Fast Determination of Ingredients in Solid Pharmaceuticals by Microwave-Enhanced In-Source Decay of Microwave Plasma Torch Mass Spectrometry.

PubMed

Su, Rui; Wang, Xinchen; Hou, Changming; Yang, Meiling; Huang, Keke; Chen, Huanwen

2017-09-01

Rapid qualitative and quantitative analysis of solid samples (e.g., pharmaceutical preparations) by using a small and low-resolution mass spectrometer without MS/MS function is still a challenge in ambient pressure ionization mass spectrometric analysis. Herein, a practically efficient method termed microwave-enhanced in-source decay (MEISD) using microwave plasma torch desorption ionization coupled with time-of-flight mass spectrometry (MPTDI-TOF MS) was developed for fast analysis of pharmaceutical tablets using a miniature TOF mass spectrometer without tandem mass function. The intensity of ISD fragmentation was evaluated under different microwave power values. Several factors, including desorption distance and time that might affect the signal intensity and fragmentation, were systematically investigated. It was observed that both the protonated molecular ions and major fragment ions from the active ingredients in tablets could be found in the full-scan mass spectra in positive ion mode, which were comparable to those obtained by a commercial LTQ-XL ion trap mass spectrometer. The structures of the ingredients could be elucidated in detail using the MEISD method, which promotes our understanding of the desorption/ionization processes in microwave plasma torch (MPT). Quantitative analysis of 10 tablets was achieved by full-scan MPTDI-TOF MS with low limit of detection (LOD, 0.763 mg/g), acceptable relative standard deviation (RSD < 7.33%, n =10), and 10 s for each tablet, showing promising applications in high throughput screening of counterfeit drugs. Graphical Abstract ᅟ.

Fast Determination of Ingredients in Solid Pharmaceuticals by Microwave-Enhanced In-Source Decay of Microwave Plasma Torch Mass Spectrometry

NASA Astrophysics Data System (ADS)

Su, Rui; Wang, Xinchen; Hou, Changming; Yang, Meiling; Huang, Keke; Chen, Huanwen

2017-09-01

Rapid qualitative and quantitative analysis of solid samples (e.g., pharmaceutical preparations) by using a small and low-resolution mass spectrometer without MS/MS function is still a challenge in ambient pressure ionization mass spectrometric analysis. Herein, a practically efficient method termed microwave-enhanced in-source decay (MEISD) using microwave plasma torch desorption ionization coupled with time-of-flight mass spectrometry (MPTDI-TOF MS) was developed for fast analysis of pharmaceutical tablets using a miniature TOF mass spectrometer without tandem mass function. The intensity of ISD fragmentation was evaluated under different microwave power values. Several factors, including desorption distance and time that might affect the signal intensity and fragmentation, were systematically investigated. It was observed that both the protonated molecular ions and major fragment ions from the active ingredients in tablets could be found in the full-scan mass spectra in positive ion mode, which were comparable to those obtained by a commercial LTQ-XL ion trap mass spectrometer. The structures of the ingredients could be elucidated in detail using the MEISD method, which promotes our understanding of the desorption/ionization processes in microwave plasma torch (MPT). Quantitative analysis of 10 tablets was achieved by full-scan MPTDI-TOF MS with low limit of detection (LOD, 0.763 mg/g), acceptable relative standard deviation (RSD < 7.33%, n =10), and 10 s for each tablet, showing promising applications in high throughput screening of counterfeit drugs. [Figure not available: see fulltext.

Structural elucidation of new urinary tamoxifen metabolites by liquid chromatography quadrupole time-of-flight mass spectrometry.

PubMed

Lu, Jianghai; He, Chunji; He, Genye; Wang, Xiaobing; Xu, Youxuan; Wu, Yun; Dong, Ying; Ouyang, Gangfeng

2014-07-01

In this study, tamoxifen metabolic profiles were investigated carefully. Tamoxifen was administered to two healthy male volunteers and one female patient suffering from breast cancer. Urinary extracts were analyzed by liquid chromatography quadruple time-of-flight mass spectrometry using full scan and targeted MS/MS techniques with accurate mass measurement. Chromatographic peaks for potential metabolites were selected by using the theoretical [M + H](+) as precursor ion in full-scan experiment and m/z 72, 58 or 44 as characteristic product ions for N,N-dimethyl, N-desmethyl and N,N-didesmethyl metabolites in targeted MS/MS experiment, respectively. Tamoxifen and 37 metabolites were detected in extraction study samples. Chemical structures of seven unreported metabolites were elucidated particularly on the basis of fragmentation patterns observed for these metabolites. Several metabolic pathways containing mono- and di-hydroxylation, methoxylation, N-desmethylation, N,N-didesmethylation, oxidation and combinations were suggested. All the metabolites were detected in the urine samples up to 1 week. Copyright © 2014 John Wiley & Sons, Ltd.

[Application of precursor ion scanning method in rapid screening of illegally added phosphodiesterase-5 inhibitors and their unknown derivatives in Chinese traditional patent medicines and health foods].

PubMed

Sun, Jing; Cao, Ling; Feng, Youlong; Tan, Li

2014-11-01

The compounds with similar structure often have similar pharmacological activities. So it is a trend for illegal addition that new derivatives of effective drugs are synthesized to avoid the statutory test. This bring challenges to crack down on illegal addition behavior, however, modified derivatives usually have similar product ions, which allow for precursor ion scanning. In this work, precursor ion scanning mode of a triple quadrupole mass spectrometer was first applied to screen illegally added drugs in complex matrix such as Chinese traditional patent medicines and healthy foods. Phosphodiesterase-5 inhibitors were used as experimental examples. Through the analysis of the structure and mass spectrum characteristics of the compounds, phosphodiesterase-5 inhibitors were classified, and their common product ions were screened by full scan of product ions of typical compounds. Then high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method with precursor ion scanning mode was established based on the optimization of MS parameters. The effect of mass parameters and the choice of fragment ions were also studied. The method was applied to determine actual samples and further refined. The results demonstrated that this method can meet the need of rapid screening of unknown derivatives of phosphodiesterase-5 inhibitors in complex matrix, and prevent unknown derivatives undetected. This method shows advantages in sensitivity, specificity and efficiency, and is worth to be further investigated.

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry

DOE PAGES

Van Berkel, Gary J.; Kertesz, Vilmos

2016-11-15

An “Open Access”-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendorprovided software libraries. Sample classification based on spectral comparison utilized themore » spectral contrast angle method. As a result, using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. In conclusion, this work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching.« less

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Berkel, Gary J.; Kertesz, Vilmos

An “Open Access”-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendorprovided software libraries. Sample classification based on spectral comparison utilized themore » spectral contrast angle method. As a result, using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. In conclusion, this work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching.« less

High-resolution liquid chromatography/electrospray ionization time-of-flight mass spectrometry combined with liquid chromatography/electrospray ionization tandem mass spectrometry to identify polyphenols from grape antioxidant dietary fiber.

PubMed

Touriño, Sonia; Fuguet, Elisabet; Jáuregui, Olga; Saura-Calixto, Fulgencio; Cascante, Marta; Torres, Josep Lluís

2008-11-01

Grape antioxidant dietary fiber (GADF) is a dietary supplement that combines the benefits of both fiber and antioxidants that help prevent cancer and cardiovascular diseases. The antioxidant polyphenolic components in GADF probably help prevent cancer in the digestive tract, where they are bioavailable. Mass spectrometry coupled to liquid chromatography is a powerful tool for the analysis of complex plant derivatives such as GADF. We use a combination of MS techniques, namely liquid chromatography/electrospray ionization time-of-flight mass spectrometry (LC/ESI-TOF-MS) and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) on a triple quadrupole, for the identification of the polyphenolic constituents of the soluble fraction of GADF. First, we separated the mixture into four fractions which were tested for phenolic constituents using the TOF system in the full scan mode. The high sensitivity and resolution of the TOF detector over the triple quadrupole facilitate the preliminary characterization of the fractions. Then we used LC/ESI-MS/MS to identify the individual phenols through MS/MS experiments (product ion scan, neutral loss scan, precursor ion scan). Finally, most of the identities were unequivocally confirmed by accurate mass measurements on the TOF spectrometer. LC/ESI-TOF-MS combined with MS/MS correctly identifies the bioactive polyphenolic components from the soluble fraction of GADF. High-resolution TOF-MS is particularly useful for identifying the structure of compounds with the same LC/ESI-MS/MS fragmentation patterns.

[Hemorrhagic adrenal pseudocyst: case report].

PubMed

Basile, G; Buffone, A; Cicciarella, G; di Mari, P; Cirino, E

2004-01-01

Adrenal cysts are usually asymptomatic; they are usually identified occasionally during ultrasound or C.T. scans (incidentaloma). Among adrenal cysts the most common types are epithelial cysts and pseudocysts. Intracystic haemorrhage is one of the possible complications of adrenal pseudocysts. We report a case of a young woman with right superior abdominal pain, fever and acute anemia. A C.T. scan showed a 10 cm. mass between the liver and the right kidney. To be sure of the nature of this mass also M.R., urography and C.T.-guided biopsy were carried out. This latter only let us make the final diagnosis of hemorrhagic adrenal pseudocyst. Thereafter, a laparotomic right adrenalectomy was performed, with full recovery of the patient. Adrenal cysts may cause differential diagnostic problems with masses of contiguous organs like kidney, liver and gallbladder. For this reason, ultrasound and C.T. scans may not be sufficient and must be completed by M.R., urography and/or C.T.-guided biopsy. Intracystic hamorrhage, spontaneous or post-traumatic, may cause to the patient acute anemia which, as soon as the diagnosis is confirmed, indicates surgery. The operation usually is a laparotomic adrenalectomy, since the laparoscopic approach is not sufficient to control large masses with active bleeding inside.

ON-SITE SOLID PHRASE EXTRACTION AND LABORATORY ...

EPA Pesticide Factsheets

Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. A I -L sample, however, usually provides too little analyte for full-scan data acquisition. An on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent has been developed. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-sol

IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ...

EPA Pesticide Factsheets

Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little analyte for full-scan data acquisition.We have developed an on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-s

Determination of thiol metabolites in human urine by stable isotope labeling in combination with pseudo-targeted mass spectrometry analysis

NASA Astrophysics Data System (ADS)

Liu, Ping; Qi, Chu-Bo; Zhu, Quan-Fei; Yuan, Bi-Feng; Feng, Yu-Qi

2016-02-01

Precursor ion scan and multiple reaction monitoring scan (MRM) are two typical scan modes in mass spectrometry analysis. Here, we developed a strategy by combining stable isotope labeling (IL) with liquid chromatography-mass spectrometry (LC-MS) under double precursor ion scan (DPI) and MRM for analysis of thiols in 5 types of human cancer urine. Firstly, the IL-LC-DPI-MS method was applied for non-targeted profiling of thiols from cancer samples. Compared to traditional full scan mode, the DPI method significantly improved identification selectivity and accuracy. 103 thiol candidates were discovered in all cancers and 6 thiols were identified by their standards. It is worth noting that pantetheine, for the first time, was identified in human urine. Secondly, the IL-LC-MRM-MS method was developed for relative quantification of thiols in cancers compared to healthy controls. All the MRM transitions of light and heavy labeled thiols were acquired from urines by using DPI method. Compared to DPI method, the sensitivity of MRM improved by 2.1-11.3 folds. In addition, the concentration of homocysteine, γ-glutamylcysteine and pantetheine enhanced more than two folds in cancer patients compared to healthy controls. Taken together, the method demonstrated to be a promising strategy for identification and comprehensive quantification of thiols in human urines.

Determination of thiol metabolites in human urine by stable isotope labeling in combination with pseudo-targeted mass spectrometry analysis

PubMed Central

Liu, Ping; Qi, Chu-Bo; Zhu, Quan-Fei; Yuan, Bi-Feng; Feng, Yu-Qi

2016-01-01

Precursor ion scan and multiple reaction monitoring scan (MRM) are two typical scan modes in mass spectrometry analysis. Here, we developed a strategy by combining stable isotope labeling (IL) with liquid chromatography-mass spectrometry (LC-MS) under double precursor ion scan (DPI) and MRM for analysis of thiols in 5 types of human cancer urine. Firstly, the IL-LC-DPI-MS method was applied for non-targeted profiling of thiols from cancer samples. Compared to traditional full scan mode, the DPI method significantly improved identification selectivity and accuracy. 103 thiol candidates were discovered in all cancers and 6 thiols were identified by their standards. It is worth noting that pantetheine, for the first time, was identified in human urine. Secondly, the IL-LC-MRM-MS method was developed for relative quantification of thiols in cancers compared to healthy controls. All the MRM transitions of light and heavy labeled thiols were acquired from urines by using DPI method. Compared to DPI method, the sensitivity of MRM improved by 2.1–11.3 folds. In addition, the concentration of homocysteine, γ-glutamylcysteine and pantetheine enhanced more than two folds in cancer patients compared to healthy controls. Taken together, the method demonstrated to be a promising strategy for identification and comprehensive quantification of thiols in human urines. PMID:26888486

Preventive doping control screening analysis of prohibited substances in human urine using rapid-resolution liquid chromatography/high-resolution time-of-flight mass spectrometry.

PubMed

Vonaparti, A; Lyris, E; Angelis, Y S; Panderi, I; Koupparis, M; Tsantili-Kakoulidou, A; Peters, R J B; Nielen, M W F; Georgakopoulos, C

2010-06-15

Unification of the screening protocols for a wide range of doping agents has become an important issue for doping control laboratories. This study presents the development and validation of a generic liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) screening method of 241 small molecule analytes from various categories of prohibited substances (stimulants, narcotics, diuretics, beta(2)-agonists, beta-blockers, hormone antagonists and modulators, glucocorticosteroids and anabolic agents). It is based on a single-step liquid-liquid extraction of hydrolyzed urine and the use of a rapid-resolution liquid chromatography/high-resolution time-of-flight mass spectrometric system acquiring continuous full scan data. Electrospray ionization in the positive mode was used. Validation parameters consisted of identification capability, limit of detection, specificity, ion suppression, extraction recovery, repeatability and mass accuracy. Detection criteria were established on the basis of retention time reproducibility and mass accuracy. The suitability of the methodology for doping control was demonstrated with positive urine samples. The preventive role of the method was proved by the case where full scan acquisition with accurate mass measurement allowed the retrospective reprocessing of acquired data from past doping control samples for the detection of a designer drug, the stimulant 4-methyl-2-hexanamine, which resulted in re-reporting a number of stored samples as positives for this particular substance, when, initially, they had been reported as negatives. Copyright (c) 2010 John Wiley & Sons, Ltd.

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry.

PubMed

Van Berkel, Gary J; Kertesz, Vilmos

2017-02-15

An "Open Access"-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendor-provided software libraries. Sample classification based on spectral comparison utilized the spectral contrast angle method. Using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. This work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

High resolution full scan liquid chromatography mass spectrometry comprehensive screening in sports antidoping urine analysis.

PubMed

Abushareeda, Wadha; Vonaparti, Ariadni; Saad, Khadija Al; Almansoori, Moneera; Meloug, Mbarka; Saleh, Amal; Aguilera, Rodrigo; Angelis, Yiannis; Horvatovich, Peter L; Lommen, Arjen; Alsayrafi, Mohammed; Georgakopoulos, Costas

2018-03-20

The aim of this paper is to present the development and validation of a high-resolution full scan (HR-FS) electrospray ionization (ESI) liquid chromatography coupled to quadrupole Orbitrap mass spectrometer (LC/Q/Orbitrap MS) platform for the screening of prohibited substances in human urine according to World Antidoping Agency (WADA) requirements. The method was also validated for quantitative analysis of six endogenous steroids (epitestosterone, testosterone, 5α-dihydrotestosterone, dehydroepiandrosterone, androsterone and etiocholanolone) in their intact sulfates form. The sample preparation comprised a combination of a hydrolyzed urine liquid-liquid extraction and the dilute & shoot addition of original urine in the extracted aliquot. The HR-FS MS acquisition mode with Polarity Switching was applied in combination of the Quadrupole-Orbitrap mass filter. The HR-FS acquisition of analytical signal, for known and unknown small molecules, allows the inclusion of all analytes detectable with LC-MS for antidoping investigations to identify the use of known or novel prohibited substances and metabolites after electronic data files' reprocessing. The method has been validated to be fit-for-purpose for the antidoping analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of trace levels of herbicides and their degradation products in surface and ground waters by gas chromatography/ion-trap mass spectrometry

USGS Publications Warehouse

Pereira, W.E.; Rostad, C.E.; Leiker, T.J.

1990-01-01

A rapid, specific and highly sensitive method is described for the determination of several commonly used herbicides and their degradation products in surface and ground waters by using gas chromatography/ion-trap mass spectrometry. The compounds included atrazine, and its degradation products desethylatrazine and desisopropylatrazine; Simazine; Cyanazine; Metolachlor; and alachlor and its degradation products, 2-chloro-2', 6'-diethylacetanilide, 2-hydroxy-2', 6'-diethylacetanilide and 2,6-diethylaniline. The method was applied to surface-water samples collected from 16 different stations along the lower Mississippi River and its major tributaries, and ground-water samples beneath a cornfield in central Nebraska. Average recovery of a surrogate herbicide, terbuthylazine, was greater than 99%. Recoveries of the compounds of interest from river water spiked at environmental levels are also presented. Full-scan mass spectra of these compounds were obtained on 1 ng or less of analyte. Data were collected in the full-scan acquisition mode. Quantitation was based on a single characteristic ion for each compound. The detection limit was 60 pg with a signal-to-noise ratio of greater than 10:1.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asano, Keiji G; Ford, Michael J; Tomkins, Bruce A

A self-aspirating heated nebulizer probe is described and demonstrated for use in the direct analysis of analytes on surfaces and in liquid samples by atmospheric pressure chemical ionization (APCI) mass spectrometry. Functionality and performance of the probe as a self-aspirating APCI source is demonstrated using reserpine and progesterone as test compounds. The utility of the probe to sample analytes directly from surfaces was demonstrated first by scanning development lanes of a reversed-phase thin-layer chromatography plate in which a three-component dye mixture, viz., Fat Red 7B, Solvent Green 3, and Solvent Blue 35, was spotted and the components were separated. Developmentmore » lanes were scanned by the sampling probe operated under computer control (x, y plane) while full-scan mass spectra were recorded using a quadrupole ion trap mass spectrometer. In addition, the ability to sample the surface of pharmaceutical tablets (viz., Extra Strength Tylenol(reg. sign) and Evista(reg. sign) tablets) and to detect the active ingredients (acetaminophen and raloxifene, respectively) selectively was demonstrated using tandem mass spectrometry (MS/MS). Finally, the capability to sample analyte solutions from the wells of a 384-well microtiter plate and to perform quantitative analyses using MS/MS detection was illustrated with cotinine standards spiked with cotinine-d{sub 3} as an internal standard.« less

Use of a least absolute shrinkage and selection operator (LASSO) model to selected ion flow tube mass spectrometry (SIFT-MS) analysis of exhaled breath to predict the efficacy of dialysis: a pilot study.

PubMed

Wang, Maggie Haitian; Chong, Ka Chun; Storer, Malina; Pickering, John W; Endre, Zoltan H; Lau, Steven Yf; Kwok, Chloe; Lai, Maria; Chung, Hau Yin; Ying Zee, Benny Chung

2016-09-28

Selected ion flow tube-mass spectrometry (SIFT-MS) provides rapid, non-invasive measurements of a full-mass scan of volatile compounds in exhaled breath. Although various studies have suggested that breath metabolites may be indicators of human disease status, many of these studies have included few breath samples and large numbers of compounds, limiting their power to detect significant metabolites. This study employed a least absolute shrinkage and selective operator (LASSO) approach to SIFT-MS data of breath samples to preliminarily evaluate the ability of exhaled breath findings to monitor the efficacy of dialysis in hemodialysis patients. A process of model building and validation showed that blood creatinine and urea concentrations could be accurately predicted by LASSO-selected masses. Using various precursors, the LASSO models were able to predict creatinine and urea concentrations with high adjusted R-square (>80%) values. The correlation between actual concentrations and concentrations predicted by the LASSO model (using precursor H 3 O + ) was high (Pearson correlation coefficient  =  0.96). Moreover, use of full mass scan data provided a better prediction than compounds from selected ion mode. These findings warrant further investigations in larger patient cohorts. By employing a more powerful statistical approach to predict disease outcomes, breath analysis using SIFT-MS technology could be applicable in future to daily medical diagnoses.

High-resolution mass spectrometry method for the detection, characterization and quantitation of pharmaceuticals in water.

PubMed

Pinhancos, Rebeca; Maass, Sara; Ramanathan, Dil M

2011-11-01

The presence of pharmaceuticals in drinking water is an emerging environmental concern. In most environmental testing laboratories, LC-MS/MS assays based on selected reaction monitoring are used as part of a battery of tests used to assure water quality. Although LC-MS/MS continues to be the best tool for detecting pharmaceuticals in water, the combined use of hybrid high-resolution mass spectrometry (HRMS) and ultrahigh pressure liquid chromatography (UHPLC) is starting to become a practical tool to study emerging environmental contaminants. The hybrid LTQ-orbitrap mass spectrometer is suitable for integrated quantitative and qualitative bioanalysis because of the following reasons: (1) the ability to collect full-scan HRMS spectra with scan speeds suitable for UHPLC separations, (2) routine measurement of mass with less than 5 ppm mass accuracy, (3) high mass resolving power, and (4) ability to perform on-the-fly polarity switching in the linear ion trap (LTQ). In the present work, we provide data demonstrating the application of UHPLC-LTQ-orbitrap for the detection, characterization and quantification of pharmaceuticals and their metabolites in drinking water. Copyright © 2011 John Wiley & Sons, Ltd.

Transformation of chlorinated paraffins to olefins during metal work and thermal exposure - Deconvolution of mass spectra and kinetics.

PubMed

Schinkel, Lena; Lehner, Sandro; Knobloch, Marco; Lienemann, Peter; Bogdal, Christian; McNeill, Kristopher; Heeb, Norbert V

2018-03-01

Chlorinated paraffins (CPs) are high production volume chemicals widely used as additives in metal working fluids. Thereby, CPs are exposed to hot metal surfaces which may induce degradation processes. We hypothesized that the elimination of hydrochloric acid would transform CPs into chlorinated olefins (COs). Mass spectrometry is widely used to detect CPs, mostly in the selected ion monitoring mode (SIM) evaluating 2-3 ions at mass resolutions R < 20'000. This approach is not suited to detected COs, because their mass spectra strongly overlap with CPs. We applied a mathematical deconvolution method based on full-scan MS data to separate interfered CP/CO spectra. Metal drilling indeed induced HCl-losses. CO proportions in exposed mixtures of chlorotridecanes increased. Thermal exposure of chlorotridecanes at 160, 180, 200 and 220 °C also induced dehydrohalogenation reactions and CO proportions also increased. Deconvolution of respective mass spectra is needed to study the CP transformation kinetics without bias from CO interferences. Apparent first-order rate constants (k app ) increased up to 0.17, 0.29 and 0.46 h -1 for penta-, hexa- and heptachloro-tridecanes exposed at 220 °C. Respective half-life times (τ 1/2 ) decreased from 4.0 to 2.4 and 1.5 h. Thus, higher chlorinated paraffins degrade faster than lower chlorinated ones. In conclusion, exposure of CPs during metal drilling and thermal treatment induced HCl losses and CO formation. It is expected that CPs and COs are co-released from such processes. Full-scan mass spectra and subsequent deconvolution of interfered signals is a promising approach to tackle the CP/CO problem, in case of insufficient mass resolution. Copyright © 2017 Elsevier Ltd. All rights reserved.

Liquid extraction surface analysis (LESA) of food surfaces employing chip-based nano-electrospray mass spectrometry.

PubMed

Eikel, Daniel; Henion, Jack

2011-08-30

An automated surface-sampling technique called liquid extraction surface analysis (LESA), coupled with infusion nano-electrospray high-resolution mass spectrometry and tandem mass spectrometry (MS/MS), is described and applied to the qualitative determination of surface chemical residues resulting from the artificial spraying of selected fresh fruits and vegetables with representative pesticides. Each of the targeted pesticides was readily detected with both high-resolution and full-scan collision-induced dissociation (CID) mass spectra. In the case of simazine and sevin, a mass resolution of 100,000 was insufficient to distinguish the isobaric protonated molecules for these compounds. When the surface of a spinach leaf was analyzed by LESA, trace levels of diazinon were readily detected on the spinach purchased directly from a supermarket before they were sprayed with the five-pesticide mixture. A 30 s rinse under hot running tap water appeared to quantitatively remove all remaining residues of this pesticide. Diazinon was readily detected by LESA analysis on the skin of the artificially sprayed spinach. Finally, incurred pyrimethanil at a level of 169 ppb in a batch slurry of homogenized apples was analyzed by LESA and this pesticide was readily detected by both high-resolution mass spectrometry and full-scan CID mass spectrometry, thus showing that pesticides may also be detected in whole fruit homogenized samples. This report shows that representative pesticides on fruit and vegetable surfaces present at levels 20-fold below generally allowed EPA tolerance levels are readily detected and confirmed by the title technologies making LESA-MS as interesting screening method for food safety purposes. Copyright © 2011 John Wiley & Sons, Ltd.

Metabolism of RCS-8, a synthetic cannabinoid with cyclohexyl structure, in human hepatocytes by high-resolution MS

PubMed Central

Wohlfarth, Ariane; Pang, Shaokun; Zhu, Mingshe; Gandhi, Adarsh S; Scheidweiler, Karl B; Huestis, Marilyn A

2015-01-01

Background Since 2008, synthetic cannabinoids are major new designer drugs of abuse. They are extensively metabolized and excreted in urine, but limited human metabolism data are available. As there are no reports on the metabolism of RCS-8, a scheduled phenylacetylindole synthetic cannabinoid with an N-cyclohexylethyl moiety, we investigated metabolism of this new designer drug by human hepatocytes and high resolution MS. Methods After human hepatocyte incubation with RCS-8, samples were analyzed on a TripleTOF 5600+ mass spectrometer with time-of-flight survey scan and information-dependent acquisition triggered product ion scans. Data mining of the accurate mass full scan and product ion spectra employed different data processing algorithms. Results and Conclusion More than 20 RCS-8 metabolites were identified, products of oxidation, demethylation, and glucuronidation. Major metabolites and targets for analytical methods were hydroxyphenyl RCS - 8 glucuronide, a variety of hydroxycyclohexyl-hydroxyphenyl RCS-8 glucuronides, hydroxyphenyl RCS-8, as well as the demethyl-hydroxycyclohexyl RCS-8 glucuronide. PMID:24946920

Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemical ionization.

PubMed

Ovchinnikova, Olga S; Van Berkel, Gary J

2010-06-30

An atmospheric pressure proximal probe thermal desorption sampling method coupled with secondary ionization by electrospray or atmospheric pressure chemical ionization was demonstrated for the mass spectrometric analysis of a diverse set of compounds (dyestuffs, pharmaceuticals, explosives and pesticides) separated on various high-performance thin-layer chromatography plates. Line scans along or through development lanes on the plates were carried out by moving the plate relative to a stationary heated probe positioned close to or just touching the stationary phase surface. Vapors of the compounds thermally desorbed from the surface were drawn into the ionization region of a combined electrospray ionization/atmospheric pressure chemical ionization source where they merged with reagent ions and/or charged droplets from a corona discharge or an electrospray emitter and were ionized. The ionized components were then drawn through the atmospheric pressure sampling orifice into the vacuum region of a triple quadrupole mass spectrometer and detected using full scan, single ion monitoring, or selected reaction monitoring mode. Studies of variable parameters and performance metrics including the proximal probe temperature, gas flow rate into the ionization region, surface scan speed, read-out resolution, detection limits, and surface type are discussed.

Multiplexed data independent acquisition (MSX-DIA) applied by high resolution mass spectrometry improves quantification quality for the analysis of histone peptides

PubMed Central

Sidoli, Simone; Fujiwara, Rina; Garcia, Benjamin A.

2016-01-01

We present the mass spectrometry (MS) based application of the innovative, although scarcely exploited, multiplexed data-independent acquisition (MSX-DIA) for the analysis of histone post-translational modifications (PTMs). Histones are golden standard for complexity in MS based proteomics, due to their large number of combinatorial modifications, leading to isobaric peptides after proteolytic digestion. DIA has thus gained popularity for the purpose as it allows for MS/MS-based quantification without upfront assay development. In this work, we evaluated the performance of traditional DIA versus MSX-DIA in terms of MS/MS spectra quality, instrument scan rate and quantification precision using histones from HeLa cells. We used an MS/MS isolation window of 10 and 6 m/z for DIA and MSX-DIA, respectively. Four MS/MS scans were multiplexed for MSX-DIA. Despite MSX-DIA was programmed to perform 2-fold more MS/MS events than traditional DIA, it acquired on average ~5% more full MS scans, indicating even faster scan rate. Results highlighted an overall decrease of background ion signals using MSX-DIA, and we illustrated specific examples where peptides of different precursor masses were co-fragmented by DIA but not MSX-DIA. Taken together, MSX-DIA proved thus to be a more favorable method for histone analysis in data independent mode. PMID:27193262

The minimal SUSY B - L model: from the unification scale to the LHC

DOE PAGES

Ovrut, Burt A.; Purves, Austin; Spinner, Sogee

2015-06-26

Here, this paper introduces a random statistical scan over the high-energy initial parameter space of the minimal SUSY B - L model — denoted as the B - L MSSM. Each initial set of points is renormalization group evolved to the electroweak scale — being subjected, sequentially, to the requirement of radiative B - L and electroweak symmetry breaking, the present experimental lower bounds on the B - L vector boson and sparticle masses, as well as the lightest neutral Higgs mass of ~125 GeV. The subspace of initial parameters that satisfies all such constraints is presented, shown to bemore » robust and to contain a wide range of different configurations of soft supersymmetry breaking masses. The low-energy predictions of each such “valid” point — such as the sparticle mass spectrum and, in particular, the LSP — are computed and then statistically analyzed over the full subspace of valid points. Finally, the amount of fine-tuning required is quantified and compared to the MSSM computed using an identical random scan. The B - L MSSM is shown to generically require less fine-tuninng.« less

Changes in the expression of N- and O-glycopeptides in patients with colorectal cancer and hepatocellular carcinoma quantified by full-MS scan FT-ICR and multiple reaction monitoring.

PubMed

Darebna, Petra; Novak, Petr; Kucera, Radek; Topolcan, Ondrej; Sanda, Miloslav; Goldman, Radoslav; Pompach, Petr

2017-02-05

Alternations in the glycosylation of proteins have been described in connection with several cancers, including hepatocellular carcinoma (HCC) and colorectal cancer. Analytical tools, which use combination of liquid chromatography and mass spectrometry, allow precise and sensitive description of these changes. In this study, we use MRM and FT-ICR operating in full-MS scan, to determine ratios of intensities of specific glycopeptides in HCC, colorectal cancer, and liver metastasis of colorectal cancer. Haptoglobin, hemopexin and complement factor H were detected after albumin depletion and the N-linked glycopeptides with fucosylated glycans were compared with their non-fucosylated forms. In addition, sialylated forms of an O-linked glycopeptide of hemopexin were quantified in the same samples. We observe significant increase in fucosylation of all three proteins and increase in bi-sialylated O-glycopeptide of hemopexin in HCC of hepatitis C viral (HCV) etiology by both LC-MS methods. The results of the MRM and full-MS scan FT-ICR analyses provide comparable quantitative readouts in spite of chromatographic, mass spectrometric and data analysis differences. Our results suggest that both workflows allow adequate relative quantification of glycopeptides and suggest that HCC of HCV etiology differs in glycosylation from colorectal cancer and liver metastasis of colorectal cancer. The article compares N- and O-glycosylation of several serum proteins in different diseases by a fast and easy sample preparation procedure in combination with high resolution Fourier transform ion cyclotron resonance mass spectrometry. The results show successful glycopeptides relative quantification in a complex peptide mixture by the high resolution instrument and the detection of glycan differences between the different types of cancer diseases. The presented method is comparable to conventional targeted MRM approach but allows additional curation of the data. Copyright © 2016 Elsevier B.V. All rights reserved.

Changes in the expression of N- and O-glycopeptides in patients with colorectal cancer and hepatocellular carcinoma quantified by full-MS scan FT-ICR and multiple reaction monitoring

PubMed Central

Darebna, Petra; Novak, Petr; Kucera, Radek; Topolcan, Ondrej; Sanda, Miloslav; Goldman, Radoslav; Pompach, Petr

2018-01-01

Alternations in the glycosylation of proteins have been described in connection with several cancers, including hepatocellular carcinoma (HCC) and colorectal cancer. Analytical tools, which use combination of liquid chromatography and mass spectrometry, allow precise and sensitive description of these changes. In this study, we use MRM and FT-ICR operating in full-MS scan, to determine ratios of intensities of specific glycopeptides in HCC, colorectal cancer, and liver metastasis of colorectal cancer. Haptoglobin, hemopexin and complement factor H were detected after albumin depletion and the N-linked glycopeptides with fucosylated glycans were compared with their non-fucosylated forms. In addition, sialylated forms of an O-linked glycopeptide of hemopexin were quantified in the same samples. We observe significant increase in fucosylation of all three proteins and increase in bisialylated O-glycopeptide of hemopexin in HCC of hepatitis C viral (HCV) etiology by both LC-MS methods. The results of the MRM and full-MS scan FT-ICR analyses provide comparable quantitative readouts in spite of chromatographic, mass spectrometric and data analysis differences. Our results suggest that both workflows allow adequate relative quantification of glycopeptides and suggest that HCC of HCV etiology differs in glycosylation from colorectal cancer and liver metastasis of colorectal cancer. Significance The article compares N- and O-glycosylation of several serum proteins in different diseases by a fast and easy sample preparation procedure in combination with high resolution Fourier transform ion cyclotron resonance mass spectrometry. The results show successful glycopeptides relative quantification in a complex peptide mixture by the high resolution instrument and the detection of glycan differences between the different types of cancer diseases. The presented method is comparable to conventional targeted MRM approach but allows additional curation of the data. PMID:27646713

Validation of the Mass-Extraction-Window for Quantitative Methods Using Liquid Chromatography High Resolution Mass Spectrometry.

PubMed

Glauser, Gaétan; Grund, Baptiste; Gassner, Anne-Laure; Menin, Laure; Henry, Hugues; Bromirski, Maciej; Schütz, Frédéric; McMullen, Justin; Rochat, Bertrand

2016-03-15

A paradigm shift is underway in the field of quantitative liquid chromatography-mass spectrometry (LC-MS) analysis thanks to the arrival of recent high-resolution mass spectrometers (HRMS). The capability of HRMS to perform sensitive and reliable quantifications of a large variety of analytes in HR-full scan mode is showing that it is now realistic to perform quantitative and qualitative analysis with the same instrument. Moreover, HR-full scan acquisition offers a global view of sample extracts and allows retrospective investigations as virtually all ionized compounds are detected with a high sensitivity. In time, the versatility of HRMS together with the increasing need for relative quantification of hundreds of endogenous metabolites should promote a shift from triple-quadrupole MS to HRMS. However, a current "pitfall" in quantitative LC-HRMS analysis is the lack of HRMS-specific guidance for validated quantitative analyses. Indeed, false positive and false negative HRMS detections are rare, albeit possible, if inadequate parameters are used. Here, we investigated two key parameters for the validation of LC-HRMS quantitative analyses: the mass accuracy (MA) and the mass-extraction-window (MEW) that is used to construct the extracted-ion-chromatograms. We propose MA-parameters, graphs, and equations to calculate rational MEW width for the validation of quantitative LC-HRMS methods. MA measurements were performed on four different LC-HRMS platforms. Experimentally determined MEW values ranged between 5.6 and 16.5 ppm and depended on the HRMS platform, its working environment, the calibration procedure, and the analyte considered. The proposed procedure provides a fit-for-purpose MEW determination and prevents false detections.

Direct Analysis in Real Time (DART) of an Organothiophosphate at Ultrahigh Resolution by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry and Tandem Mass Spectrometry

PubMed Central

Prokai, Laszlo; Stevens, Stanley M.

2016-01-01

Direct analysis in real time (DART) is a recently developed ambient ionization technique for mass spectrometry to enable rapid and sensitive analyses with little or no sample preparation. After swab-based field sampling, the organothiophosphate malathion was analyzed using DART-Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometry (MS) and tandem mass spectrometry (MS/MS). Mass resolution was documented to be over 800,000 in full-scan MS mode and over 1,000,000 for an MS/MS product ion produced by collision-induced dissociation of the protonated analyte. Mass measurement accuracy below 1 ppm was obtained for all DART-generated ions that belonged to the test compound in the mass spectra acquired using only external mass calibration. This high mass measurement accuracy, achievable at present only through FTMS, was required for unequivocal identification of the corresponding molecular formulae. PMID:26784186

Direct Analysis in Real Time (DART) of an Organothiophosphate at Ultrahigh Resolution by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry and Tandem Mass Spectrometry.

PubMed

Prokai, Laszlo; Stevens, Stanley M

2016-01-16

Direct analysis in real time (DART) is a recently developed ambient ionization technique for mass spectrometry to enable rapid and sensitive analyses with little or no sample preparation. After swab-based field sampling, the organothiophosphate malathion was analyzed using DART-Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometry (MS) and tandem mass spectrometry (MS/MS). Mass resolution was documented to be over 800,000 in full-scan MS mode and over 1,000,000 for an MS/MS product ion produced by collision-induced dissociation of the protonated analyte. Mass measurement accuracy below 1 ppm was obtained for all DART-generated ions that belonged to the test compound in the mass spectra acquired using only external mass calibration. This high mass measurement accuracy, achievable at present only through FTMS, was required for unequivocal identification of the corresponding molecular formulae.

Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision-induced dissociation behavior.

PubMed

Polet, Michael; Van Gansbeke, Wim; Van Eenoo, Peter; Deventer, Koen

2016-02-28

The detection of new anabolic steroid metabolites and new designer steroids is a challenging task in doping analysis. Switching from electron ionization gas chromatography triple quadrupole mass spectrometry (GC/EI-MS/MS) to chemical ionization (CI) has proven to be an efficient way to increase the sensitivity of GC/MS/MS analyses and facilitate the detection of anabolic steroids. CI also extends the possibilities of GC/MS/MS analyses as the molecular ion is retained in its protonated form due to the softer ionization. In EI it can be difficult to find previously unknown but expected metabolites due to the low abundance or absence of the molecular ion and the extensive (and to a large extent unpredictable) fragmentation. The main aim of this work was to study the CI and collision-induced dissociation (CID) behavior of a large number of anabolic androgenic steroids (AAS) as their trimethylsilyl derivatives in order to determine correlations between structures and CID fragmentation. Clarification of these correlations is needed for the elucidation of structures of unknown steroids and new metabolites. The ionization and CID behavior of 65 AAS have been studied using GC/CI-MS/MS with ammonia as the reagent gas. Glucuronidated AAS reference standards were first hydrolyzed to obtain their free forms. Afterwards, all the standards were derivatized to their trimethylsilyl forms. Full scan and product ion scan analyses were used to examine the ionization and CID behavior. Full scan and product ion scan analyses revealed clear correlations between AAS structure and the obtained mass spectra. These correlations were confirmed by analysis of multiple hydroxylated, methylated, chlorinated and deuterated analogs. AAS have been divided into three groups according to their ionization behavior and into seven groups according to their CID behavior. Correlations between fragmentation and structure were revealed and fragmentation pathways were postulated. Copyright © 2016 John Wiley & Sons, Ltd.

New Potential Biomarker for Methasterone Misuse in Human Urine by Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry.

PubMed

Zhang, Jianli; Lu, Jianghai; Wu, Yun; Wang, Xiaobing; Xu, Youxuan; Zhang, Yinong; Wang, Yan

2016-09-24

In this study, methasterone urinary metabolic profiles were investigated by liquid chromatography quadrupole time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. A healthy male volunteer was asked to take the drug and liquid-liquid extraction was employed to process urine samples. Chromatographic peaks for potential metabolites were hunted out with the theoretical [M - H](-) as a target ion in a full scan experiment and actual deprotonated ions were studied in targeted MS/MS experiment. Fifteen metabolites including two new sulfates (S1 and S2), three glucuronide conjugates (G2, G6 and G7), and three free metabolites (M2, M4 and M6) were detected for methasterone. Three metabolites involving G4, G5 and M5 were obtained for the first time in human urine samples. Owing to the absence of helpful fragments to elucidate the steroid ring structure of methasterone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was employed to obtain structural information of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and the potential structure was inferred using a combined MS method. Metabolite detection times were also analyzed and G2 (18-nor-17β-hydroxymethyl-2α, 17α-dimethyl-androst-13-en-3α-ol-ξ-O-glucuronide) was thought to be new potential biomarker for methasterone misuse which can be detected up to 10 days.

Characterization and identification of a C-terminal amidated mechano growth factor (MGF) analogue in black market products.

PubMed

Esposito, Simone; Deventer, Koen; Van Eenoo, Peter

2012-03-30

Mechano growth factor (MGF) is a splice variant of insulin-like growth factor that possesses anabolic properties and has not yet been approved for therapeutic use. Nevertheless, it is readily available on the black market. Although the World Anti-Doping Agency (WADA) has banned the use of MGF in sports, no routinely performed methods have been reported for its detection. In this work, two preparations from the black market containing an unknown MGF analogue were characterized. Mass spectrometry characterizations of unknown preparations and a reference human MGF were performed on an Orbitrap and a triple quadrupole mass spectrometers after separation by liquid chromatography. High accuracy measurements allowed protein identification from full scan MS data, and low-resolution full scan MS/MS provided further information on fragmentation. HCD scans of the analytes showed the presence of common b series product ions in the black market preparations and the human MGF reference standard, but all the y series ions starting from (y(1))(+) exhibited a difference of 1 m/z unit in nominal mass. This difference was demonstrated to be due to a C-terminal amidation of MGF. High-resolution data demonstrated that the black market products were both C-terminal amidated analogues of human MGF. In addition, low-resolution MS/MS characterization revealed a potentially diagnostic transition (m/z 717.8 → 431.1) for the discrimination of C-amidated MGF from the endogenous form. Qualitative identification of a MGF C-terminal amidated analogue in two black market products was successfully achieved. This report demonstrates that illegal MGF preparations are commercially available for use as doping agent in sports. Copyright © 2012 John Wiley & Sons, Ltd.

Evaluation of a semiautomated lung mass calculation technique for internal dosimetry applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Busse, Nathan; Erwin, William; Pan, Tinsu

2013-12-15

Purpose: The authors sought to evaluate a simple, semiautomated lung mass estimation method using computed tomography (CT) scans obtained using a variety of acquisition techniques and reconstruction parameters for mass correction of medical internal radiation dose-based internal radionuclide radiation absorbed dose estimates.Methods: CT scans of 27 patients with lung cancer undergoing stereotactic body radiation therapy treatment planning with PET/CT were analyzed retrospectively. For each patient, free-breathing (FB) and respiratory-gated 4DCT scans were acquired. The 4DCT scans were sorted into ten respiratory phases, representing one complete respiratory cycle. An average CT reconstruction was derived from the ten-phase reconstructions. Mid expiration breath-holdmore » CT scans were acquired in the same session for many patients. Deep inspiration breath-hold diagnostic CT scans of many of the patients were obtained from different scanning sessions at similar time points to evaluate the effect of contrast administration and maximum inspiration breath-hold. Lung mass estimates were obtained using all CT scan types, and intercomparisons made to assess lung mass variation according to scan type. Lung mass estimates using the FB CT scans from PET/CT examinations of another group of ten male and ten female patients who were 21–30 years old and did not have lung disease were calculated and compared with reference lung mass values. To evaluate the effect of varying CT acquisition and reconstruction parameters on lung mass estimation, an anthropomorphic chest phantom was scanned and reconstructed with different CT parameters. CT images of the lungs were segmented using the OsiriX MD software program with a seed point of about −850 HU and an interval of 1000. Lung volume, and mean lung, tissue, and air HUs were recorded for each scan. Lung mass was calculated by assuming each voxel was a linear combination of only air and tissue. The specific gravity of lung volume was calculated using the formula (lung HU − air HU)/(tissue HU − air HU), and mass = specific gravity × total volume × 1.04 g/cm{sup 3}.Results: The range of calculated lung masses was 0.51–1.29 kg. The average male and female lung masses during FB CT were 0.80 and 0.71 kg, respectively. The calculated lung mass varied across the respiratory cycle but changed to a lesser degree than did lung volume measurements (7.3% versus 15.4%). Lung masses calculated using deep inspiration breath-hold and average CT were significantly larger (p < 0.05) than were some masses calculated using respiratory-phase and FB CT. Increased voxel size and smooth reconstruction kernels led to high lung mass estimates owing to partial volume effects.Conclusions: Organ mass correction is an important component of patient-specific internal radionuclide dosimetry. Lung mass calculation necessitates scan-based density correction to account for volume changes owing to respiration. The range of lung masses in the authors’ patient population represents lung doses for the same absorbed energy differing from 25% below to 64% above the dose found using reference phantom organ masses. With proper management of acquisition parameters and selection of FB or midexpiration breath hold scans, lung mass estimates with about 10% population precision may be achieved.« less

Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements.

PubMed

Strano-Rossi, Sabina; Odoardi, Sara; Castrignanò, Erika; Serpelloni, Giovanni; Chiarotti, Marcello

2015-03-15

The paper describes a liquid chromatography/high resolution mass spectrometry LC/HRMS method for the simultaneous identification and quantification of stimulants (ephedrines, caffeine, anorectic drugs such as phentermine, phendimetrazine, phenmetrazine, fenfluramine, benfluorex, mephentermine, fencanfamine, sibutramine) and PDE5I (sildenafil, vardenafil and tadalafil) in food supplements using a benchtop Orbitrap mass spectrometer. The mass detector, with a nominal resolving power of 100,000 (FWHM at m/z 200), operated in full scan mode in ESI positive ionization mode. Analytes were identified by retention times, accurate masses and correspondence of experimental and calculated isotopic patterns. The limits of detection (LOD) obtained varied from 1 to 25 ng g(-1) and limits of quantification (LOQ) were 50 ng g(-1) for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000 ng g(-1), giving correlation coefficients>0.99. Accuracy (intended as %E) and repeatability (% CV) were always lower than 15%. The method was applied to the analysis of 36 dietary supplements, revealing the presence of ephedrine and/or pseudoephedrine in four of them, caffeine in eight of them and sildenafil in four of them. In one case, ephedrine was not reported on the label of the dietary supplement, as well as for caffeine in other two cases. A further confirmation of the analytes identity in positive samples was obtained through in-source fragmentation and comparison of the obtained fragments and their relative abundances with those from certified standards. As the acquisition mode is full scan, it would be also possible to re-process a previously acquired datafile for the investigation of untargeted analytes. Copyright © 2014 Elsevier B.V. All rights reserved.

IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ULTRA-TRACE SYNTHETIC MUSKS IN MUNICIPAL SEWAGE EFFLUENT USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY, FULL-SCAN MODE

EPA Science Inventory

Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little ana...

ON-SITE SOLID PHRASE EXTRACTION AND LABORATORY ANALYSIS OF ULTRA-TRACE SYNTHETIC MUSKS IN MUNICIPAL SEWAGE EFFLUENT USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY, FULL-SCAN MODE

EPA Science Inventory

Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. A I -L sample, however, usually provides too little ana...

Development and validation of a fast and simple multi-analyte procedure for quantification of 40 drugs relevant to emergency toxicology using GC-MS and one-point calibration.

PubMed

Meyer, Golo M J; Weber, Armin A; Maurer, Hans H

2014-05-01

Diagnosis and prognosis of poisonings should be confirmed by comprehensive screening and reliable quantification of xenobiotics, for example by gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-mass spectrometry (LC-MS). The turnaround time should be short enough to have an impact on clinical decisions. In emergency toxicology, quantification using full-scan acquisition is preferable because this allows screening and quantification of expected and unexpected drugs in one run. Therefore, a multi-analyte full-scan GC-MS approach was developed and validated with liquid-liquid extraction and one-point calibration for quantification of 40 drugs relevant to emergency toxicology. Validation showed that 36 drugs could be determined quickly, accurately, and reliably in the range of upper therapeutic to toxic concentrations. Daily one-point calibration with calibrators stored for up to four weeks reduced workload and turn-around time to less than 1 h. In summary, the multi-analyte approach with simple liquid-liquid extraction, GC-MS identification, and quantification over fast one-point calibration could successfully be applied to proficiency tests and real case samples. Copyright © 2013 John Wiley & Sons, Ltd.

Analytical performance of the various acquisition modes in Orbitrap MS and MS/MS.

PubMed

Kaufmann, Anton

2018-04-30

Quadrupole Orbitrap instruments (Q Orbitrap) permit high-resolution mass spectrometry (HRMS)-based full scan acquisitions and have a number of acquisition modes where the quadrupole isolates a particular mass range prior to a possible fragmentation and HRMS-based acquisition. Selecting the proper acquisition mode(s) is essential if trace analytes are to be quantified in complex matrix extracts. Depending on the particular requirements, such as sensitivity, selectivity of detection, linear dynamic range, and speed of analysis, different acquisition modes may have to be chosen. This is particularly important in the field of multi-residue analysis (e.g., pesticides or veterinary drugs in food samples) where a large number of analytes within a complex matrix have to be detected and reliably quantified. Meeting the specific detection and quantification performance criteria for every targeted compound may be challenging. It is the aim of this paper to describe the strengths and the limitations of the currently available Q Orbitrap acquisition modes. In addition, the incorporation of targeted acquisitions between full scan experiments is discussed. This approach is intended to integrate compounds that require an additional degree of sensitivity or selectivity into multi-residue methods. This article is protected by copyright. All rights reserved.

Determination of fluspirilene in human plasma by liquid chromatography-tandem mass spectrometry with electrospray ionisation.

PubMed

Swart, K J; Sutherland, F C; van Essen, G H; Hundt, H K; Hundt, A F

1998-12-18

An ultra-sensitive method for the determination of fluspirilene in plasma was established, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. The samples were extracted with hexane/isoamyl alcohol, separated on a Phenomenex Luna C18 5 mu 150 x 2.1 mm column with a mobile phase consisting of methanol-water-acetic acid (600:400:1) at a flow-rate of 0.3 ml/min. Detection was achieved by a Finnigan Matt mass spectrometer (LCQ) at unit resolution in full scan mode scanning the product ion spectrum from m/z 130-500 and monitoring the transition of the protonated molecular ion at m/z 476.2, to the sum of the largest product ions m/z 371, 342 and 274 (MS-MS). Electrospray ionisation was used for ion production. The mean recovery for fluspirilene was 90% with a lower limit of quantification of 21.50 pg/ml using 1 ml plasma for extraction. This is the first chromatographic method described for the determination of fluspirilene in plasma that is accurate and sensitive enough to be used in pharmacokinetic studies.

Hologic QDR 2000 whole-body scans: a comparison of three combinations of scan modes and analysis software

NASA Technical Reports Server (NTRS)

Spector, E.; LeBlanc, A.; Shackelford, L.

1995-01-01

This study reports on the short-term in vivo precision and absolute measurements of three combinations of whole-body scan modes and analysis software using a Hologic QDR 2000 dual-energy X-ray densitometer. A group of 21 normal, healthy volunteers (11 male and 10 female) were scanned six times, receiving one pencil-beam and one array whole-body scan on three occasions approximately 1 week apart. The following combinations of scan modes and analysis software were used: pencil-beam scans analyzed with Hologic's standard whole-body software (PB scans); the same pencil-beam analyzed with Hologic's newer "enhanced" software (EPB scans); and array scans analyzed with the enhanced software (EA scans). Precision values (% coefficient of variation, %CV) were calculated for whole-body and regional bone mineral content (BMC), bone mineral density (BMD), fat mass, lean mass, %fat and total mass. In general, there was no significant difference among the three scan types with respect to short-term precision of BMD and only slight differences in the precision of BMC. Precision of BMC and BMD for all three scan types was excellent: < 1% CV for whole-body values, with most regional values in the 1%-2% range. Pencil-beam scans demonstrated significantly better soft tissue precision than did array scans. Precision errors for whole-body lean mass were: 0.9% (PB), 1.1% (EPB) and 1.9% (EA). Precision errors for whole-body fat mass were: 1.7% (PB), 2.4% (EPB) and 5.6% (EA). EPB precision errors were slightly higher than PB precision errors for lean, fat and %fat measurements of all regions except the head, although these differences were significant only for the fat and % fat of the arms and legs. In addition EPB precision values exhibited greater individual variability than PB precision values. Finally, absolute values of bone and soft tissue were compared among the three combinations of scan and analysis modes. BMC, BMD, fat mass, %fat and lean mass were significantly different between PB scans and either of the EPB or EA scans. Differences were as large as 20%-25% for certain regional fat and BMD measurements. Additional work may be needed to examine the relative accuracy of the scan mode/software combinations and to identify reasons for the differences in soft tissue precision with the array whole-body scan mode.

Liquid chromatography-tandem mass spectrometry characterization of five new leucinostatins produced by Paecilomyces lilacinus CG-189.

PubMed

Martinez, Ana Flávia Canovas; Moraes, Luiz Alberto Beraldo

2015-03-01

The fungus Paecilomyces lilacinus produces leucinostatins—peptaibiotics that exert a range of biological activities including antimalarial, antiviral, antitumor and phytotoxicity. In this paper, we developed an analytical method employing LC-MS/MS in the precursor ion and product ion scan modes to elucidate five new leucinostatins. Direct Infusion (DI-MS) helped to identify the most abundant leucinostatins: F, D B2, S, A and K. MS/MS analysis using a triple quadrupole operating at different scan modes is a versatile tool to study natural products, especially peptaibiotics. Although DI-MS full-scan analysis is rapid and sensitive, it cannot distinguish between peptide isomers. On the other hand, LC-MS/MS operated in the precursor ion and product ion modes is time consuming, but allows identifying the structure of isomers or isobar in crude extracts.

[Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

PubMed

Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui

2014-05-01

A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were < or = 10 microg/kg, which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.

Analysis of additives in dairy products by liquid chromatography coupled to quadrupole-orbitrap mass spectrometry.

PubMed

Jia, Wei; Ling, Yun; Lin, Yuanhui; Chang, James; Chu, Xiaogang

2014-04-04

A new method combining QuEChERS with ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) was developed for the highly accurate and sensitive screening of 43 antioxidants, preservatives and synthetic sweeteners in dairy products. Response surface methodology was employed to optimize a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method for the determination of 42 different analytes in dairy products for the first time. After optimization, the maximum predicted recovery was 99.33% rate for aspartame under the optimized conditions of 10 mL acetionitrile, 1.52 g sodium acetate, 410 mg PSA and 404 mgC18. For the matrices studied, the recovery rates of the other 42 compounds ranged from 89.4% to 108.2%, with coefficient of variation <6.4%. UHPLC/ESI Q-Orbitrap Mass full scan mode acquired full MS data was used to identify and quantify additives, and data-dependent scan mode obtained fragment ion spectra for confirmation. The mass accuracy typically obtained is routinely better than 1.5ppm, and only need to calibrate once a week. The 43 compounds behave dynamic in the range 0.001-1000 μg kg(-1) concentration, with correlation coefficient >0.999. The limits of detection for the analytes are in the range 0.0001-3.6 μg kg(-1). This method has been successfully applied on screening of antioxidants, preservatives and synthetic sweeteners in commercial dairy product samples, and it is very useful for fast screening of different food additives. Copyright © 2014 Elsevier B.V. All rights reserved.

New drostanolone metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control.

PubMed

Liu, Yang; Lu, Jianghai; Yang, Sheng; Zhang, Qingying; Xu, Youxuan

2016-04-01

Drostanolone is one of the most frequently detected anabolic androgenic steroids in doping control analysis. Here, we studied drostanolone urinary metabolic profiles using liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. The drug was administered to one healthy male volunteer and liquid-liquid extraction along with direct-injection were used to analyze urine samples. Chromatographic peaks for potential metabolites were identified with the theoretical [M-H](-) as a target ion in a full scan experiment and actual deprotonated ions were analyzed in targeted MS/MS mode. Eleven metabolites including five new sulfates, five glucuronide conjugates, and one free metabolite were confirmed for drostanolone. Due to the absence of useful fragment ions to illustrate the steroid ring structure of drostanolone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was used to obtain structural details of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and a potential structure was proposed using a combined MS approach. Metabolite detection times were recorded and S4 (2α-methyl-5α-androstan-17-one-6β-ol-3α-sulfate) and G1 (2α-methyl-5α-androstan-17-one-3α-glucuronide) were thought to be new potential biomarkers for drostanolone misuse which can be detected up to 24days by liquid-liquid extraction and 7days by direct-injection analysis after intramuscular injection. S4 and G1 were also detected in two drostanolone-positive routine urine samples. Copyright © 2016 Elsevier Inc. All rights reserved.

Multiplexed data independent acquisition (MSX-DIA) applied by high resolution mass spectrometry improves quantification quality for the analysis of histone peptides.

PubMed

Sidoli, Simone; Fujiwara, Rina; Garcia, Benjamin A

2016-08-01

We present the MS-based application of the innovative, although scarcely exploited, multiplexed data-independent acquisition (MSX-DIA) for the analysis of histone PTMs. Histones are golden standard for complexity in MS based proteomics, due to their large number of combinatorial modifications, leading to isobaric peptides after proteolytic digestion. DIA has, thus, gained popularity for the purpose as it allows for MS/MS-based quantification without upfront assay development. In this work, we evaluated the performance of traditional DIA versus MSX-DIA in terms of MS/MS spectra quality, instrument scan rate and quantification precision using histones from HeLa cells. We used an MS/MS isolation window of 10 and 6 m/z for DIA and MSX-DIA, respectively. Four MS/MS scans were multiplexed for MSX-DIA. Despite MSX-DIA was programmed to perform two-fold more MS/MS events than traditional DIA, it acquired on average ∼5% more full MS scans, indicating even faster scan rate. Results highlighted an overall decrease of background ion signals using MSX-DIA, and we illustrated specific examples where peptides of different precursor masses were co-fragmented by DIA but not MSX-DIA. Taken together, MSX-DIA proved thus to be a more favorable method for histone analysis in data independent mode. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Comprehensive Workflow of Mass Spectrometry-Based Untargeted Metabolomics in Cancer Metabolic Biomarker Discovery Using Human Plasma and Urine

PubMed Central

Zou, Wei; She, Jianwen; Tolstikov, Vladimir V.

2013-01-01

Current available biomarkers lack sensitivity and/or specificity for early detection of cancer. To address this challenge, a robust and complete workflow for metabolic profiling and data mining is described in details. Three independent and complementary analytical techniques for metabolic profiling are applied: hydrophilic interaction liquid chromatography (HILIC–LC), reversed-phase liquid chromatography (RP–LC), and gas chromatography (GC). All three techniques are coupled to a mass spectrometer (MS) in the full scan acquisition mode, and both unsupervised and supervised methods are used for data mining. The univariate and multivariate feature selection are used to determine subsets of potentially discriminative predictors. These predictors are further identified by obtaining accurate masses and isotopic ratios using selected ion monitoring (SIM) and data-dependent MS/MS and/or accurate mass MSn ion tree scans utilizing high resolution MS. A list combining all of the identified potential biomarkers generated from different platforms and algorithms is used for pathway analysis. Such a workflow combining comprehensive metabolic profiling and advanced data mining techniques may provide a powerful approach for metabolic pathway analysis and biomarker discovery in cancer research. Two case studies with previous published data are adapted and included in the context to elucidate the application of the workflow. PMID:24958150

Determination of boldenone sulfoconjugate and related steroid sulfates in equine urine by high-performance liquid chromatography/tandem mass spectrometry.

PubMed

Weidolf, L O; Lee, E D; Henion, J D

1988-03-01

Sulfoconjugated anabolic steroids were separated by micro-bore high-performance liquid chromatography. The eluent was introduced into the atmospheric pressure ion source of the triple-quadrupole mass spectrometer via an ion spray liquid chromatograph/mass spectrometer interface operated in the negative ion mode. The limit of detection was 10 pg on-column by selected ion monitoring of the molecular ion and the response increased linearly over a concentration range of 2.4 orders of magnitude. Following work-up by a liquid-solid extraction procedure of equine urine samples, full-scan daughter ion spectra of boldenone sulfate could be obtained up to 17 days after a therapeutic dose of boldenone undecylenate to a horse.

Rapid screening of low-molecular-weight phenols from persimmon (Diospyros kaki) pulp using liquid chromatography/UV-visible/electrospray mass spectrometry analysis.

PubMed

Sentandreu, Enrique; Cerdán-Calero, Manuela; Halket, John M; Navarro, José L

2015-06-01

Persimmon fruits have been widely used in traditional medicine owing to their phenolic composition. This research aims to perform a rapid, detailed and affordable study of the profile of low-molecular-weight phenols from persimmon pulp. Two different HPLC-DAD/ESI-MS(n) analyses were performed using a routine three-dimensional ion trap mass spectrometer to analyze the ethanolic extract of persimmon pulp: (1) an untargeted data-dependent analysis to identify the majority of small phenols that included full MS and MS(2) scan events; (2) a targeted data-dependent analysis to identify polymerized phenols (dimers and formic acid adducts) through a source-induced dissociation analysis that included full MS and MS(2) scan events. Thirty-two low-molecular-weight phenols were detected, comprising gallic acid and its glycoside and acyl derivatives, glycosides of p-coumaric, vanillic and cinnamic acids and different flavone di-C-hexosides, most of them reported for the first time in persimmon. The use of a straightforward and affordable methodology of analysis led to obtain an up-to-date profiling of low-molecular-weight phenols in persimmon. The results can help future actions aimed to expand the understanding of the phenolic metabolome of persimmon cultivars. © 2014 Society of Chemical Industry.

Wide-field high-performance geosynchronous imaging

NASA Astrophysics Data System (ADS)

Wood, H. John; Jenstrom, Del; Wilson, Mark; Hinkal, Sanford; Kirchman, Frank

1998-01-01

The NASA Mission to Planet Earth (MTPE) Program and the National Oceanographic and Atmospheric Administration (NOAA) are sponsoring the Advanced Geosynchronous Studies (AGS) to develop technologies and system concepts for Earth observation from geosynchronous orbit. This series of studies is intended to benefit both MTPE science and the NOAA GOES Program. Within the AGS program, advanced imager trade studies have investigated two candidate concepts for near-term advanced geosynchronous imagers. One concept uses a scan mirror to direct the line of sight from a 3-axis stabilized platform. Another eliminates the need for a scan mirror by using an agile spacecraft bus to scan the entire instrument. The purpose of this paper is to discuss the optical design trades and system issues encountered in evaluating the two scanning approaches. The imager design started with a look at first principles: what is the most efficient way to image the Earth in those numerous spectral bands of interest to MTPE scientists and NOAA weather forecasters. Optical design trades included rotating filter wheels and dispersive grating instruments. The design converged on a bandpass filter instrument using four focal planes to cover the spectral range 0.45 to 13.0 micrometers. The first imager design uses a small agile spacecraft supporting an afocal optical telescope. Dichroic beamsplitters feed refractive objectives to four focal planes. The detectors are a series of long linear and rectangular arrays which are scanned in a raster fashion over the 17 degree Earth image. The use of the spacecraft attitude control system to raster the imager field-of-view (FOV) back and forth over the Earth eliminates the need for a scan mirror. However, the price paid is significant energy and time required to reverse the spacecraft slew motions at the end of each scan line. Hence, it is desired to minimize the number of scan lines needed to cover the full Earth disk. This desire, coupled with the ground coverage requirements, drives the telescope design to a 1.6 degree square FOV to provide full Earth disk coverage in less than 12 swaths. The telescope design to accommodate the FOV and image quality requirements is a 30 cm aperture three-element off-axis anastigmat. The size and mass of the imager instrument that result from this optical configuration are larger than desired. But spacecraft reaction wheel torque and power requirements to raster the imager FOV are achievable using existing spacecraft technology. However, launch mass and cost are higher than desired. In the second high-level trade study, the AGS imager team is looking at incorporating a scan mirror and having the satellite three-axis stabilized. The use of the scan mirror eliminates the long turn-around times of the spacecraft scanning approach, allowing for faster Earth coverage. Thus the field of view of the afocal telescope can be reduced by half while still satisfying ground coverage requirements. The optical design of the reduced field afocal telescope is being studied to shrink its size and improve its performance. Both a three-mirror Cassegrain afocal and a two-mirror pair of confocal paraboloids are being considered. With either telescope, the size, mass, and power requirements of this imager are significantly less than those of the first imager design. Both imager designs appear to be feasible and both meet envisioned MTPE and NOAA geosynchronous imaging needs. The AGS imager team is continuing to explore the optical trade space to further optimize imager designs.

ChromAlign: A two-step algorithmic procedure for time alignment of three-dimensional LC-MS chromatographic surfaces.

PubMed

Sadygov, Rovshan G; Maroto, Fernando Martin; Hühmer, Andreas F R

2006-12-15

We present an algorithmic approach to align three-dimensional chromatographic surfaces of LC-MS data of complex mixture samples. The approach consists of two steps. In the first step, we prealign chromatographic profiles: two-dimensional projections of chromatographic surfaces. This is accomplished by correlation analysis using fast Fourier transforms. In this step, a temporal offset that maximizes the overlap and dot product between two chromatographic profiles is determined. In the second step, the algorithm generates correlation matrix elements between full mass scans of the reference and sample chromatographic surfaces. The temporal offset from the first step indicates a range of the mass scans that are possibly correlated, then the correlation matrix is calculated only for these mass scans. The correlation matrix carries information on highly correlated scans, but it does not itself determine the scan or time alignment. Alignment is determined as a path in the correlation matrix that maximizes the sum of the correlation matrix elements. The computational complexity of the optimal path generation problem is reduced by the use of dynamic programming. The program produces time-aligned surfaces. The use of the temporal offset from the first step in the second step reduces the computation time for generating the correlation matrix and speeds up the process. The algorithm has been implemented in a program, ChromAlign, developed in C++ language for the .NET2 environment in WINDOWS XP. In this work, we demonstrate the applications of ChromAlign to alignment of LC-MS surfaces of several datasets: a mixture of known proteins, samples from digests of surface proteins of T-cells, and samples prepared from digests of cerebrospinal fluid. ChromAlign accurately aligns the LC-MS surfaces we studied. In these examples, we discuss various aspects of the alignment by ChromAlign, such as constant time axis shifts and warping of chromatographic surfaces.

Application of the MIDAS approach for analysis of lysine acetylation sites.

PubMed

Evans, Caroline A; Griffiths, John R; Unwin, Richard D; Whetton, Anthony D; Corfe, Bernard M

2013-01-01

Multiple Reaction Monitoring Initiated Detection and Sequencing (MIDAS™) is a mass spectrometry-based technique for the detection and characterization of specific post-translational modifications (Unwin et al. 4:1134-1144, 2005), for example acetylated lysine residues (Griffiths et al. 18:1423-1428, 2007). The MIDAS™ technique has application for discovery and analysis of acetylation sites. It is a hypothesis-driven approach that requires a priori knowledge of the primary sequence of the target protein and a proteolytic digest of this protein. MIDAS essentially performs a targeted search for the presence of modified, for example acetylated, peptides. The detection is based on the combination of the predicted molecular weight (measured as mass-charge ratio) of the acetylated proteolytic peptide and a diagnostic fragment (product ion of m/z 126.1), which is generated by specific fragmentation of acetylated peptides during collision induced dissociation performed in tandem mass spectrometry (MS) analysis. Sequence information is subsequently obtained which enables acetylation site assignment. The technique of MIDAS was later trademarked by ABSciex for targeted protein analysis where an MRM scan is combined with full MS/MS product ion scan to enable sequence confirmation.

Evaluation of diagnostic value of CT scan, physical examination and ultrasound based on pathological findings in patients with pelvic masses.

PubMed

Firoozabadi, Razieh Dehghani; Karimi Zarchi, Mojgan; Mansurian, Hamid Reza; Moghadam, Bita Rafiei; Teimoori, Soraya; Naseri, Ali

2011-01-01

Because benign and malignant cervical and ovarian masses occur with different percentages in different age groups, the importance of primary diagnosis and selection of a suitable surgical procedure is underlined. Diagnosis of pelvic masses is carried out using ultrasound, physical examination, CT scan and MRI. The objective of this study is to evaluate the diagnostic value of CT scan in pelvic masses in comparison with physical examination-ultrasound based on pathology of the lesion in patients undergoing laparotomic surgery. This analytic-descriptive study focused on age, sonographic findings, physical examinations, CT scan and pathological findings in 139 patients with pelvic mass, gathered with questionnaires and statistically analayzed using the SPSS software programme. Of 139 patients with pelvic mass (patients aged from 17 to 75 years old), 62 (44%) cases were diagnosed as benign and 77 (55.4%) as malignant; among them malignant tratoma serocyst adenocarsinoma with 33 (23.7%) cases and benign myoma with 21 (15.2%) cases comprised the most frequent cases. The sensitivity and specificity of sonography-physical examination were 51.9% and 87.9% respectively and the sensitivity and specificity of CT scan images were 79.2% and 91.6% respectively. It was shown that CT scan images were more consistant with pathological findings in predicting appropriate surgical procedures than do sonography-physical examinations. The sensitivity of CT scan is far higher than that of sonography-physical examination in the diagnosis of pelvic mass malignancy.

GC and GC-MS determination of fluoroacetic acid and phenoxy acid herbicides via triphasal extractive pentafluorobenzylation using a polymer-bound phase-transfer catalyst.

PubMed

Miki, A; Tsuchihashi, H; Yamashita, M

1998-01-01

A simple and sensitive gas chromatography and gas chromatography-mass spectrometry (GC-MS) procedure has been developed for fluoroacetic acid (FA) and phenoxy acid herbicides (PAHs) via triphasal extractive pentafluorobenzylation. The triphasal system consisted of an aqueous sample, the extraction solvent toluene containing pentafluorobenzyl bromide as the derivatization reagent, and polymer-bound tri-n-butyl-methylphosphonium bromide as a phase-transfer catalyst, FA spiked in beverages, such as orange juice and milk, was extracted as its pentafluorobenzyl (PFB) derivative under moderate conditions (i.e., at a pH value of 6.5 at 60 degrees C). The detection limits were 0.10-0.20 microgram/mL by GC with electron-capture detection (GC-ECD), and 0.42-0.50 microgram/mL by full-scan GC-MS. PAHs were also detectable in the same manner within the detection limits of 0.05-0.10 microgram/mL by GC-ECD and 0.13-0.25 microgram/mL by full-scan GC-MS. Urine and serum which both contained 2,4-dichlorophenoxyacetic acid could also be analyzed by GC-MS after the triphasal pentafluorobenzylation. The detection limit was 0.20 microgram/mL in the full-scan mode and 10 ng/mL in the selected ion monitoring mode both for the urine and serum.

Ultrahigh-performance liquid chromatography electrospray ionization Q-Orbitrap mass spectrometry for the analysis of 451 pesticide residues in fruits and vegetables: method development and validation.

PubMed

Wang, Jian; Chow, Willis; Chang, James; Wong, Jon W

2014-10-22

This paper presents an application of ultrahigh-performance liquid chromatography electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) for the determination of 451 pesticide residues in fruits and vegetables. Pesticides were extracted from samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS in full MS scan mode acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) (i.e., data-dependent scan mode) obtained product ion spectra for identification. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves along with the use of isotopically labeled standards or a chemical analogue as internal standards to achieve optimal method accuracy. The method performance characteristics include overall recovery, intermediate precision, and measurement uncertainty evaluated according to a nested experimental design. For the 10 matrices studied, 94.5% of the pesticides in fruits and 90.7% in vegetables had recoveries between 81 and 110%; 99.3% of the pesticides in fruits and 99.1% of the pesticides in vegetables had an intermediate precision of ≤20%; and 97.8% of the pesticides in fruits and 96.4% of the pesticides in vegetables showed measurement uncertainty of ≤50%. Overall, the UHPLC/ESI Q-Orbitrap MS demonstrated acceptable performance for the quantification of pesticide residues in fruits and vegetables. The UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) along with library matching showed great potential for identification and is being investigated further for routine practice.

The current role of high-resolution mass spectrometry in food analysis.

PubMed

Kaufmann, Anton

2012-05-01

High-resolution mass spectrometry (HRMS), which is used for residue analysis in food, has gained wider acceptance in the last few years. This development is due to the availability of more rugged, sensitive, and selective instrumentation. The benefits provided by HRMS over classical unit-mass-resolution tandem mass spectrometry are considerable. These benefits include the collection of full-scan spectra, which provides greater insight into the composition of a sample. Consequently, the analyst has the freedom to measure compounds without previous compound-specific tuning, the possibility of retrospective data analysis, and the capability of performing structural elucidations of unknown or suspected compounds. HRMS strongly competes with classical tandem mass spectrometry in the field of quantitative multiresidue methods (e.g., pesticides and veterinary drugs). It is one of the most promising tools when moving towards nontargeted approaches. Certain hardware and software issues still have to be addressed by the instrument manufacturers for it to dislodge tandem mass spectrometry from its position as the standard trace analysis tool.

Neutrino masses and their ordering: global data, priors and models

NASA Astrophysics Data System (ADS)

Gariazzo, S.; Archidiacono, M.; de Salas, P. F.; Mena, O.; Ternes, C. A.; Tórtola, M.

2018-03-01

We present a full Bayesian analysis of the combination of current neutrino oscillation, neutrinoless double beta decay and Cosmic Microwave Background observations. Our major goal is to carefully investigate the possibility to single out one neutrino mass ordering, namely Normal Ordering or Inverted Ordering, with current data. Two possible parametrizations (three neutrino masses versus the lightest neutrino mass plus the two oscillation mass splittings) and priors (linear versus logarithmic) are exhaustively examined. We find that the preference for NO is only driven by neutrino oscillation data. Moreover, the values of the Bayes factor indicate that the evidence for NO is strong only when the scan is performed over the three neutrino masses with logarithmic priors; for every other combination of parameterization and prior, the preference for NO is only weak. As a by-product of our Bayesian analyses, we are able to (a) compare the Bayesian bounds on the neutrino mixing parameters to those obtained by means of frequentist approaches, finding a very good agreement; (b) determine that the lightest neutrino mass plus the two mass splittings parametrization, motivated by the physical observables, is strongly preferred over the three neutrino mass eigenstates scan and (c) find that logarithmic priors guarantee a weakly-to-moderately more efficient sampling of the parameter space. These results establish the optimal strategy to successfully explore the neutrino parameter space, based on the use of the oscillation mass splittings and a logarithmic prior on the lightest neutrino mass, when combining neutrino oscillation data with cosmology and neutrinoless double beta decay. We also show that the limits on the total neutrino mass ∑ mν can change dramatically when moving from one prior to the other. These results have profound implications for future studies on the neutrino mass ordering, as they crucially state the need for self-consistent analyses which explore the best parametrization and priors, without combining results that involve different assumptions.

The core of tau-paired helical filaments studied by scanning transmission electron microscopy and limited proteolysis.

PubMed

von Bergen, Martin; Barghorn, Stefan; Müller, Shirley A; Pickhardt, Marcus; Biernat, Jacek; Mandelkow, Eva-Maria; Davies, Peter; Aebi, Ueli; Mandelkow, Eckhard

2006-05-23

In Alzheimer's disease and frontotemporal dementias the microtubule-associated protein tau forms intracellular paired helical filaments (PHFs). The filaments formed in vivo consist mainly of full-length molecules of the six different isoforms present in adult brain. The substructure of the PHF core is still elusive. Here we applied scanning transmission electron microscopy (STEM) and limited proteolysis to probe the mass distribution of PHFs and their surface exposure. Tau filaments assembled from the three repeat domain have a mass per length (MPL) of approximately 60 kDa/nm and filaments from full-length tau (htau40DeltaK280 mutant) have approximately 160 kDa/nm, compared with approximately 130 kDa/nm for PHFs from Alzheimer's brain. Polyanionic cofactors such as heparin accelerate assembly but are not incorporated into PHFs. Limited proteolysis combined with N-terminal sequencing and mass spectrometry of fragments reveals a protease-sensitive N-terminal half and semiresistant PHF core starting in the first repeat and reaching to the C-terminus of tau. Continued proteolysis leads to a fragment starting at the end of the first repeat and ending in the fourth repeat. PHFs from tau isoforms with four repeats revealed an additional cleavage site within the middle of the second repeat. Probing the PHFs with antibodies detecting epitopes either over longer stretches in the C-terminal half of tau or in the fourth repeat revealed that they grow in a polar manner. These data describe the physical parameters of the PHFs and enabled us to build a model of the molecular arrangement within the filamentous structures.

Influence of natural organic matter on the screening of pharmaceuticals in water by using liquid chromatography with full scan mass spectrometry.

PubMed

Rivera, Zahira Herrera; Oosterink, Efraim; Rietveld, Luuk; Schoutsen, Frans; Stolker, Linda

2011-08-26

The influence of natural organic matter on the screening of pharmaceuticals in water was determined by using high resolution liquid chromatography (HRLC) combined with full scan mass spectrometry (MS) techniques like time of flight (ToF) or Orbitrap MS. Water samples containing different amount of natural organic matter (NOM) and residues of a set of 11 pharmaceuticals were analyzed by using Exactive Orbitrap™ LC-MS. The samples were screened for residues of pharmaceuticals belonging to different classes like benzimidazoles, macrolides, penicillins, quinolones, sulfonamides, tetracyclines, tranquillizers, non-steroidal anti-inflammatory drugs (NSAIDs), anti-epileptics and lipid regulators. The method characteristics were established over a concentration range of 0.1-500 μg L(-1). The 11 pharmaceuticals were added to two effluent and two influent water samples. The NOM concentration within the samples ranged from 2 to 8 mg L(-1) of dissolved organic carbon. The HRLC-Exactive Orbitrap™ LC-MS system was set at a resolution of 50,000 (FWHM) and this selection was found sufficient for the detection of the list of pharmaceuticals. With this resolution setting, accurate mass measurements with errors below 2 ppm were found, despite of the NOM concentration of the different types of water samples. The linearities were acceptable with correlation coefficients greater than 0.95 for 30 of the 51 measured linearities. The limit of detection varies between 0.1 μg L(-1)and 100 μg L(-1). It was demonstrated that sensitivity could be affected by matrix constituents in both directions of signal reduction or enhancement. Finally it was concluded that with direct shoot method used (no sample pretreatment) all compounds, were detected but LODs depend on matrix-analyte-concentration combination. No direct relation was observed between NOM concentration and method characteristics. For accurate quantification the use of internal standards and/or sample clean-up is necessary. The direct shoot method is only applicable for qualitative screening purposes. The use of full scan MS makes it possible to search for unknown contaminants. With the use of adequate software and a database containing more than 50,000 entries a tool is available to search for unknowns. Copyright © 2011 Elsevier B.V. All rights reserved.

Conventional liquid chromatography/triple quadrupole mass spectrometer-based metabolite identification and semi-quantitative estimation approach in the investigation of dabigatran etexilate in vitro metabolism

PubMed Central

Hu, Zhe-Yi; Parker, Robert B.; Herring, Vanessa L.; Laizure, S. Casey

2012-01-01

Dabigatran etexilate (DABE) is an oral prodrug that is rapidly converted by esterases to dabigatran (DAB), a direct inhibitor of thrombin. To elucidate the esterase-mediated metabolic pathway of DABE, a high-performance liquid chromatography/mass spectrometer (LC-MS/MS)-based metabolite identification and semi-quantitative estimation approach was developed. To overcome the poor full-scan sensitivity of conventional triple quadrupole mass spectrometry, precursor-product ion pairs were predicted, to search for the potential in vitro metabolites. The detected metabolites were confirmed by the product ion scan. A dilution method was introduced to evaluate the matrix effects of tentatively identified metabolites without chemical standards. Quantitative information on detected metabolites was obtained using ‘metabolite standards’ generated from incubation samples that contain a high concentration of metabolite in combination with a correction factor for mass spectrometry response. Two in vitro metabolites of DABE (M1 and M2) were identified, and quantified by the semi-quantitative estimation approach. It is noteworthy that CES1 convert DABE to M1 while CES2 mediates the conversion of DABE to M2. M1 (or M2) was further metabolized to DAB by CES2 (or CES1). The approach presented here provides a solution to a bioanalytical need for fast identification and semi-quantitative estimation of CES metabolites in preclinical samples. PMID:23239178

Quantitative targeted and retrospective data analysis of relevant pesticides, antibiotics and mycotoxins in bakery products by liquid chromatography-single-stage Orbitrap mass spectrometry.

PubMed

De Dominicis, Emiliano; Commissati, Italo; Gritti, Elisa; Catellani, Dante; Suman, Michele

2015-01-01

In addition to 'traditional' multi-residue and multi-contaminant multiple reaction monitoring (MRM) mass spectrometric techniques devoted to quantifying a list of targeted compounds, the global food industry requires non-targeted methods capable of detecting other possible potentially hazardous compounds. Ultra-high-performance liquid chromatography combined with a single-stage Orbitrap high-resolution mass spectrometer (UHPLC-HRMS Exactive™-Orbitrap Technology) was successfully exploited for the complete selective and quantitative determination of 33 target compounds within three major cross categories (pesticides, antibiotics and mycotoxins) in bakery matrices (specifically milk, wheat flour and mini-cakes). Resolution was set at 50 000 full width at half maximum (FWHM) to achieve the right compromise between an adequate scan speed and selectivity, allowing for the limitations related to the necessary generic sample preparation approach. An exact mass with tolerance of 5 ppm and minimum peak threshold of 10 000 units were fixed as the main identification conditions, including retention time and isotopic pattern as additional criteria devoted to greatly reducing the risk of false-positive findings. The full validation for all the target analytes was performed: linearity, intermediate repeatability and recovery (28 analytes within 70-120%) were positively assessed; furthermore, limits of quantification between 5 and 100 µg kg(-1) (with most of the analytes having a limit of detection below 6 µg kg(-1)) indicate good performance, which is compatible with almost all the regulatory needs. Naturally contaminated and fortified mini-cakes, prepared through combined use of industrial and pilot plant production lines, were analysed at two different concentration levels, obtaining good overall quantitative results and providing preliminary indications of the potential of full-scan HRMS cluster analysis. The effectiveness of this analytical approach was also tested in terms of the formulation of hypotheses for the identification of other analytes not initially targeted which can have toxicological implications (e.g. 3-acetyl-deoxynivalenol and deoxynivalenol-3-glucoside), opening a window on retrospective investigation perspectives in food safety laboratories.

Algorithm-enabled partial-angular-scan configurations for dual-energy CT.

PubMed

Chen, Buxin; Zhang, Zheng; Xia, Dan; Sidky, Emil Y; Pan, Xiaochuan

2018-05-01

We seek to investigate an optimization-based one-step method for image reconstruction that explicitly compensates for nonlinear spectral response (i.e., the beam-hardening effect) in dual-energy CT, to investigate the feasibility of the one-step method for enabling two dual-energy partial-angular-scan configurations, referred to as the short- and half-scan configurations, on standard CT scanners without involving additional hardware, and to investigate the potential of the short- and half-scan configurations in reducing imaging dose and scan time in a single-kVp-switch full-scan configuration in which two full rotations are made for collection of dual-energy data. We use the one-step method to reconstruct images directly from dual-energy data through solving a nonconvex optimization program that specifies the images to be reconstructed in dual-energy CT. Dual-energy full-scan data are generated from numerical phantoms and collected from physical phantoms with the standard single-kVp-switch full-scan configuration, whereas dual-energy short- and half-scan data are extracted from the corresponding full-scan data. Besides visual inspection and profile-plot comparison, the reconstructed images are analyzed also in quantitative studies based upon tasks of linear-attenuation-coefficient and material-concentration estimation and of material differentiation. Following the performance of a computer-simulation study to verify that the one-step method can reconstruct numerically accurately basis and monochromatic images of numerical phantoms, we reconstruct basis and monochromatic images by using the one-step method from real data of physical phantoms collected with the full-, short-, and half-scan configurations. Subjective inspection based upon visualization and profile-plot comparison reveals that monochromatic images, which are used often in practical applications, reconstructed from the full-, short-, and half-scan data are largely visually comparable except for some differences in texture details. Moreover, quantitative studies based upon tasks of linear-attenuation-coefficient and material-concentration estimation and of material differentiation indicate that the short- and half-scan configurations yield results in close agreement with the ground-truth information and that of the full-scan configuration. The one-step method considered can compensate effectively for the nonlinear spectral response in full- and partial-angular-scan dual-energy CT. It can be exploited for enabling partial-angular-scan configurations on standard CT scanner without involving additional hardware. Visual inspection and quantitative studies reveal that, with the one-step method, partial-angular-scan configurations considered can perform at a level comparable to that of the full-scan configuration, thus suggesting the potential of the two partial-angular-scan configurations in reducing imaging dose and scan time in the standard single-kVp-switch full-scan CT in which two full rotations are performed. The work also yields insights into the investigation and design of other nonstandard scan configurations of potential practical significance in dual-energy CT. © 2018 American Association of Physicists in Medicine.

Laser Microdissection and Atmospheric Pressure Chemical Ionization Mass Spectrometry Coupled for Multimodal Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lorenz, Matthias; Ovchinnikova, Olga S; Kertesz, Vilmos

2013-01-01

This paper describes the coupling of ambient laser ablation surface sampling, accomplished using a laser capture microdissection system, with atmospheric pressure chemical ionization mass spectrometry for high spatial resolution multimodal imaging. A commercial laser capture microdissection system was placed in close proximity to a modified ion source of a mass spectrometer designed to allow for sampling of laser ablated material via a transfer tube directly into the ionization region. Rhodamine 6G dye of red sharpie ink in a laser etched pattern as well as cholesterol and phosphatidylcholine in a cerebellum mouse brain thin tissue section were identified and imaged frommore » full scan mass spectra. A minimal spot diameter of 8 m was achieved using the 10X microscope cutting objective with a lateral oversampling pixel resolution of about 3.7 m. Distinguishing between features approximately 13 m apart in a cerebellum mouse brain thin tissue section was demonstrated in a multimodal fashion including co-registered optical and mass spectral chemical images.« less

Experimental Characterization of Secular Frequency Scanning in Ion Trap Mass Spectrometers

NASA Astrophysics Data System (ADS)

Snyder, Dalton T.; Pulliam, Christopher J.; Wiley, Joshua S.; Duncan, Jason; Cooks, R. Graham

2016-07-01

Secular frequency scanning is implemented and characterized using both a benchtop linear ion trap and a miniature rectilinear ion trap mass spectrometer. Separation of tetraalkylammonium ions and those from a mass calibration mixture and from a pesticide mixture is demonstrated with peak widths approaching unit resolution for optimized conditions using the benchtop ion trap. The effects on the spectra of ion trap operating parameters, including waveform amplitude, scan direction, scan rate, and pressure are explored, and peaks at black holes corresponding to nonlinear (higher-order field) resonance points are investigated. Reverse frequency sweeps (increasing mass) on the Mini 12 are shown to result in significantly higher ion ejection efficiency and superior resolution than forward frequency sweeps that decrement mass. This result is accounted for by the asymmetry in ion energy absorption profiles as a function of AC frequency and the shift in ion secular frequency at higher amplitudes in the trap due to higher order fields. We also found that use of higher AC amplitudes in forward frequency sweeps biases ions toward ejection at points of higher order parametric resonance, despite using only dipolar excitation. Higher AC amplitudes also increase peak width and decrease sensitivity in both forward and reverse frequency sweeps. Higher sensitivity and resolution were obtained at higher trap pressures in the secular frequency scan, in contrast to conventional resonance ejection scans, which showed the opposite trend in resolution on the Mini 12. Mass range is shown to be naturally extended in secular frequency scanning when ejecting ions by sweeping the AC waveform through low frequencies, a method which is similar, but arguably superior, to the more usual method of mass range extension using low q resonance ejection.

Experimental Characterization of Secular Frequency Scanning in Ion Trap Mass Spectrometers.

PubMed

Snyder, Dalton T; Pulliam, Christopher J; Wiley, Joshua S; Duncan, Jason; Cooks, R Graham

2016-07-01

Secular frequency scanning is implemented and characterized using both a benchtop linear ion trap and a miniature rectilinear ion trap mass spectrometer. Separation of tetraalkylammonium ions and those from a mass calibration mixture and from a pesticide mixture is demonstrated with peak widths approaching unit resolution for optimized conditions using the benchtop ion trap. The effects on the spectra of ion trap operating parameters, including waveform amplitude, scan direction, scan rate, and pressure are explored, and peaks at black holes corresponding to nonlinear (higher-order field) resonance points are investigated. Reverse frequency sweeps (increasing mass) on the Mini 12 are shown to result in significantly higher ion ejection efficiency and superior resolution than forward frequency sweeps that decrement mass. This result is accounted for by the asymmetry in ion energy absorption profiles as a function of AC frequency and the shift in ion secular frequency at higher amplitudes in the trap due to higher order fields. We also found that use of higher AC amplitudes in forward frequency sweeps biases ions toward ejection at points of higher order parametric resonance, despite using only dipolar excitation. Higher AC amplitudes also increase peak width and decrease sensitivity in both forward and reverse frequency sweeps. Higher sensitivity and resolution were obtained at higher trap pressures in the secular frequency scan, in contrast to conventional resonance ejection scans, which showed the opposite trend in resolution on the Mini 12. Mass range is shown to be naturally extended in secular frequency scanning when ejecting ions by sweeping the AC waveform through low frequencies, a method which is similar, but arguably superior, to the more usual method of mass range extension using low q resonance ejection. Graphical Abstract ᅟ.

High Dynamic Range Pixel Array Detector for Scanning Transmission Electron Microscopy.

PubMed

Tate, Mark W; Purohit, Prafull; Chamberlain, Darol; Nguyen, Kayla X; Hovden, Robert; Chang, Celesta S; Deb, Pratiti; Turgut, Emrah; Heron, John T; Schlom, Darrell G; Ralph, Daniel C; Fuchs, Gregory D; Shanks, Katherine S; Philipp, Hugh T; Muller, David A; Gruner, Sol M

2016-02-01

We describe a hybrid pixel array detector (electron microscope pixel array detector, or EMPAD) adapted for use in electron microscope applications, especially as a universal detector for scanning transmission electron microscopy. The 128×128 pixel detector consists of a 500 µm thick silicon diode array bump-bonded pixel-by-pixel to an application-specific integrated circuit. The in-pixel circuitry provides a 1,000,000:1 dynamic range within a single frame, allowing the direct electron beam to be imaged while still maintaining single electron sensitivity. A 1.1 kHz framing rate enables rapid data collection and minimizes sample drift distortions while scanning. By capturing the entire unsaturated diffraction pattern in scanning mode, one can simultaneously capture bright field, dark field, and phase contrast information, as well as being able to analyze the full scattering distribution, allowing true center of mass imaging. The scattering is recorded on an absolute scale, so that information such as local sample thickness can be directly determined. This paper describes the detector architecture, data acquisition system, and preliminary results from experiments with 80-200 keV electron beams.

Partial scan artifact reduction (PSAR) for the assessment of cardiac perfusion in dynamic phase-correlated CT.

PubMed

Stenner, Philip; Schmidt, Bernhard; Bruder, Herbert; Allmendinger, Thomas; Haberland, Ulrike; Flohr, Thomas; Kachelriess, Marc

2009-12-01

Cardiac CT achieves its high temporal resolution by lowering the scan range from 2pi to pi plus fan angle (partial scan). This, however, introduces CT-value variations, depending on the angular position of the pi range. These partial scan artifacts are of the order of a few HU and prevent the quantitative evaluation of perfusion measurements. The authors present the new algorithm partial scan artifact reduction (PSAR) that corrects a dynamic phase-correlated scan without a priori information. In general, a full scan does not suffer from partial scan artifacts since all projections in [0, 2pi] contribute to the data. To maintain the optimum temporal resolution and the phase correlation, PSAR creates an artificial full scan pn(AF) by projectionwise averaging a set of neighboring partial scans pn(P) from the same perfusion examination (typically N approximately 30 phase-correlated partial scans distributed over 20 s and n = 1, ..., N). Corresponding to the angular range of each partial scan, the authors extract virtual partial scans pn(V) from the artificial full scan pn(AF). A standard reconstruction yields the corresponding images fn(P), fn(AF), and fn(V). Subtracting the virtual partial scan image fn(V) from the artificial full scan image fn(AF) yields an artifact image that can be used to correct the original partial scan image: fn(C) = fn(P) - fn(V) + fn(AF), where fn(C) is the corrected image. The authors evaluated the effects of scattered radiation on the partial scan artifacts using simulated and measured water phantoms and found a strong correlation. The PSAR algorithm has been validated with a simulated semianthropomorphic heart phantom and with measurements of a dynamic biological perfusion phantom. For the stationary phantoms, real full scans have been performed to provide theoretical reference values. The improvement in the root mean square errors between the full and the partial scans with respect to the errors between the full and the corrected scans is up to 54% for the simulations and 90% for the measurements. The phase-correlated data now appear accurate enough for a quantitative analysis of cardiac perfusion.

Chemical Mass Shifts in a Digital Linear Ion Trap as Analytical Identity of o-, m-, and p-Xylene.

PubMed

Sun, Lulu; Xue, Bing; Huang, Zhengxu; Cheng, Ping; Ma, Li; Ding, Li; Zhou, Zhen

2018-07-01

Chemical mass shifts between isomeric ions of o-, m-, and p-xylene were measured using a digital linear ion trap, and the directions and values of the shifts were found to be correlated to the collision cross sections of the isomers. Both forward and reverse scans were used and the chemical shifts for each pair of isomers in scans of opposite directions were in opposite signs. Using different voltage settings (namely the voltage dividing ratio-VDR) of the ion trap allows adding high order field components in the quadrupole field and results in larger chemical mass shifts. The differential chemical mass shift which combined the shifts from forward and reverse scans doubled the amount of chemical shift, e.g., 0.077 Th between o- and p-xylene, enough for identification of the type of isomer without using an additional ion mobility spectrometer. The feature of equal and opposite chemical mass shifts also allowed to null out the chemical mass shift by calculating the mean m/z value between the two opposite scans and remove or reduce the mass error caused by chemical mass shift. Graphical Abstract ᅟ.

Chemical Mass Shifts in a Digital Linear Ion Trap as Analytical Identity of o-, m-, and p-Xylene

NASA Astrophysics Data System (ADS)

Sun, Lulu; Xue, Bing; Huang, Zhengxu; Cheng, Ping; Ma, Li; Ding, Li; Zhou, Zhen

2018-04-01

Chemical mass shifts between isomeric ions of o-, m-, and p-xylene were measured using a digital linear ion trap, and the directions and values of the shifts were found to be correlated to the collision cross sections of the isomers. Both forward and reverse scans were used and the chemical shifts for each pair of isomers in scans of opposite directions were in opposite signs. Using different voltage settings (namely the voltage dividing ratio-VDR) of the ion trap allows adding high order field components in the quadrupole field and results in larger chemical mass shifts. The differential chemical mass shift which combined the shifts from forward and reverse scans doubled the amount of chemical shift, e.g., 0.077 Th between o- and p-xylene, enough for identification of the type of isomer without using an additional ion mobility spectrometer. The feature of equal and opposite chemical mass shifts also allowed to null out the chemical mass shift by calculating the mean m/z value between the two opposite scans and remove or reduce the mass error caused by chemical mass shift. [Figure not available: see fulltext.

Fast analysis of triterpenoids in Ganoderma lucidum spores by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

PubMed

Yan, Zhou; Xia, Bing; Qiu, Ming Hua; Li Sheng, Ding; Xu, Hong Xi

2013-11-01

A rapid and reliable method was established for simultaneous determination of main triterpenoids in Ganoderma lucidum spores using ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-TQ-MS). The established method was validated in terms of linearity, sensitivity, precision, accuracy and stability, and was successfully applied to determine the contents of 10 main triterpenoids in different batches of G. lucidum spores. The analysis results showed that moderate levels of triterpenoids were found in G. lucidum spores. In addition, a MS full scan with a daughter ion scan experiment was performed to identify the potential derivatives of triterpenoids present in G. lucidum spores. As a result, a total of 22 triterpenoids from different G. lucidum spores were unequivocally or tentatively identified via comparisons with authentic standards and literatures. This method provides both qualitative and quantitative results without the need for repetitive UPLC-MS analyses, thereby increasing efficiency and productivity, making it suitable for high-throughput applications. Copyright © 2013 John Wiley & Sons, Ltd.

[Simultaneous determination of nine preservatives in fruits using gas chromatography-mass spectrometry].

PubMed

Peng, Shunü; Wang, Qiuquan; Fang, Lanlan; Guo, Shanyong; Zeng, Zhouhua; Lin, Zhuguang

2014-01-01

A gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of nine typical preservatives (pyrimethanil, chlorothalonil, chlorpyrifos, triadimefon, thiabendazole, imazalil, myclobutanil, iprodione, prochloraz) in fruits. The fruit samples were subjected to ultrasonic extraction with hexane/ethyl acetate (1/1, v/v), and followed by purification using diatomite column chromatography with hexane/ethyl acetate (1/3, v/v) eluant. Qualitative and quantitative analysis of the nine preservatives were performed on the GC-MS at full-scan (SCAN) and selected ion monitoring (SIM) modes, in which triphenylphosphate was used as the internal standard. The detection limits obtained for the nine preservatives were ranged from 0.10 microg/kg to 2.16 microg/kg. The average recoveries were in the range of 75.3% to 128% at the spiked levels of 50, 100 and 200 microg/kg with the relative standard deviations (RSDs) of 1.57% to 11.6% (n = 5). The results showed that the developed method is sensitive and accurate for the determination of the nine preservatives in fruits.

ScanRanker: Quality Assessment of Tandem Mass Spectra via Sequence Tagging

PubMed Central

Ma, Ze-Qiang; Chambers, Matthew C.; Ham, Amy-Joan L.; Cheek, Kristin L.; Whitwell, Corbin W.; Aerni, Hans-Rudolf; Schilling, Birgit; Miller, Aaron W.; Caprioli, Richard M.; Tabb, David L.

2011-01-01

In shotgun proteomics, protein identification by tandem mass spectrometry relies on bioinformatics tools. Despite recent improvements in identification algorithms, a significant number of high quality spectra remain unidentified for various reasons. Here we present ScanRanker, an open-source tool that evaluates the quality of tandem mass spectra via sequence tagging with reliable performance in data from different instruments. The superior performance of ScanRanker enables it not only to find unassigned high quality spectra that evade identification through database search, but also to select spectra for de novo sequencing and cross-linking analysis. In addition, we demonstrate that the distribution of ScanRanker scores predicts the richness of identifiable spectra among multiple LC-MS/MS runs in an experiment, and ScanRanker scores assist the process of peptide assignment validation to increase confident spectrum identifications. The source code and executable versions of ScanRanker are available from http://fenchurch.mc.vanderbilt.edu. PMID:21520941

Multi-targeted interference-free determination of ten β-blockers in human urine and plasma samples by alternating trilinear decomposition algorithm-assisted liquid chromatography-mass spectrometry in full scan mode: comparison with multiple reaction monitoring.

PubMed

Gu, Hui-Wen; Wu, Hai-Long; Yin, Xiao-Li; Li, Yong; Liu, Ya-Juan; Xia, Hui; Zhang, Shu-Rong; Jin, Yi-Feng; Sun, Xiao-Dong; Yu, Ru-Qin; Yang, Peng-Yuan; Lu, Hao-Jie

2014-10-27

β-blockers are the first-line therapeutic agents for treating cardiovascular diseases and also a class of prohibited substances in athletic competitions. In this work, a smart strategy that combines three-way liquid chromatography-mass spectrometry (LC-MS) data with second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm was developed for simultaneous determination of ten β-blockers in human urine and plasma samples. This flexible strategy proved to be a useful tool to solve the problems of overlapped peaks and uncalibrated interferences encountered in quantitative LC-MS, and made the multi-targeted interference-free qualitative and quantitative analysis of β-blockers in complex matrices possible. The limits of detection were in the range of 2.0×10(-5)-6.2×10(-3) μg mL(-1), and the average recoveries were between 90 and 110% with standard deviations and average relative prediction errors less than 10%, indicating that the strategy could provide satisfactory prediction results for ten β-blockers in human urine and plasma samples only using liquid chromatography hyphenated single-quadrupole mass spectrometer in full scan mode. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring (MRM) method. T-test demonstrated that there are no significant differences between the prediction results of the two methods. Considering the advantages of fast, low-cost, high sensitivity, and no need of complicated chromatographic and tandem mass spectrometric conditions optimization, the proposed strategy is expected to be extended as an attractive alternative method to quantify analyte(s) of interest in complex systems such as cells, biological fluids, food, environment, pharmaceuticals and other complex samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Three-dimensional body scanning system for apparel mass-customization

NASA Astrophysics Data System (ADS)

Xu, Bugao; Huang, Yaxiong; Yu, Weiping; Chen, Tong

2002-07-01

Mass customization is a new manufacturing trend in which mass-market products (e.g., apparel) are quickly modified one at a time based on customers' needs. It is an effective competing strategy for maximizing customers' satisfaction and minimizing inventory costs. An automatic body measurement system is essential for apparel mass customization. This paper introduces the development of a body scanning system, body size extraction methods, and body modeling algorithms. The scanning system utilizes the multiline triangulation technique to rapidly acquire surface data on a body, and provides accurate body measurements, many of which are not available with conventional methods. Cubic B-spline curves are used to connect and smooth body curves. From the scanned data, a body form can be constructed using linear Coons surfaces. The body form can be used as a digital model of the body for 3-D garment design and for virtual try-on of a designed garment. This scanning system and its application software enable apparel manufacturers to provide custom design services to consumers seeking personal-fit garments.

In vitro metabolism study of Strychnos alkaloids using high-performance liquid chromatography combined with hybrid ion trap/time-of-flight mass spectrometry.

PubMed

Tian, Ji-Xin; Peng, Can; Xu, Lei; Tian, Yuan; Zhang, Zun-Jian

2013-06-01

In this report, the in vitro metabolism of Strychnos alkaloids was investigated using liquid chromatography/high-resolution mass spectrometry for the first time. Strychnine and brucine were selected as model compounds to determine the universal biotransformations of the Strychnos alkaloids in rat liver microsomes. The incubation mixtures were separated by a bidentate-C18 column, and then analyzed by on-line ion trap/time-of-flight mass spectrometry. With the assistance of mass defect filtering technique, full-scan accurate mass datasets were processed for the discovery of the related metabolites. The structural elucidations of these metabolites were achieved by comparing the changes in accurate molecular masses, calculating chemical component using Formula Predictor software and defining sites of biotransformation based upon accurate MS(n) spectral information. As a result, 31 metabolites were identified, of which 26 metabolites were reported for the first time. These biotransformations included hydroxylation, N-oxidation, epoxidation, methylation, dehydrogenation, de-methoxylation, O-demethylation, as well as hydrolysis reactions. Copyright © 2013 John Wiley & Sons, Ltd.

TU-F-18A-06: Dual Energy CT Using One Full Scan and a Second Scan with Very Few Projections

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, T; Zhu, L

Purpose: The conventional dual energy CT (DECT) requires two full CT scans at different energy levels, resulting in dose increase as well as imaging errors from patient motion between the two scans. To shorten the scan time of DECT and thus overcome these drawbacks, we propose a new DECT algorithm using one full scan and a second scan with very few projections by preserving structural information. Methods: We first reconstruct a CT image on the full scan using a standard filtered-backprojection (FBP) algorithm. We then use a compressed sensing (CS) based iterative algorithm on the second scan for reconstruction frommore » very few projections. The edges extracted from the first scan are used as weights in the Objectives: function of the CS-based reconstruction to substantially improve the image quality of CT reconstruction. The basis material images are then obtained by an iterative image-domain decomposition method and an electron density map is finally calculated. The proposed method is evaluated on phantoms. Results: On the Catphan 600 phantom, the CT reconstruction mean error using the proposed method on 20 and 5 projections are 4.76% and 5.02%, respectively. Compared with conventional iterative reconstruction, the proposed edge weighting preserves object structures and achieves a better spatial resolution. With basis materials of Iodine and Teflon, our method on 20 projections obtains similar quality of decomposed material images compared with FBP on a full scan and the mean error of electron density in the selected regions of interest is 0.29%. Conclusion: We propose an effective method for reducing projections and therefore scan time in DECT. We show that a full scan plus a 20-projection scan are sufficient to provide DECT images and electron density with similar quality compared with two full scans. Our future work includes more phantom studies to validate the performance of our method.« less

Bronchoalveolar carcinoma of lung masquerading as iodine avid metastasis in a patient with minimally invasive follicular carcinoma of thyroid.

PubMed

Malhotra, Gaurav; Nair, Narendra; Menon, Hari; Gujral, Sumit; Abhyankar, Amit; Baghel, Nawab S; Awasare, Sushama; Nabar, Swapna J; Abhyankar, Suman; Kand, Purushottam G

2008-01-01

A 52-year-old man with follicular thyroid carcinoma was administered 182 mCi of radioiodine (I-131) a month after total thyroidectomy. Post-therapy scan revealed diffuse uptake of radioiodine in the apical left lung. CT-guided biopsy of this mass revealed mucinous bronchoalveolar carcinoma. Immunohistochemistry for thyroglobulin was negative. An FDG PET scan showed avid uptake in the lung mass. Surgery was ruled out, so he was given chemotherapy, without benefit. The lesion continued to show I-131 uptake even while on daily T3 substitution, suggesting that the mass was thyroid stimulating hormone-independent. Because the mass showed I-131 uptake and chemotherapy was not beneficial, it was decided to treat with I-131. He was continued on T3 substitution therapy and was given 209 mCi of I-131. Follow-up CT scan a few weeks later reported a 1-cm all round reduction of the mass. I-131 scan showed avid tracer uptake in the mass. This case suggests the possibility of this therapeutic option in nonthyroidal tumors that may concentrate radioiodine.

A critical evaluation of liquid chromatography with hybrid linear ion trap-Orbitrap mass spectrometry for the determination of acidic contaminants in wastewater effluents.

PubMed

Cahill, Michael G; Dineen, Brian A; Stack, Mary A; James, Kevin J

2012-12-28

Acidic pesticide and pharmaceutical contaminants were pre-concentrated and extracted from wastewater samples (500 mL) using solid-phase extraction. Analyte recoveries were 79-96%, with % RSD values in the range, 1.7-7.4%. Analyte identification and quantification were carried out using liquid chromatography-mass spectrometry (LC-MS) with hybrid linear ion trap (LIT) Orbitrap instrumentation. Using a resolution setting of 30,000 FWHM, full-scan MS analysis was performed using heated electrospray ionization (HESI) in negative mode. The high mass resolution capabilities of the Orbitrap MS were exploited for the determination of trace contaminants allowing facile discrimination between analytes and matrix. The dependant scan functions of the Orbitrap MS using higher collisional dissociation (HCD) and LIT MS were evaluated for the confirmation of analytes at trace concentration levels. Mass accuracy for target contaminants using this method was less than 2 ppm. The limits of quantitation (LOQs) were in the range, 2.1-27 ng/L. The inter-day accuracy and precision were measured over a five-day period at two concentrations. The % relative errors were in the range, 0.30-7.7%, and the % RSD values were in the range, 1.5-5.5%. Using this method, 2,4-D, mecoprop, ibuprofen, naproxene and gemfibrozil were identified in several wastewater treatment plants in Ireland. Copyright © 2012 Elsevier B.V. All rights reserved.

Identification of organic hydroperoxides and peroxy acids using atmospheric pressure chemical ionization-tandem mass spectrometry (APCI-MS/MS): application to secondary organic aerosol

NASA Astrophysics Data System (ADS)

Zhou, Shouming; Rivera-Rios, Jean C.; Keutsch, Frank N.; Abbatt, Jonathan P. D.

2018-05-01

Molecules with hydroperoxide functional groups are of extreme importance to both the atmospheric and biological chemistry fields. In this work, an analytical method is presented for the identification of organic hydroperoxides and peroxy acids (ROOH) by direct infusion of liquid samples into a positive-ion atmospheric pressure chemical ionization-tandem mass spectrometer ((+)-APCI-MS/MS). Under collisional dissociation conditions, a characteristic neutral loss of 51 Da (arising from loss of H2O2+NH3) from ammonium adducts of the molecular ions ([M + NH4]+) is observed for ROOH standards (i.e. cumene hydroperoxide, isoprene-4-hydroxy-3-hydroperoxide (ISOPOOH), tert-butyl hydroperoxide, 2-butanone peroxide and peracetic acid), as well as the ROOH formed from the reactions of H2O2 with aldehydes (i.e. acetaldehyde, hexanal, glyoxal and methylglyoxal). This new ROOH detection method was applied to methanol extracts of secondary organic aerosol (SOA) material generated from ozonolysis of α-pinene, indicating a number of ROOH molecules in the SOA material. While the full-scan mass spectrum of SOA demonstrates the presence of monomers (m/z = 80-250), dimers (m/z = 250-450) and trimers (m/z = 450-600), the neutral loss scan shows that the ROOH products all have masses less than 300 Da, indicating that ROOH molecules may not contribute significantly to the SOA oligomeric content. We anticipate this method could also be applied to biological systems with considerable value.

UPLC/MS MS data of testosterone metabolites in human and zebrafish liver microsomes and whole zebrafish larval microsomes.

PubMed

Saad, Moayad; Bijttebier, Sebastiaan; Matheeussen, An; Verbueken, Evy; Pype, Casper; Casteleyn, Christophe; Van Ginneken, Chris; Maes, Louis; Cos, Paul; Van Cruchten, Steven

2018-02-01

This article represents data regarding a study published in Toxicology in vitro entitled " in vitro CYP-mediated drug metabolism in the zebrafish (embryo) using human reference compounds" (Saad et al., 2017) [1]. Data were acquired with ultra-performance liquid chromatography - accurate mass mass spectrometry (UPLC-amMS). A full spectrum scan was conducted for the testosterone (TST) metabolites from the microsomal stability assay in zebrafish and humans. The microsomal proteins were extracted from adult zebrafish male (MLM) and female (FLM) livers, whole body homogenates of 96 h post fertilization larvae (EM) and a pool of human liver microsomes from 50 donors (HLM). Data are expressed as the abundance from the extracted ion chromatogram of the metabolites.

Rapid in situ identification of bioactive compounds in plants by in vivo nanospray high-resolution mass spectrometry.

PubMed

Chang, Qing; Peng, Yue'e; Dan, Conghui; Shuai, Qin; Hu, Shenghong

2015-03-25

A method for the rapid in situ identification of bioactive compounds in fresh plants has been developed using in vivo nanospray coupled to high-resolution mass spectrometry (HR-MS). Using a homemade in vivo nanospray ion source, the plant liquid was drawn out from a target region and ionized in situ. The ionized bioactive compounds were then identified using Q-Orbitrap HR-MS. The accurate mass measurements of these bioactive compounds were performed by full-scan or selected ion monitoring (SIM), and tandem mass spectrometry (MS/MS) was used in the structural elucidation. Without sample pretreatment, 12 bioactive compounds in 7 different plant species were identified, namely, isoalliin in onion; butylphthalide in celery; N-methylpelletierine, pelletierine, and pseudopelletierine in pomegranate; chlorogenic acid in crabapple; solamargine, solasonine, and solasodine in nightshade; aloin and aloe-emodin in aloe; and menthone in mint. This work demonstrates that in vivo nanospray HR-MS is a good method for rapid in situ identification of bioactive compounds in plants.

Metabolism studies of benzbromarone in rats by high performance liquid chromatography-quadrupole time of flight mass spectrometry.

PubMed

Wu, Haiqing; Peng, Ying; Wang, Shaojie; Wang, Kai; Zhao, Xunchen; Jiang, Fan

2012-12-12

A high performance liquid chromatography-quadrupole time of flight mass spectrometry (HPLC-QTOF-MS) method was employed in investigation of benzbromarone metabolites in rat plasma, urine, feces and bile samples. Meanwhile, the metabolic pathways of benzbromarone in rats were discussed. The identification was achieved on a reversed-phase C(18) column with mobile phase gradient method. The QTOF-MS was operated under full scan of MS or MS/MS in negative mode. The fragments were acquired by raising collision induced dissociation (CID) energy for speculating the structures of parent ions. According to the information from the chromatograms and mass spectra, 17 metabolites were obtained. Among them, the deoxidized phase I metabolites and an array of phase II metabolites-sulfate conjugates detected in the biological samples made the work more significant. Copyright © 2012 Elsevier B.V. All rights reserved.

2D and 3D MALDI-imaging: conceptual strategies for visualization and data mining.

PubMed

Thiele, Herbert; Heldmann, Stefan; Trede, Dennis; Strehlow, Jan; Wirtz, Stefan; Dreher, Wolfgang; Berger, Judith; Oetjen, Janina; Kobarg, Jan Hendrik; Fischer, Bernd; Maass, Peter

2014-01-01

3D imaging has a significant impact on many challenges in life sciences, because biology is a 3-dimensional phenomenon. Current 3D imaging-technologies (various types MRI, PET, SPECT) are labeled, i.e. they trace the localization of a specific compound in the body. In contrast, 3D MALDI mass spectrometry-imaging (MALDI-MSI) is a label-free method imaging the spatial distribution of molecular compounds. It complements 3D imaging labeled methods, immunohistochemistry, and genetics-based methods. However, 3D MALDI-MSI cannot tap its full potential due to the lack of statistical methods for analysis and interpretation of large and complex 3D datasets. To overcome this, we established a complete and robust 3D MALDI-MSI pipeline combined with efficient computational data analysis methods for 3D edge preserving image denoising, 3D spatial segmentation as well as finding colocalized m/z values, which will be reviewed here in detail. Furthermore, we explain, why the integration and correlation of the MALDI imaging data with other imaging modalities allows to enhance the interpretation of the molecular data and provides visualization of molecular patterns that may otherwise not be apparent. Therefore, a 3D data acquisition workflow is described generating a set of 3 different dimensional images representing the same anatomies. First, an in-vitro MRI measurement is performed which results in a three-dimensional image modality representing the 3D structure of the measured object. After sectioning the 3D object into N consecutive slices, all N slices are scanned using an optical digital scanner, enabling for performing the MS measurements. Scanning the individual sections results into low-resolution images, which define the base coordinate system for the whole pipeline. The scanned images conclude the information from the spatial (MRI) and the mass spectrometric (MALDI-MSI) dimension and are used for the spatial three-dimensional reconstruction of the object performed by image registration techniques. Different strategies for automatic serial image registration applied to MS datasets are outlined in detail. The third image modality is histology driven, i.e. a digital scan of the histological stained slices in high-resolution. After fusion of reconstructed scan images and MRI the slice-related coordinates of the mass spectra can be propagated into 3D-space. After image registration of scan images and histological stained images, the anatomical information from histology is fused with the mass spectra from MALDI-MSI. As a result of the described pipeline we have a set of 3 dimensional images representing the same anatomies, i.e. the reconstructed slice scans, the spectral images as well as corresponding clustering results, and the acquired MRI. Great emphasis is put on the fact that the co-registered MRI providing anatomical details improves the interpretation of 3D MALDI images. The ability to relate mass spectrometry derived molecular information with in vivo and in vitro imaging has potentially important implications. This article is part of a Special Issue entitled: Computational Proteomics in the Post-Identification Era. Guest Editors: Martin Eisenacher and Christian Stephan. Copyright © 2013. Published by Elsevier B.V.

Annotation: a computational solution for streamlining metabolomics analysis

PubMed Central

Domingo-Almenara, Xavier; Montenegro-Burke, J. Rafael; Benton, H. Paul; Siuzdak, Gary

2017-01-01

Metabolite identification is still considered an imposing bottleneck in liquid chromatography mass spectrometry (LC/MS) untargeted metabolomics. The identification workflow usually begins with detecting relevant LC/MS peaks via peak-picking algorithms and retrieving putative identities based on accurate mass searching. However, accurate mass search alone provides poor evidence for metabolite identification. For this reason, computational annotation is used to reveal the underlying metabolites monoisotopic masses, improving putative identification in addition to confirmation with tandem mass spectrometry. This review examines LC/MS data from a computational and analytical perspective, focusing on the occurrence of neutral losses and in-source fragments, to understand the challenges in computational annotation methodologies. Herein, we examine the state-of-the-art strategies for computational annotation including: (i) peak grouping or full scan (MS1) pseudo-spectra extraction, i.e., clustering all mass spectral signals stemming from each metabolite; (ii) annotation using ion adduction and mass distance among ion peaks; (iii) incorporation of biological knowledge such as biotransformations or pathways; (iv) tandem MS data; and (v) metabolite retention time calibration, usually achieved by prediction from molecular descriptors. Advantages and pitfalls of each of these strategies are discussed, as well as expected future trends in computational annotation. PMID:29039932

Full cycle rapid scan EPR deconvolution algorithm.

PubMed

Tseytlin, Mark

2017-08-01

Rapid scan electron paramagnetic resonance (RS EPR) is a continuous-wave (CW) method that combines narrowband excitation and broadband detection. Sinusoidal magnetic field scans that span the entire EPR spectrum cause electron spin excitations twice during the scan period. Periodic transient RS signals are digitized and time-averaged. Deconvolution of absorption spectrum from the measured full-cycle signal is an ill-posed problem that does not have a stable solution because the magnetic field passes the same EPR line twice per sinusoidal scan during up- and down-field passages. As a result, RS signals consist of two contributions that need to be separated and postprocessed individually. Deconvolution of either of the contributions is a well-posed problem that has a stable solution. The current version of the RS EPR algorithm solves the separation problem by cutting the full-scan signal into two half-period pieces. This imposes a constraint on the experiment; the EPR signal must completely decay by the end of each half-scan in order to not be truncated. The constraint limits the maximum scan frequency and, therefore, the RS signal-to-noise gain. Faster scans permit the use of higher excitation powers without saturating the spin system, translating into a higher EPR sensitivity. A stable, full-scan algorithm is described in this paper that does not require truncation of the periodic response. This algorithm utilizes the additive property of linear systems: the response to a sum of two inputs is equal the sum of responses to each of the inputs separately. Based on this property, the mathematical model for CW RS EPR can be replaced by that of a sum of two independent full-cycle pulsed field-modulated experiments. In each of these experiments, the excitation power equals to zero during either up- or down-field scan. The full-cycle algorithm permits approaching the upper theoretical scan frequency limit; the transient spin system response must decay within the scan period. Separation of the interfering up- and down-field scan responses remains a challenge for reaching the full potential of this new method. For this reason, only a factor of two increase in the scan rate was achieved, in comparison with the standard half-scan RS EPR algorithm. It is important for practical use that faster scans not necessarily increase the signal bandwidth because acceleration of the Larmor frequency driven by the changing magnetic field changes its sign after passing the inflection points on the scan. The half-scan and full-scan algorithms are compared using a LiNC-BuO spin probe of known line-shape, demonstrating that the new method produces stable solutions when RS signals do not completely decay by the end of each half-scan. Copyright © 2017 Elsevier Inc. All rights reserved.

Full cycle rapid scan EPR deconvolution algorithm

NASA Astrophysics Data System (ADS)

Tseytlin, Mark

2017-08-01

Rapid scan electron paramagnetic resonance (RS EPR) is a continuous-wave (CW) method that combines narrowband excitation and broadband detection. Sinusoidal magnetic field scans that span the entire EPR spectrum cause electron spin excitations twice during the scan period. Periodic transient RS signals are digitized and time-averaged. Deconvolution of absorption spectrum from the measured full-cycle signal is an ill-posed problem that does not have a stable solution because the magnetic field passes the same EPR line twice per sinusoidal scan during up- and down-field passages. As a result, RS signals consist of two contributions that need to be separated and postprocessed individually. Deconvolution of either of the contributions is a well-posed problem that has a stable solution. The current version of the RS EPR algorithm solves the separation problem by cutting the full-scan signal into two half-period pieces. This imposes a constraint on the experiment; the EPR signal must completely decay by the end of each half-scan in order to not be truncated. The constraint limits the maximum scan frequency and, therefore, the RS signal-to-noise gain. Faster scans permit the use of higher excitation powers without saturating the spin system, translating into a higher EPR sensitivity. A stable, full-scan algorithm is described in this paper that does not require truncation of the periodic response. This algorithm utilizes the additive property of linear systems: the response to a sum of two inputs is equal the sum of responses to each of the inputs separately. Based on this property, the mathematical model for CW RS EPR can be replaced by that of a sum of two independent full-cycle pulsed field-modulated experiments. In each of these experiments, the excitation power equals to zero during either up- or down-field scan. The full-cycle algorithm permits approaching the upper theoretical scan frequency limit; the transient spin system response must decay within the scan period. Separation of the interfering up- and down-field scan responses remains a challenge for reaching the full potential of this new method. For this reason, only a factor of two increase in the scan rate was achieved, in comparison with the standard half-scan RS EPR algorithm. It is important for practical use that faster scans not necessarily increase the signal bandwidth because acceleration of the Larmor frequency driven by the changing magnetic field changes its sign after passing the inflection points on the scan. The half-scan and full-scan algorithms are compared using a LiNC-BuO spin probe of known line-shape, demonstrating that the new method produces stable solutions when RS signals do not completely decay by the end of each half-scan.

Functional imaging in differentiating bronchial masses: an initial experience with a combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan.

PubMed

Kumar, Arvind; Jindal, Tarun; Dutta, Roman; Kumar, Rakesh

2009-10-01

To evaluate the role of combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan in differentiating bronchial tumors observed in contrast enhanced computed tomography scan of chest. Prospective observational study. Place of study: All India Institute of Medical Sciences, New Delhi, India. 7 patients with bronchial mass detected in computed tomography scan of the chest were included in this study. All patients underwent (18)F-FDG PET-CT scan, (68)Ga DOTA-TOC PET-CT scan and fiberoptic bronchoscope guided biopsy followed by definitive surgical excision. The results of functional imaging studies were analyzed and the results are correlated with the final histopathology of the tumor. Histopathological examination of 7 bronchial masses revealed carcinoid tumors (2 typical, 1 atypical), inflammatory myofibroblastic tumor (1), mucoepidermoid carcinoma (1), hamartoma (1), and synovial cell sarcoma (1). The typical carcinoids had mild (18)F-FDG uptake and high (68)Ga DOTA-TOC uptake. Atypical carcinoid had moderate uptake of (18)F-FDG and high (68)Ga DOTA-TOC uptake. Inflammatory myofibroblastic tumor showed high uptake of (18)F-FDG and no uptake of (68)Ga DOTA-TOC. Mucoepidermoid carcinoma showed mild (18)F-FDG uptake and no (68)Ga DOTA-TOC uptake. Hamartoma showed no uptake on either scans. Synovial cell sarcoma showed moderate (18)F-FDG uptake and mild focal (68)Ga DOTA-TOC uptake. This initial experience with the combined use of (18)F-FDG and (68)Ga DOTA-TOC PET-CT scan reveals different uptake patterns in various bronchial tumors. Bronchoscopic biopsy will continue to be the gold standard; however, the interesting observations made in this study merits further evaluation of the utility of the combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan in larger number of patients with bronchial masses.

Paleogene stratigraphy of the Solomons Island, Maryland corehole

USGS Publications Warehouse

Gibson, Thomas G.; Bybell, Laurel M.

1994-01-01

Purge and trap capillary gas chromatography/mass spectrometry is a rapid, precise, accurate method for determining volatile organic compounds in samples of surface water and ground water. The method can be used to determine 59 selected compounds, including chlorofluorohydrocarbons, aromatic hydrocarbons, and halogenated hydrocarbons. The volatile organic compounds are removed from the sample matrix by actively purging the sample with helium. The volatile organic compounds are collected onto a sorbant trap, thermally desorbed, separated by a Megabore gas chromatographic capillary column, ionized by electron impact, and determined by a full-scan quadrupole mass spectrometer. Compound identification is confirmed by the gas chromatographic retention time and by the resultant mass spectrum. Unknown compounds detected in a sample can be tentatively identified by comparing the unknown mass spectrum to reference spectra in the mass-spectra computer-data system library compiled by the National Institute of Standards and Technology. Method detection limits for the selected compounds range from 0.05 to 0.2 microgram per liter. Recoveries for the majority of the selected compounds ranged from 80 to 120 percent, with relative standard deviations of less than 10 percent.

Rotating-unbalanced-mass Devices for Scanning Balloon-borne Experiments, Free-flying Spacecraft, and Space Shuttle/space Station Experiments

NASA Technical Reports Server (NTRS)

Polites, Michael E.

1990-01-01

A new method is presented for scanning balloon-borne experiments, free-flying spacecraft, and gimballed experiments mounted to the space shuttle or the space station. It uses rotating-unbalanced-mass (RUM) devices for generating circular, line, or raster scan patterns and an auxiliary control system for target acquisition, keeping the scan centered on the target, and producing complementary motion for raster scanning. It is ideal for applications where the only possible way to accomplish the required scan is to physically scan the entire experiment or spacecraft as in x ray and gamma ray experiments. In such cases, this new method should have advantages over prior methods in terms of either power, weight, cost, performance, stability, or a combination of these.

Wide-field reflective scanning optical systems

NASA Technical Reports Server (NTRS)

Abel, I. R.

1973-01-01

Catoptric optical scanning system provides relatively fast line-scan rate for two-dimensional coverage. Rapid scan rates require low focal ratios between components and smallest possible masses. System is relatively free from monochromatic defects and chromatic aberrations.

The application of a novel high-resolution mass spectrometry-based analytical strategy to rapid metabolite profiling of a dual drug combination in humans.

PubMed

Xing, Jie; Zang, Meitong; Liu, Huixiang

2017-11-15

Metabolite profiling of combination drugs in complex matrix is a big challenge. Development of an effective data mining technique for simultaneously extracting metabolites of one parent drug from both background matrix and combined drug-related signals could be a solution. This study presented a novel high resolution mass spectrometry (HRMS)-based data-mining strategy to fast and comprehensive metabolite identification of combination drugs in human. The model drug combination was verapamil-irbesartan (VER-IRB), which is widely used in clinic to treat hypertension. First, mass defect filter (MDF), as a targeted data mining tool, worked effectively except for those metabolites with similar MDF values. Second, the accurate mass-based background subtraction (BS), as an untargeted data-mining tool, was able to recover all relevant metabolites of VER-IRB from the full-scan MS dataset except for trace metabolites buried in the background noise and/or combined drug-related signals. Third, the novel ring double bond (RDB; valence values of elements in structure) filter, could show rich structural information in more sensitive full-scan MS chromatograms; however, it had a low capability to remove background noise and was difficult to differentiate the metabolites with RDB coverage. Fourth, an integrated strategy, i.e., untargeted BS followed by RDB, was effective for metabolite identification of VER and IRB, which have different RDB values. Majority of matrix signals were firstly removed using BS. Metabolite ions for each parent drug were then isolated from remaining background matrix and combined drug-related signals by imposing of preset RDB values/ranges around the parent drug and selected core substructures. In parallel, MDF was used to recover potential metabolites with similar RDB. As a result, a total of 74 metabolites were found for VER-IRB in human plasma and urine, among which ten metabolites have not been previously reported in human. The results demonstrated that the combination of accurate mass-based multiple data-mining techniques, i.e., untargeted background subtraction followed by ring double bond filtering in parallel with targeted mass defect filtering, can be a valuable tool for rapid metabolite profiling of combination drug. Copyright © 2017 Elsevier B.V. All rights reserved.

Frequency-scanning MALDI linear ion trap mass spectrometer for large biomolecular ion detection.

PubMed

Lu, I-Chung; Lin, Jung Lee; Lai, Szu-Hsueh; Chen, Chung-Hsuan

2011-11-01

This study presents the first report on the development of a matrix-assisted laser desorption ionization (MALDI) linear ion trap mass spectrometer for large biomolecular ion detection by frequency scan. We designed, installed, and tested this radio frequency (RF) scan linear ion trap mass spectrometer and its associated electronics to dramatically extend the mass region to be detected. The RF circuit can be adjusted from 300 to 10 kHz with a set of operation amplifiers. To trap the ions produced by MALDI, a high pressure of helium buffer gas was employed to quench extra kinetic energy of the heavy ions produced by MALDI. The successful detection of the singly charged secretory immunoglobulin A ions indicates that the detectable mass-to-charge ratio (m/z) of this system can reach ~385 000 or beyond.

WE-EF-207-07: Dual Energy CT with One Full Scan and a Second Sparse-View Scan Using Structure Preserving Iterative Reconstruction (SPIR)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, T; Zhu, L

Purpose: Conventional dual energy CT (DECT) reconstructs CT and basis material images from two full-size projection datasets with different energy spectra. To relax the data requirement, we propose an iterative DECT reconstruction algorithm using one full scan and a second sparse-view scan by utilizing redundant structural information of the same object acquired at two different energies. Methods: We first reconstruct a full-scan CT image using filtered-backprojection (FBP) algorithm. The material similarities of each pixel with other pixels are calculated by an exponential function about pixel value differences. We assume that the material similarities of pixels remains in the second CTmore » scan, although pixel values may vary. An iterative method is designed to reconstruct the second CT image from reduced projections. Under the data fidelity constraint, the algorithm minimizes the L2 norm of the difference between pixel value and its estimation, which is the average of other pixel values weighted by their similarities. The proposed algorithm, referred to as structure preserving iterative reconstruction (SPIR), is evaluated on physical phantoms. Results: On the Catphan600 phantom, SPIR-based DECT method with a second 10-view scan reduces the noise standard deviation of a full-scan FBP CT reconstruction by a factor of 4 with well-maintained spatial resolution, while iterative reconstruction using total-variation regularization (TVR) degrades the spatial resolution at the same noise level. The proposed method achieves less than 1% measurement difference on electron density map compared with the conventional two-full-scan DECT. On an anthropomorphic pediatric phantom, our method successfully reconstructs the complicated vertebra structures and decomposes bone and soft tissue. Conclusion: We develop an effective method to reduce the number of views and therefore data acquisition in DECT. We show that SPIR-based DECT using one full scan and a second 10-view scan can provide high-quality DECT images and accurate electron density maps as conventional two-full-scan DECT.« less

Results of a laboratory experiment that tests rotating unbalanced-mass devices for scanning gimbaled payloads and free-flying spacecraft

NASA Technical Reports Server (NTRS)

Alhorn, D. C.; Polites, M. E.

1994-01-01

Rotating unbalanced-mass (RUM) devices are a new way to scan space-based, balloon-borne, and ground-based gimbaled payloads, like x-ray and gamma-ray telescopes. They can also be used to scan free-flying spacecraft. Circular scans, linear scans, and raster scans can be generated. A pair of RUM devices generates the basic scan motion and an auxiliary control system using torque motors, control moment gyros, or reaction wheels keeps the scan centered on the target and produces some complementary motion for raster scanning. Previous analyses and simulation results show that this approach offers significant power savings compared to scanning only with the auxiliary control system, especially with large payloads and high scan frequencies. However, these claims have never been proven until now. This paper describes a laboratory experiment which tests the concept of scanning a gimbaled payload with RUM devices. A description of the experiment is given and test results that prove the concept are presented. The test results are compared with those from a computer simulation model of the experiment and the differences are discussed.

Dynamic transfer applied to secondary ion imaging over large scanned fields with the nanoSIMS 50 at high mass resolution

NASA Astrophysics Data System (ADS)

Slodzian, Georges; Wu, Ting-Di; Duprat, Jean; Engrand, Cécile; Guerquin-Kern, Jean-Luc

2017-12-01

Dynamic transfer is an adaptive optical approach used for coupling a scanning ion probe with the mass spectrometer designed for analyzing sputtered ions emanating from the probe impact. Its tuning is of crucial importance for getting uniform signal collection over large scanning fields and therefore scanning images free of vignetting in a context of high mass resolution. Revisiting the optical design of the NanoSIMS 50 instrument, where the same set of lenses focuses the primary ion probe on the sample and collects secondary ions from the sample, led us to develop novel experimental procedures to achieve dynamic transfer tuning and overcome instrumental imperfections. It is the case for scanning distortion that may be induced by the octopole used for correcting probe astigmatism and may cause irreducible vignetting on scanning images. We show that it is possible to develop complete tuning procedures by compromising temporarily on the sharpness of the probe focus. Most importantly, we show that, in a context of high mass resolution, the transfer does not significantly disturb isotopic ratios over large scanned fields provided external coils are properly adjusted to compensate ambient magnetic fields. Deepening the procedures led us to demonstrate that the scanning center of the probe may not coincide with the imaging center of COOL, Coaxial Objective Lenses forming the probe and extracting secondary ions. We have checked that bringing those two centers into coincidence resulted in a better image quality over large fields. In the present work, we show how to handle the secondary beam in order to position it before it enters the spectrometer. That capability is essential for optimizing transmission at high mass resolution by aligning the secondary beam axis on a given entrance axis of the spectrometer. These results led us to propose several instrumental improvements including the crucial interest of an additional octopole upstream in the primary ion probe column to prevent scanning distortion when performing astigmatism correction and the possibility of offsetting primary beam deviating plates to bring scanning and imaging centers in coincidence.

Unbiased Scanning Method and Data Banking Approach Using Ultra-High Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry for Quantitative Comparison of Metabolite Exposure in Plasma across Species Analyzed at Different Dates.

PubMed

Gao, Hongying; Deng, Shibing; Obach, R Scott

2015-12-01

An unbiased scanning methodology using ultra high-performance liquid chromatography coupled with high-resolution mass spectrometry was used to bank data and plasma samples for comparing the data generated at different dates. This method was applied to bank the data generated earlier in animal samples and then to compare the exposure to metabolites in animal versus human for safety assessment. With neither authentic standards nor prior knowledge of the identities and structures of metabolites, full scans for precursor ions and all ion fragments (AIF) were employed with a generic gradient LC method to analyze plasma samples at positive and negative polarity, respectively. In a total of 22 tested drugs and metabolites, 21 analytes were detected using this unbiased scanning method except that naproxen was not detected due to low sensitivity at negative polarity and interference at positive polarity; and 4'- or 5-hydroxy diclofenac was not separated by a generic UPLC method. Statistical analysis of the peak area ratios of the analytes versus the internal standard in five repetitive analyses over approximately 1 year demonstrated that the analysis variation was significantly different from sample instability. The confidence limits for comparing the exposure using peak area ratio of metabolites in animal plasma versus human plasma measured over approximately 1 year apart were comparable to the analysis undertaken side by side on the same days. These statistical analysis results showed it was feasible to compare data generated at different dates with neither authentic standards nor prior knowledge of the analytes.

Advantages and limitations of computed tomography scans for treatment planning of lung cancer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mira, J.G.; Potter, J.L.; Fullerton, G.D.

1982-09-01

Forty-five Chest computed tomography (CT) scans performed on patients with lung carcinoma (LC) were evaluated in an attempt to understand the pattern of intrathoracic tumor spread and the advantages and limitations this technique offers for treatment planning when compared to planning done by conventional X rays. The following findings can help treatment planning. (1) When regular X rays do not show location (i.e., hemithorax opacification), CT scan will show it in 68% of patients. If regular X rays show a well localized mass, unsuspected tumor extensions were disclosed in 78% of these patients. Hence, CT scans should be done inmore » all LC patients prior to treatment planning; (2) Mediastinal masses frequently spread anteriorly toward the sternum and posteriorly around the vertebral bodies toward the cord and costal pleura. This should be considered for radiotherapy boost techniques; (3) Lung masses spread in one third of cases toward the lateral costal pleura. Thus, the usual 1-2cm of safety margin around the LC are not sufficient in some cases; (4) Tumor size can appear much smaller in regular X rays than in CT scans. Hence, CT scans are necessary for accurate staging and evaluation of tumor response. Some CT scan limitations are: (1) Atelectasis blends with tumor in approximately half of the patients, thus obscuring tumor boundaries; (2) CT numbers and contrast enhancement did not help to differentiate between these two structures; and (3) Limited definition of CT scan prevents investigation of suspected microscopic spread around tumor masses.« less

Gas chromatography-mass spectrometry analysis of essential oils from five parts of Chaihu (Radix Bupleuri Chinensis).

PubMed

Meng, Jie; Chen, Xingfu; Yang, Wenyu; Song, Jiuhua; Zhang, Yu; Li, Zhifei; Yang, Xingwang; Yang, Zhanguo

2014-12-01

To analyze the essential oils from flowers, leaves, stems, roots, and fruits of Chaihu (Radix Bupleuri Chinensis). We extracted essential oils from different parts of Chaihu (Radix Bupleuri Chinensis) using a steam distillation method. The essential oils were analyzed by gas chromatography-mass spectrometry (GC-MS). Data were collected in full scan mode (m/z 60-600). Volatile components were identified based on their retention indices and by comparing their mass spectra with those in the National Institute of Standards and Technology 2005 database, assisted by tandem mass spectrometry information. The relative content of each constituent was determined by area normalization. We identified 111 components, of which 12 were common to all 5 parts, 30 were found only in roots, 14 were found only in flowers, 6 were found only in leaves, 4 were found only in stems, and 17 were found only in fruits. Our results show that the stems, flowers, leaves, and fruits of Chaihu (Radix Bupleuri Chinensis) contain a high concentration of essential oils, and that the exact composition of the essential oils differs among the plant parts. To develop new medicines and make full use of the Chaihu (Radix Bupleuri Chinensis) resource, it is important to characterize the essential oils from different parts of the plant. In future research, it will be important to determine the pharmacological effects of the various components and the essential oil mixtures.

Feasibility of using a miniature NIR spectrometer to measure volumic mass during alcoholic fermentation.

PubMed

Fernández-Novales, Juan; López, María-Isabel; González-Caballero, Virginia; Ramírez, Pilar; Sánchez, María-Teresa

2011-06-01

Volumic mass-a key component of must quality control tests during alcoholic fermentation-is of great interest to the winemaking industry. Transmitance near-infrared (NIR) spectra of 124 must samples over the range of 200-1,100-nm were obtained using a miniature spectrometer. The performance of this instrument to predict volumic mass was evaluated using partial least squares (PLS) regression and multiple linear regression (MLR). The validation statistics coefficient of determination (r(2)) and the standard error of prediction (SEP) were r(2) = 0.98, n = 31 and r(2) = 0.96, n = 31, and SEP = 5.85 and 7.49 g/dm(3) for PLS and MLR equations developed to fit reference data for volumic mass and spectral data. Comparison of results from MLR and PLS demonstrates that a MLR model with six significant wavelengths (P < 0.05) fit volumic mass data to transmittance (1/T) data slightly worse than a more sophisticated PLS model using the full scanning range. The results suggest that NIR spectroscopy is a suitable technique for predicting volumic mass during alcoholic fermentation, and that a low-cost NIR instrument can be used for this purpose.

Novel strategy for the determination of illegal adulterants in health foods and herbal medicines using high-performance liquid chromatography with high-resolution mass spectrometry.

PubMed

Wang, Zhe; Wu, Caisheng; Wang, Gangli; Zhang, Qingsheng; Zhang, Jinlan

2015-03-01

The detection, confirmation, and quantification of multiple illegal adulterants in health foods and herbal medicines by using a single analytical method are a challenge. This paper reports on a new strategy to meet this challenge by employing high-performance liquid chromatography coupled with high-resolution mass spectrometry and a mass spectral tree similarity filter technique. This analytical method can rapidly collect high-resolution, high-accuracy, optionally multistage mass data for compounds in samples. After a preliminary screening by retention time and high-resolution mass spectral data, known illegal adulterants can be detected. The mass spectral tree similarity filter technique has been applied to rapidly confirm these adulterants and simultaneously discover unknown ones. By using full-scan mass spectra as stem and data-dependent subsequent stage mass spectra to form branches, mass spectrometry data from detected compounds are converted into mass spectral trees. The known or unknown illegal adulterants in the samples are confirmed or discovered based on the similarity between their mass spectral trees and those of the references in a library, and they are finally quantified against standard curves. This new strategy has been tested by using 50 samples, and the illegal adulterants were rapidly and effectively detected, confirmed and quantified. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly sensitive and selective analysis of urinary steroids by comprehensive two-dimensional gas chromatography combined with positive chemical ionization quadrupole mass spectrometry

PubMed Central

Zhang, Ying; Tobias, Herbert J.; Brenna, J. Thomas

2014-01-01

Comprehensive two dimensional gas chromatography (GC×GC) provides greater separation space than conventional GC. Because of fast peak elution, a time of flight mass spectrometer (TOFMS) is the usual structure-specific detector of choice. The quantitative capabilities of a novel GC×GC fast quadrupole MS were investigated with electron ionization (EI), and CH4 or NH3 positive chemical ionization (PCI) for analysis of endogenous urinary steroids targeted in anti-doping tests. Average precisions for steroid quantitative analysis from replicate urine extractions were 6% (RSD) for EI and 8% for PCI-NH3. The average limits of detection (LOD) calculated by quantification ions for 12 target steroids spiked into steroid-free urine matrix (SFUM) were 2.6 ng mL−1 for EI, 1.3 ng mL−1 for PCI-CH4, and 0.3 ng mL−1 for PCI-NH3, all in mass scanning mode. The measured limits of quantification (LOQ) with full mass scan GC×GC-qMS were comparable with the LOQ values measured by one-dimensional GC-MS in single ion monitoring (SIM) mode. PCI-NH3 yields fewer fragments and greater (pseudo)molecular ion abundances than EI or PCI-CH4. These data show a benchtop GC×GC-qMS system has the sensitivity, specificity, and resolution to analyze urinary steroids at normal urine concentrations, and that PCI-NH3, not currently available on most GC×GC-TOFMS instruments, is of particular value for generation of structure-specific ions. PMID:22606686

Full information acquisition in scanning probe microscopy and spectroscopy

DOEpatents

Jesse, Stephen; Belianinov, Alex; Kalinin, Sergei V.; Somnath, Suhas

2017-04-04

Apparatus and methods are described for scanning probe microscopy and spectroscopy based on acquisition of full probe response. The full probe response contains valuable information about the probe-sample interaction that is lost in traditional scanning probe microscopy and spectroscopy methods. The full probe response is analyzed post data acquisition using fast Fourier transform and adaptive filtering, as well as multivariate analysis. The full response data is further compressed to retain only statistically significant components before being permanently stored.

Definition and design of an experiment to test raster scanning with rotating unbalanced-mass devices on gimbaled payloads

NASA Technical Reports Server (NTRS)

Lightsey, W. D.; Alhorn, D. C.; Polites, M. E.

1992-01-01

An experiment designed to test the feasibility of using rotating unbalanced-mass (RUM) devices for line and raster scanning gimbaled payloads, while expending very little power is described. The experiment is configured for ground-based testing, but the scan concept is applicable to ground-based, balloon-borne, and space-based payloads, as well as free-flying spacecraft. The servos used in scanning are defined; the electronic hardware is specified; and a computer simulation model of the system is described. Simulation results are presented that predict system performance and verify the servo designs.

Full-Body CT Scans - What You Need to Know

MedlinePlus

... Medical Imaging Medical X-ray Imaging Full-Body CT Scans - What You Need to Know Share Tweet ... new service for health-conscious people: "Whole-body CT screening." This typically involves scanning the body from ...

Diagnostic Accuracy of B-mode USG and Doppler Scan for Ovarian Lesions

PubMed Central

Agarwal, Vinish Kumar

2016-01-01

Introduction Ultrasonography (USG) is considered as the primary imaging modality for confirmation of ovarian mass and to differentiate them in to benign or malignant. Aim The present study was conducted with the aim to evaluate accuracy of B- mode USG and Doppler scan (Colour Doppler + Spectral Doppler) for ovarian lesions. Materials and Methods The patients included in the study were from those referred with either palpable adnexal mass or incidentally detected adnexal masses. Total 250 women were evaluated by USG, Doppler scan. Only fifty patients who had true ovarian mass intraoperatively and on histopathology were included in study, rest masses were excluded. Study parameters were morphological indexing on B- Mode USG, flow study, vessel arrangement, and vessel morphology and vessel location in Colour Doppler and resistive index and pulsatility index in spectral Doppler. Results Total 50 women were included in present study. Out of these 46% were pre-menopausal while 54% were menopaused women, 66.7% of post-menopausal women had malignant ovarian masses compared to 8.7% of premenopausal. Sensitivity, specificity, positive predictive value and negative predictive value of B-Mode USG for ovarian masses were 94.44%, 48.15%, 54.84% and 92.86% respectively, with p-value = 0.007, while sensitivity, specificity, positive predictive value and negative predictive value of Doppler scan were 85%, 90%, 85% and 90% respectively, with p-value = 0.0001. Conclusion USG and its different techniques are accepted as the primary imaging modality for early stage diagnosis of an ovarian malignancy. Statistical analysis suggests that Doppler Scan (Colour + Spectral) was more accurate (88%) than B-Mode USG (67%), but author is in view that both of these modalities should be used in conjunction to screen the ovarian lesions. PMID:27790544

Estimating Mass Properties of Dinosaurs Using Laser Imaging and 3D Computer Modelling

PubMed Central

Bates, Karl T.; Manning, Phillip L.; Hodgetts, David; Sellers, William I.

2009-01-01

Body mass reconstructions of extinct vertebrates are most robust when complete to near-complete skeletons allow the reconstruction of either physical or digital models. Digital models are most efficient in terms of time and cost, and provide the facility to infinitely modify model properties non-destructively, such that sensitivity analyses can be conducted to quantify the effect of the many unknown parameters involved in reconstructions of extinct animals. In this study we use laser scanning (LiDAR) and computer modelling methods to create a range of 3D mass models of five specimens of non-avian dinosaur; two near-complete specimens of Tyrannosaurus rex, the most complete specimens of Acrocanthosaurus atokensis and Strutiomimum sedens, and a near-complete skeleton of a sub-adult Edmontosaurus annectens. LiDAR scanning allows a full mounted skeleton to be imaged resulting in a detailed 3D model in which each bone retains its spatial position and articulation. This provides a high resolution skeletal framework around which the body cavity and internal organs such as lungs and air sacs can be reconstructed. This has allowed calculation of body segment masses, centres of mass and moments or inertia for each animal. However, any soft tissue reconstruction of an extinct taxon inevitably represents a best estimate model with an unknown level of accuracy. We have therefore conducted an extensive sensitivity analysis in which the volumes of body segments and respiratory organs were varied in an attempt to constrain the likely maximum plausible range of mass parameters for each animal. Our results provide wide ranges in actual mass and inertial values, emphasizing the high level of uncertainty inevitable in such reconstructions. However, our sensitivity analysis consistently places the centre of mass well below and in front of hip joint in each animal, regardless of the chosen combination of body and respiratory structure volumes. These results emphasize that future biomechanical assessments of extinct taxa should be preceded by a detailed investigation of the plausible range of mass properties, in which sensitivity analyses are used to identify a suite of possible values to be tested as inputs in analytical models. PMID:19225569

Estimating mass properties of dinosaurs using laser imaging and 3D computer modelling.

PubMed

Bates, Karl T; Manning, Phillip L; Hodgetts, David; Sellers, William I

2009-01-01

Body mass reconstructions of extinct vertebrates are most robust when complete to near-complete skeletons allow the reconstruction of either physical or digital models. Digital models are most efficient in terms of time and cost, and provide the facility to infinitely modify model properties non-destructively, such that sensitivity analyses can be conducted to quantify the effect of the many unknown parameters involved in reconstructions of extinct animals. In this study we use laser scanning (LiDAR) and computer modelling methods to create a range of 3D mass models of five specimens of non-avian dinosaur; two near-complete specimens of Tyrannosaurus rex, the most complete specimens of Acrocanthosaurus atokensis and Strutiomimum sedens, and a near-complete skeleton of a sub-adult Edmontosaurus annectens. LiDAR scanning allows a full mounted skeleton to be imaged resulting in a detailed 3D model in which each bone retains its spatial position and articulation. This provides a high resolution skeletal framework around which the body cavity and internal organs such as lungs and air sacs can be reconstructed. This has allowed calculation of body segment masses, centres of mass and moments or inertia for each animal. However, any soft tissue reconstruction of an extinct taxon inevitably represents a best estimate model with an unknown level of accuracy. We have therefore conducted an extensive sensitivity analysis in which the volumes of body segments and respiratory organs were varied in an attempt to constrain the likely maximum plausible range of mass parameters for each animal. Our results provide wide ranges in actual mass and inertial values, emphasizing the high level of uncertainty inevitable in such reconstructions. However, our sensitivity analysis consistently places the centre of mass well below and in front of hip joint in each animal, regardless of the chosen combination of body and respiratory structure volumes. These results emphasize that future biomechanical assessments of extinct taxa should be preceded by a detailed investigation of the plausible range of mass properties, in which sensitivity analyses are used to identify a suite of possible values to be tested as inputs in analytical models.

Screening and identification of glyceollins and their metabolites by electrospray ionization tandem mass spectrometry with precursor ion scanning

USDA-ARS?s Scientific Manuscript database

A method has been developed for screening glyceollins and their metabolites based upon precursor ion scanning. Under higher-energy collision conditions, employing a triple quadrupole mass spectrometer in the negative ion mode, deprotonated glyceollin precursors yield a diagnostic radical product ion...

Importance of Standardized DXA Protocol for Assessing Physique Changes in Athletes.

PubMed

Nana, Alisa; Slater, Gary J; Hopkins, Will G; Halson, Shona L; Martin, David T; West, Nicholas P; Burke, Louise M

2016-06-01

The implications of undertaking DXA scans using best practice protocols (subjects fasted and rested) or a less precise but more practical protocol in assessing chronic changes in body composition following training and a specialized recovery technique were investigated. Twenty-one male cyclists completed an overload training program, in which they were randomized to four sessions per week of either cold water immersion therapy or control groups. Whole-body DXA scans were undertaken with best practice protocol (Best) or random activity protocol (Random) at baseline, after 3 weeks of overload training, and after a 2-week taper. Magnitudes of changes in total, lean and fat mass from baseline-overload, overload-taper and baseline-taper were assessed by standardization (Δmean/SD). The standard deviations of change scores for total and fat-free soft tissue mass (FFST) from Random scans (2-3%) were approximately double those observed in the Best (1-2%), owing to extra random errors associated with Random scans at baseline. There was little difference in change scores for fat mass. The effect of cold water immersion therapy on baseline-taper changes in FFST was possibly harmful (-0.7%; 90% confidence limits ±1.2%) with Best scans but unclear with Random scans (0.9%; ±2.0%). Both protocols gave similar possibly harmful effects of cold water immersion therapy on changes in fat mass (6.9%; ±13.5% and 5.5%; ±14.3%, respectively). An interesting effect of cold water immersion therapy on training-induced changes in body composition might have been missed with a less precise scanning protocol. DXA scans should be undertaken with Best.

An unusual cause of intractable heel pain.

PubMed

Ghani, Samuel; Fazal, Muhammad Ali

2011-01-01

We report a case of severe heel pain that did not respond to noninvasive measures. Magnetic resonance imaging scans revealed a soft tissue mass that after complete surgical excision was found to be an epidermal cyst. The patient experienced full resolution of the symptoms after excision of the epidermal cyst. To our knowledge, intractable heel pain due to an epidermal cyst is rare. We were unable to identify a previous publication describing the presence of an epidermal cyst localized to the heel without a history of previous trauma. From our experience with the present case, we believe that clinicians should consider the possibility of an epidermal inclusion cyst and should have a low threshold for obtaining magnetic resonance imaging scans, in particular, before the initiation of invasive treatment, in the case of intractable heel pain. Copyright © 2011 American College of Foot and Ankle Surgeons. Published by Elsevier Inc. All rights reserved.

A novel approach to transforming a non-targeted metabolic profiling method to a pseudo-targeted method using the retention time locking gas chromatography/mass spectrometry-selected ions monitoring.

PubMed

Li, Yong; Ruan, Qiang; Li, Yanli; Ye, Guozhu; Lu, Xin; Lin, Xiaohui; Xu, Guowang

2012-09-14

Non-targeted metabolic profiling is the most widely used method for metabolomics. In this paper, a novel approach was established to transform a non-targeted metabolic profiling method to a pseudo-targeted method using the retention time locking gas chromatography/mass spectrometry-selected ion monitoring (RTL-GC/MS-SIM). To achieve this transformation, an algorithm based on the automated mass spectral deconvolution and identification system (AMDIS), GC/MS raw data and a bi-Gaussian chromatographic peak model was developed. The established GC/MS-SIM method was compared with GC/MS-full scan (the total ion current and extracted ion current, TIC and EIC) methods, it was found that for a typical tobacco leaf extract, 93% components had their relative standard deviations (RSDs) of relative peak areas less than 20% by the SIM method, while 88% by the EIC method and 81% by the TIC method. 47.3% components had their linear correlation coefficient higher than 0.99, compared with 5.0% by the EIC and 6.2% by TIC methods. Multivariate analysis showed the pooled quality control samples clustered more tightly using the developed method than using GC/MS-full scan methods, indicating a better data quality. With the analysis of the variance of the tobacco samples from three different planting regions, 167 differential components (p<0.05) were screened out using the RTL-GC/MS-SIM method, but 151 and 131 by the EIC and TIC methods, respectively. The results show that the developed method not only has a higher sensitivity, better linearity and data quality, but also does not need complicated peak alignment among different samples. It is especially suitable for the screening of differential components in the metabolic profiling investigation. Copyright © 2012 Elsevier B.V. All rights reserved.

Application of ultra-high-performance liquid chromatography coupled with LTQ-Orbitrap mass spectrometry for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements.

PubMed

Cheng, Qiaoyuan; Shou, Linjun; Chen, Cen; Shi, Shi; Zhou, Minghao

2017-10-01

In this paper, an ultra-high-performance liquid chromatography coupled with linear ion trap quadrupole Orbitrap high resolution mass spectrometry (UHPLC-LTQ-Orbitrap HRMS) method was developed and validated for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements. 13 wt-loss drugs were well separated by the gradient elution of 10mmol/L ammonium acetate - 0.05% formic acid H 2 O and acetonitrile at a flow rate of 0.2mL/min within 12min. The MS analysis was operated under the positive ion and in full MS/dd-MS 2 (data-dependent MS 2 ) mode. The full MS scan with resolution at 60 000 FWHM and narrow mass windows at 5ppm acquired data for identification and quantitation, and dd-MS 2 scan with resolution at 15 000 FWHM obtained product ions for confirmation. The method validation showed good linearity with coefficients of determination (r 2 ) higher than 0.9951 for all analytes. Meantime, all the LOD and LLOQ values were in the respective range of 0.3-2 and 1-9ng/g. The accuracy, intra- and inter-day precision were in the ranges of -1.7 to 3.4%, 1.7-5.0% and 1.9-4.4%, respectively. The mean recoveries ranged from 85.4 to 107.1%, while the absolute and relative matrix effect were in the corresponding range of 98.2-108.6% and 2.6-8.7%. Among 120 batches of weight loss plant dietary supplements, sibutramine and fluoxertine or both were positive in 29 samples. In general, LTQ-Orbitrap HRMS technology was a powerful tool for the analysis of illegal ingredients in dietary supplements. Copyright © 2017 Elsevier B.V. All rights reserved.

Fast scan control for deflection type mass spectrometers

NASA Technical Reports Server (NTRS)

Yeager, P. R.; Gaetano, G.; Hughes, D. B. (Inventor)

1974-01-01

A high speed scan device is reported that allows most any scanning sector mass spectrometer to measure preselected gases at a very high sampling rate. The device generates a rapidly changing staircase output which is applied to the accelerator of the spectrometer and it also generates defocusing pulses that are applied to one of the deflecting plates of the spectrometer which when shorted to ground deflects the ion beam away from the collector. A defocusing pulse occurs each time there is a change in the staircase output.

B-scan ultrasonography for the detection of space-occupying ocular masses.

PubMed

Miller, W W; Cartee, R E

1985-07-01

A noninvasive technique, B-scan ultrasonography, was used to obtain detailed cross-sectional images of ocular and orbital structure and form. When a low-frequency probe (5 MHz) was used, tissue penetration was excellent; however, axial resolution was limited. The technique was used in a study of 2 cats and 1 dog. The use of low-frequency B-scan ultrasound should aid in the diagnostic examinations of space-occupying masses in the posterior portion of the ocular bulb and the orbit.

A NEW MASS SPECTROMETRIC TECHNIQUE FOR ...

EPA Pesticide Factsheets

Most organic compounds are not found in mass spectral libraries and cannot be easily identified from low resolution mass spectra. Ion Composition Elucidation (ICE) utilizes selected ion recording with a double focusing mass spectrometer in a new way to determine exact masses and relative abundances of ions more rapidly and with greater accuracy than by full scanning. These measurements are made as analytes from a complex mixture elute from a GC column into the ion source. The exact masses and relative abundances establish the elemental compositions of the ions in a mass spectrum, which limits the possible identify of the compound sufficiently to make searches of the chemical and commercial literature feasible. ICE has two facets: Mass Peak Profiling from Selected Ion Recording Data (MPPSIRD) for data acquisition and a Profile Generation Model (PGM) for automated data interpretation. NTPSIRD and the PGM will be described and several applications of ICE will be shown: tentative identification of a compound that provided a mass spectrum with I I plausible NIST library matches; confirmation of the presence of temazepam, a sedative and one of the 200 most prescribed drugs in 1999. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this T

UHPLC-Q-TOF-MS/MS Method Based on Four-Step Strategy for Metabolism Study of Fisetin in Vitro and in Vivo.

PubMed

Zhang, Xia; Yin, Jintuo; Liang, Caijuan; Sun, Yupeng; Zhang, Lantong

2017-12-20

Fisetin has been identified as an anticancer agent with antiangiogenic properties in mice. However, its metabolism in vitro (rat liver microsomes) and in vivo (rats) is presently not characterized. In this study, ultra-high-performance liquid chromatography coupled with hybrid triple quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) was employed for data acquiring, and a four-step analytical strategy was developed to screen and identify metabolites. First, full-scan was applied, which was dependent on a multiple mass defect filter (MMDF) combined with dynamic background subtraction (DBS). Then PeakView 1.2 and Metabolitepilot 1.5 software were used to load data to seek possible metabolites. Finally, metabolites were identified according to mass measurement and retention time. Moreover, isomers were distinguished based on Clog P parameter. Based on the proposed method, 53 metabolites in vivo and 14 metabolites in vitro were characterized. Moreover, metabolic pathways mainly included oxidation, reduction, hydrogenation, methylation, sulfation, and glucuronidation.

Examination of forensic entomology evidence using computed tomography scanning: case studies and refinement of techniques for estimating maggot mass volumes in bodies.

PubMed

Johnson, Aidan; Archer, Melanie; Leigh-Shaw, Lyndie; Pais, Mike; O'Donnell, Chris; Wallman, James

2012-09-01

A new technique has recently been developed for estimating the volume of maggot masses on deceased persons using post-mortem CT scans. This allows volume to be measured non-invasively and factored into maggot mass temperature calculations for both casework and research. Examination of admission scans also allows exploration of entomological evidence in anatomical areas not usually exposed by autopsy (e.g. nasal cavities and facial sinuses), and before autopsy disrupts the maggot distribution on a body. This paper expands on work already completed by providing the x-ray attenuation coefficient by way of Hounsfield unit (HU) values for various maggot species, maggot masses and human tissue adjacent to masses. Specifically, this study looked at the HU values for four forensically important blowfly larvae: Lucilia cuprina, L. sericata, Calliphora stygia and C. vicina. The Calliphora species had significantly lower HU values than the Lucilia species. This might be explained by histological analysis, which revealed a non-significant trend, suggesting that Calliphora maggots have a higher fat content than the Lucilia maggots. It is apparent that the variation in the x-ray attenuation coefficient usually precludes its use as a tool for delineating the maggot mass from human tissue and that morphology is the dominant method for delineating a mass. This paper also includes three case studies, which reveal different applications for interpreting entomological evidence using post-mortem CT scans.

Precision of guided scanning procedures for full-arch digital impressions in vivo.

PubMed

Zimmermann, Moritz; Koller, Christina; Rumetsch, Moritz; Ender, Andreas; Mehl, Albert

2017-11-01

System-specific scanning strategies have been shown to influence the accuracy of full-arch digital impressions. Special guided scanning procedures have been implemented for specific intraoral scanning systems with special regard to the digital orthodontic workflow. The aim of this study was to evaluate the precision of guided scanning procedures compared to conventional impression techniques in vivo. Two intraoral scanning systems with implemented full-arch guided scanning procedures (Cerec Omnicam Ortho; Ormco Lythos) were included along with one conventional impression technique with irreversible hydrocolloid material (alginate). Full-arch impressions were taken three times each from 5 participants (n = 15). Impressions were then compared within the test groups using a point-to-surface distance method after best-fit model matching (OraCheck). Precision was calculated using the (90-10%)/2 quantile and statistical analysis with one-way repeated measures ANOVA and post hoc Bonferroni test was performed. The conventional impression technique with alginate showed the lowest precision for full-arch impressions with 162.2 ± 71.3 µm. Both guided scanning procedures performed statistically significantly better than the conventional impression technique (p < 0.05). Mean values for group Cerec Omnicam Ortho were 74.5 ± 39.2 µm and for group Ormco Lythos 91.4 ± 48.8 µm. The in vivo precision of guided scanning procedures exceeds conventional impression techniques with the irreversible hydrocolloid material alginate. Guided scanning procedures may be highly promising for clinical applications, especially for digital orthodontic workflows.

Identification and structural characterisation of triterpene saponins from the root of Ardisia mamillata Hance by HPLC-ESI-QTOF-MS/MS.

PubMed

Zhang, Er-Fei; Ling, Yun; Yin, Zi; Zhang, Qing

2018-04-01

Triterpene saponins in medicinal plants attract scientific attentions for their structural diversity and significant bioactivities. In this work, a high-performance liquid chromatography coupled to electrospray ionisation and quadrupole time-of-flight mass spectrometry (HPLC-ESI-QTOF-MS/MS) method is used to rapidly separate and identify triterpene saponins from the extract of Ardisia mamillata Hance (AMH). In the full scan mass spectrum, the accurate determination of molecular formula is obtained by the predominant ion [M + HCOO] - in negative ion mode. As a result, 30 triterpene saponins are identified or tentatively identified in the plant extract. Of these, 17 triterpene saponins are new compounds. In conclusion, the HPLC-ESI-QTOF-MS/MS is an efficient technique to separate and identify triterpene saponins in complex matrices of medicinal plant.

Determination of fusarium mycotoxins in wheat, maize and animal feed using on-line clean-up with high resolution mass spectrometry.

PubMed

Ates, E; Mittendorf, K; Stroka, J; Senyuva, H

2013-01-01

An automated method involving on-line clean-up and analytical separation in a single run using TurboFlow™ reversed phase liquid chromatography coupled to a high resolution mass spectrometer has been developed for the simultaneous determination of deoxynivalenol, T2 toxin, HT2 toxin, zearalenone and fumonisins B1 and B2 in maize, wheat and animal feed. Detection was performed in full scan mode at a resolution of R = 100,000 full width at half maximum with high energy collision cell dissociation for the determination of fragment ions with a mass accuracy below 5 ppm. The extract from homogenised samples, after blending with a 0.1% aqueous mixture of 0.1% formic acid/acetonitrile (43:57) for 45 min, was injected directly onto the TurboFlow™ (TLX) column for automated on-line clean-up followed by analytical separation and accurate mass detection. The TurboFlow™ column enabled specific binding of target mycotoxins, whereas higher molecular weight compounds, like fats, proteins and other interferences with different chemical properties, were removed to waste. Single laboratory method validation was performed by spiking blank materials with mycotoxin standards. The recovery and repeatability was determined by spiking at three concentration levels (50, 100 and 200% of legislative limits) with six replicates. Average recovery, relative standard deviation and intermediate precision values were 71 to 120%, 1 to 19% and 4 to 19%, respectively. The method accuracy was confirmed with certified reference materials and participation in proficiency testing.

Toward the Atomic-Level Mass Analysis of Biomolecules by the Scanning Atom Probe.

PubMed

Nishikawa, Osamu; Taniguchi, Masahiro

2017-04-01

In 1994, a new type of atom probe instrument, named the scanning atom probe (SAP), was proposed. The unique feature of the SAP is the introduction of a small extraction electrode, which scans over a specimen surface and confines the high field, required for field evaporation of surface atoms in a small space, between the specimen and the electrode. Thus, the SAP does not require a sharp specimen tip. This indicates that the SAP can mass analyze the specimens which are difficult to form in a sharp tip, such as organic materials and biomolecules. Clean single wall carbon nanotubes (CNT), made by high-pressure carbon monoxide process are found to be the best substrates for biomolecules. Various amino acids and dipeptide biomolecules were successfully mass analyzed, revealing characteristic clusters formed by strongly bound atoms in the specimens. The mass analysis indicates that SAP analysis of biomolecules is not only qualitative, but also quantitative.

Target analysis of primary aromatic amines combined with a comprehensive screening of migrating substances in kitchen utensils by liquid chromatography-high resolution mass spectrometry.

PubMed

Sanchis, Yovana; Coscollà, Clara; Roca, Marta; Yusà, Vicent

2015-06-01

An analytical strategy including both the quantitative target analysis of 8 regulated primary aromatic amines (PAAs), as well as a comprehensive post-run target screening of 77 migrating substances, was developed for nylon utensils, using liquid chromatography-orbitrap-high resolution mass spectrometry (LC-HRMS) operating in full scan mode. The accurate mass data were acquired with a resolving power of 50,000 FWHM (scan speed, 2 Hz), and by alternating two acquisition events, ESI+ with and without fragmentation. The target method was validated after statistical optimization of the main ionization and fragmentation parameters. The quantitative method presented appropriate performance to be used in official monitoring with recoveries ranging from 78% to 112%, precision in terms of Relative Standard Deviation (RSD) was less than 15%, and the limits of quantification were between 2 and 2.5 µg kg(-1). For post-target screening, a customized theoretical database was built for food contact material migrants, including bisphenols, phthalates, and other amines. For identification purposes, accurate exact mass (<5 ppm) and some diagnostic ions including fragments were used. The strategy was applied to 10 real samples collected from different retailers in the Valencian Region (Spain) during 2014. Six out of eight target PAAs were detected in at least one sample in the target analysis. The most frequently detected compounds were 4,4'-methylenedianiline and aniline, with concentrations ranging from 2.4 to 19,715 µg kg(-1) and 2.5 to 283 µg kg(-1), respectively. Two phthalates were identified and confirmed in the post-run target screening analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

XGlycScan: An Open-source Software For N-linked Glycosite Assignment, Quantification and Quality Assessment of Data from Mass Spectrometry-based Glycoproteomic Analysis.

PubMed

Aiyetan, Paul; Zhang, Bai; Zhang, Zhen; Zhang, Hui

2014-01-01

Mass spectrometry based glycoproteomics has become a major means of identifying and characterizing previously N-linked glycan attached loci (glycosites). In the bottom-up approach, several factors which include but not limited to sample preparation, mass spectrometry analyses, and protein sequence database searches result in previously N-linked peptide spectrum matches (PSMs) of varying lengths. Given that multiple PSM scan map to a glycosite, we reason that identified PSMs are varying length peptide species of a unique set of glycosites. Because associated spectra of these PSMs are typically summed separately, true glycosite associated spectra counts are lost or complicated. Also, these varying length peptide species complicate protein inference as smaller sized peptide sequences are more likely to map to more proteins than larger sized peptides or actual glycosite sequences. Here, we present XGlycScan. XGlycScan maps varying length peptide species to glycosites to facilitate an accurate quantification of glycosite associated spectra counts. We observed that this reduced the variability in reported identifications of mass spectrometry technical replicates of our sample dataset. We also observed that mapping identified peptides to glycosites provided an assessment of search-engine identification. Inherently, XGlycScan reported glycosites reduce the complexity in protein inference. We implemented XGlycScan in the platform independent Java programing language and have made it available as open source. XGlycScan's source code is freely available at https://bitbucket.org/paiyetan/xglycscan/src and its compiled binaries and documentation can be freely downloaded at https://bitbucket.org/paiyetan/xglycscan/downloads. The graphical user interface version can also be found at https://bitbucket.org/paiyetan/xglycscangui/src and https://bitbucket.org/paiyetan/xglycscangui/downloads respectively.

Development of a sensitive method for the determination of acrylamide in coffee using high-performance liquid chromatography coupled to a hybrid quadrupole Orbitrap mass spectrometer.

PubMed

Pugajeva, Iveta; Jaunbergs, Janis; Bartkevics, Vadims

2015-01-01

The emerging trend towards high-resolution mass spectrometry (MS) alternatives was evaluated by the application of Orbitrap MS for the determination of acrylamide in coffee samples. The high resolving power of the Orbitrap MS provided the high selectivity and sensitivity that enabled quantitative analysis of acrylamide in complex matrices, such as coffee. Several sample preparation methods and scanning modes of the MS (full MS, t-SIM, t-MS2) were assessed in order to optimise parameters of the analytical method. The final procedure involved the extraction of acrylamide with acetonitrile, solid-phase extraction with dispersive primary secondary amine (PSA) and amino columns, and the detection by ultra-performance liquid chromatography coupled to a hybrid quadrupole-Orbitrap MS (HPLC-Q-Orbitrap) operated in targeted MS2 scanning mode. The repeatability of the method at the lowest calibration level (10 μg kg(-1)), expressed as relative standard deviation, was 7.8% and the average recovery of acrylamide was 111%. The proposed method was applied to the determination of acrylamide in 22 samples of roasted coffee obtained from the Latvian retail market. Acrylamide concentration in coffee samples was in the range of 166-503 μg kg(-1).

The effect of respiratory motion on pulmonary nodule location during electromagnetic navigation bronchoscopy.

PubMed

Chen, Alexander; Pastis, Nicholas; Furukawa, Brian; Silvestri, Gerard A

2015-05-01

Electromagnetic navigation has improved the diagnostic yield of peripheral bronchoscopy for pulmonary nodules. For these procedures, a thin-slice chest CT scan is performed prior to bronchoscopy at full inspiration and is used to create virtual airway reconstructions that are used as a map during bronchoscopy. Movement of the lung occurs with respiratory variation during bronchoscopy, and the location of pulmonary nodules during procedures may differ significantly from their location on the initial planning full-inspiratory chest CT scan. This study was performed to quantify pulmonary nodule movement from full inspiration to end-exhalation during tidal volume breathing in patients undergoing electromagnetic navigation procedures. A retrospective review of electromagnetic navigation procedures was performed for which two preprocedure CT scans were performed prior to bronchoscopy. One CT scan was performed at full inspiration, and a second CT scan was performed at end-exhalation during tidal volume breathing. Pulmonary lesions were identified on both CT scans, and distances between positions were recorded. Eighty-five pulmonary lesions were identified in 46 patients. Average motion of all pulmonary lesions was 17.6 mm. Pulmonary lesions located in the lower lobes moved significantly more than upper lobe nodules. Size and distance from the pleura did not significantly impact movement. Significant movement of pulmonary lesions occurs between full inspiration and end-exhalation during tidal volume breathing. This movement from full inspiration on planning chest CT scan to tidal volume breathing during bronchoscopy may significantly affect the diagnostic yield of electromagnetic navigation bronchoscopy procedures.

Imaging MS Methodology for More Chemical Information in Less Data Acquisition Time Utilizing a Hybrid Linear Ion Trap-Orbitrap Mass Spectrometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perdian, D. C.; Lee, Young Jin

2010-11-15

A novel mass spectrometric imaging method is developed to reduce the data acquisition time and provide rich chemical information using a hybrid linear ion trap-orbitrap mass spectrometer. In this method, the linear ion trap and orbitrap are used in tandem to reduce the acquisition time by incorporating multiple linear ion trap scans during an orbitrap scan utilizing a spiral raster step plate movement. The data acquisition time was decreased by 43-49% in the current experiment compared to that of orbitrap-only scans; however, 75% or more time could be saved for higher mass resolution and with a higher repetition rate laser.more » Using this approach, a high spatial resolution of 10 {micro}m was maintained at ion trap imaging, while orbitrap spectra were acquired at a lower spatial resolution, 20-40 {micro}m, all with far less data acquisition time. Furthermore, various MS imaging methods were developed by interspersing MS/MS and MSn ion trap scans during orbitrap scans to provide more analytical information on the sample. This method was applied to differentiate and localize structural isomers of several flavonol glycosides from an Arabidopsis flower petal in which MS/MS, MSn, ion trap, and orbitrap images were all acquired in a single data acquisition.« less

Screening of Carotenoids in Tomato Fruits by Using Liquid Chromatography with Diode Array-Linear Ion Trap Mass Spectrometry Detection.

PubMed

Gentili, Alessandra; Caretti, Fulvia; Ventura, Salvatore; Pérez-Fernández, Virginia; Venditti, Alessandro; Curini, Roberta

2015-08-26

This paper presents an analytical strategy for a large-scale screening of carotenoids in tomato fruits by exploiting the potentialities of the triple quadrupole-linear ion trap hybrid mass spectrometer (QqQLIT). The method involves separation on C30 reversed-phase column and identification by means of diode array detection (DAD) and atmospheric pressure chemical ionization-mass spectrometry (APCI-MS). The authentic standards of six model compounds were used to optimize the separative conditions and to predict the chromatographic behavior of untargeted carotenoids. An information dependent acquisition (IDA) was performed with (i) enhanced-mass scan (EMS) as the survey scan, (ii) enhanced-resolution (ER) scan to obtain the exact mass of the precursor ions (16-35 ppm), and (iii) enhanced product ion (EPI) scan as dependent scan to obtain structural information. LC-DAD-multiple reaction monitoring (MRM) chromatograms were also acquired for the identification of targeted carotenoids occurring at low concentrations; for the first time, the relative abundance between the MRM transitions (ion ratio) was used as an extra tool for the MS distinction of structural isomers and the related families of geometrical isomers. The whole analytical strategy was high-throughput, because a great number of experimental data could be acquired with few analytical steps, and cost-effective, because only few standards were used; when applied to characterize some tomato varieties ('Tangerine', 'Pachino', 'Datterino', and 'Camone') and passata of 'San Marzano' tomatoes, our method succeeded in identifying up to 44 carotenoids in the 'Tangerine'" variety.

Doping control analysis of 46 polar drugs in horse plasma and urine using a 'dilute-and-shoot' ultra high performance liquid chromatography-high resolution mass spectrometry approach.

PubMed

Kwok, Wai Him; Choi, Timmy L S; Kwok, Karen Y; Chan, George H M; Wong, Jenny K Y; Wan, Terence S M

2016-06-17

The high sensitivity of ultra high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS) allows the identification of many prohibited substances without pre-concentration, leading to the development of simple and fast 'dilute-and-shoot' methods for doping control for human and equine sports. While the detection of polar drugs in plasma and urine is difficult using liquid-liquid or solid-phase extraction as these substances are poorly extracted, the 'dilute-and-shoot' approach is plausible. This paper describes a 'dilute-and-shoot' UHPLC-HRMS screening method to detect 46 polar drugs in equine urine and plasma, including some angiotensin-converting enzyme (ACE) inhibitors, sympathomimetics, anti-epileptics, hemostatics, the new doping agent 5-aminoimidazole-4-carboxamide-1-β-d-ribofuranoside (AICAR), as well as two threshold substances, namely dimethyl sulfoxide and theobromine. For plasma, the sample (200μL) was protein precipitated using trichloroacetic acid, and the resulting supernatant was diluted using Buffer A with an overall dilution factor of 3. For urine, the sample (20μL) was simply diluted 50-fold with Buffer A. The diluted plasma or urine sample was then analysed using a UHPLC-HRMS system in full-scan ESI mode. The assay was validated for qualitative identification purpose. This straightforward and reliable approach carried out in combination with other screening procedures has increased the efficiency of doping control analysis in the laboratory. Moreover, since the UHPLC-HRMS data were acquired in full-scan mode, the method could theoretically accommodate an unlimited number of existing and new doping agents, and would allow a retrospectively search for drugs that have not been targeted at the time of analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Modeling Of A Monocular, Full-Color, Laser-Scanning, Helmet-Mounted Display for Aviator Situational Awareness

DTIC Science & Technology

2017-03-27

USAARL Report No. 2017-10 Modeling of a Monocular, Full -Color, Laser- Scanning, Helmet-Mounted Display for Aviator Situational Awareness By Thomas...RESPONSIBLE PERSON 19b. TELEPHONE NUMBER (Include area code) 27-03-2017 Final 2002-2003 Modeling of a Monocular, Full -Color, Laser-Scanning, Helmet...was the idea of modeling HMDs by producing computer imagery for an observer to evaluate the quality of symbology. HMD, ANVIS, HGU-56P, Virtual

Identification of damage in plates using full-field measurement with a continuously scanning laser Doppler vibrometer system

NASA Astrophysics Data System (ADS)

Chen, Da-Ming; Xu, Y. F.; Zhu, W. D.

2018-05-01

An effective and reliable damage identification method for plates with a continuously scanning laser Doppler vibrometer (CSLDV) system is proposed. A new constant-speed scan algorithm is proposed to create a two-dimensional (2D) scan trajectory and automatically scan a whole plate surface. Full-field measurement of the plate can be achieved by applying the algorithm to the CSLDV system. Based on the new scan algorithm, the demodulation method is extended from one dimension for beams to two dimensions for plates to obtain a full-field operating deflection shape (ODS) of the plate from velocity response measured by the CSLDV system. The full-field ODS of an associated undamaged plate is obtained by using polynomials with proper orders to fit the corresponding full-field ODS from the demodulation method. A curvature damage index (CDI) using differences between curvatures of ODSs (CODSs) associated with ODSs that are obtained by the demodulation method and the polynomial fit is proposed to identify damage. An auxiliary CDI obtained by averaging CDIs at different excitation frequencies is defined to further assist damage identification. An experiment of an aluminum plate with damage in the form of 10.5% thickness reduction in a damage area of 0.86% of the whole scan area is conducted to investigate the proposed method. Six frequencies close to natural frequencies of the plate and one randomly selected frequency are used as sinusoidal excitation frequencies. Two 2D scan trajectories, i.e., a horizontally moving 2D scan trajectory and a vertically moving 2D scan trajectory, are used to obtain ODSs, CODSs, and CDIs of the plate. The damage is successfully identified near areas with consistently high values of CDIs at different excitation frequencies along the two 2D scan trajectories; the damage area is also identified by auxiliary CDIs.

Discovery of C5-C17 poly- and perfluoroalkyl substances in water by in-line SPE-HPLC-Orbitrap with in-source fragmentation flagging.

PubMed

Liu, Yanna; Pereira, Alberto Dos Santos; Martin, Jonathan W

2015-04-21

The presence of unknown organofluorine compounds in environmental samples has prompted the development of nontargeted analytical methods capable of detecting new perfluoroalkyl and polyfluoroalkyl substances (PFASs). By combining high volume injection with high performance liquid chromatography (HPLC) and ultrahigh resolution Orbitrap mass spectrometry, a sensitive (0.003-0.2 ng F/mL for model mass-labeled PFASs) untargeted workflow was developed for discovery and characterization of novel PFASs in water. In the first step, up to 5 mL of water is injected to in-line solid phase extraction, chromatographed by HPLC, and detected by electrospray ionization with mass spectral acquisition in parallel modes cycling back and forth: (i) full scan with ultrahigh resolving power (RP = 120,000, mass accuracy ≤3 ppm), and (ii) in-source fragmentation flagging scans designed to yield marker fragment ions including [C2F5](-) (m/z 118.992), [C3F7](-) (m/z 168.988), [SO4H](-) (m/z 96.959), and [Cl](-) (m/z 34.9). For flagged PFASs, plausible empirical formulas were generated from accurate masses, isotopic patterns, and fragment ions. In the second step, another injection is made to collect high resolution MS/MS spectra of suspect PFAS ions, allowing further confirmation of empirical formulas while also enabling preliminary structural characterization. The method was validated by applying it to an industrial wastewater, and 36 new PFASs were discovered. Of these, 26 were confidently assigned to 3 new PFAS classes that have not previously been reported in the environment: polyfluorinated sulfates (CnFn+3Hn-2SO4(-); n = 5, 7, 9, 11, 13, and 15), chlorine substituted perfluorocarboxylates (ClCnF2nCO2(-); n = 4-11), and hydro substituted perfluorocarboxylates (HCnF2nCO2(-); n = 5-16). Application of the technique to environmental water samples is now warranted.

Precursor and Neutral Loss Scans in an RF Scanning Linear Quadrupole Ion Trap

NASA Astrophysics Data System (ADS)

Snyder, Dalton T.; Szalwinski, Lucas J.; Schrader, Robert L.; Pirro, Valentina; Hilger, Ryan; Cooks, R. Graham

2018-03-01

Methodology for performing precursor and neutral loss scans in an RF scanning linear quadrupole ion trap is described and compared to the unconventional ac frequency scan technique. In the RF scanning variant, precursor ions are mass selectively excited by a fixed frequency resonance excitation signal at low Mathieu q while the RF amplitude is ramped linearly to pass ions through the point of excitation such that the excited ion's m/z varies linearly with time. Ironically, a nonlinear ac frequency scan is still required for ejection of the product ions since their frequencies vary nonlinearly with the linearly varying RF amplitude. In the case of the precursor scan, the ejection frequency must be scanned so that it is fixed on a product ion m/z throughout the RF scan, whereas in the neutral loss scan, it must be scanned to maintain a constant mass offset from the excited precursor ions. Both simultaneous and sequential permutation scans are possible; only the former are demonstrated here. The scans described are performed on a variety of samples using different ionization sources: protonated amphetamine ions generated by nanoelectrospray ionization (nESI), explosives ionized by low-temperature plasma (LTP), and chemical warfare agent simulants sampled from a surface and analyzed with swab touch spray (TS). We lastly conclude that the ac frequency scan variant of these MS/MS scans is preferred due to electronic simplicity. In an accompanying manuscript, we thus describe the implementation of orthogonal double resonance precursor and neutral loss scans on the Mini 12 using constant RF voltage. [Figure not available: see fulltext.

Horizon scanning of new and emerging medical technology in Australia: its relevance to Medical Services Advisory Committee health technology assessments and public funding.

PubMed

O'Malley, Sue P; Jordan, Ernest

2009-07-01

In 1998, a formal process using full health technology assessments (HTAs) was implemented to determine the suitability for public subsidy of new and emerging medical technologies in the Australian private healthcare sector. This process is overseen by the Medical Services Advisory Committee (MSAC). In 2004, horizon scanning was introduced in Australia with the stated objective of identifying new and emerging medical technologies into the public healthcare sector, with consideration to the publicly subsidized private healthcare sector. How well horizon scanning works in identifying new and emerging technologies suitable for government subsidized funding in the private healthcare sector is examined in this study. A descriptive evaluation of the impact of horizon scanning as an early alert and awareness system identifying new and emerging technologies before these technologies are submitted to MSAC for a full HTA. All MSAC HTAs commenced after the introduction of horizon scanning in 2004 were cross-checked with the list of Prioritizing Summaries or Horizon Scanning Reports to determine whether a prior Prioritizing Summary or Horizon Scanning Report had been carried out. Of the forty-three technologies that were the subject of a full MSAC HTAs in the time period examined, only eleven had been the subject of either a Prioritizing Summary or Horizon Scanning Report. As a result of a full MSAC HTA, twelve of the technologies that were not the subject of a Prioritizing Summary or Horizon Scanning Report were given positive recommendations for public funding. Horizon scanning was set up to scan the introduction of new and emerging medical technologies into the public healthcare sector, with consideration to the publicly subsidized private healthcare sector. Based on the number of new and emerging technologies that have been the subject of a full MSAC HTA without first being subjected to either a Prioritizing Summary or Horizon Scanning Report, horizon scanning in Australia does not function as an "early alert and awareness system" for funding in the publicly subsidized private healthcare sector in Australia.

High resolution measurement of earthquake impacts on rock slope stability and damage using pre- and post-earthquake terrestrial laser scans

NASA Astrophysics Data System (ADS)

Hutchinson, Lauren; Stead, Doug; Rosser, Nick

2017-04-01

Understanding the behaviour of rock slopes in response to earthquake shaking is instrumental in response and relief efforts following large earthquakes as well as to ongoing risk management in earthquake affected areas. Assessment of the effects of seismic shaking on rock slope kinematics requires detailed surveys of the pre- and post-earthquake condition of the slope; however, at present, there is a lack of high resolution monitoring data from pre- and post-earthquake to facilitate characterization of seismically induced slope damage and validate models used to back-analyze rock slope behaviour during and following earthquake shaking. Therefore, there is a need for additional research where pre- and post- earthquake monitoring data is available. This paper presents the results of a direct comparison between terrestrial laser scans (TLS) collected in 2014, the year prior to the 2015 earthquake sequence, with that collected 18 months after the earthquakes and two monsoon cycles. The two datasets were collected using Riegl VZ-1000 and VZ-4000 full waveform laser scanners with high resolution (c. 0.1 m point spacing as a minimum). The scans cover the full landslide affected slope from the toe to the crest. The slope is located in Sindhupalchok District, Central Nepal which experienced some of the highest co-seismic and post-seismic landslide intensities across Nepal due to the proximity to the epicenters (<20 km) of both of the main aftershocks on April 26, 2015 (M 6.7) and May 12, 2015 (M7.3). During the 2015 earthquakes and subsequent 2015 and 2016 monsoons, the slope experienced rockfall and debris flows which are evident in satellite imagery and field photographs. Fracturing of the rock mass associated with the seismic shaking is also evident at scales not accessible through satellite and field observations. The results of change detection between the TLS datasets with an emphasis on quantification of seismically-induced slope damage is presented. Patterns in the distribution and expression of rock mass damage are also explored. The findings presented herein provide insight into the response of rock slopes to seismic shaking and highlight the application of remote sensing to understand slope behaviour.

A New Group of Disinfection Byproducts in Drinking Water: Trihalo-hydroxy-cyclopentene-diones.

PubMed

Pan, Yang; Li, Wenbin; Li, Aimin; Zhou, Qing; Shi, Peng; Wang, Ying

2016-07-19

We report the detection, synthesis, preparative isolation, structure characterization and identification, and formation of a new group of drinking water disinfection byproducts (DBPs): trihalo-hydroxy-cyclopentene-diones (trihalo-HCDs). With ultra performance liquid chromatography (UPLC)/electrospray ionization-triple quadruple mass spectrometry analyses (full scans, multiple reaction monitoring, and product ion scans) and high-resolution mass spectrometry analyses (full scans), the new group of DBPs was identified with formulae and proposed with structures. However, due to a lack of commercially available standard compounds, structure identification of this new group of DBPs was challenging. 2,4,6-Trihydroxybenzaldehyde was found to be a good precursor for the synthesis of the tribromo species (m/z 345/347/349/351) in the new group of DBPs by reacting with bromine at a 2,4,6-trihydroxybenzaldehyde-to-bromine molar ratio of 1:8. With UPLC/photodiode array analysis (simultaneous 2- and 3-dimensional operations), the new DBP was determined to have a maximum UV absorption at the wavelength of 280 nm. Through isolation with high performance liquid chromatography/UV-triggered collections followed by lyophilization, the pure standard of the new DBP was obtained. Characterized with Fourier transform infrared spectroscopy, the pure standard of the new DBP was finally identified to be tribromo-HCD, and thus the new group of DBPs was identified to be trihalo-HCDs. On the basis of the disclosed structure, formation pathways of tribromo-HCD through reactions of three different precursors and bromine were proposed and partially verified. Moreover, increasing the bromide level in source water shifted the formation of trihalo-HCDs from being more chlorinated to being more brominated; with an increase in the contact time from 1 h to 5 d, the formation of trihalo-HCDs kept increasing in chloramination, whereas they kept decreasing in chlorination; with an increase in the pH from 6.0 to 8.5, the formation of trihalo-HCDs was decreased by ∼80%. Notably, the concentrations of tribromo-HCD in eight Chinese tap water samples were from below the detection limit to 0.53 μg/L.

A rare adult renal neuroblastoma better imaged by 18F-FDG than by 68Ga-dotanoc in the PET/CT scan.

PubMed

Jain, Tarun Kumar; Singh, Sharwan Kumar; Sood, Ashwani; Ashwathanarayama, Abhiram Gj; Basher, Rajender Kumar; Shukla, Jaya; Mittal, Bhagwant Rai

2017-01-01

Primary renal neuroblastoma is an uncommon tumor in children and extremely rare in adults. We present a case of a middle aged female having a large retroperitoneal mass involving the right kidney with features of neuroblastoma on pre-operative histopathology. Whole-body fluorine-18-fluoro-deoxyglucose positron emission tomography ( 18 F-FDG PET/CT) and 68 Ga-dotanoc PET/CT scans performed for staging and therapeutic potential revealed a tracer avid mass replacing the right kidney and also pelvic lymph nodes. The 18 F-FDG PET/CT scan showed better both the primary lesion and the metastases in the pelvic lymph nodes than the 68 Ga-dotanoc scan supporting diagnosis and treatment planning.

Aerobic activated sludge transformation of vincristine and identification of the transformation products.

PubMed

Kosjek, Tina; Negreira, Noelia; Heath, Ester; López de Alda, Miren; Barceló, Damià

2018-01-01

This study aims to identify (bio)transformation products of vincristine, a plant alkaloid chemotherapy drug. A batch biotransformation experiment was set-up using activated sludge at two concentration levels with and without the addition of a carbon source. Sample analysis was performed on an ultra-high performance liquid chromatograph coupled to a high-resolution hybrid quadrupole-Orbitrap tandem mass spectrometer. To identify molecular ions of vincristine transformation products and to propose molecular and chemical structures, we performed data-dependent acquisition experiments combining full-scan mass spectrometry data with product ion spectra. In addition, the use of non-commercial detection and prediction algorithms such as MZmine 2 and EAWAG-BBD Pathway Prediction System, was proven to be proficient for screening for transformation products in complex wastewater matrix total ion chromatograms. In this study eleven vincristine transformation products were detected, nine of which were tentatively identified. Copyright © 2017 Elsevier B.V. All rights reserved.

H.M.'s contributions to neuroscience: a review and autopsy studies.

PubMed

Augustinack, Jean C; van der Kouwe, André J W; Salat, David H; Benner, Thomas; Stevens, Allison A; Annese, Jacopo; Fischl, Bruce; Frosch, Matthew P; Corkin, Suzanne

2014-11-01

H.M., Henry Molaison, was one of the world's most famous amnesic patients. His amnesia was caused by an experimental brain operation, bilateral medial temporal lobe resection, carried out in 1953 to relieve intractable epilepsy. He died on December 2, 2008, and that night we conducted a wide variety of in situ MRI scans in a 3 T scanner at the Massachusetts General Hospital (Mass General) Athinoula A. Martinos Center for Biomedical Imaging. For the in situ experiments, we acquired a full set of standard clinical scans, 1 mm isotropic anatomical scans, and multiple averages of 440 μm isotropic anatomical scans. The next morning, H.M.'s body was transported to the Mass General Morgue for autopsy. The photographs taken at that time provided the first documentation of H.M.'s lesions in his physical brain. After tissue fixation, we obtained ex vivo structural data at ultra-high resolution using 3 T and 7 T magnets. For the ex vivo acquisitions, the highest resolution images were 210 μm isotropic. Based on the MRI data, the anatomical areas removed during H.M.'s experimental operation were the medial temporopolar cortex, piriform cortex, virtually all of the entorhinal cortex, most of the perirhinal cortex and subiculum, the amygdala (except parts of the dorsal-most nuclei-central and medial), anterior half of the hippocampus, and the dentate gyrus (posterior head and body). The posterior parahippocampal gyrus and medial temporal stem were partially damaged. Spared medial temporal lobe tissue included the dorsal-most amygdala, the hippocampal-amygdalo-transition-area, ∼2 cm of the tail of the hippocampus, a small part of perirhinal cortex, a small portion of medial hippocampal tissue, and ∼2 cm of posterior parahippocampal gyrus. H.M.'s impact on the field of memory has been remarkable, and his contributions to neuroscience continue with a unique dataset that includes in vivo, in situ, and ex vivo high-resolution MRI. Copyright © 2014 Wiley Periodicals, Inc.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harnsberger, H.R.; Datz, F.L.; Knochel, J.Q.

A patient with postpolycythemic myeloid metaplasia developed an enlarging abdominal mass documented on TCT scanning. To distinguish between lymphoma and extramedullary hematopoiesis, marrow elements were imaged with /sup 111/In chloride and /sup 99m/Tc sulfur colloid. Because the mass failed to accumulate either tracer, a presumptive diagnosis of lymphoma was made and exploratory surgery was performed. The excised mass was found to consist of enlarged lymph nodes containing extramedullary hematopoiesis. Caution should be exercised in the use of /sup 111/In or /sup 99m/Tc SC bone-marrow scans to diagnose sites of extramedullary hematopoiesis.

Goddard Conference on Mass Storage Systems and Technologies, volume 2

NASA Technical Reports Server (NTRS)

Kobler, Ben (Editor); Hariharan, P. C. (Editor)

1993-01-01

Papers and viewgraphs from the conference are presented. Discussion topics include the IEEE Mass Storage System Reference Model, data archiving standards, high-performance storage devices, magnetic and magneto-optic storage systems, magnetic and optical recording technologies, high-performance helical scan recording systems, and low end helical scan tape drives. Additional discussion topics addressed the evolution of the identifiable unit for processing (file, granule, data set, or some similar object) as data ingestion rates increase dramatically, and the present state of the art in mass storage technology.

An integrated strategy to improve data acquisition and metabolite identification by time-staggered ion lists in UHPLC/Q-TOF MS-based metabolomics.

PubMed

Wang, Yang; Feng, Ruibing; He, Chengwei; Su, Huanxing; Ma, Huan; Wan, Jian-Bo

2018-08-05

The narrow linear range and the limited scan time of the given ion make the quantification of the features challenging in liquid chromatography-mass spectrometry (LC-MS)-based untargeted metabolomics with the full-scan mode. And metabolite identification is another bottleneck of untargeted analysis owing to the difficulty of acquiring MS/MS information of most metabolites detected. In this study, an integrated workflow was proposed using the newly established multiple ion monitoring mode with time-staggered ion lists (tsMIM) and target-directed data-dependent acquisition with time-staggered ion lists (tsDDA) to improve data acquisition and metabolite identification in UHPLC/Q-TOF MS-based untargeted metabolomics. Compared to the conventional untargeted metabolomics, the proprosed workflow exhibited the better repeatability before and after data normalization. After selecting features with the significant change by statistical analysis, MS/MS information of all these features can be obtained by tsDDA analysis to facilitate metabolite identification. Using time-staggered ion lists, the workflow is more sensitive in data acquisition, especially for the low-abundant features. Moreover, the metabolites with low abundance tend to be wrongly integrated and triggered by full scan-based untargeted analysis with MS E acquisition mode, which can be greatly improved by the proposed workflow. The integrated workflow was also successfully applied to discover serum biosignatures for the genetic modification of fat-1 in mice, which indicated its practicability and great potential in future metabolomics studies. Copyright © 2018 Elsevier B.V. All rights reserved.

[MRI and CT-scan in presumed benign ovarian tumors].

PubMed

Thomassin-Naggara, I; Bazot, M

2013-12-01

Radiological examinations are required for the assessment of complex or indeterminate ovarian masses, mainly using MRI and CT-scan. MRI provides better tissue characterization than Doppler ultrasound or CT-scan (LE2). Pelvic MRI is recommended in case of an indeterminate or complex ovarian ultrasonographic mass (grade B). The protocol of a pelvic MRI should include morphological T1 and T2 sequences (grade B). In case of solid portion, perfusion and diffusion sequences are recommended (grade C). In case of doubt about the diagnosis of ovarian origin, pelvic MRI is preferred over the CT-scan (grade C). MRI is the technique of choice for the difference between functional and organic ovarian lesion diagnosis (grade C). It can be useful in case of clinical diagnostic uncertainty between polycystic ovary syndrome and ovarian hyperstimulation and multilocular ovarian tumor syndrome (grade C). No MRI classification for ovarian masses is currently validated. The establishment of a presumption of risk of malignancy is required in a MRI report of adnexal mass with if possible a guidance on the histological diagnosis. In the absence of clinical or sonographic diagnosis, pelvic CT-scan is recommended in the context of acute painful pelvic mass in non-pregnant patients (grade C). It specifies the anomalies and allows the differential diagnosis with digestive and urinary diseases (LE4). Given the lack of data in the literature, the precautionary principle must be applied to the realization of a pelvic MRI in a pregnant patient. A risk-benefit balance should be evaluated case by case by the clinician and the radiologist and information should be given to the patient. In an emergency situation during pregnancy, pelvic MRI is an alternative to CT-scan for the exploration of acute pelvic pain in case of uncertain sonographic diagnosis (grade C). Copyright © 2013. Published by Elsevier Masson SAS.

Impact of digital intraoral scan strategies on the impression accuracy using the TRIOS Pod scanner.

PubMed

Müller, Philipp; Ender, Andreas; Joda, Tim; Katsoulis, Joannis

2016-04-01

Little information is available on the impact of different scan strategies on the accuracy of full-arch scans with intraoral scanners. The aim of this in-vitro study was to investigate the trueness and precision of full-arch maxillary digital impressions comparing three scan strategies. Three scan strategies (A, B, and C) were applied each five times on one single model (A, first buccal surfaces, return from occlusal-palatal; B, first occlusal-palatal, return buccal; C, S-type one-way). The TRIOS Pod scanner (3shape, Copenhagen, Denmark) with a color detector was used for these digital impressions. A cast of a maxillary dentate jaw was fabricated and scanned with an industrial reference scanner. This full-arch data record was digitally superimposed with the test scans (trueness) and within-group comparison was performed for each group (precision). The values within the 90/10 percentiles from the digital superimposition were used for calculation and group comparisons with nonparametric tests (ANOVA, post-hoc Bonferroni). The trueness (mean ± standard deviation) was 17.9 ± 16.4 μm for scan strategy A, 17.1 ± 13.7 μm for B, and 26.8 ± 14.7 μm for C without statistically significant difference. The precision was lowest for scan strategy A (35.0 ± 51.1 μm) and significantly different to B (7.9 ± 5.6 μm) and C (8.5 ± 6.3 μm). Scan strategy B may be recommended as it provides the highest trueness and precision in full-arch scans and therefore minimizes inaccuracies in the final reconstruction.

Rapid analysis of controlled substances using desorption electrospray ionization mass spectrometry.

PubMed

Rodriguez-Cruz, Sandra E

2006-01-01

The recently developed technique of desorption electrospray ionization (DESI) has been applied to the rapid analysis of controlled substances. Experiments have been performed using a commercial ThermoFinnigan LCQ Advantage MAX ion-trap mass spectrometer with limited modifications. Results from the ambient sampling of licit and illicit tablets demonstrate the ability of the DESI technique to detect the main active ingredient(s) or controlled substance(s), even in the presence of other higher-concentration components. Full-scan mass spectrometry data provide preliminary identification by molecular weight determination, while rapid analysis using the tandem mass spectrometry (MS/MS) mode provides fragmentation data which, when compared to the laboratory-generated ESI-MS/MS spectral library, provide structural information and final identification of the active ingredient(s). The consecutive analysis of tablets containing different active components indicates there is no cross-contamination or interference from tablet to tablet, demonstrating the reliability of the DESI technique for rapid sampling (one tablet/min or better). Active ingredients have been detected for tablets in which the active component represents less than 1% of the total tablet weight, demonstrating the sensitivity of the technique. The real-time sampling of cannabis plant material is also presented.

Combining targeted and nontargeted data analysis for liquid chromatography/high-resolution mass spectrometric analyses.

PubMed

Croley, Timothy R; White, Kevin D; Wong, Jon; Callahan, John H; Musser, Steven M; Antler, Margaret; Lashin, Vitaly; McGibbon, Graham A

2013-03-01

Increasing importation of food and the diversity of potential contaminants have necessitated more analytical testing of these foods. Historically, mass spectrometric methods for testing foods were confined to monitoring selected ions (SIM or MRM), achieving sensitivity by focusing on targeted ion signals. A limiting factor in this approach is that any contaminants not included on the target list are not typically identified and retrospective data mining is limited. A potential solution is to utilize high-resolution MS to acquire accurate mass full-scan data. Based on the instrumental resolution, these data can be correlated to the actual mass of a contaminant, which would allow for identification of both target compounds and compounds that are not on a target list (nontargets). The focus of this research was to develop software algorithms to provide rapid and accurate data processing of LC/MS data to identify both targeted and nontargeted analytes. Software from a commercial vendor was developed to process LC/MS data and the results were compared to an alternate, vendor-supplied solution. The commercial software performed well and demonstrated the potential for a fully automated processing solution. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A dual-reflective electrothermal MEMS micromirror for full circumferential scanning endoscopic imaging

NASA Astrophysics Data System (ADS)

Wu, Lei; Xie, Huikai

2008-02-01

This paper reports the design, fabrication and measurements of a dual-reflective, single-crystal silicon based micromirror that can perform full circumferential scanning (FCS) for endoscopic optical coherence tomography (EOCT). In the proposed FCS-EOCT probe, two optical fibers are used to deliver light beams to either surface of the micromirror, which can rotate +/-45° (or 90°) and thus a 180° optical scanning is obtained from each mirror surface, resulting in full circumferential scans. A novel surface- and bulk-combined micromachining process based on SOI wafers is developed for fabricating the dual reflective micromirror. The single-crystal-silicon device layer of SOI wafers is used for mirror flatness, and Al is coated on both sides for high reflectivity. With one light beam delivered to each mirror surface, full 360° scans have been observed. Other measured data include the resonant frequency: 328Hz, radius of curvatures: - 124 mm (front surface) and 127 mm (back surface), and the reflectances: 81.3% (front surface) and 79.0% (back surface).

Mass preserving registration for lung CT

NASA Astrophysics Data System (ADS)

Gorbunova, Vladlena; Lo, Pechin; Loeve, Martine; Tiddens, Harm A.; Sporring, Jon; Nielsen, Mads; de Bruijne, Marleen

2009-02-01

In this paper, we evaluate a novel image registration method on a set of expiratory-inspiratory pairs of computed tomography (CT) lung scans. A free-form multi resolution image registration technique is used to match two scans of the same subject. To account for the differences in the lung intensities due to differences in inspiration level, we propose to adjust the intensity of lung tissue according to the local expansion or compression. An image registration method without intensity adjustment is compared to the proposed method. Both approaches are evaluated on a set of 10 pairs of expiration and inspiration CT scans of children with cystic fibrosis lung disease. The proposed method with mass preserving adjustment results in significantly better alignment of the vessel trees. Analysis of local volume change for regions with trapped air compared to normally ventilated regions revealed larger differences between these regions in the case of mass preserving image registration, indicating that mass preserving registration is better at capturing localized differences in lung deformation.

Wave propagation modeling in composites reinforced by randomly oriented fibers

NASA Astrophysics Data System (ADS)

Kudela, Pawel; Radzienski, Maciej; Ostachowicz, Wieslaw

2018-02-01

A new method for prediction of elastic constants in randomly oriented fiber composites is proposed. It is based on mechanics of composites, the rule of mixtures and total mass balance tailored to the spectral element mesh composed of 3D brick elements. Selected elastic properties predicted by the proposed method are compared with values obtained by another theoretical method. The proposed method is applied for simulation of Lamb waves in glass-epoxy composite plate reinforced by randomly oriented fibers. Full wavefield measurements conducted by the scanning laser Doppler vibrometer are in good agreement with simulations performed by using the time domain spectral element method.

Interpretation of Secondary Organic Aerosol Formation from Diesel Exhaust Photooxidation in an Environmental Chamber

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nakao, Shunsuke; Shrivastava, ManishKumar B.; Nguyen, Anh

2011-04-14

Secondary organic aerosol (SOA) formation from diesel exhaust in a smog chamber was investigated. Particle volume measurement based on mobility diameter is shown to underestimate SOA formation from diesel exhaust due to the external void space of agglomerate particles, in which case mass-based measurement technique is necessary. Rapid determination of particle effective density as a function of particle mass was performed by an Aerosol Particle Mass analyzer – Scanning Mobility Particle Sizer (APM-SMPS) to obtain particle mass concentration and fractal dimension. Continuous aging of aerosol was observed in terms of atomic ratio (O/C), from 0.05 to 0.25 in 12 hours,more » underscoring the importance of multi-generational oxidation of low-volatile organic vapors emitted from diesel engine as the significant source of oxygenated SOA. Experimental conditions possibly have strong impacts on physical evolution of diesel particulates in a smog chamber. Higher particle effective densities were observed when raw exhaust was injected into a full bag as opposed to filling a bag with diluted exhaust using an ejector diluter. When longer transfer line was used for injecting diesel exhaust into the smog chamber, rapid particle coagulation was observed, leading to increasing particle volume concentration in dark while its mass concentration is decreasing.« less

Laser-Aided Directed Energy Deposition of Steel Powder over Flat Surfaces and Edges.

PubMed

Caiazzo, Fabrizia; Alfieri, Vittorio

2018-03-16

In the framework of Additive Manufacturing of metals, Directed Energy Deposition of steel powder over flat surfaces and edges has been investigated in this paper. The aims are the repair and overhaul of actual, worn-out, high price sensitive metal components. A full-factorial experimental plan has been arranged, the results have been discussed in terms of geometry, microhardness and thermal affection as functions of the main governing parameters, laser power, scanning speed and mass flow rate; dilution and catching efficiency have been evaluated as well to compare quality and effectiveness of the process under conditions of both flat and edge depositions. Convincing results are presented to give grounds for shifting the process to actual applications: namely, no cracks or pores have been found in random cross-sections of the samples in the processing window. Interestingly an effect of the scanning conditions has been proven on the resulting hardness in the fusion zone; therefore, the mechanical characteristics are expected to depend on the processing parameters.

Laser-Aided Directed Energy Deposition of Steel Powder over Flat Surfaces and Edges

PubMed Central

2018-01-01

In the framework of Additive Manufacturing of metals, Directed Energy Deposition of steel powder over flat surfaces and edges has been investigated in this paper. The aims are the repair and overhaul of actual, worn-out, high price sensitive metal components. A full-factorial experimental plan has been arranged, the results have been discussed in terms of geometry, microhardness and thermal affection as functions of the main governing parameters, laser power, scanning speed and mass flow rate; dilution and catching efficiency have been evaluated as well to compare quality and effectiveness of the process under conditions of both flat and edge depositions. Convincing results are presented to give grounds for shifting the process to actual applications: namely, no cracks or pores have been found in random cross-sections of the samples in the processing window. Interestingly an effect of the scanning conditions has been proven on the resulting hardness in the fusion zone; therefore, the mechanical characteristics are expected to depend on the processing parameters. PMID:29547571

The role of gas in determining image quality and resolution during in situ scanning transmission electron microscopy experiments

DOE PAGES

Zhu, Yuanyuan; Browning, Nigel D.

2017-05-24

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelasticmore » scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. Furthermore, we demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.« less

Low-dose head computed tomography in children: a single institutional experience in pediatric radiation risk reduction: clinical article.

PubMed

Morton, Ryan P; Reynolds, Renee M; Ramakrishna, Rohan; Levitt, Michael R; Hopper, Richard A; Lee, Amy; Browd, Samuel R

2013-10-01

In this study, the authors describe their experience with a low-dose head CT protocol for a preselected neurosurgical population at a dedicated pediatric hospital (Seattle Children's Hospital), the largest number of patients with this protocol reported to date. All low-dose head CT scans between October 2011 and November 2012 were reviewed. Two different low-dose radiation dosages were used, at one-half or one-quarter the dose of a standard head CT scan, based on patient characteristics agreed upon by the neurosurgery and radiology departments. Patient information was also recorded, including diagnosis and indication for CT scan. Six hundred twenty-four low-dose head CT procedures were performed within the 12-month study period. Although indications for the CT scans varied, the most common reason was to evaluate the ventricles and catheter placement in hydrocephalic patients with shunts (70%), followed by postoperative craniosynostosis imaging (12%). These scans provided adequate diagnostic imaging, and no patient required a follow-up full-dose CT scan as a result of poor image quality on a low-dose CT scan. Overall physician comfort and satisfaction with interpretation of the images was high. An additional 2150 full-dose head CT scans were performed during the same 12-month time period, making the total number of CT scans 2774. This value compares to 3730 full-dose head CT scans obtained during the year prior to the study when low-dose CT and rapid-sequence MRI was not a reliable option at Seattle Children's Hospital. Thus, over a 1-year period, 22% of the total CT scans were able to be converted to low-dose scans, and full-dose CT scans were able to be reduced by 42%. The implementation of a low-dose head CT protocol substantially reduced the amount of ionizing radiation exposure in a preselected population of pediatric neurosurgical patients. Image quality and diagnostic utility were not significantly compromised.

A 51-Year-Old Woman With an Increasing Chest Wall Mass Years After Resection of an Early Stage Lung Cancer.

PubMed

Dhakal, Ajay; Chen, Hongbin; Dexter, Elisabeth U

2017-12-01

A 51-year-old woman was found to have a new 14 × 6 mm soft tissue mass under the right serratus muscle on a CT scan of the chest performed for routine surveillance due to her history of stage I lung cancer. A follow-up CT scan performed 4 months later showed that the mass had increased in size to 22 × 8 mm. The patient presents to the oncology clinic to discuss the results of the CT scan. She has no pain or swelling on the right lateral chest and no cough, fever, or shortness of breath. She is at her baseline health with good appetite and functional status. Copyright © 2017 American College of Chest Physicians. Published by Elsevier Inc. All rights reserved.

Detection of anabolic and androgenic steroids and/or their esters in horse hair using ultra-high performance liquid chromatography-high resolution mass spectrometry.

PubMed

Kwok, Karen Y; Choi, Timmy L S; Kwok, Wai Him; Wong, Jenny K Y; Wan, Terence S M

2017-04-14

Anabolic and androgenic steroids (AASs) are a class of prohibited substances banned in horseracing at all times. The common approach for controlling the misuse of AASs in equine sports is by detecting the presence of AASs and/or their metabolites in urine and blood samples using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). This approach, however, often falls short as the duration of effect for many AASs are longer than their detection time in both urine and blood. As a result, there is a high risk that such AASs could escape detection in their official race-day samples although they may have been used during the long period of training. Hair analysis, on the other hand, can afford significantly longer detection windows. In addition, the identification of synthetic ester derivatives of AASs in hair, particularly for the endogenous ones, can provide unequivocal proof of their exogenous origin. This paper describes the development of a sensitive method (at sub to low parts-per-billion or ppb levels) for detecting 48 AASs and/or their esters in horse hair using ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS). Decontaminated horse hair was pulverised and subjected to in-situ liquid-liquid extraction in a mixture of hexane - ethyl acetate (7:3, v/v) and phosphate buffer (0.1M, pH 9.5), followed by additional clean-up using mixed-mode solid-phase extraction. The final extract was analysed using UHPLC-HRMS in the positive electrospray ionisation (ESI) mode with both full scan and parallel reaction monitoring (PRM). This method was validated for qualitative identification purposes. Validation data, including method specificity, method sensitivity, extraction recovery, method precision and matrix effect are presented. Method applicability was demonstrated by the successful detection and confirmation of testosterone propionate in a referee hair sample. To our knowledge, this was the first report of a comprehensive screening method for detecting as many as 48 AASs and/or their esters in horse hair. Moreover, retrospective analysis of non-targeted AASs and/or their esters was made feasible by re-examining the full scan UHPLC-HRMS data acquired. Copyright © 2017 Elsevier B.V. All rights reserved.

Modification of endoscopic medial maxillectomy: a novel approach for inverted papilloma of the maxillary sinus.

PubMed

Ghosh, A; Pal, S; Srivastava, A; Saha, S

2015-02-01

To describe modification to endoscopic medial maxillectomy for treating extensive Krouse stage II or III inverted papilloma of the nasal and maxillary sinus. Ten patients with inverted papilloma arising from the nasoantral area underwent diagnostic nasal endoscopy, contrast-enhanced computed tomography scanning of the paranasal sinus and pre-operative biopsy of the nasal mass. They were all managed using endoscopic medial maxillectomy and followed up for seven months to three years without recurrence. Most patients were aged 41-60 years at presentation, and most were male. Presenting symptoms were nasal obstruction, mass in the nasal cavity and epistaxis. In each case, computed tomography imaging showed a mass involving the nasal cavity and maxillary sinus, with bony remodelling. The endoscopic medial maxillectomy approach was modified by making an incision in the pyriform aperture and removing part of the anterolateral wall of the maxilla bone en bloc. Modified endoscopic medial maxillectomy providing full access to the maxillary and ethmoid sinuses is described in detail. This effective, reproducible technique is associated with reduced operative time and morbidity.

Quantitative determination of major active components in Ginkgo biloba dietary supplements by liquid chromatography/mass spectrometry.

PubMed

Ding, Shujing; Dudley, Ed; Plummer, Sue; Tang, Jiandong; Newton, Russell P; Brenton, A Gareth

2006-01-01

A reversed-phase high-performance liquid chromatography/electrospray ionisation mass spectrometry (RP-HPLC/ESI-MS) method was developed and validated for the simultaneous determination of ten major active components in Ginkgo biloba extract (bilobalide, ginkgolides A, B, C, quercetin, kaempferol, isorhamnetin, rutin hydrate, quercetin-3-beta-D-glucoside and quercitrin hydrate) which have not been previously reported to be quantified in a single analysis. The ten components exhibit baseline separation in 50 min by C18 chromatography using a water/1:1 (v/v) methanol/acetonitrile gradient. Quantitation was performed using negative ESI-MS in selected ion monitoring (SIM) mode. Good reproducibility and recovery were obtained by this method. The sensitivity of both UV and different mass spectrometry modes (full scan, selected ion monitoring (SIM), and selected reaction monitoring (SRM)) were compared and both quantitation with and without internal standard were evaluated. The analysis of Ginkgo biloba commercial products showed remarkable variations in the rutin and quercetin content as well as the terpene lactone contents although all the products satisfy the conventional quality control method. Copyright 2006 John Wiley & Sons, Ltd.

Studies on the metabolism and toxicological detection of the Eschscholtzia californica alkaloids californine and protopine in urine using gas chromatography-mass spectrometry.

PubMed

Paul, Liane D; Maurer, Hans H

2003-06-05

Eschscholtzia californica preparations are in use as phytopharmaceuticals and as herbal drugs. Studies are described on the metabolism and the toxicological analysis of the Eschscholtzia californica alkaloids californine and protopine in rat urine using gas chromatography-mass spectrometry. The identified metabolites indicated that californine is extensively metabolized by N-demethylation and/or single or double demethylenation with consecutive catechol-O-methylation of one of the hydroxy groups. Protopine, however, only undergoes extensive demethylenation of the 2,3-methylenedioxy group followed by catechol-O-methylation. All phenolic hydroxy metabolites were found to be partly conjugated. The authors' systematic toxicological analysis procedure using full-scan gas chromatography-mass spectrometry after acid hydrolysis, liquid-liquid extraction and microwave-assisted acetylation allowed the detection of the main metabolites of californine and protopine in rat urine after a dose which should correspond to that of drug users. Therefore, use of Eschscholtzia californica preparations should also be detectable in human urine by the authors' systematic toxicological analysis procedure.

Ultra performance liquid chromatography atmospheric pressure photoionization high resolution mass spectrometric method for determination of multiclass pesticide residues in grape and mango juices.

PubMed

Deme, Pragney; Upadhyayula, Vijayasarathi V R

2015-04-15

A novel analytical method was developed for determination of organochlorine, synthetic pyrethroid, organophosphate and carbamate pesticide residues in fruit juices using ultra performance liquid chromatography-atmospheric pressure photoionization-high resolution mass spectrometry (UPLC-APPI-HRMS). The analytes were extracted from fruit juices by dispersive solid-phase extraction using multi-walled carbon nanotubes (MWCNTs). The analysis was carried out in full scan mode using dual ionization mode of APPI in the mass range of 100-650 units. The limit of detection and limit of quantification values for the pesticides were in the range of 0.025-0.15 ng mL(-1) and 0.1-0.5 ng mL(-1) respectively. The matrix effect of the method was found to be low and extraction recoveries were in the range of 60-110%. Some of the real fruits juice samples showed the presence of some pesticides in the range of 6.5-24.8 ng L(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of atelectasis changes on tissue mass and dose during lung radiotherapy.

PubMed

Guy, Christopher L; Weiss, Elisabeth; Jan, Nuzhat; Reshko, Leonid B; Christensen, Gary E; Hugo, Geoffrey D

2016-11-01

To characterize mass and density changes of lung parenchyma in non-small cell lung cancer (NSCLC) patients following midtreatment resolution of atelectasis and to quantify the impact this large geometric change has on normal tissue dose. Baseline and midtreatment CT images and contours were obtained for 18 NSCLC patients with atelectasis. Patients were classified based on atelectasis volume reduction between the two scans as having either full, partial, or no resolution. Relative mass and density changes from baseline to midtreatment were calculated based on voxel intensity and volume for each lung lobe. Patients also had clinical treatment plans available which were used to assess changes in normal tissue dose constraints from baseline to midtreatment. The midtreatment image was rigidly aligned with the baseline scan in two ways: (1) bony anatomy and (2) carina. Treatment parameters (beam apertures, weights, angles, monitor units, etc.) were transferred to each image. Then, dose was recalculated. Typical IMRT dose constraints were evaluated on all images, and the changes from baseline to each midtreatment image were investigated. Atelectatic lobes experienced mean (stdev) mass changes of -2.8% (36.6%), -24.4% (33.0%), and -9.2% (17.5%) and density changes of -66.0% (6.4%), -25.6% (13.6%), and -17.0% (21.1%) for full, partial, and no resolution, respectively. Means (stdev) of dose changes to spinal cord D max , esophagus D mean , and lungs D mean were 0.67 (2.99), 0.99 (2.69), and 0.50 Gy (2.05 Gy), respectively, for bone alignment and 0.14 (1.80), 0.77 (2.95), and 0.06 Gy (1.71 Gy) for carina alignment. Dose increases with bone alignment up to 10.93, 7.92, and 5.69 Gy were found for maximum spinal cord, mean esophagus, and mean lung doses, respectively, with carina alignment yielding similar values. 44% and 22% of patients had at least one metric change by at least 5 Gy (dose metrics) or 5% (volume metrics) for bone and carina alignments, respectively. Investigation of GTV coverage showed mean (stdev) changes in V Rx , D max , and D min of -5.5% (13.5%), 2.5% (4.2%), and 0.8% (8.9%), respectively, for bone alignment with similar results for carina alignment. Resolution of atelectasis caused mass and density decreases, on average, and introduced substantial changes in normal tissue dose metrics in a subset of the patient cohort.

Effect of atelectasis changes on tissue mass and dose during lung radiotherapy

PubMed Central

Guy, Christopher L.; Weiss, Elisabeth; Jan, Nuzhat; Reshko, Leonid B.; Christensen, Gary E.; Hugo, Geoffrey D.

2016-01-01

Purpose: To characterize mass and density changes of lung parenchyma in non-small cell lung cancer (NSCLC) patients following midtreatment resolution of atelectasis and to quantify the impact this large geometric change has on normal tissue dose. Methods: Baseline and midtreatment CT images and contours were obtained for 18 NSCLC patients with atelectasis. Patients were classified based on atelectasis volume reduction between the two scans as having either full, partial, or no resolution. Relative mass and density changes from baseline to midtreatment were calculated based on voxel intensity and volume for each lung lobe. Patients also had clinical treatment plans available which were used to assess changes in normal tissue dose constraints from baseline to midtreatment. The midtreatment image was rigidly aligned with the baseline scan in two ways: (1) bony anatomy and (2) carina. Treatment parameters (beam apertures, weights, angles, monitor units, etc.) were transferred to each image. Then, dose was recalculated. Typical IMRT dose constraints were evaluated on all images, and the changes from baseline to each midtreatment image were investigated. Results: Atelectatic lobes experienced mean (stdev) mass changes of −2.8% (36.6%), −24.4% (33.0%), and −9.2% (17.5%) and density changes of −66.0% (6.4%), −25.6% (13.6%), and −17.0% (21.1%) for full, partial, and no resolution, respectively. Means (stdev) of dose changes to spinal cord Dmax, esophagus Dmean, and lungs Dmean were 0.67 (2.99), 0.99 (2.69), and 0.50 Gy (2.05 Gy), respectively, for bone alignment and 0.14 (1.80), 0.77 (2.95), and 0.06 Gy (1.71 Gy) for carina alignment. Dose increases with bone alignment up to 10.93, 7.92, and 5.69 Gy were found for maximum spinal cord, mean esophagus, and mean lung doses, respectively, with carina alignment yielding similar values. 44% and 22% of patients had at least one metric change by at least 5 Gy (dose metrics) or 5% (volume metrics) for bone and carina alignments, respectively. Investigation of GTV coverage showed mean (stdev) changes in VRx, Dmax, and Dmin of −5.5% (13.5%), 2.5% (4.2%), and 0.8% (8.9%), respectively, for bone alignment with similar results for carina alignment. Conclusions: Resolution of atelectasis caused mass and density decreases, on average, and introduced substantial changes in normal tissue dose metrics in a subset of the patient cohort. PMID:27806593

Comparison of scatter rejection and low-contrast performance of scan equalization digital radiography (SEDR), slot-scan digital radiography, and full-field digital radiography systems for chest phantom imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu Xinming; Shaw, Chris C.; Lai, Chao-Jen

Purpose: To investigate and compare the scatter rejection properties and low-contrast performance of the scan equalization digital radiography (SEDR) technique to the slot-scan and conventional full-field digital radiography techniques for chest imaging. Methods: A prototype SEDR system was designed and constructed with an a-Se flat-panel (FP) detector to improve image quality in heavily attenuating regions of an anthropomorphic chest phantom. Slot-scanning geometry was used to reject scattered radiation without attenuating primary x rays. The readout scheme of the FP was modified to erase accumulated scatter signals prior to image readout. A 24-segment beam width modulator was developed to regulate x-raymore » exposures regionally and compensate for the low x-ray flux in heavily attenuating regions. To measure the scatter-to-primary ratios (SPRs), a 2 mm thick lead plate with a 2-D array of aperture holes was used to measure the primary signals, which were then subtracted from those obtained without the lead plate to determine scatter components. A 2-D array of aluminum beads (3 mm in diameter) was used as the low-contrast objects to measure the contrast ratios (CRs) and contrast-to-noise ratios (CNRs) for evaluating the low-contrast performance in chest phantom images. A set of two images acquired with the same techniques were subtracted from each other to measure the noise levels. SPRs, CRs, and CNRs of the SEDR images were measured in four anatomical regions of chest phantom images and compared to those of slot-scan images and full-field images acquired with and without antiscatter grid. Results: The percentage reduction of SPR (percentage of SPRs reduced with scatter removal/rejection methods relative to that for nongrid full-field imaging) averaged over four anatomical regions was measured to be 80%, 83%, and 71% for SEDR, slot-scan, and full-field with grid, respectively. The average CR over four regions was found to improve over that for nongrid full-field imaging by 259%, 279%, and 145% for SEDR, slot-scan, and full-field with grid, respectively. The average CNR over four regions was found to improve over that for nongrid full-field imaging by 201% for SEDR as compared to 133% for the slot-scan technique and 14% for the antiscatter grid method. Conclusions: Both SEDR and slot-scan techniques outperformed the antiscatter grid method used in standard full-field radiography. For imaging with the same effective exposure, the SEDR technique offers no advantage over the slot-scan method in terms of SPRs and CRs. However, it improves CNRs significantly, especially in heavily attenuating regions. The improvement of low-contrast performance may help improve the detection of the lung nodules or other abnormalities and may offer SEDR the potential for dose reduction in chest radiography.« less

Levator claviculae muscle discovered during physical examination for cervical lymphadenopathy.

PubMed

Rosenheimer, J L; Loewy, J; Lozanoff, S

2000-01-01

During a routine physical examination of an adult female with a history of breast cancer and cervical lymphadenopathy, a mass was noted in the right supraclavicular region. The mass was unilateral and easily palpable along the superior border near the median aspect of the clavicle. Plain film radiography, performed to determine whether the mass represented an enlarged jugulo-omohyoid lymph node, revealed an elongated opaque mass in this region. Computed tomographic (CT) and magnetic resonance (MR) images were subsequently obtained. Sequential axial CT scans revealed a cylindrical mass that appeared to be independent of contiguous muscles, including the sternocleidomastoid, anterior, and middle scalene muscles. This mass attached inferiorly to the clavicle and superiorly to the transverse process of the sixth cervical vertebra. Sagittal, coronal, and axial MR scans confirmed the presence of a well-defined superficial mass. It is concluded that the mass represents a levator claviculae (cleidocervical) muscle. This observation underscores the importance of understanding soft tissue variants that may be encountered during a routine physical examination. Copyright 2000 Wiley-Liss, Inc.

Using Power Spectrum Analysis to Evaluate 18O-Water Labeling Data Acquired from Low Resolution Mass Spectrometers

PubMed Central

Sadygov, Rovshan G.; Zhao, Yingxin; Haidacher, Sigmund J.; Starkey, Jonathan M.; Tilton, Ronald G.; Denner, Larry

2010-01-01

We describe a method for ratio estimations in 18O-water labeling experiments acquired from low resolution isotopically resolved data. The method is implemented in a software package specifically designed for use in experiments making use of zoom-scan mode data acquisition. Zoom-scan mode data allows commonly used ion trap mass spectrometers to attain isotopic resolution, which make them amenable to use in labeling schemes such as 18O-water labeling, but algorithms and software developed for high resolution instruments may not be appropriate for the lower resolution data acquired in zoom-scan mode. The use of power spectrum analysis is proposed as a general approach which may be uniquely suited to these data types. The software implementation uses power spectrum to remove high-frequency noise, and band-filter contributions from co-eluting species of differing charge states. From the elemental composition of a peptide sequence we generate theoretical isotope envelopes of heavy-light peptide pairs in five different ratios; these theoretical envelopes are correlated with the filtered experimental zoom scans. To automate peptide quantification in high-throughput experiments, we have implemented our approach in a computer program, MassXplorer. We demonstrate the application of MassXplorer to two model mixtures of known proteins, and to a complex mixture of mouse kidney cortical extract. Comparison with another algorithm for ratio estimations demonstrates the increased precision and automation of MassXplorer. PMID:20568695

Dual energy CT with one full scan and a second sparse-view scan using structure preserving iterative reconstruction (SPIR)

NASA Astrophysics Data System (ADS)

Wang, Tonghe; Zhu, Lei

2016-09-01

Conventional dual-energy CT (DECT) reconstruction requires two full-size projection datasets with two different energy spectra. In this study, we propose an iterative algorithm to enable a new data acquisition scheme which requires one full scan and a second sparse-view scan for potential reduction in imaging dose and engineering cost of DECT. A bilateral filter is calculated as a similarity matrix from the first full-scan CT image to quantify the similarity between any two pixels, which is assumed unchanged on a second CT image since DECT scans are performed on the same object. The second CT image from reduced projections is reconstructed by an iterative algorithm which updates the image by minimizing the total variation of the difference between the image and its filtered image by the similarity matrix under data fidelity constraint. As the redundant structural information of the two CT images is contained in the similarity matrix for CT reconstruction, we refer to the algorithm as structure preserving iterative reconstruction (SPIR). The proposed method is evaluated on both digital and physical phantoms, and is compared with the filtered-backprojection (FBP) method, the conventional total-variation-regularization-based algorithm (TVR) and prior-image-constrained-compressed-sensing (PICCS). SPIR with a second 10-view scan reduces the image noise STD by a factor of one order of magnitude with same spatial resolution as full-view FBP image. SPIR substantially improves over TVR on the reconstruction accuracy of a 10-view scan by decreasing the reconstruction error from 6.18% to 1.33%, and outperforms TVR at 50 and 20-view scans on spatial resolution with a higher frequency at the modulation transfer function value of 10% by an average factor of 4. Compared with the 20-view scan PICCS result, the SPIR image has 7 times lower noise STD with similar spatial resolution. The electron density map obtained from the SPIR-based DECT images with a second 10-view scan has an average error of less than 1%.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory : determination of polycyclic aromatic hydrocarbon compounds in sediment by gas chromatography/mass spectrometry

USGS Publications Warehouse

Olson, Mary C.; Iverson, Jana L.; Furlong, Edward T.; Schroeder, Michael P.

2004-01-01

A method for the determination of 28 polycyclic aromatic hydrocarbons (PAHs) and 25 alkylated PAH homolog groups in sediment samples is described. The compounds are extracted from sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography. The compounds are identified and uantitated using capillary-column gas chromatography/mass spectrometry. The report presents performance data for full-scan ion monitoring. Method detection limits in laboratory reagent matrix samples range from 1.3 to 5.1 micrograms per kilogram for the 28 PAHs. The 25 groups of alkylated PAHs are homologs of five groups of isomeric parent PAHs. Because of the lack of authentic standards, these homologs are reported semiquantitatively using a response factor from a parent PAH or a specific alkylated PAH. Precision data for the alkylated PAH homologs are presented using two different standard reference manuals produced by the National Institute of Standards and Technology: SRM 1941b and SRM 1944. The percent relative standard deviations for identified alkylated PAH homolog groups ranged from 1.55 to 6.98 for SRM 1941b and from 6.11 to 12.0 for SRM 1944. Homolog group concentrations reported under this method include the concentrations of individually identified compounds that are members of the group. Organochlorine (OC) pesticides--including toxaphene, polychlorinated biphenyls (PCBs), and organophosphate (OP) pesticides--can be isolated simultaneously using this method. In brief, sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethan (95 percent) and methanol (5 percent). The extract is concentrated and then filtered through a 0.2-micrometer polytetrafluoroethylene syringe filter. The PAH fraction is isolated by quantitatively injecting an aliquot of sample onto two polystyrene-divinylbenzene gel-permeation chromatographic columns connected in series. The compounds are eluted with dichloromethane, a PAH fraction is collected, and a portion of the coextracted interferences, including elemental sulfur, is separated and discarded. The extract is solvent exchanged, the volume is reduced, and internal standard is added. Sample analysis is completed using a gas chromatograph/mass spectrometer and full-scan acquisition.

Preparation and Electrochemical Characterization of Mesoporous Polyaniline-Silica Nanocomposites as an Electrode Material for Pseudocapacitors

PubMed Central

Zu, Lei; Cui, Xiuguo; Jiang, Yanhua; Hu, Zhongkai; Lian, Huiqin; Liu, Yang; Jin, Yushun; Li, Yan; Wang, Xiaodong

2015-01-01

Mesoporous polyaniline-silica nanocomposites with a full interpenetrating structure for pseudocapacitors were synthesized via the vapor phase approach. The morphology and structure of the nanocomposites were deeply investigated by scanning electron microscopy, infrared spectroscopy, X-ray diffraction, thermal gravimetric analysis and nitrogen adsorption-desorption tests. The results present that the mesoporous nanocomposites possess a uniform particle morphology and full interpenetrating structure, leading to a continuous conductive polyaniline network with a large specific surface area. The electrochemical performances of the nanocomposites were tested in a mixed solution of sulfuric acid and potassium iodide. With the merits of a large specific surface area and suitable pore size distribution, the nanocomposite showed a large specific capacitance (1702.68 farad (F)/g) due to its higher utilization of the active material. This amazing value is almost three-times larger than that of bulk polyaniline when the same mass of active material was used. PMID:28788006

Broad screening and identification of β-agonists in feed and animal body fluid and tissues using ultra-high performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry combined with spectra library search.

PubMed

Li, Tingting; Cao, Jingjing; Li, Zhen; Wang, Xian; He, Pingli

2016-02-01

Broad screening and identification of β-agonists in feed, serum, urine, muscle and liver samples was achieved in a quick and highly sensitive manner using ultra high performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) combined with a spectra library search. Solid-phase extraction technology was employed for sample purification and enrichment. After extraction and purification, the samples were analyzed using a Q-Orbitrap high-resolution mass spectrometer under full-scan and data-dependent MS/MS mode. The acquired mass spectra were compared with an in-house library (compound library and MS/MS mass spectral library) built with TraceFinder Software which contained the M/Z of the precursor ion, chemical formula, retention time, character fragment ions and the entire MS/MS spectra of 32 β-agonist standards. Screening was achieved by comparing 5 key mass spectral results and positive matches were marked. Using the developed method, the identification results from 10 spiked samples and 238 actual samples indicated that only 2% of acquired mass spectra produced false identities. The method validation results showed that the limit of detection ranged from 0.021-3.854 μg kg(-1)and 0.015-1.198 ng mL(-1) for solid and liquid samples, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Accuracy and Radiation Dose Reduction of Limited-Range CT in the Evaluation of Acute Appendicitis in Pediatric Patients.

PubMed

Jin, Michael; Sanchez, Thomas R; Lamba, Ramit; Fananapazir, Ghaneh; Corwin, Michael T

2017-09-01

The purpose of this article is to determine the accuracy and radiation dose reduction of limited-range CT prescribed from the top of L2 to the top of the pubic symphysis in children with suspected acute appendicitis. We performed a retrospective study of 210 consecutive pediatric patients from December 11, 2012, through December 11, 2014, who underwent abdominopelvic CT for suspected acute appendicitis. Two radiologists independently reviewed the theoretic limited scans from the superior L2 vertebral body to the top of the pubic symphysis, to assess for visualization of the appendix, acute appendicitis, alternative diagnoses, and incidental findings. Separately, the same parameters were assessed on the full scan by the same two reviewers. Whole-body effective doses were determined for the full- and limited-range scans and were compared using the paired t test. The appendix or entire cecum was visualized on the limited scan in all cases, and no cases of acute appendicitis were missed on the simulated limited scan compared with the full scan. Two alternative diagnoses were missed with the limited scan: one case of hydronephrosis and one of acute acalculous cholecystitis. The mean effective dose for the original scan was 5.6 mSv and that for the simulated limited scan was 3.0 mSv, resulting in a dose reduction of 46.4% (p < 0.001). A limited-range CT examination performed from the top of L2 to the top of the pubic symphysis is as accurate as a full-range abdominopelvic CT in evaluating pediatric patients with suspected appendicitis and reduces the dose by approximately 46%.

Detection of periimplant fenestration and dehiscence with the use of two scan modes and the smallest voxel sizes of a cone-beam computed tomography device.

PubMed

de-Azevedo-Vaz, Sergio Lins; Vasconcelos, Karla de Faria; Neves, Frederico Sampaio; Melo, Saulo Leonardo Sousa; Campos, Paulo Sérgio Flores; Haiter-Neto, Francisco

2013-01-01

To assess the accuracy of cone-beam computed tomography (CBCT) in periimplant fenestration and dehiscence detection, and to determine the effects of 2 voxel sizes and scan modes. One hundred titanium implants were placed in bovine ribs in which periimplant fenestration and dehiscence were simulated. CBCT images were acquired with the use of 3 protocols of the i-CAT NG unit: A) 0.2 mm voxel size half-scan (180°); B) 0.2 mm voxel size full-scan (360°); and C) 0.12 mm voxel size full scan (360°). Receiver operating characteristic curves and diagnostic values were obtained. The Az values were compared with the use of analysis of variance. The Az value for dehiscence in protocol A was significantly lower than those of B or C (P < .01). They did not statistically differ for fenestration (P > .05). Protocol B yielded the highest values. The voxel sizes did not affect fenestration and dehiscence detection, and for dehiscence full-scan performed better than half-scan. Copyright © 2013 Elsevier Inc. All rights reserved.

Application of Gas Chromatography-Tandem Mass Spectrometry (GC/MS/MS) for the Analysis of Deuterium Enrichment of Water

PubMed Central

Walker, Dillon K.; Thaden, John J.; Deutz, Nicolaas E.P.

2015-01-01

Incorporation of deuterium from deuterium oxide (2H2O) into biological components is a commonly used approach in metabolic studies. Determining the dilution of deuterium in the body water pool (BW) can be used to estimate body composition. We describe three sensitive GC-MS/MS methods to measure water enrichment in BW . Samples were reacted with NaOH and U-13C3-acetone in an autosampler vial to promote deuterium exchange with U-13C3-acetone hydrogens. Headspace injections were made of U-13C3-acetone-saturated air onto a 30m DB-1MS column in EI-mode. Subjects ingested 30ml 2H2O and plasma samples were collected. BW was determined by standard equation. DXA scans were performed to calculate body mass, body volume and bone mineral content. A 4 compartmental model was used to estimate body composition (fat and fat free mass). Full scan experiments generated a m/z 45 peak and to a lesser extent a m/z 61 peak. Product fragment ions further monitored included 45 and 46 using selected ion monitoring (SIM;Method1), the 61>45 and 62>46 transition using multiple reaction monitoring (MRM;Method2) and the Neutral Loss, 62>45, transition (Method3). MRM methods were optimized for collision energy (CE) and collision-induced dissociation (CID) argon gas pressure with 6eV CE and 1.5 mTorr CID gas being optimal. Method2 was used for finally determination of 2H2O enrichment of subjects due to lower natural background. We have developed a sensitive method to determine 2H2O enrichment in body water to enable measurement of FM and FFM. PMID:26169138

Comprehensive analytical strategy for biomonitoring of pesticides in urine by liquid chromatography–orbitrap high resolution masss pectrometry.

PubMed

Roca, M; Leon, N; Pastor, A; Yusà, V

2014-12-29

In this study we propose an analytical strategy that combines a target approach for the quantitative analysis of contemporary pesticide metabolites with a comprehensive post-target screening for the identification of biomarkers of exposure to environmental contaminants in urine using liquid chromatography coupled to high-resolution mass spectrometry (LC–HRMS). The quantitative method for the target analysis of 29 urinary metabolites of organophosphate (OP) insecticides, synthetic pyrethroids, herbicides and fungicides was validated after a previous statistical optimization of the main factors governing the ion source ionization and a fragmentation study using the high energy collision dissociation (HCD) cell. The full scan accurate mass data were acquired with a resolving power of 50,000 FWHM (scan speed, 2 Hz), in both ESI+ and ESI− modes, and with and without HCD-fragmentation. The method – LOQ was lower than 3.2 μg L−1 for the majority of the analytes. For post-target screening a customized theoretical database was built, for the identification of 60 metabolites including pesticides, PAHs, phenols, and other metabolites of environmental pollutants. For identification purposes, accurate exact mass with less than 5 ppm, and diagnostic ions including isotopes and/or fragments were used. The analytical strategy was applied to 20 urine sample collected from children living in Valencia Region. Eleven target metabolites were detected with concentrations ranging from 1.18 to 131 μg L−1. Likewise, several compounds were tentatively identified in the post-target analysis belonging to the families of phthalates, phenols and parabenes. The proposed strategy is suitable for the determination of target pesticide biomarkers in urine in the framework of biomonitoring studies, and appropriate for the identification of other non-target metabolites.

VOC removal and deodorization of effluent gases from an industrial plant by photo-oxidation, chemical oxidation, and ozonization.

PubMed

Domeño, Celia; Rodríguez-Lafuente, Angel; Martos, J M; Bilbao, Rafael; Nerín, Cristina

2010-04-01

The efficiency of photo-oxidation, chemical oxidation by sodium hypochlorite, and ozonization for the industrial-scale removal of volatile organic compounds (VOCs) and odors from gaseous emissions was studied by applying these treatments (in an experimental system) to substances passing through an emission stack of a factory producing maize derivatives. Absorption and ozonization were the most efficient treatment, removing 75% and 98% of VOCs, respectively, while photo-oxidation only removed about 59%. The emitted chemical compounds and odors were identified and quantified by gas chromatography-mass spectrometry (in full-scan mode). In addition to presenting the results, their implications for selecting optimal processes for treating volatile emissions are discussed.

Determination of exposure multiples of human metabolites for MIST assessment in preclinical safety species without using reference standards or radiolabeled compounds.

PubMed

Ma, Shuguang; Li, Zhiling; Lee, Keun-Joong; Chowdhury, Swapan K

2010-12-20

A simple, reliable, and accurate method was developed for quantitative assessment of metabolite coverage in preclinical safety species by mixing equal volumes of human plasma with blank plasma of animal species and vice versa followed by an analysis using high-resolution full-scan accurate mass spectrometry. This approach provided comparable results (within (±15%) to those obtained from regulated bioanalysis and did not require synthetic standards or radiolabeled compounds. In addition, both qualitative and quantitative data were obtained from a single LC-MS analysis on all metabolites and, therefore, the coverage of any metabolite of interest can be obtained.

Defect scanning technology in the works

Treesearch

Philip A. Araman; R. Conners

1994-01-01

This article describes the defect scanning technology being developed by Virginia Tech and U.S. Forest Service scientists in Blacksburg, Virginia to scan full sized hardwood lumber at industrial speeds.

Accuracy, reliability, and efficiency of intraoral scanners for full-arch impressions: a systematic review of the clinical evidence.

PubMed

Goracci, Cecilia; Franchi, Lorenzo; Vichi, Alessandro; Ferrari, Marco

2016-08-01

The interest on intraoral scanners for digital impressions has been growing and new devices are continuously introduced on the market. It is timely to verify whether the several scanners proposed for full-arch digital impressions have been tested under clinical conditions for validity, repeatability, reproducibility, as well as for time efficiency, and patient acceptance. An electronic search of the literature was conducted through PubMed, Scopus, Cochrane Library, Web of Science, and Embase, entering the query terms 'digital impression', 'intraoral digital impression', 'intraoral scanning', 'intraoral scanner', 'intraoral digital scanner', combined by the Boolean operator 'OR'. No language or time limitation was applied. Only studies where digital full-arch impressions had been recorded intraorally were considered. In only eight studies full-arch scans had been performed intraorally. Only four studies reported data on validity, repeatability, reproducibility of digital measurements and their samples were limited to subjects in complete permanent dentition. Only two intraoral scanners, Lava COS and iTero, were tested. Scanning times were measured in six studies and varied largely. Patients' acceptance of intraoral scanning was evaluated in four studies, but it was not specifically assessed for children. The scientific evidence so far collected on intraoral scanning is neither exhaustive, nor up-to-date. Data from full-arch scans performed in children should be collected. For a meaningful assessment of time efficiency, agreement should be reached on the procedural steps to be included in the computation of scanning time. © The Author 2015. Published by Oxford University Press on behalf of the European Orthodontic Society. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Study of the scan uniformity from an i-CAT cone beam computed tomography dental imaging system.

PubMed

Bryant, J A; Drage, N A; Richmond, S

2008-10-01

As part of an ongoing programme to improve diagnosis and treatment planning relevant to implant placement, orthodontic treatment and dentomaxillofacial surgery, a study has been made of the spatial accuracy and density response of an i-CAT, a cone beam CT (CBCT) dental imaging system supplied by Imaging Sciences International Inc. Custom-made phantoms using acrylic sheet and water were used for measurements on spatial accuracy, density response and noise. The measurements were made over a period of several months on a clinical machine rather than on a machine dedicated to research. Measurements on a precision grid showed the spatial accuracy to be universally within the tolerance of +/-1 pixel. The density response and the noise in the data were found to depend strongly on the mass in the slice being scanned. The density response was subject to two effects. The first effect changes the whole slice uniformly and linearly depends on the total mass in the slice. The second effect exists when there is mass outside the field of view, dubbed the "exo-mass" effect. This effect lowers the measured CT number rapidly at the scan edge furthest from the exo-mass and raises it on the adjacent edge. The noise also depended quasi-linearly on the mass in the slice. Some general performance rules were drafted to describe these effects and a preliminary correction algorithm was constructed.

Effect of High-Intensity Interval Training on Total, Abdominal and Visceral Fat Mass: A Meta-Analysis.

PubMed

Maillard, Florie; Pereira, Bruno; Boisseau, Nathalie

2018-02-01

High-intensity interval training (HIIT) is promoted as a time-efficient strategy to improve body composition. The aim of this meta-analysis was to assess the efficacy of HIIT in reducing total, abdominal, and visceral fat mass in normal-weight and overweight/obese adults. Electronic databases were searched to identify all related articles on HIIT and fat mass. Stratified analysis was performed using the nature of HIIT (cycling versus running, target intensity), sex and/or body weight, and the methods of measuring body composition. Heterogeneity was also determined RESULTS: A total of 39 studies involving 617 subjects were included (mean age 38.8 years ± 14.4, 52% females). HIIT significantly reduced total (p = 0.003), abdominal (p = 0.007), and visceral (p = 0.018) fat mass, with no differences between the sexes. A comparison showed that running was more effective than cycling in reducing total and visceral fat mass. High-intensity (above 90% peak heart rate) training was more successful in reducing whole body adiposity, while lower intensities had a greater effect on changes in abdominal and visceral fat mass. Our analysis also indicated that only computed tomography scan or magnetic resonance imaging showed significant abdominal and/or visceral fat-mass loss after HIIT interventions. HIIT is a time-efficient strategy to decrease fat-mass deposits, including those of abdominal and visceral fat mass. There was some evidence of the greater effectiveness of HIIT running versus cycling, but owing to the wide variety of protocols used and the lack of full details about cycling training, further comparisons need to be made. Large, multicenter, prospective studies are required to establish the best HIIT protocols for reducing fat mass according to subject characteristics.

Novel approach in LC-MS/MS using MRM to generate a full profile of acyl-CoAs: discovery of acyl-dephospho-CoAs.

PubMed

Li, Qingling; Zhang, Shenghui; Berthiaume, Jessica M; Simons, Brigitte; Zhang, Guo-Fang

2014-03-01

A metabolomic approach to selectively profile all acyl-CoAs was developed using a programmed multiple reaction monitoring (MRM) method in LC-MS/MS and was employed in the analysis of various rat organs. The programmed MRM method possessed 300 mass ion transitions with the mass difference of 507 between precursor ion (Q1) and product ion (Q3), and the precursor ion started from m/z 768 and progressively increased one mass unit at each step. Acyl-dephospho-CoAs resulting from the dephosphorylation of acyl-CoAs were identified by accurate MS and fragmentation. Acyl-dephospho-CoAs were also quantitatively scanned by the MRM method with the mass difference of 427 between Q1 and Q3 mass ions. Acyl-CoAs and dephospho-CoAs were assayed with limits of detection ranging from 2 to 133 nM. The accuracy of the method was demonstrated by assaying a range of concentrations of spiked acyl-CoAs with the results of 80-114%. The distribution of acyl-CoAs reflects the metabolic status of each organ. The physiological role of dephosphorylation of acyl-CoAs remains to be further characterized. The methodology described herein provides a novel strategy in metabolomic studies to quantitatively and qualitatively profile all potential acyl-CoAs and acyl-dephospho-CoAs.

Validation study of an interpolation method for calculating whole lung volumes and masses from reduced numbers of CT-images in ponies.

PubMed

Reich, H; Moens, Y; Braun, C; Kneissl, S; Noreikat, K; Reske, A

2014-12-01

Quantitative computer tomographic analysis (qCTA) is an accurate but time intensive method used to quantify volume, mass and aeration of the lungs. The aim of this study was to validate a time efficient interpolation technique for application of qCTA in ponies. Forty-one thoracic computer tomographic (CT) scans obtained from eight anaesthetised ponies positioned in dorsal recumbency were included. Total lung volume and mass and their distribution into four compartments (non-aerated, poorly aerated, normally aerated and hyperaerated; defined based on the attenuation in Hounsfield Units) were determined for the entire lung from all 5 mm thick CT-images, 59 (55-66) per animal. An interpolation technique validated for use in humans was then applied to calculate qCTA results for lung volumes and masses from only 10, 12, and 14 selected CT-images per scan. The time required for both procedures was recorded. Results were compared statistically using the Bland-Altman approach. The bias ± 2 SD for total lung volume calculated from interpolation of 10, 12, and 14 CT-images was -1.2 ± 5.8%, 0.1 ± 3.5%, and 0.0 ± 2.5%, respectively. The corresponding results for total lung mass were -1.1 ± 5.9%, 0.0 ± 3.5%, and 0.0 ± 3.0%. The average time for analysis of one thoracic CT-scan using the interpolation method was 1.5-2 h compared to 8 h for analysis of all images of one complete thoracic CT-scan. The calculation of pulmonary qCTA data by interpolation from 12 CT-images was applicable for equine lung CT-scans and reduced the time required for analysis by 75%. Copyright © 2014 Elsevier Ltd. All rights reserved.

Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

USGS Publications Warehouse

Wolf, Ruth E.; Adams, Monique

2015-01-01

Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

Mass Determination of Rous Sarcoma Virus Virions by Scanning Transmission Electron Microscopy

PubMed Central

Vogt, Volker M.; Simon, Martha N.

1999-01-01

The internal structural protein of retroviruses, Gag, comprises most of the mass of the virion, and Gag itself can give rise to virus-like particles when expressed in appropriate cells. Previously the stoichiometry of Gag in virions was inferred from indirect measurements carried out 2 decades ago. We now have directly determined the masses of individual particles of the prototypic avian retrovirus, Rous sarcoma virus (RSV), by using scanning transmission electron microscopy. In this technique, the number of scattered electrons in the dark-field image integrated over an individual freeze-dried virus particle on a grid is directly proportional to its mass. The RSV virions had a mean mass of 2.5 × 108 Da, corresponding to about 1,500 Gag molecules per virion. The population of virions was not homogeneous, with about one-third to two-thirds of the virions deviating from the mean by more than 10% of the mass in two respective preparations. The mean masses for virions carrying genomes of 7.4 or 9.3 kb were indistinguishable, suggesting that mass variability is not due to differences in RNA incorporation. PMID:10400808

Characterization of metabolites of larotaxel in rat by liquid chromatography coupled with Q exactive high-resolution benchtop quadrupole orbitrap mass spectrometer.

PubMed

Liu, Zhenzhen; Hou, Pengyi; Liu, Lian; Qian, Feng

2018-03-01

1. Liquid-chromatography (LC) high-resolution (HR) mass spectrometry (MS) analysis can record HR full scans for drug metabolism studies. Larotaxel is a taxane analog that has the potential for the treatment of various types of cancer. 2. In this study, the metabolism of larotaxel was evaluated after an intravenous dose of 8 mg/kg via the caudal vein to healthy rats and its metabolites were characterized by high performance liquid chromatography coupled with a Q Exactive high-resolution benchtop quadrupole orbitrap mass spectrometer. Rat bio-samples were separated on a Capcell Pak C 18 column (2.1 i.d. × 100 mm; 2.7 μm) with mobile phase of acetonitrile and water. 3. As a result, a total of 34 metabolites were detected and identified by comparing the molecular masses, retention times and spectral patterns of the analytes with those of the parent drug. Three metabolites were confirmed by comparison with reference substances. 4. The prominent metabolites were mainly hydroxyl, dihydroxyl, trihydroxyl and 10-desacetyl analogs of larotaxel, some of which resulted from oxidation of the tert-butyl groups on the side chain and further oxidation and cyclization of the tert-butyl hydroxylated metabolites.

Structural analysis of an intact monoclonal antibody by online electrochemical reduction of disulfide bonds and Fourier transform ion cyclotron resonance mass spectrometry.

PubMed

Nicolardi, Simone; Deelder, André M; Palmblad, Magnus; van der Burgt, Yuri E M

2014-06-03

Structural confirmation and quality control of recombinant monoclonal antibodies (mAbs) by top-down mass spectrometry is still challenging due to the size of the proteins, disulfide content, and post-translational modifications such as glycosylation. In this study we have applied electrochemistry (EC) to overcome disulfide bridge complexity in top-down analysis of mAbs. To this end, an electrochemical cell was coupled directly to an electrospray ionization (ESI) source and a Fourier transform ion cyclotron resonance (FTICR) mass spectrometer (MS) equipped with a 15 T magnet. By performing online EC-assisted reduction of interchain disulfide bonds in an intact mAb, the released light chains could be selected for tandem mass spectrometry (MS/MS) analysis without interference from heavy-chain fragments. Moreover, the acquisition of full MS scans under denaturing conditions allowed profiling of all abundant mAb glycoforms. Ultrahigh-resolution FTICR-MS measurements provided fully resolved isotopic distributions of intact mAb and enabled the identification of the most abundant adducts and other interfering species. Furthermore, it was found that reduction of interchain disulfide bonds occurs in the ESI source dependent on capillary voltage and solvent composition. This phenomenon was systematically evaluated and compared with the results obtained from reduction in the electrochemical cell.

Comparative Study of Three Methods for Affinity Measurements: Capillary Electrophoresis Coupled with UV Detection and Mass Spectrometry, and Direct Infusion Mass Spectrometry

NASA Astrophysics Data System (ADS)

Mironov, Gleb G.; Logie, Jennifer; Okhonin, Victor; Renaud, Justin B.; Mayer, Paul M.; Berezovski, Maxim V.

2012-07-01

We present affinity capillary electrophoresis and mass spectrometry (ACE-MS) as a comprehensive separation technique for label-free solution-based affinity analysis. The application of ACE-MS for measuring affinity constants between eight small molecule drugs [ibuprofen, s-flurbiprofen, diclofenac, phenylbutazone, naproxen, folic acid, resveratrol, and 4,4'-(propane-1,3-diyl) dibenzoic acid] and β-cyclodextrin is described. We couple on-line ACE with MS to combine the separation and kinetic capability of ACE together with the molecular weight and structural elucidation of MS in one system. To understand the full potential of ACE-MS, we compare it with two other methods: Direct infusion mass spectrometry (DIMS) and ACE with UV detection (ACE-UV). After the evaluation, DIMS provides less reliable equilibrium dissociation constants than separation-based ACE-UV and ACE-MS, and cannot be used solely for the study of noncovalent interactions. ACE-MS determines apparent dissociation constants for all reacting small molecules in a mixture, even in cases when drugs overlap with each other during separation. The ability of ACE-MS to interact, separate, and rapidly scan through m/z can facilitate the simultaneous affinity analysis of multiple interacting pairs, potentially leading to the high-throughput screening of drug candidates.

3D laser scanning in civil engineering - measurements of volume of earth masses

NASA Astrophysics Data System (ADS)

Pawłowicz, J. A.; Szafranko, E.; Harasymiuk, J.

2018-03-01

Considering the constant drive to improve and accelerate building processes as well as possible applications of the latest technological achievements in civil engineering practice, the author has proposed to use 3D laser scanning in the construction industry. For example, data achieved through a 3D laser scanning process will facilitate making inventories of parameters of buildings in a very short time, will enable one to check irregularly shaped masses of earth, heavy and practically impossible to calculate precisely using traditional techniques. The other part of the research, performed in the laboratory, consisted of measurements of a model mound of earth. All the measurements were made with a 3D SkanStation C10 laser scanner manufactured by Leica. The data were analyzed. The results suggest that there are great opportunities for using the laser scanning technology in civil engineering

Comprehensive quantification of triacylglycerols in soybean seeds by electrospray ionization mass spectrometry with multiple neutral loss scans

DOE PAGES

Li, Maoyin; Butka, Emily; Wang, Xuemin

2014-10-10

Soybean seeds are an important source of vegetable oil and biomaterials. The content of individual triacylglycerol species (TAG) in soybean seeds is difficult to quantify in an accurate and rapid way. The present study establishes an approach to quantify TAG species in soybean seeds utilizing an electrospray ionization tandem mass spectrometry with multiple neutral loss scans. Ten neutral loss scans were performed to detect the fatty acyl chains of TAG, including palmitic (P, 1650), linolenic (Ln, 1853), linoleic (L, 1852), oleic (O, 1851), stearic (S, 1850), eicosadienoic (2052), gadoleic (2051), arachidic (2050), erucic (2251), and behenic (2250). The abundance ofmore » ten fatty acyl chains at 46 TAG masses (mass-to-charge ratio, m/z) were determined after isotopic deconvolution and correction by adjustment factors at each TAG mass. The direct sample infusion and multiple internal standards correction allowed a rapid and accurate quantification of TAG species. Ninety-three TAG species were resolved and their levels were determined.The most abundant TAG species were LLL, OLL, LLLn, PLL, OLLn, OOL, POL, and SLL. Many new species were detected and quantified. As a result, this shotgun lipidomics approach should facilitate the study of TAG metabolism and genetic breeding of soybean seeds for desirable TAG content and composition.« less

Quantitative and Qualitative Aspects of Gas-Metal-Oxide Mass Transfer in High-Temperature Confocal Scanning Laser Microscopy

NASA Astrophysics Data System (ADS)

Piva, Stephano P. T.; Pistorius, P. Chris; Webler, Bryan A.

2018-05-01

During high-temperature confocal scanning laser microscopy (HT-CSLM) of liquid steel samples, thermal Marangoni flow and rapid mass transfer between the sample and its surroundings occur due to the relatively small sample size (diameter around 5 mm) and large temperature gradients. The resulting evaporation and steel-slag reactions tend to change the chemical composition in the metal. Such mass transfer effects can change observed nonmetallic inclusions. This work quantifies oxide-metal-gas mass transfer of solutes during HT-CSLM experiments using computational simulations and experimental data for (1) dissolution of MgO inclusions in the presence and absence of slag and (2) Ca, Mg-silicate inclusion changes upon exposure of a Si-Mn-killed steel to an oxidizing gas atmosphere.

High mass resolution, high angular acceptance time-of-flight mass spectroscopy for planetary missions under the Planetary Instrument Definition and Development Program (PIDDP)

NASA Technical Reports Server (NTRS)

Young, David T.

1991-01-01

This final report covers three years and several phases of work in which instrumentation for the Planetary Instrument Definition and Development Program (PIDDP) were successfully developed. There were two main thrusts to this research: (1) to develop and test methods for electrostatically scanning detector field-of-views, and (2) to improve the mass resolution of plasma mass spectrometers to M/delta M approximately 25, their field-of-view (FOV) to 360 degrees, and their E-range to cover approximately 1 eV to 50 keV. Prototypes of two different approaches to electrostatic scanning were built and tested. The Isochronous time-of-flight (TOF) and the linear electric field 3D TOF devices were examined.

Body composition estimation from selected slices: equations computed from a new semi-automatic thresholding method developed on whole-body CT scans

PubMed Central

Villa, Chiara; Brůžek, Jaroslav

2017-01-01

Background Estimating volumes and masses of total body components is important for the study and treatment monitoring of nutrition and nutrition-related disorders, cancer, joint replacement, energy-expenditure and exercise physiology. While several equations have been offered for estimating total body components from MRI slices, no reliable and tested method exists for CT scans. For the first time, body composition data was derived from 41 high-resolution whole-body CT scans. From these data, we defined equations for estimating volumes and masses of total body AT and LT from corresponding tissue areas measured in selected CT scan slices. Methods We present a new semi-automatic approach to defining the density cutoff between adipose tissue (AT) and lean tissue (LT) in such material. An intra-class correlation coefficient (ICC) was used to validate the method. The equations for estimating the whole-body composition volume and mass from areas measured in selected slices were modeled with ordinary least squares (OLS) linear regressions and support vector machine regression (SVMR). Results and Discussion The best predictive equation for total body AT volume was based on the AT area of a single slice located between the 4th and 5th lumbar vertebrae (L4-L5) and produced lower prediction errors (|PE| = 1.86 liters, %PE = 8.77) than previous equations also based on CT scans. The LT area of the mid-thigh provided the lowest prediction errors (|PE| = 2.52 liters, %PE = 7.08) for estimating whole-body LT volume. We also present equations to predict total body AT and LT masses from a slice located at L4-L5 that resulted in reduced error compared with the previously published equations based on CT scans. The multislice SVMR predictor gave the theoretical upper limit for prediction precision of volumes and cross-validated the results. PMID:28533960

Body composition estimation from selected slices: equations computed from a new semi-automatic thresholding method developed on whole-body CT scans.

PubMed

Lacoste Jeanson, Alizé; Dupej, Ján; Villa, Chiara; Brůžek, Jaroslav

2017-01-01

Estimating volumes and masses of total body components is important for the study and treatment monitoring of nutrition and nutrition-related disorders, cancer, joint replacement, energy-expenditure and exercise physiology. While several equations have been offered for estimating total body components from MRI slices, no reliable and tested method exists for CT scans. For the first time, body composition data was derived from 41 high-resolution whole-body CT scans. From these data, we defined equations for estimating volumes and masses of total body AT and LT from corresponding tissue areas measured in selected CT scan slices. We present a new semi-automatic approach to defining the density cutoff between adipose tissue (AT) and lean tissue (LT) in such material. An intra-class correlation coefficient (ICC) was used to validate the method. The equations for estimating the whole-body composition volume and mass from areas measured in selected slices were modeled with ordinary least squares (OLS) linear regressions and support vector machine regression (SVMR). The best predictive equation for total body AT volume was based on the AT area of a single slice located between the 4th and 5th lumbar vertebrae (L4-L5) and produced lower prediction errors (|PE| = 1.86 liters, %PE = 8.77) than previous equations also based on CT scans. The LT area of the mid-thigh provided the lowest prediction errors (|PE| = 2.52 liters, %PE = 7.08) for estimating whole-body LT volume. We also present equations to predict total body AT and LT masses from a slice located at L4-L5 that resulted in reduced error compared with the previously published equations based on CT scans. The multislice SVMR predictor gave the theoretical upper limit for prediction precision of volumes and cross-validated the results.

Volumetric LiDAR scanning of a wind turbine wake and comparison with a 3D analytical wake model

NASA Astrophysics Data System (ADS)

Carbajo Fuertes, Fernando; Porté-Agel, Fernando

2016-04-01

A correct estimation of the future power production is of capital importance whenever the feasibility of a future wind farm is being studied. This power estimation relies mostly on three aspects: (1) a reliable measurement of the wind resource in the area, (2) a well-established power curve of the future wind turbines and, (3) an accurate characterization of the wake effects; the latter being arguably the most challenging one due to the complexity of the phenomenon and the lack of extensive full-scale data sets that could be used to validate analytical or numerical models. The current project addresses the problem of obtaining a volumetric description of a full-scale wake of a 2MW wind turbine in terms of velocity deficit and turbulence intensity using three scanning wind LiDARs and two sonic anemometers. The characterization of the upstream flow conditions is done by one scanning LiDAR and two sonic anemometers, which have been used to calculate incoming vertical profiles of horizontal wind speed, wind direction and an approximation to turbulence intensity, as well as the thermal stability of the atmospheric boundary layer. The characterization of the wake is done by two scanning LiDARs working simultaneously and pointing downstream from the base of the wind turbine. The direct LiDAR measurements in terms of radial wind speed can be corrected using the upstream conditions in order to provide good estimations of the horizontal wind speed at any point downstream of the wind turbine. All this data combined allow for the volumetric reconstruction of the wake in terms of velocity deficit as well as turbulence intensity. Finally, the predictions of a 3D analytical model [1] are compared to the 3D LiDAR measurements of the wind turbine. The model is derived by applying the laws of conservation of mass and momentum and assuming a Gaussian distribution for the velocity deficit in the wake. This model has already been validated using high resolution wind-tunnel measurements and large-eddy simulation (LES) data of miniature wind turbine wakes, as well as LES data of real-scale wind-turbine wakes, but not yet with full-scale wind turbine wake measurements. [1] M. Bastankhah and F. Porté-Agel. A New Analytical Model For Wind-Turbine Wakes, in Renewable Energy, vol. 70, p. 116-123, 2014.

Catalysts at work: From integral to spatially resolved X-ray absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grunwaldt, Jan-Dierk; Kimmerle, Bertram; Baiker, Alfons

2009-09-25

Spectroscopic studies on heterogeneous catalysts have mostly been done in an integral mode. However, in many cases spatial variations in catalyst structure can occur, e.g. during impregnation of pre-shaped particles, during reaction in a catalytic reactor, or in microstructured reactors as the present overview shows. Therefore, spatially resolved molecular information on a microscale is required for a comprehensive understanding of theses systems, partly in ex situ studies, partly under stationary reaction conditions and in some cases even under dynamic reaction conditions. Among the different available techniques, X-ray absorption spectroscopy (XAS) is a well-suited tool for this purpose as the differentmore » selected examples highlight. Two different techniques, scanning and full-field X-ray microscopy/tomography, are described and compared. At first, the tomographic structure of impregnated alumina pellets is presented using full-field transmission microtomography and compared to the results obtained with a scanning X-ray microbeam technique to analyse the catalyst bed inside a catalytic quartz glass reactor. On the other hand, by using XAS in scanning microtomography, the structure and the distribution of Cu(0), Cu(I), Cu(II) species in a Cu/ZnO catalyst loaded in a quartz capillary microreactor could be reconstructed quantitatively on a virtual section through the reactor. An illustrating example for spatially resolved XAS under reaction conditions is the partial oxidation of methane over noble metal-based catalysts. In order to obtain spectroscopic information on the spatial variation of the oxidation state of the catalyst inside the reactor XAS spectra were recorded by scanning with a micro-focussed beam along the catalyst bed. Alternatively, full-field transmission imaging was used to efficiently determine the distribution of the oxidation state of a catalyst inside a reactor under reaction conditions. The new technical approaches together with quantitative data analysis and an appropriate in situ catalytic experiment allowed drawing important conclusions on the reaction mechanism, and the analytical strategy might be similarly applied in other case studies. The corresponding temperature profiles and the catalytic performance were measured by means of an IR-camera and mass spectrometric analysis. In a more advanced experiment the ignition process of the partial oxidation of methane was followed in a spatiotemporal manner which demonstrates that spatially resolved spectroscopic information can even be obtained in the subsecond scale.« less

Clinical anthropometrics and body composition from 3D whole-body surface scans.

PubMed

Ng, B K; Hinton, B J; Fan, B; Kanaya, A M; Shepherd, J A

2016-11-01

Obesity is a significant worldwide epidemic that necessitates accessible tools for robust body composition analysis. We investigated whether widely available 3D body surface scanners can provide clinically relevant direct anthropometrics (circumferences, areas and volumes) and body composition estimates (regional fat/lean masses). Thirty-nine healthy adults stratified by age, sex and body mass index (BMI) underwent whole-body 3D scans, dual energy X-ray absorptiometry (DXA), air displacement plethysmography and tape measurements. Linear regressions were performed to assess agreement between 3D measurements and criterion methods. Linear models were derived to predict DXA body composition from 3D scan measurements. Thirty-seven external fitness center users underwent 3D scans and bioelectrical impedance analysis for model validation. 3D body scan measurements correlated strongly to criterion methods: waist circumference R 2 =0.95, hip circumference R 2 =0.92, surface area R 2 =0.97 and volume R 2 =0.99. However, systematic differences were observed for each measure due to discrepancies in landmark positioning. Predictive body composition equations showed strong agreement for whole body (fat mass R 2 =0.95, root mean square error (RMSE)=2.4 kg; fat-free mass R 2 =0.96, RMSE=2.2 kg) and arms, legs and trunk (R 2 =0.79-0.94, RMSE=0.5-1.7 kg). Visceral fat prediction showed moderate agreement (R 2 =0.75, RMSE=0.11 kg). 3D surface scanners offer precise and stable automated measurements of body shape and composition. Software updates may be needed to resolve measurement biases resulting from landmark positioning discrepancies. Further studies are justified to elucidate relationships between body shape, composition and metabolic health across sex, age, BMI and ethnicity groups, as well as in those with metabolic disorders.

High-grade malignant transformation of a radiation-naïve nasopharyngeal angiofibroma.

PubMed

Allensworth, Jordan J; Troob, Scott H; Lanciault, Christian; Andersen, Peter E

2016-04-01

Nasopharyngeal angiofibromas are typically considered benign vascular neoplasms, with descriptions of high-grade sarcomatous change found only in lesions with prior radiotherapy. We describe the first reported case of high-grade malignant change in a nasopharyngeal angiofibroma naive to radiation. A 45-year-old man presented with left-sided nasal congestion and fullness and was found to have a left-sided nasopharyngeal mass with intracranial extension on CT scan. A biopsy of the mass revealed nasopharyngeal angiofibroma. The patient opted for MRI surveillance, which revealed interval growth 3 years later. Decompression surgery revealed only angiofibroma, but resection 9 months later demonstrated high-grade sarcoma and concomitant angiofibroma. The patient had residual disease which progressed through chemoradiation, and is now pursuing clinical trial enrollment. Malignant transformation of nasopharyngeal angiofibroma is extremely rare. As highlighted by this report, high-grade undifferentiated lesions may arise in tumors without previous radiation. © 2016 Wiley Periodicals, Inc. Head Neck 38: E2425-E2427, 2016. © 2016 Wiley Periodicals, Inc.

DetectTLC: Automated Reaction Mixture Screening Utilizing Quantitative Mass Spectrometry Image Feature

PubMed Central

Kaddi, Chanchala D.; Bennett, Rachel V.; Paine, Martin R. L.; Banks, Mitchel D.; Weber, Arthur L.; Fernández, Facundo M.; Wang, May D.

2016-01-01

Full characterization of complex reaction mixtures is necessary to understand mechanisms, optimize yields, and elucidate secondary reaction pathways. Molecular-level information for species in such mixtures can be readily obtained by coupling mass spectrometry imaging (MSI) with thin layer chromatography (TLC) separations. User-guided investigation of imaging data for mixture components with known m/z values is generally straightforward; however, spot detection for unknowns is highly tedious, and limits the applicability of MSI in conjunction with TLC. To accelerate imaging data mining, we developed DetectTLC, an approach that automatically identifies m/z values exhibiting TLC spot-like regions in MS molecular images. Furthermore, DetectTLC can also spatially match m/z values for spots acquired during alternating high and low collision-energy scans, pairing product ions with precursors to enhance structural identification. As an example, DetectTLC is applied to the identification and structural confirmation of unknown, yet significant, products of abiotic pyrazinone and aminopyrazine nucleoside analog synthesis. PMID:26508443

A quantitative approach for pesticide analysis in grape juice by direct interfacing of a matrix compatible SPME phase to dielectric barrier discharge ionization-mass spectrometry.

PubMed

Mirabelli, Mario F; Gionfriddo, Emanuela; Pawliszyn, Janusz; Zenobi, Renato

2018-02-12

We evaluated the performance of a dielectric barrier discharge ionization (DBDI) source for pesticide analysis in grape juice, a fairly complex matrix due to the high content of sugars (≈20% w/w) and pigments. A fast sample preparation method based on direct immersion solid-phase microextraction (SPME) was developed, and novel matrix compatible SPME fibers were used to reduce in-source matrix suppression effects. A high resolution LTQ Orbitrap mass spectrometer allowed for rapid quantification in full scan mode. This direct SPME-DBDI-MS approach was proven to be effective for the rapid and direct analysis of complex sample matrices, with limits of detection in the parts-per-trillion (ppt) range and inter- and intra-day precision below 30% relative standard deviation (RSD) for samples spiked at 1, 10 and 10 ng ml -1 , with overall performance comparable or even superior to existing chromatographic approaches.

New designer drug p-methoxymethamphetamine: studies on its metabolism and toxicological detection in urine using gas chromatography-mass spectrometry.

PubMed

Staack, Roland F; Fehn, Josef; Maurer, Hans H

2003-06-05

Studies are described on the metabolism and the toxicological analysis of the new designer drug rac-p-methoxymethamphetamine (PMMA) in rat urine using gas chromatography-mass spectrometry (GC-MS). The identified metabolites indicated that PMMA was extensively metabolized mainly by O-demethylation to pholedrine and to a minor extent to p-methoxyamphetamine (PMA), 1-hydroxypholedrine diastereomers (one being oxilofrine), 4'-hydroxy-3'-methoxymethamphetamine and 4'-hydroxy-3'-methoxyamphetamine. The authors' systematic toxicological analysis (STA) procedure using full-scan GC-MS after acid hydrolysis, liquid-liquid extraction and microwave-assisted acetylation allowed the detection of the main metabolites of PMMA in rat urine after a dose corresponding to that of drug users. Therefore, this procedure should be suitable for detection of PMMA intake in human urine via its metabolites. However, it must be considered that pholedrine and oxilofrine are also in therapeutic use. Differentiation of PMMA, PMA and/or pholedrine intake is discussed.

WFC3 Micro-arcsecond astrometry of the possible SNIa progenitor BPM 71214

NASA Astrophysics Data System (ADS)

Debes, John

2012-10-01

We propose to use the newly commissioned scanning mode on WFC3 to obtain astrometric measurements of the ~0.008 AU WD/M dwarf binary BPM 71214. This system is a fascinating mystery for post-common envelope binary evolution and may be a SN1a progenitor. COS spectra of the WD in the system shows that it is rapidly rotating with a vsin i of 200 km/s, implying that it has already accreted significant mass from its companion, but mass transfer has since stopped. The COS spectra imply a near Chandrasekar mass for the WD, while optical spectroscopy suggests a mass of 0.8 M_Sun. We propose to take four orbits of WFC3 observations in scanning mode to obtain astrometric measurements of this system at a per-measurement precision of ~30~micro-arcseconds. Such measurements will definitively constrain the mass of the WD and fully solve for both masses in the binary.

Simultaneous and Sequential MS/MS Scan Combinations and Permutations in a Linear Quadrupole Ion Trap.

PubMed

Snyder, Dalton T; Szalwinski, Lucas J; Cooks, R Graham

2017-10-17

Methods of performing precursor ion scans as well as neutral loss scans in a single linear quadrupole ion trap have recently been described. In this paper we report methodology for performing permutations of MS/MS scan modes, that is, ordered combinations of precursor, product, and neutral loss scans following a single ion injection event. Only particular permutations are allowed; the sequences demonstrated here are (1) multiple precursor ion scans, (2) precursor ion scans followed by a single neutral loss scan, (3) precursor ion scans followed by product ion scans, and (4) segmented neutral loss scans. (5) The common product ion scan can be performed earlier in these sequences, under certain conditions. Simultaneous scans can also be performed. These include multiple precursor ion scans, precursor ion scans with an accompanying neutral loss scan, and multiple neutral loss scans. We argue that the new capability to perform complex simultaneous and sequential MS n operations on single ion populations represents a significant step in increasing the selectivity of mass spectrometry.

A precise measurement of the top quark mass in dilepton final states using 9.7 fb$$^{-1}$$ of D{Ø} Run II data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Huanzhao

2015-05-16

The top quark is a very special fundamental particle in the Standard Model (SM) mainly due to its heavy mass. The top quark has extremely short lifetime and decays before hadronization. This reduces the complexity for the measurement of its mass. The top quark couples very strongly to the Higgs boson since the fermion-Higgs Yukawa coupling linearly depends on the fermion’s mass. Therefore, the top quark is also heavily involved in Higgs production and related study. A precise measurement of the top quark mass is very important, as it allows for self-consistency check of the SM, and also gives a insight about the stability of our universe in the SM context. This dissertation presents my work on the measurement of the top quark mass in dilepton final states of tmore » $$\\bar{t}$$ events in p$$\\bar{p}$$ collisions at √s = 1.96 TeV, using the full DØ Run II data corresponding to an integrated luminosity of 9.7 fb -1 at the Fermilab Tevatron. I extracted the top quark mass by reconstructing event kinematics, and integrating over expected neutrino rapidity distributions to obtain solutions over a scanned range of top quark mass hypotheses. The analysis features a comprehensive optimization that I made to minimize the expected statistical uncertainty. I also improve the calibration of jets in dilepton events by using the calibration determined in t$$\\bar{t}$$ → lepton+jets events, which reduces the otherwise limiting systematic uncertainty from the jet energy scale. The measured mass is 173.11 ± 1.34(stat) +0.83 -0.72(sys) GeV .« less

The oxidation of aluminum at high temperature studied by Thermogravimetric Analysis and Differential Scanning Calorimetry.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Coker, Eric Nicholas

2013-10-01

The oxidation in air of high-purity Al foil was studied as a function of temperature using Thermogravimetric Analysis with Differential Scanning Calorimetry (TGA/DSC). The rate and/or extent of oxidation was found to be a non-linear function of the temperature. Between 650 and 750 ÀC very little oxidation took place; at 850 ÀC oxidation occurred after an induction period, while at 950 ÀC oxidation occurred without an induction period. At oxidation temperatures between 1050 and 1150 ÀC rapid passivation of the surface of the aluminum foil occurred, while at 1250 ÀC and above, an initial rapid mass increase was observed, followedmore » by a more gradual increase in mass. The initial rapid increase was accompanied by a significant exotherm. Cross-sections of oxidized specimens were characterized by scanning electron microscopy (SEM); the observed alumina skin thicknesses correlated qualitatively with the observed mass increases.« less

An efficient scan diagnosis methodology according to scan failure mode for yield enhancement

NASA Astrophysics Data System (ADS)

Kim, Jung-Tae; Seo, Nam-Sik; Oh, Ghil-Geun; Kim, Dae-Gue; Lee, Kyu-Taek; Choi, Chi-Young; Kim, InSoo; Min, Hyoung Bok

2008-12-01

Yield has always been a driving consideration during fabrication of modern semiconductor industry. Statistically, the largest portion of wafer yield loss is defective scan failure. This paper presents efficient failure analysis methods for initial yield ramp up and ongoing product with scan diagnosis. Result of our analysis shows that more than 60% of the scan failure dies fall into the category of shift mode in the very deep submicron (VDSM) devices. However, localization of scan shift mode failure is very difficult in comparison to capture mode failure because it is caused by the malfunction of scan chain. Addressing the biggest challenge, we propose the most suitable analysis method according to scan failure mode (capture / shift) for yield enhancement. In the event of capture failure mode, this paper describes the method that integrates scan diagnosis flow and backside probing technology to obtain more accurate candidates. We also describe several unique techniques, such as bulk back-grinding solution, efficient backside probing and signal analysis method. Lastly, we introduce blocked chain analysis algorithm for efficient analysis of shift failure mode. In this paper, we contribute to enhancement of the yield as a result of the combination of two methods. We confirm the failure candidates with physical failure analysis (PFA) method. The direct feedback of the defective visualization is useful to mass-produce devices in a shorter time. The experimental data on mass products show that our method produces average reduction by 13.7% in defective SCAN & SRAM-BIST failure rates and by 18.2% in wafer yield rates.

Anabolic steroids detected in bodybuilding dietary supplements - a significant risk to public health.

PubMed

Abbate, V; Kicman, A T; Evans-Brown, M; McVeigh, J; Cowan, D A; Wilson, C; Coles, S J; Walker, C J

2015-07-01

Twenty-four products suspected of containing anabolic steroids and sold in fitness equipment shops in the United Kingdom (UK) were analyzed for their qualitative and semi-quantitative content using full scan gas chromatography-mass spectrometry (GC-MS), accurate mass liquid chromatography-mass spectrometry (LC-MS), high pressure liquid chromatography with diode array detection (HPLC-DAD), UV-Vis, and nuclear magnetic resonance (NMR) spectroscopy. In addition, X-ray crystallography enabled the identification of one of the compounds, where reference standard was not available. Of the 24 products tested, 23 contained steroids including known anabolic agents; 16 of these contained steroids that were different to those indicated on the packaging and one product contained no steroid at all. Overall, 13 different steroids were identified; 12 of these are controlled in the UK under the Misuse of Drugs Act 1971. Several of the products contained steroids that may be considered to have considerable pharmacological activity, based on their chemical structures and the amounts present. This could unwittingly expose users to a significant risk to their health, which is of particular concern for naïve users. Copyright © 2014 John Wiley & Sons, Ltd.

Structural Characterization of New Peptide Variants Produced by Cyanobacteria from the Brazilian Atlantic Coastal Forest Using Liquid Chromatography Coupled to Quadrupole Time-of-Flight Tandem Mass Spectrometry

PubMed Central

Sanz, Miriam; Andreote, Ana Paula Dini; Fiore, Marli Fatima; Dörr, Felipe Augusto; Pinto, Ernani

2015-01-01

Cyanobacteria from underexplored and extreme habitats are attracting increasing attention in the search for new bioactive substances. However, cyanobacterial communities from tropical and subtropical regions are still largely unknown, especially with respect to metabolite production. Among the structurally diverse secondary metabolites produced by these organisms, peptides are by far the most frequently described structures. In this work, liquid chromatography/electrospray ionization coupled to high resolution quadrupole time-of-flight tandem mass spectrometry with positive ion detection was applied to study the peptide profile of a group of cyanobacteria isolated from the Southeastern Brazilian coastal forest. A total of 38 peptides belonging to three different families (anabaenopeptins, aeruginosins, and cyanopeptolins) were detected in the extracts. Of the 38 peptides, 37 were detected here for the first time. New structural features were proposed based on mass accuracy data and isotopic patterns derived from full scan and MS/MS spectra. Interestingly, of the 40 surveyed strains only nine were confirmed to be peptide producers; all of these strains belonged to the order Nostocales (three Nostoc sp., two Desmonostoc sp. and four Brasilonema sp.). PMID:26096276

Molecular Ionization-Desorption Analysis Source (MIDAS) for Mass Spectrometry: Thin-Layer Chromatography.

PubMed

Winter, Gregory T; Wilhide, Joshua A; LaCourse, William R

2016-02-01

Molecular ionization-desorption analysis source (MIDAS), which is a desorption atmospheric pressure chemical ionization (DAPCI) type source, for mass spectrometry has been developed as a multi-functional platform for the direct sampling of surfaces. In this article, its utility for the analysis of thin-layer chromatography (TLC) plates is highlighted. Amino acids, which are difficult to visualize without staining reagents or charring, were detected and identified directly from a TLC plate. To demonstrate the full potential of MIDAS, all active ingredients from an analgesic tablet, separated on a TLC plate, were successfully detected using both positive and negative ion modes. The identity of each of the compounds was confirmed from their mass spectra and compared against standards. Post separation, the chemical signal (blue permanent marker) as reference marks placed at the origin and solvent front were used to calculate retention factor (Rf) values from the resulting ion chromatogram. The quantitative capabilities of the device were exhibited by scanning caffeine spots on a TLC plate of increasing sample amount. A linear curve based on peak are, R2 = 0.994, was generated for seven spots ranging from 50 to 1000 ng of caffeine per spot.

Molecular Ionization-Desorption Analysis Source (MIDAS) for Mass Spectrometry: Thin-Layer Chromatography

NASA Astrophysics Data System (ADS)

Winter, Gregory T.; Wilhide, Joshua A.; LaCourse, William R.

2016-02-01

Molecular ionization-desorption analysis source (MIDAS), which is a desorption atmospheric pressure chemical ionization (DAPCI) type source, for mass spectrometry has been developed as a multi-functional platform for the direct sampling of surfaces. In this article, its utility for the analysis of thin-layer chromatography (TLC) plates is highlighted. Amino acids, which are difficult to visualize without staining reagents or charring, were detected and identified directly from a TLC plate. To demonstrate the full potential of MIDAS, all active ingredients from an analgesic tablet, separated on a TLC plate, were successfully detected using both positive and negative ion modes. The identity of each of the compounds was confirmed from their mass spectra and compared against standards. Post separation, the chemical signal (blue permanent marker) as reference marks placed at the origin and solvent front were used to calculate retention factor (Rf) values from the resulting ion chromatogram. The quantitative capabilities of the device were exhibited by scanning caffeine spots on a TLC plate of increasing sample amount. A linear curve based on peak are, R2 = 0.994, was generated for seven spots ranging from 50 to 1000 ng of caffeine per spot.

Recurrent pulmonary embolism due to echinococcosis secondary to hepatic surgery for hydatid cysts.

PubMed

Damiani, Mario Francesco; Carratù, Pierluigi; Tatò, Ilaria; Vizzino, Heleanna; Florio, Carlo; Resta, Onofrio

2012-01-01

We describe the case of a 53-year-old man with recurrent pulmonary embolism due to intra-arterial cysts from Echinococcus. Both the patient's medical history and the computed tomographic (CT) scan abnormalities led to the diagnosis. The CT scan, performed during hospitalization in our ward, showed cystic masses in the left main pulmonary artery and in the descending branch of the right pulmonary artery. Within cystic masses, thin septa were visible, giving a chambered appearance, which was suggestive of a group of daughter cysts. In the past, our patient underwent multiple operations for recurring echinococcal cysts of the liver. After the last intervention, 4 years earlier, his postoperative course was complicated by pulmonary embolism: a CT scan showed a filling defect in the descending branch of the right pulmonary artery, which was caused by the same cystic mass as 4 years later, although smaller. This mass, not properly treated, increased in diameter. Moreover, after 4 years, there has been a new episode of embolism, which involved the left main pulmonary artery. This is the first case in which there are repeated episodes of pulmonary embolism echinococcosis after hepatic surgery for removal of hydatid cysts.

Background correction in separation techniques hyphenated to high-resolution mass spectrometry - Thorough correction with mass spectrometry scans recorded as profile spectra.

PubMed

Erny, Guillaume L; Acunha, Tanize; Simó, Carolina; Cifuentes, Alejandro; Alves, Arminda

2017-04-07

Separation techniques hyphenated with high-resolution mass spectrometry have been a true revolution in analytical separation techniques. Such instruments not only provide unmatched resolution, but they also allow measuring the peaks accurate masses that permit identifying monoisotopic formulae. However, data files can be large, with a major contribution from background noise and background ions. Such unnecessary contribution to the overall signal can hide important features as well as decrease the accuracy of the centroid determination, especially with minor features. Thus, noise and baseline correction can be a valuable pre-processing step. The methodology that is described here, unlike any other approach, is used to correct the original dataset with the MS scans recorded as profiles spectrum. Using urine metabolic studies as examples, we demonstrate that this thorough correction reduces the data complexity by more than 90%. Such correction not only permits an improved visualisation of secondary peaks in the chromatographic domain, but it also facilitates the complete assignment of each MS scan which is invaluable to detect possible comigration/coeluting species. Copyright © 2017 Elsevier B.V. All rights reserved.

Automated tandem mass spectrometry by orthogonal acceleration TOF data acquisition and simultaneous magnet scanning for the characterization of petroleum mixtures.

PubMed

Roussis, S G

2001-08-01

The automated acquisition of the product ion spectra of all precursor ions in a selected mass range by using a magnetic sector/orthogonal acceleration time-of-flight (oa-TOF) tandem mass spectrometer for the characterization of complex petroleum mixtures is reported. Product ion spectra are obtained by rapid oa-TOF data acquisition and simultaneous scanning of the magnet. An analog signal generator is used for the scanning of the magnet. Slow magnet scanning rates permit the accurate profiling of precursor ion peaks and the acquisition of product ion spectra for all isobaric ion species. The ability of the instrument to perform both high- and low-energy collisional activation experiments provides access to a large number of dissociation pathways useful for the characterization of precursor ions. Examples are given that illustrate the capability of the method for the characterization of representative petroleum mixtures. The structural information obtained by the automated MS/MS experiment is used in combination with high-resolution accurate mass measurement results to characterize unknown components in a polar extract of a refinery product. The exhaustive mapping of all precursor ions in representative naphtha and middle-distillate fractions is presented. Sets of isobaric ion species are separated and their structures are identified by interpretation from first principles or by comparison with standard 70-eV EI libraries of spectra. The utility of the method increases with the complexity of the samples.

Simultaneous quantification of paeoniflorin, nobiletin, tangeretin, liquiritigenin, isoliquiritigenin, liquiritin and formononetin from Si-Ni-San extract in rat plasma and tissues by liquid chromatography-tandem mass spectrometry.

PubMed

Li, Tianxue; Yan, Zhixiang; Zhou, Chen; Sun, Jian; Jiang, Chuan; Yang, Xinghao

2013-08-01

In this study, a sensitive and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of seven bioactive components including paeoniflorin, nobiletin, tangeretin, liquiritigenin, isoliquiritigenin, liquiritin and formononetin in rat plasma and tissues after oral administration of Si-Ni-San extract using astragaloside IV as internal standard (IS). The plasma and tissue samples were extracted by solid-phase extraction. Chromatographic separation was accomplished on a C18 column with a multiple-step gradient elution. The quantification was obtained by scanning with multiple reaction monitoring via an electrospray ionization source that was operated by switching between the positive and negative modes in two MS/MS scan segments. Full validation of the assay was implemented. In conclusion, this method demonstrated good linearity and specificity. The lower limits of quantification for the analytes were <7.5 ng/mL. Intra- and inter-day precisions (RSD) were <12.5% and accuracy (RE) ranged from -10.2 to 7.3%. The average recoveries of the analytes from rat plasma and tissues were >65.2% and 58.6%, respectively. The validated method was further applied to the determination of actual rat plasma and tissues after oral administration of Si-Ni-San extract. The results provided a meaningful basis for the clinical application of this prescription. Copyright © 2013 John Wiley & Sons, Ltd.

Studies on the metabolism of five model drugs by fungi colonizing cadavers using LC-ESI-MS/MS and GC-MS analysis.

PubMed

Martínez-Ramírez, Jorge A; Voigt, Kerstin; Peters, Frank T

2012-09-01

It is well-known that cadavers may be colonized by microorganisms, but there is limited information if or to what extent these microbes are capable of metabolizing drugs or poisons, changing the concentrations and metabolic pattern of such compounds in postmortem samples. The aim of the present study was to develop a fungal biotransformation system as an in vitro model to investigate potential postmortem metabolism by fungi. Five model drugs (amitriptyline, metoprolol, mirtazapine, promethazine, and zolpidem) were each incubated with five model fungi known to colonize cadavers (Absidia repens, Aspergillus repens, Aspergillus terreus, Gliocladium viride, and Mortierella polycephala) and with Cunninghamella elegans (positive control). Incubations were performed in Sabouraud medium at 25 °C for 5 days. After centrifugation, a part of the supernatants was analyzed by liquid chromatography-tandem mass spectrometry with product ion scanning. Another part was analyzed by full scan gas chromatography-mass spectrometry after extraction and derivatization. All model drugs were metabolized by the control fungus resulting in two (metoprolol) to ten (amitriptyline) metabolites. Of the model fungi, only Abs. repens and M. polycephala metabolized the model drugs: amitriptyline was metabolized to six and five, metoprolol to two and two, mirtazapine to five and three, promethazine to six and nine, and zolpidem to three and four metabolites, respectively. The main metabolic reactions were demethylation, oxidation, and hydroxylation. The presented in vitro model is applicable to studying drug metabolism by fungi colonizing cadavers.

Three-step HPLC-ESI-MS/MS procedure for screening and identifying non-target flavonoid derivatives

NASA Astrophysics Data System (ADS)

Rak, Gábor; Fodor, Péter; Abrankó, László

2010-02-01

A three-step HPLC-ESI-MS/MS procedure is designed for screening and identification of non-target flavonoid derivatives of selected flavonoid aglycones. In this method the five commonly appearing aglycones (apigenin, luteolin, myricetin, naringenin and quercetin) were selected. The method consists of three individual mass spectrometric experiments of which the first two were implemented within a single chromatographic acquisition. The third step was carried out during a replicate chromatographic run using the same RP-HPLC conditions. The first step, a multiple reaction monitoring (MRM) scan of the aglycones was performed to define the number of derivatives relating to the selected aglycones. For this purpose the characteristic aglycone parts of the unknowns were used as specific tags of the molecules, which were generated as in-source fragments. Secondly, a full scan MS experiment is performed to identify the masses of the potential derivatives of the selected aglycones. Finally, the third step had the capability to confirm the supposed derivatives. The developed method was applied to a commercially available black currant juice to demonstrate its capability to detect and identify various flavonoid glycosides without any preliminary information about their presence in the sample. As a result 13 compounds were detected and identified in total. Namely, 3 different myricetin glycosides and the myricetin aglycone 2 luteolin glycosides plus the aglycone and 3 quercetin glycosides plus the aglycone could be identified from the tested black currant sample. In the case of apigenin and naringenin only the aglycones could be detected.

Diagnostic performance of shear wave elastography of the breast according to scanning orientation.

PubMed

Kim, Solip; Choi, SeonHyeong; Choi, Yoonjung; Kook, Shin-Ho; Park, Hee Jin; Chung, Eun Chul

2014-10-01

To evaluate the influence of the scanning orientation on diagnostic performance measured by the mean elasticity, maximum elasticity, and fat-to-lesion elasticity ratio on ultrasound-based shear wave elastography in differentiating breast cancers from benign lesions. In this study, a total of 260 breast masses from 235 consecutive patients were observed from March 2012 to November 2012. For each lesion, the mean elasticity value, maximum elasticity value, and fat-to-lesion ratio were measured along two orthogonal directions, and all values were compared with pathologic results. There were 59 malignant and 201 benign lesions. Malignant masses showed higher mean elasticity, maximum elasticity, and fat-to-lesion ratio values than benign lesions (P < .0001). The areas under the receiver operating characteristic curves were as follows: average mean elasticity on both views, 0.870; mean elasticity on the transverse view, 0.866; maximum elasticity on both views, 0.865; maximum elasticity on the transverse view, 0.864; mean elasticity on the longitudinal view, 0.849; fat-to-lesion ratio on both views, 0.849; maximum elasticity on the longitudinal view, 0.845; fat-to-lesion ratio on the transverse view, 0.841; and fat-to-lesion ratio on the longitudinal view, 0.814. Intraclass correlation coefficients for agreement between the scanning directions were as follows: mean elasticity, 0.852; maximum elasticity, 0.842; fat-to-lesion ratio, 0.746, for masses; and mean elasticity, 0.392, for anterior mammary fat. Mean elasticity, maximum elasticity, and fat-to-lesion elasticity ratio values were helpful in differentiating benign and malignant breast masses. The scanning orientation did not significantly affect the diagnostic performance of shear wave elastography for breast masses. © 2014 by the American Institute of Ultrasound in Medicine.

Evaluating Mass Analyzers as Candidates for Small, Portable, Rugged Single Point Mass Spectrometers for Analysis of Permanent Gases

NASA Technical Reports Server (NTRS)

Arkin, C. Richard; Ottens, Andrew K.; Diaz, Jorge A.; Griffin, Timothy P.; Follestein, Duke; Adams, Fredrick; Steinrock, T. (Technical Monitor)

2001-01-01

For Space Shuttle launch safety, there is a need to monitor the concentration of H2, He, O2 and Ar around the launch vehicle. Currently a large mass spectrometry system performs this task, using long transport lines to draw in samples. There is great interest in replacing this stationary system with several miniature, portable, rugged mass spectrometers which act as point sensors which can be placed at the sampling point. Five commercial and two non-commercial analyzers are evaluated. The five commercial systems include the Leybold Inficon XPR-2 linear quadrupole, the Stanford Research (SRS-100) linear quadrupole, the Ferran linear quadrupole array, the ThermoQuest Polaris-Q quadrupole ion trap, and the IonWerks Time-of-Flight (TOF). The non-commercial systems include a compact double focusing sector (CDFMS) developed at the University of Minnesota, and a quadrupole ion trap (UF-IT) developed at the University of Florida. The System Volume is determined by measuring the entire system volume including the mass analyzer, its associated electronics, the associated vacuum system, the high vacuum pump and rough pump. Also measured are any ion gauge controllers or other required equipment. Computers are not included. Scan Time is the time required for one scan to be acquired and the data to be transferred. It is determined by measuring the time required acquiring a known number of scans and dividing by said number of scans. Limit of Detection is determined first by performing a zero-span calibration (using a 10-point data set). Then the limit of detection (LOD) is defined as 3 times the standard deviation of the zero data set. (An LOD of 10 ppm or less is considered acceptable.)

Goddard Conference on Mass Storage Systems and Technologies, Volume 1

NASA Technical Reports Server (NTRS)

Kobler, Ben (Editor); Hariharan, P. C. (Editor)

1993-01-01

Copies of nearly all of the technical papers and viewgraphs presented at the Goddard Conference on Mass Storage Systems and Technologies held in Sep. 1992 are included. The conference served as an informational exchange forum for topics primarily relating to the ingestion and management of massive amounts of data and the attendant problems (data ingestion rates now approach the order of terabytes per day). Discussion topics include the IEEE Mass Storage System Reference Model, data archiving standards, high-performance storage devices, magnetic and magneto-optic storage systems, magnetic and optical recording technologies, high-performance helical scan recording systems, and low end helical scan tape drives. Additional topics addressed the evolution of the identifiable unit for processing purposes as data ingestion rates increase dramatically, and the present state of the art in mass storage technology.

The characteristics of dose at mass interface on lung cancer Stereotactic Body Radiotherapy (SBRT) simulation

NASA Astrophysics Data System (ADS)

Wulansari, I. H.; Wibowo, W. E.; Pawiro, S. A.

2017-05-01

In lung cancer cases, there exists a difficulty for the Treatment Planning System (TPS) to predict the dose at or near the mass interface. This error prediction might influence the minimum or maximum dose received by lung cancer. In addition to target motion, the target dose prediction error also contributes in the combined error during the course of treatment. The objective of this work was to verify dose plan calculated by adaptive convolution algorithm in Pinnacle3 at the mass interface against a set of measurement. The measurement was performed using Gafchromic EBT 3 film in static and dynamic CIRS phantom with amplitudes of 5 mm, 10 mm, and 20 mm in superior-inferior motion direction. Static and dynamic phantom were scanned with fast CT and slow CT before planned. The results showed that adaptive convolution algorithm mostly predicted mass interface dose lower than the measured dose in a range of -0,63% to 8,37% for static phantom in fast CT scanning and -0,27% to 15,9% for static phantom in slow CT scanning. In dynamic phantom, this algorithm was predicted mass interface dose higher than measured dose up to -89% for fast CT and varied from -17% until 37% for slow CT. This interface of dose differences caused the dose mass decreased in fast CT, except for 10 mm motion amplitude, and increased in slow CT for the greater amplitude of motion.

Reversible suprasellar pituitary mass secondary to hypothyroidism

DOE Office of Scientific and Technical Information (OSTI.GOV)

Atchison, J.A.; Lee, P.A.; Albright, A.L.

1989-12-08

Sellar enlargement and suprasellar extension of a pituitary mass, demonstrated by magnetic resonance imaging or computed tomographic scanning in three children with primary hypothyroidism, resolved after treatment with levothyroxine sodium. This condition, a logical consequence of the pathogenesis of primary hypothyroidism, must be considered in patients with pituitary and suprasellar masses.

Airport full-body screening: what is the risk?

PubMed

Mehta, Pratik; Smith-Bindman, Rebecca

2011-06-27

In the past year, the Transportation Security Administration has deployed full-body scanners in airports across the United States in response to heightened security needs. Several groups have opposed the scans, citing privacy concerns and fear of the radiation emitted by the backscatter x-ray scanners, 1 of the 2 types of machines in use. The radiation doses emitted by the scans are extremely small; the scans deliver an amount of radiation equivalent to 3 to 9 minutes of the radiation received through normal daily living. Furthermore, since flying itself increases exposure to ionizing radiation, the scan will contribute less than 1% of the dose a flyer will receive from exposure to cosmic rays at elevated altitudes. The estimation of cancer risks associated with these scans is difficult, but using the only available models, the risk would be extremely small, even among frequent flyers. We conclude that there is no significant threat of radiation from the scans.

Unravelling associations between unassigned mass spectrometry peaks with frequent itemset mining techniques.

PubMed

Vu, Trung Nghia; Mrzic, Aida; Valkenborg, Dirk; Maes, Evelyne; Lemière, Filip; Goethals, Bart; Laukens, Kris

2014-01-01

Mass spectrometry-based proteomics experiments generate spectra that are rich in information. Often only a fraction of this information is used for peptide/protein identification, whereas a significant proportion of the peaks in a spectrum remain unexplained. In this paper we explore how a specific class of data mining techniques termed "frequent itemset mining" can be employed to discover patterns in the unassigned data, and how such patterns can help us interpret the origin of the unexpected/unexplained peaks. First a model is proposed that describes the origin of the observed peaks in a mass spectrum. For this purpose we use the classical correlative database search algorithm. Peaks that support a positive identification of the spectrum are termed explained peaks. Next, frequent itemset mining techniques are introduced to infer which unexplained peaks are associated in a spectrum. The method is validated on two types of experimental proteomic data. First, peptide mass fingerprint data is analyzed to explain the unassigned peaks in a full scan mass spectrum. Interestingly, a large numbers of experimental spectra reveals several highly frequent unexplained masses, and pattern mining on these frequent masses demonstrates that subsets of these peaks frequently co-occur. Further evaluation shows that several of these co-occurring peaks indeed have a known common origin, and other patterns are promising hypothesis generators for further analysis. Second, the proposed methodology is validated on tandem mass spectrometral data using a public spectral library, where associations within the mass differences of unassigned peaks and peptide modifications are explored. The investigation of the found patterns illustrates that meaningful patterns can be discovered that can be explained by features of the employed technology and found modifications. This simple approach offers opportunities to monitor accumulating unexplained mass spectrometry data for emerging new patterns, with possible applications for the development of mass exclusion lists, for the refinement of quality control strategies and for a further interpretation of unexplained spectral peaks in mass spectrometry and tandem mass spectrometry.

A systematic review of presacral extramedullary haematopoiesis: a diagnosis to be considered for presacral masses.

PubMed

Zhou, P P; Clark, E; Kapadia, M R

2016-11-01

Presacral masses are uncommon and have malignant potential; treatment typically includes surgical excision. However, there are conditions such as extramedullary haematopoiesis (EMH) which are benign. The present study aimed to summarize the presentation of presacral EMH in our institution, to review the literature and to offer management strategies for this rare condition. The literature was searched for articles related to presacral EMH, and case reports were collected from articles meeting the inclusion criteria. We collected data on patient demographics, diagnostic investigation, management and the results of treatment. Thirty-nine patients were included in the systematic review. Initial imaging included computed tomography (CT), magnetic resonance imaging (MRI) or ultrasound (US) suggestive of EMH. Some patients then underwent a technetium scan (n = 7, 18%), biopsy of the presacral lesion (n = 27, 69%) or excision of the entire mass (n = 3, 8%). All patients who underwent technetium scan were confirmed to have EMH, demonstrating enhancement similar to bone marrow. Patients who underwent technetium scan and presacral mass biopsy had concordant results confirming presacral EMH (n = 5, 13%). Data on management were available for 35/39 (90%) with most patients followed by clinical observation (n = 20, 51%). Symptomatic patients were treated with radiotherapy (15%), surgical excision (15%) or hydroxyurea (5%) and blood transfusions (10%). Most (81%, n = 17/21) patients whose outcome was reported remained asymptomatic or experienced pain relief. Although uncommon, EMH should be considered in the differential diagnosis of a presacral mass. Presacral EMH is a benign condition that can be suspected on CT or MRI and confirmed with technetium scan. Patients may not necessarily need to undergo biopsy to confirm haematopoietic elements. Unlike other presacral masses, patients diagnosed with presacral EMH can be managed by observation. If symptomatic, radiotherapy or surgical excision may be offered. Colorectal Disease © 2016 The Association of Coloproctology of Great Britain and Ireland.

Options for veterinary drug analysis using mass spectrometry.

PubMed

Le Bizec, Bruno; Pinel, Gaud; Antignac, Jean-Philippe

2009-11-13

Several classes of chemical compounds, exhibiting many different chemical properties, are classified under the generic term of "veterinary drugs", among which are the antimicrobial medicines such as antibiotics or dyes, and drugs exhibiting growth promoting properties like steroids, beta-agonist compounds, thyrostats or growth hormones. For food safety purposes, the resort to these substances in animal breeding has been submitted to strict regulation within the European Union for more than 15 years. Systems of control have therefore been set up within the same period of time to ensure compliance with the regulation. The current strategy relies on targeted analytical approaches focusing on the detection of residues of the administered compounds or their metabolites in different kinds of feed, food or biological matrices. If screening methods, which provide rapid discrimination between compliant and suspect samples, may be based on several techniques such as immunoassays or mass spectrometry, confirmatory methods mainly rely on the latter, which provides adequate specificity and sensitivity for unambiguous identification of the target analytes in biological matrices at trace level. The present article reviews the main mass spectrometric strategies, from the very first, nonetheless still efficient, single MS and multidimensional and high-resolution MS through to advanced isotope ratio MS. Several applications in the field of residue analysis illustrate each of these approaches and focus on the balance between issues related to the compounds of interest (chemistry, matrix, concentration, ...) and the large offer of mass spectrometric-related technical possibilities, from the choice of the ionization conditions (EI, NCI, PCI, reagent gases, ESI+, ESI-), to the mass analyzers (single quadrupole, triple quadrupole, ion traps, time-of-flight, magnetic sectors, isotope ratio mass spectrometer) and corresponding acquisition modes (full scan, LR-SIM, HR-SIM, SRM, precursor scan, ...). All the displayed strategies, from the importance of sample preparation to MS analysis to potential derivatization steps and chromatographic separation parameters are discussed in that context. Besides the advantages of each strategy, main issues associated to such MS approaches are commented with an emphasis not only on such critical points as ion suppression and resolution, but also on the adequacy of the current regulation regarding the evolution of the technology. Finally, future trends which may lead to strong and positive impacts in the field of residue analysis are presented, including latest developments and improvements in chromatography or software dedicated to signal acquisition and data analysis.

Scanning transmission ion microscopy mass measurements for quantitative trace element analysis within biological samples and validation using atomic force microscopy thickness measurements

NASA Astrophysics Data System (ADS)

Devès, Guillaume; Cohen-Bouhacina, Touria; Ortega, Richard

2004-10-01

We used the nuclear microprobe techniques, micro-PIXE (particle-induced X-ray emission), micro-RBS (Rutherford backscattering spectrometry) and scanning transmission ion microscopy (STIM) in order to perform the characterization of trace element content and spatial distribution within biological samples (dehydrated cultured cells, tissues). The normalization of PIXE results was usually expressed in terms of sample dry mass as determined by micro-RBS recorded simultaneously to micro-PIXE. However, the main limit of RBS mass measurement is the sample mass loss occurring during irradiation and which could be up to 30% of the initial sample mass. We present here a new methodology for PIXE normalization and quantitative analysis of trace element within biological samples based on dry mass measurement performed by mean of STIM. The validation of STIM cell mass measurements was obtained in comparison with AFM sample thickness measurements. Results indicated the reliability of STIM mass measurement performed on biological samples and suggested that STIM should be performed for PIXE normalization. Further information deriving from direct confrontation of AFM and STIM analysis could as well be obtained, like in situ measurements of cell specific gravity within cells compartment (nucleolus and cytoplasm).

Identification of the chemical components of Saussurea involucrata by high-resolution mass spectrometry and the mass spectral trees similarity filter technique.

PubMed

Jia, Zhixin; Wu, Caisheng; Jin, Hongtao; Zhang, Jinlan

2014-11-15

Saussurea involucrata is a rare traditional Chinese medicine (TCM) that displays anti-fatigue, anti-inflammatory and anti-tumor effects. In this paper, the different chemical components of Saussurea involucrata were characterized and identified over a wide dynamic range by high-performance liquid chromatography coupled with high-resolution hybrid mass spectrometry (HPLC/HRMS/MS(n)) and the mass spectral trees similarity filter (MTSF) technique. The aerial parts of Saussurea involucrata were extracted with 75% ethanol. The partial extract was separated on a chromatography column to concentrate the low-concentration compounds. Mass data were acquired using full-scan mass analysis (resolving power 50,000) with data-dependent incorporation of dynamic exclusion analysis. The identified compounds were used as templates to construct a database of mass spectral trees. Data for the unknown compounds were matched with those templates and matching candidate structures were obtained. The detected compounds were characterized based on matching to candidate structures by the MTSF technique and were further identified by their accurate mass weight, multiple-stage analysis and fragmentation patterns and through comparison with literature data. A total of 38 compounds were identified including 19 flavones, 11 phenylpropanoids and 8 sphingolipids. Among them, 7 flavonoids, 8 phenylpropanoids and 8 sphingolipids were identified for the first time in Saussurea involucrata. HPLC/HRMS/MS(n) combined with MTSF was successfully used to discover and identify the chemical compounds in Saussurea involucrata. The results indicated that this combined technique was extremely useful for the rapid detection and identification of the chemical components in TCMs. Copyright © 2014 John Wiley & Sons, Ltd.

Comparison of bioimpedance analysis scan, hemoglobin and urea reduction ratio in hemodialysis patients following and not following monitoring program for improving quality of life

NASA Astrophysics Data System (ADS)

Muzasti, R. A.; Lubis, H. R.

2018-03-01

Hemodialysis (HD) is the renal replacement therapy in end-stage renal disease (ESRD), at least 2-3 times a week, impacting substantial changes in daily life. Therefore a monitoring program is needed to improve the quality of life (QoL) of HD patients. Indicators in monitoring QoL include phase angle (PhA), muscle and fat mass, and body fluid composition through Bio Scan impedance analysis (BIA) Scan, hemoglobin level, and urea reduction ratio (URR). An analytic study with the cross-sectional design was performed in 168 patients at Klinik Spesialis Ginjal Hipertensi (KSGH) Rasyida, Medan to compare BIA Scan profiles, hemoglobin levels, and URR in HD patients who follow and do not follow the monitoring program for improving QoL {Program Pemantauan Peningkatan Kualitas Hidup (P3KH)}. Each variable was analyzed by independent T-test, it is significant if p <0.05. This study showed that there were differences in BMI (p = 0.006), fat mass (p = 0.010), extracellular water / intracellular water (ECW / ICW) (p = 0.046), and haemoglobin p = 0.001). Although it was better in the program group, statistically there was no difference of PhA (p = 0.136), muscle mass (p = 0.842), and URR (p = 0.232).

Can a Single Sagittal Magnetic Resonance Imaging Slice Represent Whole Fatty Infiltration in Chronic Rotator Cuff Tears at the Supraspinatus?

PubMed

Lee, Yong-Beom; Yang, Cheol-Jung; Li, Cheng Zhen; Zhuan, Zhong; Kwon, Seung-Cheol; Noh, Kyu-Cheol

2018-03-01

This study aimed to investigate whether fatty infiltration (FI) measured on a single sagittal magnetic resonance imaging (MRI) slice can represent FI of the whole supraspinatus muscle. This study retrospectively reviewed the MRIs of 106 patients (age 50-79 years) divided into three rotator cuff tear-size groups: medium, large, and massive. Fat mass and muscle mass on all T1-weighted sagittal MRI scans (FA and MA) were measured. Of the total MRI scans, the Y-view was defined as the most lateral image of the junction of the scapular spine with the scapular body on the oblique sagittal T1-weighted image. Fat mass and muscle mass seen on this Y-view single slice were recorded as F1 and M1, respectively. Fat mass and muscle mass were also assessed on MRI scans lateral and medial to the Y-view. The means of fat mass and muscle mass on these three slices were recorded as F3 and M3, respectively. Average FI ratios (fat mass/muscle mass) of the three assessment methods (F1/M1, FA/MA, and F3/M3) were compared. Intraclass correlation coefficients (ICCs) were calculated for inter- and intraobserver reliability. ICCs showed higher reliability (> 0.8) for all measurements. F1/M1 values were not statistically different from FA/MA and F3/M3 values ( p > 0.05), except in males with medium and large tears. F3/M3 and FA/MA were not statistically different. The difference between F1/M1 and FA/MA did not exceed 2%. A single sagittal MRI slice can represent the whole FI in chronic rotator cuff tears, except in some patient groups. We recommend measurement of FI using a single sagittal MRI slice, given the effort required for repeated measurements.

Can a Single Sagittal Magnetic Resonance Imaging Slice Represent Whole Fatty Infiltration in Chronic Rotator Cuff Tears at the Supraspinatus?

PubMed Central

Lee, Yong-Beom; Yang, Cheol-Jung; Li, Cheng Zhen; Zhuan, Zhong; Kwon, Seung-Cheol

2018-01-01

Background This study aimed to investigate whether fatty infiltration (FI) measured on a single sagittal magnetic resonance imaging (MRI) slice can represent FI of the whole supraspinatus muscle. Methods This study retrospectively reviewed the MRIs of 106 patients (age 50–79 years) divided into three rotator cuff tear-size groups: medium, large, and massive. Fat mass and muscle mass on all T1-weighted sagittal MRI scans (FA and MA) were measured. Of the total MRI scans, the Y-view was defined as the most lateral image of the junction of the scapular spine with the scapular body on the oblique sagittal T1-weighted image. Fat mass and muscle mass seen on this Y-view single slice were recorded as F1 and M1, respectively. Fat mass and muscle mass were also assessed on MRI scans lateral and medial to the Y-view. The means of fat mass and muscle mass on these three slices were recorded as F3 and M3, respectively. Average FI ratios (fat mass/muscle mass) of the three assessment methods (F1/M1, FA/MA, and F3/M3) were compared. Intraclass correlation coefficients (ICCs) were calculated for inter- and intraobserver reliability. Results ICCs showed higher reliability (> 0.8) for all measurements. F1/M1 values were not statistically different from FA/MA and F3/M3 values (p > 0.05), except in males with medium and large tears. F3/M3 and FA/MA were not statistically different. The difference between F1/M1 and FA/MA did not exceed 2%. Conclusions A single sagittal MRI slice can represent the whole FI in chronic rotator cuff tears, except in some patient groups. We recommend measurement of FI using a single sagittal MRI slice, given the effort required for repeated measurements. PMID:29564048

Accuracy in Dental Medicine, A New Way to Measure Trueness and Precision

PubMed Central

Ender, Andreas; Mehl, Albert

2014-01-01

Reference scanners are used in dental medicine to verify a lot of procedures. The main interest is to verify impression methods as they serve as a base for dental restorations. The current limitation of many reference scanners is the lack of accuracy scanning large objects like full dental arches, or the limited possibility to assess detailed tooth surfaces. A new reference scanner, based on focus variation scanning technique, was evaluated with regards to highest local and general accuracy. A specific scanning protocol was tested to scan original tooth surface from dental impressions. Also, different model materials were verified. The results showed a high scanning accuracy of the reference scanner with a mean deviation of 5.3 ± 1.1 µm for trueness and 1.6 ± 0.6 µm for precision in case of full arch scans. Current dental impression methods showed much higher deviations (trueness: 20.4 ± 2.2 µm, precision: 12.5 ± 2.5 µm) than the internal scanning accuracy of the reference scanner. Smaller objects like single tooth surface can be scanned with an even higher accuracy, enabling the system to assess erosive and abrasive tooth surface loss. The reference scanner can be used to measure differences for a lot of dental research fields. The different magnification levels combined with a high local and general accuracy can be used to assess changes of single teeth or restorations up to full arch changes. PMID:24836007

New method for scanning spacecraft and balloon-borne/space-based experiments

NASA Technical Reports Server (NTRS)

Polites, Michael E.

1991-01-01

A new method is presented for scanning balloon-borne experiments, free-flying spacecraft, and gimballed experiments mounted to the space shuttle or the space station. It uses rotating-unbalanced-mass (RUM) devices for generating circular, line, or raster scan patterns and an auxiliary control system for target acquisition, keeping the scan centered on the target, and producing complementary motion for raster scanning. It is ideal for applications where the only possible way to accomplish the required scan is to physically scan the entire experiment or spacecraft as in X-ray and gamma ray experiments. In such cases, this new method should have advantages over prior methods in terms of either power, weight, cost, performance, stability, or a combination of these.

Ultrastructure of a Thermotolerant Basidiomycete Possibly Suitable for Production of Food Protein

PubMed Central

Hofsten, Bengt V.; Hofsten, Angelica V.

1974-01-01

The imperfect cellulolytic fungus Sporotrichum pulverulentum, which is commonly found growing in wood-chip piles, was grown in submerged culture on wheat shorts and other cereal flours. These substrates were broken down in 1 to 4 days at 30 to 40 C, and the mycelial mass was easily harvested by filtration. Scanning electron micrographs of hyphae in mycelial pellets are presented, and thin sections of conidia and hyphae were studied in a transmission electron microscope. Dolipores in septa of hyphae were observed, and cell walls are shown to be lamellar, which is characteristic of the Basidiomycetes. Actively growing hyphae are full of cytoplasm with numerous mitochondria, whereas old mycelial pellets contain highly vacuolated and almost empty cells. Images PMID:4833364

Commissioning of full energy scanning irradiation with carbon-ion beams ranging from 55.6 to 430 MeV/u at the NIRS-HIMAC

NASA Astrophysics Data System (ADS)

Hara, Y.; Furukawa, T.; Mizushima, K.; Inaniwa, T.; Saotome, N.; Tansho, R.; Saraya, Y.; Shirai, T.; Noda, K.

2017-09-01

Since 2011, a three-dimensional (3D) scanning irradiation system has been utilized for treatments at the National Institute of Radiological Sciences-Heavy Ion Medical Accelerator in Chiba (NIRS-HIMAC). In 2012, a hybrid depth scanning method was introduced for the depth direction, in which 11 discrete beam energies are used in conjunction with the range shifter. To suppress beam spread due to multiple scattering and nuclear reactions, we then developed a full energy scanning method. Accelerator tuning and beam commissioning tests prior to a treatment with this method are time-consuming, however. We therefore devised a new approach to obtain the pencil beam dataset, including consideration of the contribution of large-angle scattered (LAS) particles, which reduces the time spent on beam data preparation. The accuracy of 3D dose delivery using this new approach was verified by measuring the dose distributions for different target volumes. Results confirmed that the measured dose distributions agreed well with calculated doses. Following this evaluation, treatments using the full energy scanning method were commenced in September 2015.

Metabolic profiling of roots of liquorice (Glycyrrhiza glabra) from different geographical areas by ESI/MS/MS and determination of major metabolites by LC-ESI/MS and LC-ESI/MS/MS.

PubMed

Montoro, Paola; Maldini, Mariateresa; Russo, Mariateresa; Postorino, Santo; Piacente, Sonia; Pizza, Cosimo

2011-02-20

Liquid chromatography electrospray mass spectrometry (LC-ESI/MS) has been applied to the full characterization of saponins and phenolics in hydroalcoholic extracts of roots of liquorice (Glycyrrhiza glabra). Relative quantitative analyses of the samples with respect to the phenolic constituents and to a group of saponins related to glycyrrhizic acid were performed using LC-ESI/MS. For the saponin constituents, full scan LC-MS/MS fragmentation of the protonated (positive ion mode) or deprotonated (negative ion mode) molecular species generated diagnostic fragment ions that provided information concerning the triterpene skeleton and the number and nature of the substituents. On the basis of the specific fragmentation of glycyrrhizic acid, an LC-MS/MS method was developed in order to quantify the analyte in the liquorice root samples. Chinese G. glabra roots contained the highest levels of glycyrrhizic acid, followed by those from Italy (Calabria). Copyright © 2010 Elsevier B.V. All rights reserved.

MW-assisted synthesis of LiFePO 4 for high power applications

NASA Astrophysics Data System (ADS)

Beninati, Sabina; Damen, Libero; Mastragostino, Marina

LiFePO 4/C was prepared by solid-state reaction from Li 3PO 4, Fe 3(PO 4) 2·8H 2O, carbon and glucose in a few minutes in a scientific MW (microwave) oven with temperature and power control. The material was characterized by X-ray diffraction, scanning electron microscopy and by TGA analysis to evaluate carbon content. The electrochemical characterization as positive electrode in EC (ethylene carbonate)-DMC (dimethylcarbonate) 1 M LiPF 6 was performed by galvanostatic charge-discharge cycles at C/10 to evaluate specific capacity and by sequences of 10 s discharge-charge pulses, at different high C-rates (5-45C) to evaluate pulse-specific power in simulate operative conditions for full-HEV application. The maximum pulse-specific power and, particularly, pulse efficiency values are quite high and make MW synthesis a very promising route for mass production of LiFePO 4/C for full-HEV batteries at low energy costs.

SU-C-206-07: A Practical Sparse View Ultra-Low Dose CT Acquisition Scheme for PET Attenuation Correction in the Extended Scan Field-Of-View

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miao, J; Fan, J; Gopinatha Pillai, A

Purpose: To further reduce CT dose, a practical sparse-view acquisition scheme is proposed to provide the same attenuation estimation as higher dose for PET imaging in the extended scan field-of-view. Methods: CT scans are often used for PET attenuation correction and can be acquired at very low CT radiation dose. Low dose techniques often employ low tube voltage/current accompanied with a smooth filter before backprojection to reduce CT image noise. These techniques can introduce bias in the conversion from HU to attenuation values, especially in the extended CT scan field-of-view (FOV). In this work, we propose an ultra-low dose CTmore » technique for PET attenuation correction based on sparse-view acquisition. That is, instead of an acquisition of full amount of views, only a fraction of views are acquired. We tested this technique on a 64-slice GE CT scanner using multiple phantoms. CT scan FOV truncation completion was performed based on the published water-cylinder extrapolation algorithm. A number of continuous views per rotation: 984 (full), 246, 123, 82 and 62 have been tested, corresponding to a CT dose reduction of none, 4x, 8x, 12x and 16x. We also simulated sparse-view acquisition by skipping views from the fully-acquired view data. Results: FBP reconstruction with Q. AC filter on reduced views in the full extended scan field-of-view possesses similar image quality to the reconstruction on acquired full view data. The results showed a further potential for dose reduction compared to the full acquisition, without sacrificing any significant attenuation support to the PET. Conclusion: With the proposed sparse-view method, one can potential achieve at least 2x more CT dose reduction compared to the current Ultra-Low Dose (ULD) PET/CT protocol. A pre-scan based dose modulation scheme can be combined with the above sparse-view approaches, which can even further reduce the CT scan dose during a PET/CT exam.« less

MS/MS Automated Selected Ion Chromatograms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Monroe, Matthew

2005-12-12

This program can be used to read a LC-MS/MS data file from either a Finnigan ion trap mass spectrometer (.Raw file) or an Agilent Ion Trap mass spectrometer (.MGF and .CDF files) and create a selected ion chromatogram (SIC) for each of the parent ion masses chosen for fragmentation. The largest peak in each SIC is also identified, with reported statistics including peak elution time, height, area, and signal to noise ratio. It creates several output files, including a base peak intensity (BPI) chromatogram for the survey scan, a BPI for the fragmentation scans, an XML file containing the SICmore » data for each parent ion, and a "flat file" (ready for import into a database) containing summaries of the SIC data statistics.« less

Measurement of the integrated Luminosities of cross-section scan data samples around the $${\\rm{\\psi }}$$(3770) mass region

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ablikim, M.; Achasov, M. N.; Ahmed, S.

To investigate the nature of the (3770) resonance and to measure the cross section for e +e -→Dmore » $$\\bar{D}$$, a cross-section scan data sample, distributed among 41 center-of-mass energy points from 3.73 to 3.89 GeV, was taken with the BESIII detector operated at the BEPCII collider in the year 2010. By analyzing the large angle Bhabha scattering events, we measure the integrated luminosity of the data sample at each center-of-mass energy point. The total integrated luminosity of the data sample is 76.16±0.04±0.61 pb -1, where the first uncertainty is statistical and the second systematic.« less

Sarcoidosis with Pancreatic Mass, Endobronchial Nodules, and Miliary Opacities in the Lung.

PubMed

Matsuura, Shun; Mochizuka, Yasutaka; Oishi, Kyohei; Miyashita, Koichi; Naoi, Hyogo; Mochizuki, Eisuke; Mikura, Shinichiro; Tsukui, Masaru; Koshimizu, Naoki; Ohata, Akihiko; Suda, Takahumi

2017-11-15

Sarcoidosis affects multiple organs and rarely has unusual manifestations. A 78-year-old woman was referred to our hospital for coughing symptoms. A chest computed tomography (CT) scan revealed bilateral diffuse miliary patterns and right pleural effusion. Bronchoscopy showed multiple nodules in the carina and the bronchus intermedius. A CT scan of her abdomen revealed hypovascular lesions involving the pancreatic head and body. A transbronchial lung biopsy, bronchial mucosal biopsy, and endoscopic ultrasound-guided fine-needle aspiration of the pancreatic mass demonstrated non-caseating granulomas. We diagnosed the patient with sarcoidosis. She received no treatment for sarcoidosis and has been followed up for one year, during which no pulmonary disease progression had been observed and the pancreatic masses partially regressed.

Measurement of the integrated Luminosities of cross-section scan data samples around the $${\\rm{\\psi }}$$(3770) mass region

DOE PAGES

Ablikim, M.; Achasov, M. N.; Ahmed, S.; ...

2018-05-01

To investigate the nature of the (3770) resonance and to measure the cross section for e +e -→Dmore » $$\\bar{D}$$, a cross-section scan data sample, distributed among 41 center-of-mass energy points from 3.73 to 3.89 GeV, was taken with the BESIII detector operated at the BEPCII collider in the year 2010. By analyzing the large angle Bhabha scattering events, we measure the integrated luminosity of the data sample at each center-of-mass energy point. The total integrated luminosity of the data sample is 76.16±0.04±0.61 pb -1, where the first uncertainty is statistical and the second systematic.« less

Scanning transmission ion micro-tomography (STIM-T) of biological specimens.

PubMed

Schwertner, Micheal; Sakellariou, Arthur; Reinert, Tilo; Butz, Tilman

2006-05-01

Computed tomography (CT) was applied to sets of Scanning Transmission Ion Microscopy (STIM) projections recorded at the LIPSION ion beam laboratory (Leipzig) in order to visualize the 3D-mass distribution in several specimens. Examples for a test structure (copper grid) and for biological specimens (cartilage cells, cygospore) are shown. Scanning Transmission Micro-Tomography (STIM-T) at a resolution of 260 nm was demonstrated for the first time. Sub-micron features of the Cu-grid specimen were verified by scanning electron microscopy. The ion energy loss measured during a STIM-T experiment is related to the mass density of the specimen. Typically, biological specimens can be analysed without staining. Only shock freezing and freeze-drying is required to preserve the ultra-structure of the specimen. The radiation damage to the specimen during the experiment can be neglected. This is an advantage compared to other techniques like X-ray micro-tomography. At present, the spatial resolution is limited by beam position fluctuations and specimen vibrations.

Detection of new emerging type-A trichothecenes by untargeted mass spectrometry.

PubMed

González-Jartín, Jesús M; Alfonso, Amparo; Sainz, María J; Vieytes, Mercedes R; Botana, Luis M

2018-02-01

Mycotoxins occur naturally as agricultural contaminants all over the world. The toxic effects of some of their metabolites are known and their presence regulated in food and feed. This paper describes two methods for the detection of toxins of type-A trichothecenes group, and their modified forms, using mass spectrometry. Ultra-performance liquid chromatography coupled to mass spectrometry-ion trap-time of flight (UPLC-MS-IT-TOF) was employed to characterize the fragmentation pathways of 10 type-A trichothecenes, and characteristic ions were tentatively identified in scan mode through their accurate masses. Unknown signals were detected in a F. sporotrichioides extract, which afterwards were identified as seven modified forms of neosolaniol (NEO) and T-2 toxin. Then, UPLC coupled to tandem mass spectrometry (MS/MS) was employed to develop a precursor ion scanning method that can be used as a screening tool to detect any modified type-A trichothecenes. Copyright © 2017 Elsevier B.V. All rights reserved.

Melting temperature and enthalpy variations of phase change materials (PCMs): a differential scanning calorimetry (DSC) analysis

NASA Astrophysics Data System (ADS)

Sun, Xiaoqin; Lee, Kyoung Ok; Medina, Mario A.; Chu, Youhong; Li, Chuanchang

2018-06-01

Differential scanning calorimetry (DSC) analysis is a standard thermal analysis technique used to determine the phase transition temperature, enthalpy, heat of fusion, specific heat and activation energy of phase change materials (PCMs). To determine the appropriate heating rate and sample mass, various DSC measurements were carried out using two kinds of PCMs, namely N-octadecane paraffin and calcium chloride hexahydrate. The variations in phase transition temperature, enthalpy, heat of fusion, specific heat and activation energy were observed within applicable heating rates and sample masses. It was found that the phase transition temperature range increased with increasing heating rate and sample mass; while the heat of fusion varied without any established pattern. The specific heat decreased with the increase of heating rate and sample mass. For accuracy purpose, it is recommended that for PCMs with high thermal conductivity (e.g. hydrated salt) the focus will be on heating rate rather than sample mass.

A novel tactile-guided detection and three-dimensional localization of clinically significant breast masses.

PubMed

Mojra, A; Najarian, S; Kashani, S M Towliat; Panahi, F

2012-01-01

This paper presents a novel robotic sensory system 'Robo-Tac-BMI', which manipulates an indentation probe for the detection and three-dimensional localization of an abnormal mass embedded in the breast tissue. The Robo-Tac-BMI is designed based on artificial tactile sensing technology which is a new non-invasive method for mimicking the surgeon's palpation quantitatively. The intelligent processor of the device provides an overall stiffness map of the scanned areas. The extracted stiffness parameters provide a decisive factor for certifying the mass existence. Results are validated by 'gold standard' tests. Following the mass detection, its 3D localization is of essential importance in the treatment procedures. The planar 2D coordinate is readily available for all points on the tissue surface. Mass depth estimation is achieved by a comprehensive model utilizing the logistic regression algorithm and a Receiver Operating Characteristic (ROC) Curve for the highest accuracy. Statistical analysis is performed over 27 cases with 346 scanned areas. Copyright © 2012 Informa UK, Ltd.

Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues.

PubMed

Farré, M; Picó, Y; Barceló, D

2014-02-07

The analysis of pesticides residues using a last generation high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS) was explored. Pesticides were extracted from fruits, fish, bees and sediments by QuEChERS and from water by solid-phase with Oasis HLB cartridges. Ultra-high pressure liquid chromatography (UHPLC)-LTQ-Orbitrap mass spectrometer acquired full scan MS data for quantification, and data dependent (dd) MS(2) and MS(3) product ion spectra for identification and/or confirmation. The regression coefficients (r(2)) for the calibration curves (two order of magnitude up to the lowest calibration level) in the study were ≥0.99. The LODs for 54 validated compounds were ≤2ngmL(-1) (analytical standards). The relative standard deviation (RSD), which was used to estimate precision, was always lower than 22%. The recovery of extraction and matrix effects ranged from 58 to 120% and from -92 to 52%, respectively. Mass accuracy was always ≤4ppm, corresponding to a maximum mass error of 1.6millimass units (mmu). This procedure was then successfully applied to pesticide residues in a set of the above-mentioned food and environmental samples. In addition to target analytes, this method enables the simultaneous detection/identification of non-target pesticides, pharmaceuticals, drugs of abuse, mycotoxins, and their metabolites. Copyright © 2013 Elsevier B.V. All rights reserved.

Composite electrodes for electrochemical supercapacitors.

PubMed

Li, Jun; Yang, Quanmin; Zhitomirsky, Igor

2010-01-07

Manganese dioxide nanofibers with length ranged from 0.1 to 1 μm and a diameter of about 4-6 nm were prepared by a chemical precipitation method. Composite electrodes for electrochemical supercapacitors were fabricated by impregnation of the manganese dioxide nanofibers and multiwalled carbon nanotubes (MWCNT) into porous Ni plaque current collectors. Obtained composite electrodes, containing 85% of manganese dioxide and 15 mass% of MWCNT, as a conductive additive, with total mass loading of 7-15 mg cm-2, showed a capacitive behavior in 0.5-M Na2SO4 solutions. The decrease in stirring time during precipitation of the nanofibers resulted in reduced agglomeration and higher specific capacitance (SC). The highest SC of 185 F g-1 was obtained at a scan rate of 2 mV s-1 for mass loading of 7 mg cm-2. The SC decreased with increasing scan rate and increasing electrode mass.

Imaging and review of a large pre-auricular pilomatrixoma in a child.

PubMed

Whittemore, Kenneth R; Cohen, Michael

2012-05-28

A 10-year-old girl presented with a mildly tender mass in the right preauricular region. The mass became larger, and the overlying skin turned purple. There was no clinical response to a course of either cephalexin or clarithromycin. The remainder of the head and neck examination was normal including normal facial nerve function. Lyme titers and a computed tomographic (CT) scan with contrast of the facial region were obtained. The CT scan demonstrated the lesion to be superficial to the parotid gland. The lyme titer was elevated and doxycycline was begun. The mass appeared to reduce in size after doxycycline treatment, but then grew and turned erythematous. The lesion was surgically excised and was vascular with calcification and cheesy inclusions. The mass was quite close to the skin and the clinical diagnosis at the time of surgery was a pilomatrixoma, which was corroborated on pathological evaluation.

Composite Electrodes for Electrochemical Supercapacitors

NASA Astrophysics Data System (ADS)

Li, Jun; Yang, Quan Min; Zhitomirsky, Igor

2010-03-01

Manganese dioxide nanofibers with length ranged from 0.1 to 1 μm and a diameter of about 4-6 nm were prepared by a chemical precipitation method. Composite electrodes for electrochemical supercapacitors were fabricated by impregnation of the manganese dioxide nanofibers and multiwalled carbon nanotubes (MWCNT) into porous Ni plaque current collectors. Obtained composite electrodes, containing 85% of manganese dioxide and 15 mass% of MWCNT, as a conductive additive, with total mass loading of 7-15 mg cm-2, showed a capacitive behavior in 0.5-M Na2SO4 solutions. The decrease in stirring time during precipitation of the nanofibers resulted in reduced agglomeration and higher specific capacitance (SC). The highest SC of 185 F g-1 was obtained at a scan rate of 2 mV s-1 for mass loading of 7 mg cm-2. The SC decreased with increasing scan rate and increasing electrode mass.

Composite Electrodes for Electrochemical Supercapacitors

PubMed Central

2010-01-01

Manganese dioxide nanofibers with length ranged from 0.1 to 1 μm and a diameter of about 4–6 nm were prepared by a chemical precipitation method. Composite electrodes for electrochemical supercapacitors were fabricated by impregnation of the manganese dioxide nanofibers and multiwalled carbon nanotubes (MWCNT) into porous Ni plaque current collectors. Obtained composite electrodes, containing 85% of manganese dioxide and 15 mass% of MWCNT, as a conductive additive, with total mass loading of 7–15 mg cm−2, showed a capacitive behavior in 0.5-M Na2SO4 solutions. The decrease in stirring time during precipitation of the nanofibers resulted in reduced agglomeration and higher specific capacitance (SC). The highest SC of 185 F g−1 was obtained at a scan rate of 2 mV s−1 for mass loading of 7 mg cm−2. The SC decreased with increasing scan rate and increasing electrode mass. PMID:20672101

Coronary artery calcium: a multi-institutional, multimanufacturer international standard for quantification at cardiac CT.

PubMed

McCollough, Cynthia H; Ulzheimer, Stefan; Halliburton, Sandra S; Shanneik, Kaiss; White, Richard D; Kalender, Willi A

2007-05-01

To develop a consensus standard for quantification of coronary artery calcium (CAC). A standard for CAC quantification was developed by a multi-institutional, multimanufacturer international consortium of cardiac radiologists, medical physicists, and industry representatives. This report specifically describes the standardization of scan acquisition and reconstruction parameters, the use of patient size-specific tube current values to achieve a prescribed image noise, and the use of the calcium mass score to eliminate scanner- and patient size-based variations. An anthropomorphic phantom containing calibration inserts and additional phantom rings were used to simulate small, medium-size, and large patients. The three phantoms were scanned by using the recommended protocols for various computed tomography (CT) systems to determine the calibration factors that relate measured CT numbers to calcium hydroxyapatite density and to determine the tube current values that yield comparable noise values. Calculation of the calcium mass score was standardized, and the variance in Agatston, volume, and mass scores was compared among CT systems. Use of the recommended scanning parameters resulted in similar noise for small, medium-size, and large phantoms with all multi-detector row CT scanners. Volume scores had greater interscanner variance than did Agatston and calcium mass scores. Use of a fixed calcium hydroxyapatite density threshold (100 mg/cm(3)), as compared with use of a fixed CT number threshold (130 HU), reduced interscanner variability in Agatston and calcium mass scores. With use of a density segmentation threshold, the calcium mass score had the smallest variance as a function of patient size. Standardized quantification of CAC yielded comparable image noise, spatial resolution, and mass scores among different patient sizes and different CT systems and facilitated reduced radiation dose for small and medium-size patients.

Large photocathode 20-inch PMT testing methods for the JUNO experiment

NASA Astrophysics Data System (ADS)

Anfimov, N.

2017-06-01

The 20 kt Liquid Scintillator (LS) JUNO detector is being constructed by the International Collaboration in China, with the primary goal of addressing the question of neutrino mass ordering (hierarchy). The main challenge for JUNO is to achieve a record energy resolution, ~ 3% at 1 MeV of energy released in the LS, which is required to perform the neutrino mass hierarchy determination. About 20 000 large 20'' PMTs with high Photon Detection Efficiency (PDE) and good photocathode uniformity will ensure an approximately 80% surface coverage of the JUNO detector. The JUNO collaboration is preparing equipment for the mass tests of all PMTs using 4 dedicated containers. Each container consists of 36 drawers. Each drawer will test a single PMT. This approach allows us to test 144 PMTs in parallel. The primary measurement in the container will be the PMT response to illumination of its photocathode by a low-intensity uniform light. Each of the 20000 PMTs will undergo the container test. Additionally, a dedicated scanning system was constructed for sampled tests of PMTs that allows us to study the variation of the PDE over the entire PMT photocathode surface. A sophisticated laboratory for PMT testing was recently built. It includes a dark room where the scanning station is housed. The core of the scanning station is a rotating frame with 7 LED sources of calibrated short light flashes that are placed along the photocathode surface covering zenith angles from the top of a PMT to its equator. It allows for the testing of individual PMTs in all relevant aspects by scanning the photocathode and identifying any potential problems. The collection efficiency of a large PMT is known to be very sensitive to the Earth Magnetic Field (EMF), therefore, understanding the necessary level of EMF suppression is crucial for the JUNO Experiment. A dark room with Helmholtz coils compensating the EMF components is available for these tests at a JUNO facility. The Hamamatsu R12860 20'' PMT is a candidate for the JUNO experiment. In this article the container design and mass-testing method, the scanning setup and scanning method are briefly described and preliminary results for performance test of this PMT are reported.

Injected mass deposition thresholds for lithium granule instigated triggering of edge localized modes on EAST

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lunsford, R.; Sun, Zhen; Maingi, Rajesh

The ability of an injected lithium granule to promptly trigger an edge localized mode (ELM) has been established in multiple experiments. By horizontally injecting granules ranging in diameter from 200 microns to 1mm in diameter into the low field side of EAST H-mode discharges we have determined that granules with diameter > 600 microns are successful in triggering ELMs more than 95% of the time. Granules were radially injected from the outer midplane with velocities ~ 80 m/s into EAST upper-single null discharges with an ITER like tungsten monoblock divertor. ELM triggering was a prompt response to granule injection, andmore » for granules of a sufficient size there was no evidence of a "trigger lag" phenomenon as observed in full metal machines. We also demonstrated that the triggering efficiency decreased with granule size during dynamic size scans. These granules were individually tracked throughout their injection cycle in order to determine their efficacy at triggering an ELM. Furthermore, by simulating the granule injection with an experimentally benchmarked neutral gas shielding (NGS) model, the ablatant mass deposition required to promptly trigger an ELM is calculated and the fractional mass deposition is determined. Simulated 900 micron granules capable of triggering an ELM show a peaked mass deposition of 3.9 x 10 17 atoms per mm of penetration at a depth of approximately 5 cm past the separatrix.« less

Injected mass deposition thresholds for lithium granule instigated triggering of edge localized modes on EAST

DOE PAGES

Lunsford, R.; Sun, Zhen; Maingi, Rajesh; ...

2017-12-19

The ability of an injected lithium granule to promptly trigger an edge localized mode (ELM) has been established in multiple experiments. By horizontally injecting granules ranging in diameter from 200 microns to 1mm in diameter into the low field side of EAST H-mode discharges we have determined that granules with diameter > 600 microns are successful in triggering ELMs more than 95% of the time. Granules were radially injected from the outer midplane with velocities ~ 80 m/s into EAST upper-single null discharges with an ITER like tungsten monoblock divertor. ELM triggering was a prompt response to granule injection, andmore » for granules of a sufficient size there was no evidence of a "trigger lag" phenomenon as observed in full metal machines. We also demonstrated that the triggering efficiency decreased with granule size during dynamic size scans. These granules were individually tracked throughout their injection cycle in order to determine their efficacy at triggering an ELM. Furthermore, by simulating the granule injection with an experimentally benchmarked neutral gas shielding (NGS) model, the ablatant mass deposition required to promptly trigger an ELM is calculated and the fractional mass deposition is determined. Simulated 900 micron granules capable of triggering an ELM show a peaked mass deposition of 3.9 x 10 17 atoms per mm of penetration at a depth of approximately 5 cm past the separatrix.« less

Metabolic profiling for the identification of Huntington biomarkers by on-line solid-phase extraction capillary electrophoresis mass spectrometry combined with advanced data analysis tools.

PubMed

Pont, Laura; Benavente, Fernando; Jaumot, Joaquim; Tauler, Romà; Alberch, Jordi; Ginés, Silvia; Barbosa, José; Sanz-Nebot, Victoria

2016-03-01

In this work, an untargeted metabolomic approach based on sensitive analysis by on-line solid-phase extraction capillary electrophoresis mass spectrometry (SPE-CE-MS) in combination with multivariate data analysis is proposed as an efficient method for the identification of biomarkers of Huntington's disease (HD) progression in plasma. For this purpose, plasma samples from wild-type (wt) and HD (R6/1) mice of different ages (8, 12, and 30 weeks), were analyzed by C18 -SPE-CE-MS in order to obtain the characteristic electrophoretic profiles of low molecular mass compounds. Then, multivariate curve resolution alternating least squares (MCR-ALS) was applied to the multiple full scan MS datasets. This strategy permitted the resolution of a large number of metabolites being characterized by their electrophoretic peaks and their corresponding mass spectra. A total number of 29 compounds were relevant to discriminate between wt and HD plasma samples, as well as to follow-up the HD progression. The intracellular signaling was found to be the most affected metabolic pathway in HD mice after 12 weeks of birth, when mice already showed motor coordination deficiencies and cognitive decline. This fact agreed with the atrophy and dysfunction of specific neurons, loss of several types of receptors, and changed expression of neurotransmitters. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The impact of a focused vascular lower limb arterial duplex (F-VLAD) scan in management decisions for acute limb ischaemia.

PubMed

Normahani, Pasha; Aslam, Mohammed; Standfield, Nigel J; Jaffer, Usman

2017-01-01

To establish the diagnostic accuracy of a 'focused vascular lower limb arterial duplex scan (F-VLAD)' developed to facilitate rapid decision-making for acute limb ischaemia (ALI). Ten cases of ALI were identified from our patient database; clinical details, history and examination findings were extracted from the clinical notes. Original 'full' duplex ultrasound (DUS) pictorial reports were 're-formatted' to include only anatomical segments included in the 'F-VLAD' scan. The series of 10 reports were emailed to 1741 vascular surgeons. Each recipient received a random mixture of full and F-VLAD scans. Participants were asked regarding next step in management and confidence in decision-making (Likert scale; 1 strongly disagree, 5 strongly agree). The cases were again sent out to the same database and respondents were asked as to the cause of ischaemia (embolic or thrombosis). Eighty-one participants responded to the first survey and 43 participants to the second survey. Participants felt more confident making decisions regarding management using the full duplex report compared to the F-VLAD report (4 (3-4) vs 3 (2-4), median (IQR); p<0.001). However, there was no significant difference in diagnostic accuracy (differentiating embolus from thrombosis) when comparing the F-VLAD and full DUS reports (85.4% vs 88.3%; p=0.461). F-VLAD and 'full' DUS reports had comparable sensitivity (85.1% vs 86.8%), specificity (85.6% vs 89.2%),positive predictive value (PPV) (80.4% vs 81.9%) and negative predictive value (NPV) (89.2% vs 92.2%), respectively. The F-VLAD scan has comparable accuracy to a traditional full DUS in diagnosing the underlying aetiology of ALI. This may facilitate surgeon-performed point-of-care DUS.

Application of cation-exchange solid-phase extraction for the analysis of amino alcohols from water and human plasma for verification of Chemical Weapons Convention.

PubMed

Kanaujia, Pankaj K; Tak, Vijay; Pardasani, Deepak; Gupta, A K; Dubey, D K

2008-03-28

The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.

Detecting a wide range of environmental contaminants in human blood samples--combining QuEChERS with LC-MS and GC-MS methods.

PubMed

Plassmann, Merle M; Schmidt, Magdalena; Brack, Werner; Krauss, Martin

2015-09-01

Exposure to environmental pollution and consumer products may result in an uptake of chemicals into human tissues. Several studies have reported the presence of diverse environmental contaminants in human blood samples. However, previously developed multi-target methods for the analysis of human blood include a fairly limited amount of compounds stemming from one or two related compound groups. Thus, the sample preparation method QuEChERS (quick easy cheap effective rugged and safe) was tested for the extraction of 64 analytes covering a broad compound domain followed by detection using liquid and gas chromatography coupled to mass spectrometry (LC- and GC-MS). Forty-seven analytes showed absolute recoveries above 70% in the first QuEChERS step, being a simple liquid-liquid extraction (LLE) using acetonitrile and salt. The second QuEChERS step, being a dispersive solid phase extraction, did not result in an overall improvement of recoveries or removal of background signals. Using solely the LLE step, eight analytes could subsequently be detected in human blood samples from the German Environmental Specimen Bank. Using a LC-multiple reaction monitoring (MRM) method with a triple quadrupole instrument, better recoveries were achieved than with an older LC-high-resolution (HR) MS full scan orbitrap instrument, which required a higher concentration factor of the extracts. However, the application of HRMS full scan methods could be used for the detection of additional compounds retrospectively.

A gas chromatography-mass spectrometry method for the determination of delta-aminolevulinic acid in plant leaves.

PubMed

Hijaz, Faraj; Killiny, Nabil

2016-05-20

Delta-aminolevulinic (δ-ALA) acid is an important intermediate for tetrapyrroles biosynthesis and it has recently received great attention in plant physiology and human toxicology. However, the colorimetric method which is the most common method for determination of δ-ALA is time consuming and is not specific. In this study, a method for determination of δ-ALA in plant tissues was developed based on the trimethylsilyl (TMS) derivative of the pyrrole formed from the reaction of δ-ALA with ethyl acetoacetate via Knorr condensation. The δ-ALA in the HCl extract was reacted with ethyl acetoacetate to form a pyrrole. Then, the pyrrole compound was extracted using ethyl acetate and the solvent was evaporated to dryness. The dried sample was derivatized to its TMS ester and analyzed using GC-MS. The concentration of δ-ALA in citrus leaves incubated with levulinic acid was also determined by the conventional colorimetric method. The linear range was 10-200ppm in the full scan mode and 0.1-20ppm in the selected ion monitoring (SIM). The limit of detection was 6ppm in the full scan and 0.05ppm in SIM mode, representing a four-fold increase in sensitivity compared to the colorimetric method. The GC-MS method developed in this study is simple, accurate, sensitive, and could also be used to measure δ-ALA in other biological samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A combined morphometric analysis of foot form and its association with sex, stature, and body mass.

PubMed

Domjanic, Jacqueline; Seidler, Horst; Mitteroecker, Philipp

2015-08-01

Morphometric analysis of footprints is a classic means for orthopedic diagnosis. In forensics and physical anthropology, it is commonly used for the estimation of stature and body mass. We studied individual variation and sexual dimorphism of foot dimensions and footprint shape by a combination of classic foot measurements and geometric morphometric methods. Left and right feet of 134 healthy adult males and females were scanned twice with a 3D optical laser scanner, and stature as well as body mass were recorded. Foot length and width were measured on the 3D scans. The 2D footprints were extracted as the plantar-most 2 mm of the 3D scans and measured with 85 landmarks and semilandmarks. Both foot size and footprint shape are sexually dimorphic and relate to stature and body mass. While dimorphism in foot length largely results from dimorphism in stature, dimorphism in footprint shape partly owes to the dimorphism in BMI. Stature could be estimated well based on foot length (R(2)  = 0.76), whereas body mass was more closely related to foot width (R(2)  = 0.62). Sex could be estimated correctly for 95% of the individuals based on a combination of foot width and length. Geometric morphometrics proved to be an effective tool for the detailed analysis of footprint shape. However, for the estimation of stature, body mass, and sex, shape variables did not considerably improve estimates based on foot length and width. © 2015 Wiley Periodicals, Inc.

Clinical anthropometrics and body composition from 3D whole-body surface scans

PubMed Central

Ng, BK; Hinton, BJ; Fan, B; Kanaya, AM; Shepherd, JA

2017-01-01

BACKGROUND/OBJECTIVES Obesity is a significant worldwide epidemic that necessitates accessible tools for robust body composition analysis. We investigated whether widely available 3D body surface scanners can provide clinically relevant direct anthropometrics (circumferences, areas and volumes) and body composition estimates (regional fat/lean masses). SUBJECTS/METHODS Thirty-nine healthy adults stratified by age, sex and body mass index (BMI) underwent whole-body 3D scans, dual energy X-ray absorptiometry (DXA), air displacement plethysmography and tape measurements. Linear regressions were performed to assess agreement between 3D measurements and criterion methods. Linear models were derived to predict DXA body composition from 3D scan measurements. Thirty-seven external fitness center users underwent 3D scans and bioelectrical impedance analysis for model validation. RESULTS 3D body scan measurements correlated strongly to criterion methods: waist circumference R2 = 0.95, hip circumference R2 = 0.92, surface area R2 = 0.97 and volume R2 = 0.99. However, systematic differences were observed for each measure due to discrepancies in landmark positioning. Predictive body composition equations showed strong agreement for whole body (fat mass R2 = 0.95, root mean square error (RMSE) = 2.4 kg; fat-free mass R2 = 0.96, RMSE = 2.2 kg) and arms, legs and trunk (R2 = 0.79–0.94, RMSE = 0.5–1.7 kg). Visceral fat prediction showed moderate agreement (R2 = 0.75, RMSE = 0.11 kg). CONCLUSIONS 3D surface scanners offer precise and stable automated measurements of body shape and composition. Software updates may be needed to resolve measurement biases resulting from landmark positioning discrepancies. Further studies are justified to elucidate relationships between body shape, composition and metabolic health across sex, age, BMI and ethnicity groups, as well as in those with metabolic disorders. PMID:27329614

Optical 3D scans for orthodontic diagnostics performed on full-arch impressions. Completeness of surface structure representation.

PubMed

Vogel, Annike B; Kilic, Fatih; Schmidt, Falko; Rübel, Sebastian; Lapatki, Bernd G

2015-11-01

The purpose of this work was to evaluate the completeness of surface structure representation offered by full-arch impression scans in different situations of tooth (mal)alignment and whether this completeness could be improved by performing rescans on the same impressions reduced sequentially to different levels of gingival height and by adding extra single scans to the number of single scans recommended by the manufacturer. Three pairs of full-arch resin models were used as reference, characterized either by normal occlusion, by anterior diastematic protrusion (and edentulous spaces in the lower posterior segments), or by anterior crowding. An alginate impression of each arch was taken and digitized with a structured-light scanner, followed by three rescans with the impression cut back to 10, 5, and 1 mm of gingival height. Both the initial scan and the rescans were performed both with 19 basic single scans and with 10 extra single scans. Each impression scan was analyzed for quantitative completeness relative to its homologous direct scan of the original resin model. In addition, the topography of voids in the resultant digital model was assessed by visual inspection. Compared to the homologous reference scans of the original resin models, completeness of the original impression scans--in the absence of both gingival cutback and extra single scans--was 97.23 ± 0.066% in the maxilla or 95.72 ± 0.070% in the mandible with normal occlusion, 91.11 ± 0.132% or 96.07 ± 0.109% in the arches with anterior diastematic protrusion, and 98.24 ± 0.085% or 93.39 ± 0.146% in those with anterior crowding. Gingival cutback and extra single scans were found to improve these values up to 100.35 ± 0.066% or 99.53 ± 0.070% in the arches with normal occlusion, 91.77 ± 0.132% or 97.95 ± 0.109% in those with anterior diastematic protrusion, and 98.59 ± 0.085% or 98.96 ± 0.146% in those with anterior crowding. In strictly quantitative terms, the impression scans did capture relatively large percentages of the total surface. However, the topographic examinations revealed that regions essential for orthodontic model analysis were missing. The malocclusion models were particularly affected. Thus, impression scans performed with structured-light scanners cannot replace scans of positive casts for diagnostic use in orthodontics.

Development of a GC-APCI-QTOFMS library for new psychoactive substances and comparison to a commercial ESI library.

PubMed

Mesihää, Samuel; Ketola, Raimo A; Pelander, Anna; Rasanen, Ilpo; Ojanperä, Ilkka

2017-03-01

Gas chromatography coupled to atmospheric pressure chemical ionization quadrupole time-of-flight mass spectrometry (GC-APCI-QTOFMS) was evaluated for the identification of new psychoactive substances (NPS). An in-house high mass resolution GC-APCI-QTOFMS test library was developed for 29 nitrogen-containing drugs belonging mostly to synthetic stimulants. The library was based on 12 intra-day measurements of each compound at three different collision energies, 10, 20 and 40 eV. The in-house library mass spectra were compared to mass spectra from a commercial library constructed by liquid chromatography-electrospray ionization (LC-ESI) QTOFMS. The reversed library search scores between the in-house GC-APCI library and the commercial LC-ESI library were compared once a week during a 5-week period by using data measured by GC-APCI-QTOFMS. The protonated molecule was found for all drugs in the full scan mode, and the drugs were successfully identified by both libraries in the targeted MS/MS mode. The GC-APCI library score averaged over all collision energies was as high as 94.4/100 with a high repeatability, while the LC-ESI library score was also high (89.7/100) with a repeatability only slightly worse. These results highlight the merits of GC-APCI-QTOFMS in the analysis of NPS even in situations where the reference standards are not immediately available, taking advantage of the accurate mass measurement of the protonated molecule and product ions, and comparison to existing soft-ionization mass spectral libraries. Graphical abstract Tandem mass spectra obtained from GC-APCI-QTOFMS are comparable to LC-ESI-QTOFMS library spectra.

Accurate mass screening and identification of emerging contaminants in environmental samples by liquid chromatography-hybrid linear ion trap Orbitrap mass spectrometry.

PubMed

Hogenboom, A C; van Leerdam, J A; de Voogt, P

2009-01-16

The European Reach legislation will possibly drive producers to develop newly designed chemicals that will be less persistent, bioaccumulative or toxic. If this innovation leads to an increased use of more hydrophilic chemicals it may result in higher mobilities of chemicals in the aqueous environment. As a result, the drinking water companies may face stronger demands on removal processes as the hydrophilic compounds inherently are more difficult to remove. Monitoring efforts will also experience a shift in focus to more water-soluble compounds. Screening source waters on the presence of (emerging) contaminants is an essential step in the control of the water cycle from source to tap water. In this article, some of our experiences are presented with the hybrid linear ion trap (LTQ) FT Orbitrap mass spectrometer, in the area of chemical water analysis. A two-pronged strategy in mass spectrometric research was employed: (i) exploring effluent, surface, ground- and drinking-water samples searching for accurate masses corresponding to target compounds (and their product ions) known from, e.g. priority lists or the scientific literature and (ii) full-scan screening of water samples in search of 'unknown' or unexpected masses, followed by MS(n) experiments to elucidate the structure of the unknowns. Applications of both approaches to emerging water contaminants are presented and discussed. Results are presented for target analysis search for pharmaceuticals, benzotriazoles, illicit drugs and for the identification of unknown compounds in a groundwater sample and in a polar extract of a landfill soil sample (a toxicity identification evaluation bioassay sample). The applications of accurate mass screening and identification described in this article demonstrate that the LC-LTQ FT Orbitrap MS is well equipped to meet the challenges posed by newly emerging polar contaminants.

(Full field) optical coherence tomography and applications

NASA Astrophysics Data System (ADS)

Buchroithner, Boris; Hannesschläger, Günther; Leiss-Holzinger, Elisabeth; Prylepa, Andrii; Heise, Bettina

2018-03-01

This paper illustrates specific features and use of optical coherence tomography (OCT) in the raster-scanning and in comparison in the full field version of this imaging technique. Cases for nondestructive testing are discussed alongside other application schemes. In particular monitoring time-dependent processes and probing of birefringent specimens are considered here. In the context of polymer testing birefringence mapping may often provide information about internal strain and stress states. Recent results obtained with conventional raster-scanning OCT systems, with (dual and single-shot) full field OCT configurations, and with polarization-sensitive versions of (full field) OCT are presented here.

Evaluation of the nutrition screening tool for childhood cancer (SCAN).

PubMed

Murphy, Alexia J; White, Melinda; Viani, Karina; Mosby, Terezie T

2016-02-01

Malnutrition is a serious concern for children with cancer and nutrition screening may offer a simple alternative to nutrition assessment for identifying children with cancer who are at risk of malnutrition. The present paper aimed to evaluate the nutrition screening tool for childhood cancer (SCAN). SCAN was developed after an extensive review of currently available tools and published screening recommendation, consideration of pediatric oncology nutrition guidelines, piloting questions, and consulting with members of International Pediatric Oncology Nutrition Group. In Study 1, the accuracy and validity of SCAN against pediatric subjective global nutrition assessment (pediatric SGNA) was determined. In Study 2, subjects were classified as 'at risk of malnutrition' and 'not at risk of malnutrition' according to SCAN and measures of height, weight, body mass index (BMI) and body composition were compared between the groups. The validation of SCAN against pediatric SGNA showed SCAN had 'excellent' accuracy (0.90, 95% CI 0.78-1.00; p < 0.001), 100% sensitivity, 39% specificity, 56% positive predictive value and 100% negative predictive value. When subjects in Study 2 were classified into 'at risk of malnutrition' and 'not at risk of malnutrition' according to SCAN, the 'at risk of malnutrition' group had significantly lower values for weight Z score (p = 0.001), BMI Z score (p = 0.001) and fat mass index (FMI) (p = 0.04), than the 'not at risk of malnutrition' group. This study shows that SCAN is a simple, quick and valid tool which can be used to identify children with cancer who are at risk of malnutrition. Copyright © 2015 Elsevier Ltd and European Society for Clinical Nutrition and Metabolism. All rights reserved.

A genome-wide linkage scan for quantitative trait loci underlying obesity related phenotypes in 434 Caucasian families.

PubMed

Zhao, Lan-Juan; Xiao, Peng; Liu, Yong-Jun; Xiong, Dong-Hai; Shen, Hui; Recker, Robert R; Deng, Hong-Wen

2007-03-01

To identify quantitative trait loci (QTLs) that contribute to obesity, we performed a large-scale whole genome linkage scan (WGS) involving 4,102 individuals from 434 Caucasian families. The most pronounced linkage evidence was found at the genomic region 20p11-12 for fat mass (LOD = 3.31) and percentage fat mass (PFM) (LOD = 2.92). We also identified several regions showing suggestive linkage signals (threshold LOD = 1.9) for obesity phenotypes, including 5q35, 8q13, 10p12, and 17q11.

Application and validation of long-range terrestrial laser scanning to monitor the mass balance of very small glaciers in the Swiss Alps

NASA Astrophysics Data System (ADS)

Fischer, Mauro; Huss, Matthias; Kummert, Mario; Hoelzle, Martin

2016-06-01

Due to the relative lack of empirical field data, the response of very small glaciers (here defined as being smaller than 0.5 km2) to current atmospheric warming is not fully understood yet. Investigating their mass balance, e.g. using the direct glaciological method, is a prerequisite to fill this knowledge gap. Terrestrial laser scanning (TLS) techniques operating in the near infrared range can be applied for the creation of repeated high-resolution digital elevation models and consecutive derivation of annual geodetic mass balances of very small glaciers. This method is promising, as laborious and potentially dangerous field measurements as well as the inter- and extrapolation of point measurements can be circumvented. However, it still needs to be validated. Here, we present TLS-derived annual surface elevation and geodetic mass changes for five very small glaciers in Switzerland (Glacier de Prapio, Glacier du Sex Rouge, St. Annafirn, Schwarzbachfirn, and Pizolgletscher) and two consecutive years (2013/14-2014/15). The scans were acquired with a long-range Riegl -6000 especially designed for surveying snow- and ice-covered terrain. Zonally variable conversion factors for firn and bare ice surfaces were applied to convert geodetic volume to mass changes. We compare the geodetic results to direct glaciological mass balance measurements coinciding with the TLS surveys and assess the uncertainties and errors included in both methods. Average glacier-wide mass balances were negative in both years, showing stronger mass losses in 2014/15 (-1.65 m w.e.) compared to 2013/14 (-0.59 m w.e.). Geodetic mass balances were slightly less negative but in close agreement with the direct glaciological ones (R2 = 0.91). Due to the dense in situ measurements, the uncertainties in the direct glaciological mass balances were small compared to the majority of measured glaciers worldwide (±0.09 m w.e. yr-1 on average), and similar to uncertainties in the TLS-derived geodetic mass balances (±0.13 m w.e. yr-1).

Fast determination of 3-ethenylpyridine as a marker of environmental tobacco smoke at trace level using direct atmospheric pressure chemical ionization tandem mass spectrometry

NASA Astrophysics Data System (ADS)

Jiang, Cheng-Yong; Sun, Shi-Hao; Zhang, Qi-Dong; Liu, Jun-Hui; Zhang, Jian-Xun; Zong, Yong-Li; Xie, Jian-Ping

2013-03-01

A method with atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS) was developed and applied to direct analysis of Environmental Tobacco Smoke (ETS), using 3-ethenylpyridine (3-EP) as a vapour-phase marker. In this study, the ion source of APCI-MS/MS was modified and direct analysis of gas sample was achieved by the modified instrument. ETS samples were directly introduced, via an atmospheric pressure inlet, into the APCI source. Ionization was carried out in positive-ion APCI mode and 3-EP was identified by both full scan mode and daughter scan mode. Quantification of 3-EP was performed by multiple reaction monitoring (MRM) mode. The calibration curve was obtained in the range of 1-250 ng L-1 with a satisfactory regression coefficient of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.5 ng L-1 and 1.6 ng L-1, respectively. The precision of the method, calculated as relative standard deviation (RSD), was characterized by repeatability (RSD 3.92%) and reproducibility (RSD 4.81%), respectively. In real-world ETS samples analysis, compared with the conventional GC-MS method, the direct APCI-MS/MS has shown better reliability and practicability in the determination of 3-EP at trace level. The developed method is simple, fast, sensitive and repeatable; furthermore, it could provide an alternative way for the determination of other volatile pollutants in ambient air at low levels.

Optimization of parameters affecting signal intensity in an LTQ-orbitrap in negative ion mode: A design of experiments approach.

PubMed

Lemonakis, Nikolaos; Skaltsounis, Alexios-Leandros; Tsarbopoulos, Anthony; Gikas, Evagelos

2016-01-15

A multistage optimization of all the parameters affecting detection/response in an LTQ-orbitrap analyzer was performed, using a design of experiments methodology. The signal intensity, a critical issue for mass analysis, was investigated and the optimization process was completed in three successive steps, taking into account the three main regions of an orbitrap, the ion generation, the ion transmission and the ion detection regions. Oleuropein and hydroxytyrosol were selected as the model compounds. Overall, applying this methodology the sensitivity was increased more than 24%, the resolution more than 6.5%, whereas the elapsed scan time was reduced nearly to its half. A high-resolution LTQ Orbitrap Discovery mass spectrometer was used for the determination of the analytes of interest. Thus, oleuropein and hydroxytyrosol were infused via the instruments syringe pump and they were analyzed employing electrospray ionization (ESI) in the negative high-resolution full-scan ion mode. The parameters of the three main regions of the LTQ-orbitrap were independently optimized in terms of maximum sensitivity. In this context, factorial design, response surface model and Plackett-Burman experiments were performed and analysis of variance was carried out to evaluate the validity of the statistical model and to determine the most significant parameters for signal intensity. The optimum MS conditions for each analyte were summarized and the method optimum condition was achieved by maximizing the desirability function. Our observation showed good agreement between the predicted optimum response and the responses collected at the predicted optimum conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

[Rapid screening of acidity regulators in dairy by ion chromatography-high resolution mass spectrometry].

PubMed

Yun, Huan; Liu, Xin; Cui, Jie; Yang, Jing; Liu, Ying

2017-08-08

A method for screening of acidity regulators in dairy based on ion chromatography-high resolution mass spectrometry technology (IC-HRMS) was set up. The dairy samples were extracted by KOH (pH 7-8) and Oasis MAX SPE column, and separated by a Dionex IonPac AS11-HC column (250 mm×4 mm). All the acidity regulators were detected by Orbitrap full scan mode. Taking six organic acids as an example, the calibration curves showed good linearities in the range of 0.05-5.00 mg/L, and the correlation coefficients ( r ) were higher than 0.99. By detecting the spiked samples, the recoveries were in the range of 74.3%-115.5% with the relative standard deviations (RSDs) between 0.64% and 4.81%. Malic acid, citric acid, lactic acid, succinic acid and adipic acid could be detected by IC-HRMS in the commercial dairy samples. The results indicate that the method is simple, rapid and suitable for the qualitative screening of acidity regulators in dairy products.

Comprehensive thin-layer chromatography mass spectrometry of flavanols from Juniperus communis L. and Punica granatum L.

PubMed

Smrke, Samo; Vovk, Irena

2013-05-10

The coupling of thin-layer chromatography with mass spectrometry (TLC-MS) for the analysis of monomeric flavanols and proanthocyanidins in samples presented as complex matrices has been studied. The elution conditions for TLC-MS were optimised and full scans were compared with selected reaction monitoring for the MS detection of compounds. The performance of silica gel and cellulose plates with different developing solvents in TLC-MS was assessed. Cellulose plates provided superior sensitivity while ionisation suppression was encountered with silica plates. The use of a HILIC guard column beyond the elution head was found to facilitate detection of monomer compounds on silica plates. A new comprehensive TLC×MS procedure for screening flavanols in the entire chromatogram was developed as an alternative to the use of 4-dimethylaminocinnamaldehyde to determine the locations of compounds on the plate. This new procedure was applied to detect flavanols in the peel of Punica granatum L. fruits and in seeds of Juniperus communis L., in which flavanols and proanthocyanidin dimers and trimers were detected for the first time. Copyright © 2013 Elsevier B.V. All rights reserved.

Ultra high performance liquid chromatography-quadrupole-time of flight analysis for the identification and the determination of resveratrol and its metabolites in mouse plasma.

PubMed

Menet, M C; Cottart, C H; Taghi, M; Nivet-Antoine, V; Dargère, D; Vibert, F; Laprévote, O; Beaudeux, J-L

2013-01-25

Resveratrol is a polyphenol that has numerous interesting biological properties, but, per os, it is quickly metabolized. Some of its metabolites are more concentrated than resveratrol, may have greater biological activities, and may act as a kind of store for resveratrol. Thus, to understand the biological impact of resveratrol on a physiological system, it is crucial to simultaneously analyze resveratrol and its metabolites in plasma. This study presents an analytical method based on UHPLC-Q-TOF mass spectrometry for the quantification of resveratrol and of its most common hydrophilic metabolites. The use of (13)C- and D-labeled standards specific to each molecule led to a linear calibration curve on a larger concentration range than described previously. The use of high resolution mass spectrometry in the full scan mode enabled simultaneous identification and quantification of some hydrophilic metabolites not previously described in mice. In addition, UHPLC separation, allowing run times lower than 10 min, can be used in studies that requiring analysis of many samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Metabolic profile modifications in milk after enrofloxacin administration studied by liquid chromatography coupled with high resolution mass spectrometry.

PubMed

Junza, A; Saurina, J; Barrón, D; Minguillón, C

2016-08-19

High resolution accurate mass spectrometry (HRMS) operating in full scan MS mode was used in the search and identification of metabolites in raw milk from cows medicated with enrofloxacin. Data consisting of m/z features were taken throughout the entire chromatogram of milk samples from medicated animals and were compared with blank samples. Twenty six different compounds were identified. Some of them were attributed to structures related to enrofloxacin while others were dipeptides or tripeptides. Additionally, enrofloxacin was administered in a controlled treatment for three days. Milk was collected daily from the first day of treatment and until four days after in the search for the identified compounds. The obtained data were chemometrically treated by Principal Component Analysis. Samples were classified by this method into three different groups corresponding to days 1-2, day 3 and days 4-7 considering the different concentration profile evolution of metabolites during the days studied. Tentative metabolic pathways were designed to rationalize the presence of the newly identified compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

Advanced Automation for Ion Trap Mass Spectrometry-New Opportunities for Real-Time Autonomous Analysis

NASA Technical Reports Server (NTRS)

Palmer, Peter T.; Wong, C. M.; Salmonson, J. D.; Yost, R. A.; Griffin, T. P.; Yates, N. A.; Lawless, James G. (Technical Monitor)

1994-01-01

The utility of MS/MS for both target compound analysis and the structure elucidation of unknowns has been described in a number of references. A broader acceptance of this technique has not yet been realized as it requires large, complex, and costly instrumentation which has not been competitive with more conventional techniques. Recent advancements in ion trap mass spectrometry promise to change this situation. Although the ion trap's small size, sensitivity, and ability to perform multiple stages of mass spectrometry have made it eminently suitable for on-line, real-time monitoring applications, advance automation techniques are required to make these capabilities more accessible to non-experts. Towards this end we have developed custom software for the design and implementation of MS/MS experiments. This software allows the user to take full advantage of the ion trap's versatility with respect to ionization techniques, scan proxies, and ion accumulation/ejection methods. Additionally, expert system software has been developed for autonomous target compound analysis. This software has been linked to ion trap control software and a commercial data system to bring all of the steps in the analysis cycle under control of the expert system. These software development efforts and their utilization for a number of trace analysis applications will be described.

Metabolic Profiling of Hoodia, Chamomile, Terminalia Species and Evaluation of Commercial Preparations Using Ultrahigh-Performance Liquid Chromatography Quadrupole-Time-of-Flight Mass Spectrometry.

PubMed

Avula, Bharathi; Wang, Yan-Hong; Isaac, Giorgis; Yuk, Jimmy; Wrona, Mark; Yu, Kate; Khan, Ikhlas A

2017-11-01

Ultrahigh-performance liquid chromatography quadrupole-time-of-flight mass spectrometry (UHPLC-QToF-MS) profiling was used for the identification of marker compounds and generation of metabolic patterns that could be interrogated using chemometric modeling software. UHPLC-QToF-MS was used to generate comprehensive fingerprints of three botanicals ( Hoodia, Terminalia , and chamomile), each having different classes of compounds. Detection of a broad range of ions was carried out in full scan mode in both positive and negative modes over the range m/z 100-1700 using high-resolution mass spectrometry. Multivariate statistical analysis was used to extract relevant chemical information from the data to easily differentiate between Terminalia species, chamomile varieties, and quality control of Hoodia products. Using nontargeted analysis, identification of 37 compounds contributed to the differences between Terminalia species, 26 flavonoids were identified to show the differences between German and Roman chamomile, and 43 pregnane glycosides were identified from Hoodia gordonii samples. The UHPLC-QToF-MS-based chemical fingerprinting with principal component analysis was able to correctly distinguish botanicals and their commercial products. This work can be used as a basis to assure the quality of botanicals and commercial products. Georg Thieme Verlag KG Stuttgart · New York.

Comparison of divided and full pupil configurations for line-scanning confocal microscopy in human skin and oral mucosa

NASA Astrophysics Data System (ADS)

Larson, Bjorg; Abeytunge, Sanjeewa; Glazowski, Chris; Rajadhyaksha, Milind

2012-02-01

Confocal point-scanning microscopy has been showing promise in the detection, diagnosing and mapping of skin lesions in clinical settings. The noninvasive technique allows provides optical sectioning and cellular resolution for in vivo diagnosis of melanoma and basal cell carcinoma and pre-operative and intra-operative mapping of margins. The imaging has also enabled more accurate "guided" biopsies while minimizing the otherwise large number of "blind" biopsies. Despite these translational advances, however, point-scanning technology remains relatively complex and expensive. Line-scanning technology may offer an alternative approach to accelerate translation to the clinic. Line-scanning, using fewer optical components, inexpensive linear-array detectors and custom electronics, may enable smaller, simpler and lower-cost confocal microscopes. A line is formed using a cylindrical lens and scanned through the back focal plane of the objective with a galvanometric scanner. A linear CCD is used for detection. Two pupil configurations were compared for performance in imaging human tissue. In the full-pupil configuration, illumination and detection is made through the full objective pupil. In the divided pupil approach, half the pupil is illuminated and the other half is used for detection. The divided pupil configuration loses spatial and axial resolution due to a diminished NA, but the sectioning capability and rejection of background is improved. Imaging in skin and oral mucosa illustrate the performance of the two configurations.

Suspect screening of maternal serum to identify new environmental chemical biomonitoring targets using liquid chromatography-quadrupole time-of-flight mass spectrometry.

PubMed

Gerona, Roy R; Schwartz, Jackie M; Pan, Janet; Friesen, Matthew M; Lin, Thomas; Woodruff, Tracey J

2018-03-01

The use and advantages of high-resolution mass spectrometry (MS) as a discovery tool for environmental chemical monitoring has been demonstrated for environmental samples but not for biological samples. We developed a method using liquid chromatography-quadrupole time-of-flight MS (LC-QTOF/MS) for discovery of previously unmeasured environmental chemicals in human serum. Using non-targeted data acquisition (full scan MS analysis) we were able to screen for environmental organic acids (EOAs) in 20 serum samples from second trimester pregnant women. We define EOAs as environmental organic compounds with at least one dissociable proton which are utilized in commerce. EOAs include environmental phenols, phthalate metabolites, perfluorinated compounds, phenolic metabolites of polybrominated diphenyl ethers and polychlorinated biphenyls, and acidic pesticides and/or predicted acidic pesticide metabolites. Our validated method used solid phase extraction, reversed-phase chromatography in a C18 column with gradient elution, electrospray ionization in negative polarity and automated tandem MS (MS/MS) data acquisition to maximize true positive rates. We identified "suspect EOAs" using Agilent MassHunter Qualitative Analysis software, to match chemical formulas generated from each sample run with molecular formulas in our unique database of 693 EOAs assembled from multiple environmental literature sources. We found potential matches for 282 (41%) of the EOAs in our database. Sixty-five of these suspect EOAs were detected in at least 75% of the samples; only 19 of these compounds are currently biomonitored in National Health and Nutrition Examination Survey. We confirmed two of three suspect EOAs by LC-QTOF/MS using a targeted method developed through LC-MS/MS, reporting the first confirmation of benzophenone-1 and bisphenol S in pregnant women's sera. Our suspect screening workflow provides an approach to comprehensively scan environmental chemical exposures in humans. This can provide a better source of exposure information to help improve exposure and risk evaluation of industrial chemicals.

Pre-menarcheal physical activity predicts post-menarcheal lean mass and core strength, but not fat mass

PubMed Central

Day, M.A.; Dowthwaite, J.N.; Rosenbaum, P.F.; Roedel, G.G.; Brocker, A.A.; Scerpella, T.A.

2015-01-01

Objectives: Youth exercise is associated with improved body composition, but details regarding timing and persistence are limited. We examined pre- and circum-menarcheal organized physical activity exposure (PA) as a factor in development of early post-menarcheal lean mass, fat mass and muscle strength. Methods: Participants in a longitudinal study of musculoskeletal growth using dual energy X-ray absorptiometry (DXA) were included based on: 1) Whole body DXA scans: 0.5-1.5 years pre-menarche, 0.5-1.5 years post-menarche; 2) PA records for ≥6 months preceding the first DXA (PREPA) and for the inter-DXA interval (CIRCUMPA). Dominant arm grip strength and sit-ups tests coincided with DXA scans; PA, height and maturity were recorded semi-annually. Regressions correlated PA with lean mass/fat mass/strength, accounting for maturity, body size, and baseline values. Results Seventy girls [baseline: 11.8 yrs (sd 1.0), follow-up: 13.9 years (sd 1.0)] demonstrated circum-menarcheal gains of 25-29% for lean and fat mass and 33% for grip strength. PREPA correlated with pre- and post-menarcheal lean mass, sit-ups and pre-menarcheal fat mass (p<0.05), but not grip strength. CIRCUMPA correlated with only post-menarcheal sub-head lean mass (p=0.03). Conclusions: Lean mass and core strength at 1-year post-menarche were more strongly predicted by pre-menarcheal organized PA than by recent circum-menarcheal PA. PMID:26636280

Dual parallel mass spectrometry for lipid and vitamin D analysis

USDA-ARS?s Scientific Manuscript database

There are numerous options for mass spectrometric analysis of lipids, including different types of ionization, and a wide variety of experiments using different scan modes that can be conducted. Atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) provide complementary ...

Topic model-based mass spectrometric data analysis in cancer biomarker discovery studies.

PubMed

Wang, Minkun; Tsai, Tsung-Heng; Di Poto, Cristina; Ferrarini, Alessia; Yu, Guoqiang; Ressom, Habtom W

2016-08-18

A fundamental challenge in quantitation of biomolecules for cancer biomarker discovery is owing to the heterogeneous nature of human biospecimens. Although this issue has been a subject of discussion in cancer genomic studies, it has not yet been rigorously investigated in mass spectrometry based proteomic and metabolomic studies. Purification of mass spectometric data is highly desired prior to subsequent analysis, e.g., quantitative comparison of the abundance of biomolecules in biological samples. We investigated topic models to computationally analyze mass spectrometric data considering both integrated peak intensities and scan-level features, i.e., extracted ion chromatograms (EICs). Probabilistic generative models enable flexible representation in data structure and infer sample-specific pure resources. Scan-level modeling helps alleviate information loss during data preprocessing. We evaluated the capability of the proposed models in capturing mixture proportions of contaminants and cancer profiles on LC-MS based serum proteomic and GC-MS based tissue metabolomic datasets acquired from patients with hepatocellular carcinoma (HCC) and liver cirrhosis as well as synthetic data we generated based on the serum proteomic data. The results we obtained by analysis of the synthetic data demonstrated that both intensity-level and scan-level purification models can accurately infer the mixture proportions and the underlying true cancerous sources with small average error ratios (<7 %) between estimation and ground truth. By applying the topic model-based purification to mass spectrometric data, we found more proteins and metabolites with significant changes between HCC cases and cirrhotic controls. Candidate biomarkers selected after purification yielded biologically meaningful pathway analysis results and improved disease discrimination power in terms of the area under ROC curve compared to the results found prior to purification. We investigated topic model-based inference methods to computationally address the heterogeneity issue in samples analyzed by LC/GC-MS. We observed that incorporation of scan-level features have the potential to lead to more accurate purification results by alleviating the loss in information as a result of integrating peaks. We believe cancer biomarker discovery studies that use mass spectrometric analysis of human biospecimens can greatly benefit from topic model-based purification of the data prior to statistical and pathway analyses.

Muscle Mass Depletion Associated with Poor Outcome of Sepsis in the Emergency Department.

PubMed

Lee, YoonJe; Park, Hyun Kyung; Kim, Won Young; Kim, Myung Chun; Jung, Woong; Ko, Byuk Sung

2018-05-08

Muscle mass depletion has been suggested to predict morbidity and mortality in various diseases. However, it is not well known whether muscle mass depletion is associated with poor outcome in sepsis. We hypothesized that muscle mass depletion is associated with poor outcome in sepsis. Retrospective observational study was conducted in an emergency department during a 9-year period. Medical records of 627 patients with sepsis were reviewed. We divided the patients into 2 groups according to 28-day mortality and compared the presence of muscle mass depletion assessed by the cross-sectional area of the psoas muscle at the level of the third lumbar vertebra on abdomen CT scans. Univariate and multivariate logistic regression analyses were conducted to examine the association of scarcopenia on the outcome of sepsis. A total of 274 patients with sepsis were finally included in the study: 45 (16.4%) did not survive on 28 days and 77 patients (28.1%) were identified as having muscle mass depletion. The presence of muscle mass depletion was independently associated with 28-day mortality on multivariate logistic analysis (OR 2.79; 95% CI 1.35-5.74, p = 0.01). Muscle mass depletion evaluated by CT scan was associated with poor outcome of sepsis patients. Further studies on the appropriateness of specific treatment for muscle mass depletion with sepsis are needed. © 2018 S. Karger AG, Basel.

LC-MS Data Processing with MAVEN: A Metabolomic Analysis and Visualization Engine

PubMed Central

Clasquin, Michelle F.; Melamud, Eugene; Rabinowitz, Joshua D.

2014-01-01

MAVEN is an open-source software program for interactive processing of LC-MS-based metabolomics data. MAVEN enables rapid and reliable metabolite quantitation from multiple reaction monitoring data or high-resolution full-scan mass spectrometry data. It automatically detects and reports peak intensities for isotope-labeled metabolites. Menu-driven, click-based navigation allows visualization of raw and analyzed data. Here we provide a User Guide for MAVEN. Step-by-step instructions are provided for data import, peak alignment across samples, identification of metabolites that differ strongly between biological conditions, quantitation and visualization of isotope-labeling patterns, and export of tables of metabolite-specific peak intensities. Together, these instructions describe a workflow that allows efficient processing of raw LC-MS data into a form ready for biological analysis. PMID:22389014

LC-MS data processing with MAVEN: a metabolomic analysis and visualization engine.

PubMed

Clasquin, Michelle F; Melamud, Eugene; Rabinowitz, Joshua D

2012-03-01

MAVEN is an open-source software program for interactive processing of LC-MS-based metabolomics data. MAVEN enables rapid and reliable metabolite quantitation from multiple reaction monitoring data or high-resolution full-scan mass spectrometry data. It automatically detects and reports peak intensities for isotope-labeled metabolites. Menu-driven, click-based navigation allows visualization of raw and analyzed data. Here we provide a User Guide for MAVEN. Step-by-step instructions are provided for data import, peak alignment across samples, identification of metabolites that differ strongly between biological conditions, quantitation and visualization of isotope-labeling patterns, and export of tables of metabolite-specific peak intensities. Together, these instructions describe a workflow that allows efficient processing of raw LC-MS data into a form ready for biological analysis.

The Atmosphere of Mars and the MAVEN Mission: Cross-calibrating NGIMS and IUVS

NASA Astrophysics Data System (ADS)

AlAwar, Khalid; Lillis, Robert; Fillingim, Matthew

2016-10-01

The Mars Atmosphere and Volatile EvolutioN (MAVEN) has two instruments which are used to determine the neutral gas composition of Mars atmosphere: the Imaging UltraViolet Spectrograph (IUVS) and the Neutral Gas and Ion Mass Spectrometer (NGIMS). A detailed comparison between the two is needed in order to verify the integrity of both datasets.Our approach is divided into two stages. First, we compare neutral densities measured by NGIMS in situ and those derived from remote scans of the nearby planetary limb by IUVS, both taken at periapsis. The data resulting from the comparison show that the data is consistent between the two instruments for periapsis near the subsolar point The second stage is to validate the retrievals from the IUVS FUV scans of the Martian disk made from apoapsis by comparing with the NGIMS in situ density measurements. We first process the NGIMS data to be in the same units as the disk scan, i.e. ratios of CO2/CO and CO2/O in the topside column in which the altitude-integrated number density of CO2 is 1016 , cm-2). Since NGIMS is taken at periapsis and IUVS Disk scans are taken at apoapsis, it is not possible to compare data results from the same or nearby orbits. Ideally, it would be best to compare data at the same seasons, however this is not possible because MAVEN has not yet completed a full martian year. Our approach to overcome this obstacle was to review all times where valid data is available and examine data sets occurring at similar environmental conditions. We will present these results.

Longitudinal DXA Studies: Minimum scanning interval for pediatric assessment of body fat

USDA-ARS?s Scientific Manuscript database

The increased prevalence of obesity in the United States, has led to the increased use of dual-energy X-ray absorptiometry (DXA) for assessment of body fat mass (TBF) in pediatric populations. We examined DXA precision, in order to determine suitable scanning intervals for the measurement of change...

Precursor Ion Scan Mode-Based Strategy for Fast Screening of Polyether Ionophores by Copper-Induced Gas-Phase Radical Fragmentation Reactions.

PubMed

Crevelin, Eduardo J; Possato, Bruna; Lopes, João L C; Lopes, Norberto P; Crotti, Antônio E M

2017-04-04

The potential of copper(II) to induce gas-phase fragmentation reactions in macrotetrolides, a class of polyether ionophores produced by Streptomyces species, was investigated by accurate-mass electrospray tandem mass spectrometry (ESI-MS/MS). Copper(II)/copper(I) transition directly induced production of diagnostic acylium ions with m/z 199, 185, 181, and 167 from α-cleavages of [macrotetrolides + Cu] 2+ . A UPLC-ESI-MS/MS methodology based on the precursor ion scan of these acylium ions was developed and successfully used to identify isodinactin (1), trinactin (2), and tetranactin (3) in a crude extract of Streptomyces sp. AMC 23 in the precursor ion scan mode. In addition, copper(II) was also used to induce radical fragmentation reactions in the carboxylic acid polyether ionophore nigericin. The resulting product ions with m/z 755 and 585 helped to identify nigericin in a crude extract of Streptomyces sp. Eucal-26 by means of precursor ion scan experiments, demonstrating that copper-induced fragmentation reactions can potentially identify different classes of polyether ionophores rapidly and selectively.

Submicron mass spectrometry imaging of single cells by combined use of mega electron volt time-of-flight secondary ion mass spectrometry and scanning transmission ion microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siketić, Zdravko; Bogdanović Radović, Ivančica; Jakšić, Milko

In order to better understand biochemical processes inside an individual cell, it is important to measure the molecular composition at the submicron level. One of the promising mass spectrometry imaging techniques that may be used to accomplish this is Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS), using MeV energy heavy ions for excitation. MeV ions have the ability to desorb large intact molecules with a yield that is several orders of magnitude higher than conventional SIMS using keV ions. In order to increase the spatial resolution of the MeV TOF-SIMS system, we propose an independent TOF trigger using a STIM (scanningmore » transmission ion microscopy) detector that is placed just behind the thin transmission target. This arrangement is suitable for biological samples in which the STIM detector simultaneously measures the mass distribution in scanned samples. The capability of the MeV TOF-SIMS setup was demonstrated by imaging the chemical composition of CaCo-2 cells.« less

Automated and real-time segmentation of suspicious breast masses using convolutional neural network

PubMed Central

Gregory, Adriana; Denis, Max; Meixner, Duane D.; Bayat, Mahdi; Whaley, Dana H.; Fatemi, Mostafa; Alizad, Azra

2018-01-01

In this work, a computer-aided tool for detection was developed to segment breast masses from clinical ultrasound (US) scans. The underlying Multi U-net algorithm is based on convolutional neural networks. Under the Mayo Clinic Institutional Review Board protocol, a prospective study of the automatic segmentation of suspicious breast masses was performed. The cohort consisted of 258 female patients who were clinically identified with suspicious breast masses and underwent clinical US scan and breast biopsy. The computer-aided detection tool effectively segmented the breast masses, achieving a mean Dice coefficient of 0.82, a true positive fraction (TPF) of 0.84, and a false positive fraction (FPF) of 0.01. By avoiding positioning of an initial seed, the algorithm is able to segment images in real time (13–55 ms per image), and can have potential clinical applications. The algorithm is at par with a conventional seeded algorithm, which had a mean Dice coefficient of 0.84 and performs significantly better (P< 0.0001) than the original U-net algorithm. PMID:29768415

An automated gas chromatography time-of-flight mass spectrometry instrument for the quantitative analysis of halocarbons in air

NASA Astrophysics Data System (ADS)

Obersteiner, F.; Bönisch, H.; Engel, A.

2016-01-01

We present the characterization and application of a new gas chromatography time-of-flight mass spectrometry instrument (GC-TOFMS) for the quantitative analysis of halocarbons in air samples. The setup comprises three fundamental enhancements compared to our earlier work (Hoker et al., 2015): (1) full automation, (2) a mass resolving power R = m/Δm of the TOFMS (Tofwerk AG, Switzerland) increased up to 4000 and (3) a fully accessible data format of the mass spectrometric data. Automation in combination with the accessible data allowed an in-depth characterization of the instrument. Mass accuracy was found to be approximately 5 ppm in mean after automatic recalibration of the mass axis in each measurement. A TOFMS configuration giving R = 3500 was chosen to provide an R-to-sensitivity ratio suitable for our purpose. Calculated detection limits are as low as a few femtograms by means of the accurate mass information. The precision for substance quantification was 0.15 % at the best for an individual measurement and in general mainly determined by the signal-to-noise ratio of the chromatographic peak. Detector non-linearity was found to be insignificant up to a mixing ratio of roughly 150 ppt at 0.5 L sampled volume. At higher concentrations, non-linearities of a few percent were observed (precision level: 0.2 %) but could be attributed to a potential source within the detection system. A straightforward correction for those non-linearities was applied in data processing, again by exploiting the accurate mass information. Based on the overall characterization results, the GC-TOFMS instrument was found to be very well suited for the task of quantitative halocarbon trace gas observation and a big step forward compared to scanning, quadrupole MS with low mass resolving power and a TOFMS technique reported to be non-linear and restricted by a small dynamical range.

Dark matter interpretations of ATLAS searches for the electroweak production of supersymmetric particles in s = 8 $$ \\sqrt{s}=8 $$ TeV proton-proton collisions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aaboud, M.; Aad, G.; Abbott, B.

2016-09-01

A selection of searches by the ATLAS experiment at the LHC for the electroweak production of SUSY particles are used to study their impact on the constraints on dark matter candidates. The searches use 20 fb-1 of proton-proton collision data at s√=8s=8 TeV. A likelihood-driven scan of a five-dimensional effective model focusing on the gaugino-higgsino and Higgs sector of the phenomenological minimal supersymmetric Standard Model is performed. This scan uses data from direct dark matter detection experiments, the relic dark matter density and precision flavour physics results. Further constraints from the ATLAS Higgs mass measurement and SUSY searches at LEPmore » are also applied. A subset of models selected from this scan are used to assess the impact of the selected ATLAS searches in this five-dimensional parameter space. These ATLAS searches substantially impact those models for which the mass m(χ~01)m(χ~10) of the lightest neutralino is less than 65 GeV, excluding 86% of such models. The searches have limited impact on models with larger m(χ~01)m(χ~10) due to either heavy electroweakinos or compressed mass spectra where the mass splittings between the produced particles and the lightest supersymmetric particle is small.« less

Dark matter interpretations of ATLAS searches for the electroweak production of supersymmetric particles in $$ \\sqrt{s}=8 $$ TeV proton-proton collisions

DOE PAGES

Aaboud, M.; Aad, G.; Abbott, B.; ...

2016-09-30

A selection of searches by the ATLAS experiment at the LHC for the electroweak production of SUSY particles are used to study their impact on the constraints on dark matter candidates. The searches use 20 fb -1 of proton-proton collision data at √s=8 TeV. A likelihood-driven scan of a five-dimensional effective model focusing on the gaugino-higgsino and Higgs sector of the phenomenological minimal supersymmetric Standard Model is performed. This scan uses data from direct dark matter detection experiments, the relic dark matter density and precision flavour physics results. Further constraints from the ATLAS Higgs mass measurement and SUSY searches at LEP are also applied. A subset of models selected from this scan are used to assess the impact of the selected ATLAS searches in this five-dimensional parameter space. These ATLAS searches substantially impact those models for which the mass m(more » $$\\tilde{χ}$$$0\\atop{1}$$) of the lightest neutralino is less than 65 GeV, excluding 86% of such models. The searches have limited impact on models with larger m($$\\tilde{χ}$$$0\\atop{1}$$) due to either heavy electroweakinos or compressed mass spectra where the mass splittings between the produced particles and the lightest supersymmetric particle is small.« less

Method for dose-reduced 3D catheter tracking on a scanning-beam digital x-ray system using dynamic electronic collimation

NASA Astrophysics Data System (ADS)

Dunkerley, David A. P.; Funk, Tobias; Speidel, Michael A.

2016-03-01

Scanning-beam digital x-ray (SBDX) is an inverse geometry x-ray fluoroscopy system capable of tomosynthesis-based 3D catheter tracking. This work proposes a method of dose-reduced 3D tracking using dynamic electronic collimation (DEC) of the SBDX scanning x-ray tube. Positions in the 2D focal spot array are selectively activated to create a regionof- interest (ROI) x-ray field around the tracked catheter. The ROI position is updated for each frame based on a motion vector calculated from the two most recent 3D tracking results. The technique was evaluated with SBDX data acquired as a catheter tip inside a chest phantom was pulled along a 3D trajectory. DEC scans were retrospectively generated from the detector images stored for each focal spot position. DEC imaging of a catheter tip in a volume measuring 11.4 cm across at isocenter required 340 active focal spots per frame, versus 4473 spots in full-FOV mode. The dose-area-product (DAP) and peak skin dose (PSD) for DEC versus full field-of-view (FOV) scanning were calculated using an SBDX Monte Carlo simulation code. DAP was reduced to 7.4% to 8.4% of the full-FOV value, consistent with the relative number of active focal spots (7.6%). For image sequences with a moving catheter, PSD was 33.6% to 34.8% of the full-FOV value. The root-mean-squared-deviation between DEC-based 3D tracking coordinates and full-FOV 3D tracking coordinates was less than 0.1 mm. The 3D distance between the tracked tip and the sheath centerline averaged 0.75 mm. Dynamic electronic collimation can reduce dose with minimal change in tracking performance.

Validity and reliability of total body volume and relative body fat mass from a 3-dimensional photonic body surface scanner

PubMed Central

Mähler, Anja; Boschmann, Michael; Jeran, Stephanie

2017-01-01

Objective Three-dimensional photonic body surface scanners (3DPS) feature a tool to estimate total body volume (BV) from 3D images of the human body, from which the relative body fat mass (%BF) can be calculated. However, information on validity and reliability of these measurements for application in epidemiological studies is limited. Methods Validity was assessed among 32 participants (men, 50%) aged 20–58 years. BV and %BF were assessed using a 3DPS (VitusSmart XXL) and air displacement plethysmography (ADP) with a BOD POD® device using equations by Siri and Brozek. Three scans were obtained per participant (standard, relaxed, exhaled scan). Validity was evaluated based on the agreement of 3DPS with ADP using Bland Altman plots, correlation analysis and Wilcoxon signed ranks test for paired samples. Reliability was investigated in a separate sample of 18 participants (men, 67%) aged 25–66 years using intraclass correlation coefficients (ICC) based on two repeated 3DPS measurements four weeks apart. Results Mean BV and %BF were higher using 3DPS compared to ADP, (3DPS-ADP BV difference 1.1 ± 0.9 L, p<0.01; %BF difference 7.0 ± 5.6, p<0.01), yet the disagreement was not associated with gender, age or body mass index (BMI). Reliability was excellent for 3DPS BV (ICC, 0.998) and good for 3DPS %BF (ICC, 0.982). Results were similar for the standard scan and the relaxed scan but somewhat weaker for the exhaled scan. Conclusions Although BV and %BF are higher than ADP measurements, our data indicate good validity and reliability for an application of 3DPS in epidemiological studies. PMID:28672039

Validity and reliability of total body volume and relative body fat mass from a 3-dimensional photonic body surface scanner.

PubMed

Adler, Carolin; Steinbrecher, Astrid; Jaeschke, Lina; Mähler, Anja; Boschmann, Michael; Jeran, Stephanie; Pischon, Tobias

2017-01-01

Three-dimensional photonic body surface scanners (3DPS) feature a tool to estimate total body volume (BV) from 3D images of the human body, from which the relative body fat mass (%BF) can be calculated. However, information on validity and reliability of these measurements for application in epidemiological studies is limited. Validity was assessed among 32 participants (men, 50%) aged 20-58 years. BV and %BF were assessed using a 3DPS (VitusSmart XXL) and air displacement plethysmography (ADP) with a BOD POD® device using equations by Siri and Brozek. Three scans were obtained per participant (standard, relaxed, exhaled scan). Validity was evaluated based on the agreement of 3DPS with ADP using Bland Altman plots, correlation analysis and Wilcoxon signed ranks test for paired samples. Reliability was investigated in a separate sample of 18 participants (men, 67%) aged 25-66 years using intraclass correlation coefficients (ICC) based on two repeated 3DPS measurements four weeks apart. Mean BV and %BF were higher using 3DPS compared to ADP, (3DPS-ADP BV difference 1.1 ± 0.9 L, p<0.01; %BF difference 7.0 ± 5.6, p<0.01), yet the disagreement was not associated with gender, age or body mass index (BMI). Reliability was excellent for 3DPS BV (ICC, 0.998) and good for 3DPS %BF (ICC, 0.982). Results were similar for the standard scan and the relaxed scan but somewhat weaker for the exhaled scan. Although BV and %BF are higher than ADP measurements, our data indicate good validity and reliability for an application of 3DPS in epidemiological studies.

THE MASS ACCOMMODATION COEFFICIENT OF AMMONIUM NITRATE AEROSOL. (R823514)

EPA Science Inventory

The mass transfer rate of pure ammonium nitrate between the aerosol and gas phases was
quantified experimentally by the use of the tandem differential mobility analyzer/scanning mobility
particle sizer (TDMA/SMPS) technique. Ammonium nitrate particles 80-220 nm in diameter<...

Determination of densified biomass mass properties using 3D laser scanning and image analysis

USDA-ARS?s Scientific Manuscript database

Biomass densification is viewed as the indispensable feedstock preprocessing operation for efficient transport, storage, material flow through machines, and handling activities. Accurate mass properties of densified biomass such as surface area, volume, and envelope density form fundamental data for...

Cluster formation in laser-induced ablation and evaporation of solids observed by laser ionization time-of-flight mass spectrometry and scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Tench, R. J.; Balooch, M.; Bernardez, L.; Allen, Mike J.; Siekhaus, W. J.; Olander, D. R.; Wang, W.

1990-04-01

Laser ionization time-of-flight mass analysis (LIMA) used pulses (5ns) of a frequency-quadrupled Nd-YAG laser (266 nm) focused onto spots of 4 to 100 microns diameter to ablate material, and a reflectron time of flight tube to mass-analyze the plume. The observed mass spectra for Si, Pt, SiC, and UO 2 varied in the distribution of ablation products among atoms, molecules and clusters, depending on laser power density and target material. Cleaved surfaces of highly oriented pyrolytic graphite (HOPG) positioned at room temperature either 10 cm away from materials ablated at 10(exp -5) Torr by 1 to 3 excimer laser (308 nm) pulses of 20 ns duration or 1 m away from materials vaporized at 10(exp -8) Torr by 10 Nd-Glass laser pulses of 1 ms duration were analyzed by Scanning Tunneling Microscopy (STM) in air with angstrom resolution. Clusters up to 30 A in diameter were observed.

Aerial thermography for energy conservation

NASA Technical Reports Server (NTRS)

Jack, J. R.

1978-01-01

Thermal infrared scanning from an aircraft is a convenient and commercially available means for determining relative rates of energy loss from building roofs. The need to conserve energy as fuel costs makes the mass survey capability of aerial thermography an attractive adjunct to community energy awareness programs. Background information on principles of aerial thermography is presented. Thermal infrared scanning systems, flight and environmental requirements for data acquisition, preparation of thermographs for display, major users and suppliers of thermography, and suggested specifications for obtaining aerial scanning services were reviewed.

Assessment of the relationship between renal volume and renal function after minimally-invasive partial nephrectomy: the role of computed tomography and nuclear renal scan.

PubMed

Bertolo, Riccardo; Fiori, Cristian; Piramide, Federico; Amparore, Daniele; Barrera, Monica; Sardo, Diego; Veltri, Andrea; Porpiglia, Francesco

2018-05-14

To evaluate the correlation between the loss of renal function as assessed by Tc99MAG-3 renal scan and the loss of renal volume as calculated by volumetric assessment on CT-scan in patients who underwent minimally-invasive partial nephrectomy (PN). PN prospectively-maintained database was retrospectively queried for patients who underwent minimally-invasive PN (2012-2017) for renal mass

Categorisation of full waveform data provided by laser scanning devices

NASA Astrophysics Data System (ADS)

Ullrich, Andreas; Pfennigbauer, Martin

2011-11-01

In 2004, a laser scanner device for commercial airborne laser scanning applications, the RIEGL LMS-Q560, was introduced to the market, making use of a radical alternative approach to the traditional analogue signal detection and processing schemes found in LIDAR instruments so far: digitizing the echo signals received by the instrument for every laser pulse and analysing these echo signals off-line in a so-called full waveform analysis in order to retrieve almost all information contained in the echo signal using transparent algorithms adaptable to specific applications. In the field of laser scanning the somewhat unspecific term "full waveform data" has since been established. We attempt a categorisation of the different types of the full waveform data found in the market. We discuss the challenges in echo digitization and waveform analysis from an instrument designer's point of view and we will address the benefits to be gained by using this technique, especially with respect to the so-called multi-target capability of pulsed time-of-flight LIDAR instruments.

Active Brown Fat During 18F-FDG PET/CT Imaging Defines a Patient Group with Characteristic Traits and an Increased Probability of Brown Fat Redetection.

PubMed

Gerngroß, Carlos; Schretter, Johanna; Klingenspor, Martin; Schwaiger, Markus; Fromme, Tobias

2017-07-01

Brown adipose tissue (BAT) provides a means of nonshivering thermogenesis. In humans, active BAT can be visualized by 18 F-FDG uptake as detected by PET combined with CT. The retrospective analysis of clinical scans is a valuable source to identify anthropometric parameters that influence BAT mass and activity and thus the potential efficacy of envisioned drugs targeting this tissue to treat metabolic disease. Methods: We analyzed 2,854 18 F-FDG PET/CT scans from 1,644 patients and identified 98 scans from 81 patients with active BAT. We quantified the volume of active BAT depots (mean values in mL ± SD: total BAT, 162 ± 183 [ n = 98]; cervical, 40 ± 37 [ n = 53]; supraclavicular, 66 ± 68 [ n = 71]; paravertebral, 51 ± 53 [ n = 69]; mediastinal, 43 ± 40 [ n = 51]; subphrenic, 21 ± 21 [ n = 29]). Because only active BAT is detectable by 18 F-FDG uptake, these numbers underestimate the total amount of BAT. Considering only 32 scans of the highest activity as categorized by a visual scoring strategy, we determined a mean total BAT volume of 308 ± 208 mL. In 30 BAT-positive patients with 3 or more repeated scans, we calculated a much higher mean probability to redetect active BAT (52% ± 25%) as compared with the overall prevalence of 4.9%. We calculated a BAT activity index (BFI) based on volume and intensity of individual BAT depots. Results: We detected higher total BFI in younger patients ( P = 0.009), whereas sex, body mass index, height, mass, outdoor temperature, and blood parameters did not affect total or depot-specific BAT activity. Surprisingly, renal creatinine clearance as estimated from mass, age, and plasma creatinine was a significant predictor of BFI on the total ( P = 0.005) as well as on the level of several individual depots. In summary, we detected a high amount of more than 300 mL of BAT tissue. Conclusion: BAT-positive patients represent a group with a higher than usual probability to activate BAT during a scan. Estimated renal creatinine clearance correlated with the extent of activated BAT in a given scan. These data imply an efficacy of drugs targeting BAT to treat metabolic disease that is at the same time higher and subject to a larger individual variation than previously assumed. © 2017 by the Society of Nuclear Medicine and Molecular Imaging.

Contributions of lean mass and fat mass to bone mineral density: a study in postmenopausal women.

PubMed

Ho-Pham, Lan T; Nguyen, Nguyen D; Lai, Thai Q; Nguyen, Tuan V

2010-03-26

The relative contribution of lean and fat to the determination of bone mineral density (BMD) in postmenopausal women is a contentious issue. The present study was undertaken to test the hypothesis that lean mass is a better determinant of BMD than fat mass. This cross-sectional study involved 210 postmenopausal women of Vietnamese background, aged between 50 and 85 years, who were randomly sampled from various districts in Ho Chi Minh City (Vietnam). Whole body scans, femoral neck, and lumbar spine BMD were measured by DXA (QDR 4500, Hologic Inc., Waltham, MA). Lean mass (LM) and fat mass (FM) were derived from the whole body scan. Furthermore, lean mass index (LMi) and fat mass index (FMi) were calculated as ratio of LM or FM to body height in metre squared (m2). In multiple linear regression analysis, both LM and FM were independent and significant predictors of BMD at the spine and femoral neck. Age, lean mass and fat mass collectively explained 33% variance of lumbar spine and 38% variance of femoral neck BMD. Replacing LM and FM by LMi and LMi did not alter the result. In both analyses, the influence of LM or LMi was greater than FM and FMi. Simulation analysis suggested that a study with 1000 individuals has a 78% chance of finding the significant effects of both LM and FM, and a 22% chance of finding LM alone significant, and zero chance of finding the effect of fat mass alone. These data suggest that both lean mass and fat mass are important determinants of BMD. For a given body size -- measured either by lean mass or height --women with greater fat mass have greater BMD.

A New Method to Obtain the Black Carbon Mixing State of Biomass and Combustion Aerosols

NASA Astrophysics Data System (ADS)

Irwin, M.; Liu, D.; Joshi, R.; Allan, J. D.; Coe, H.; Flynn, M.; Olfert, J. S.; Broda, K.; Fu, P.; Sun, Y.; Ge, X.; Wang, J.

2017-12-01

Black carbon particles (BC) significantly contribute to warming effects in the atmosphere, altering weather systems, and pose significant health risks. These impacts are especially efficient at regional hotspots with high emissions of pollutants, such as in fast-developing megacities. These urban environments have the most population exposure, and improving the understanding of the sources and the processing of pollutants in these environments is critical in guiding policy making. Here we present the results of BC characterization in Beijing during the winter of 2016 (10th Nov-10th Dec), as part of a large joint UK-China field experiment. During this experiment, we successfully gathered 4 weeks of continuous measurements, including several severe pollution events in Beijing. MethodologyThe mixing state of BC, which is how BC is associated with non-BC material (its coating) within a particle, is crucial to determine its lifetime in the atmosphere and also its optical properties. However precisely quantifying the BC mixing state has posed a challenge, in part due to complex particle morphology. We have applied morphology-independent measurements of BC mixing state on a single-particle basis throughout this experiment: mono-dispersed particle mass (MP) is selected using a Centrifugal Particle Mass Analyser (CPMA, Cambustion Ltd) and a single particle soot photometer (SP2, DMT inc.) was used downstream of the CPMA to measure the refractory BC mass (MrBC). The full scan of CPMA masses (21 mass bins covering most of MP) are performed every half hour, following polydispersed particles measured without running CPMA.

Identification of multiple constituents in Chinese medicinal prescription Shensong Yangxin capsule by ultra-fast liquid chromatography combined with quadrupole time-of-flight mass spectrometry.

PubMed

Liu, Minyan; Zhao, Shaohua; Wang, Yufeng; Liu, Ting; Li, Song; Wang, Hongtao; Tu, Pengfei

2015-02-01

A practical method using ultra-fast liquid chromatography in tandem with quadrupole time-of-flight mass spectrometry combined with dynamic background subtraction technology was developed for the rapid separation and identification of the complicated constituents in the Shensong Yangxin capsule (SSYX). The chromatographic separation was performed on a C18 column (2.1 × 100 mm, 2.6 μm) with a gradient elution program using methanol and 0.1% formic acid aqueous solution as the mobile phase at a flow rate of 0.4 mL min(-1). Accurate mass measurements of the molecular ions in the full scan and the characteristic fragment ions triggered by information-dependent acquisition provided reliable identification criteria. Thus, 99 compounds, including saponins, phenolic acids, tanshinones, lignans, terpenoids, alkaloids and flavonoids, were unambiguously or tentatively identified in 40 min by comparing their retention times and accurate mass measurements for each molecular ion and its subsequent fragment ions with those of authentic standards or literature data. Simultaneously, all the compounds were further assigned to the individual raw materials. In conclusion, these results will provide a basis for quality control and further study of SSYX, and the proposed technique based on high-resolution mass spectrometry would be expected to be adaptable to the analysis of complicated constituents in various complex matrices. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Wide-range screening of psychoactive substances by FIA-HRMS: identification strategies.

PubMed

Alechaga, Élida; Moyano, Encarnación; Galceran, Maria Teresa

2015-06-01

Recreational drugs (illicit drugs, human and veterinary medicines, legal highs, etc.) often contain lacing agents and adulterants which are not related to the main active ingredient. Serious side effects and even the death of the consumer have been related to the consumption of mixtures of psychoactive substances and/or adulterants, so it is important to know the actual composition of recreational drugs. In this work, a method based on flow injection analysis (FIA) coupled with high-resolution mass spectrometry (HRMS) is proposed for the fast identification of psychoactive substances in recreational drugs and legal highs. The FIA and HRMS working conditions were optimized in order to detect a wide range of psychoactive compounds. As most of the psychoactive substances are acid-base compounds, methanol-0.1 % aqueous formic acid (1:1 v/v) as a carrier solvent and electrospray in both positive ion mode and negative ion mode were used. Two data acquisition modes, full scan at high mass resolution (HRMS) and data-dependent tandem mass spectrometry (ddMS/HRMS) with a quadrupole-Orbitrap mass analyzer were used, resulting in sufficient selectivity for identification of the components of the samples. A custom-made database containing over 450 substances, including psychoactive compounds and common adulterants, was built to perform a high-throughput target and suspect screening. Moreover, online accurate mass databases and mass fragmenter software were used to identify unknowns. Some examples, selected among the analyzed samples of recreational drugs and legal highs using the FIA-HRMS(ddMS/HRMS) method developed, are discussed to illustrate the screening strategy used in this study. The results showed that many of the analyzed samples were adulterated, and in some cases the sample composition did not match that of the supposed marketed substance.

Cerebral edema, mass effects, and regional blood volume in man.

PubMed

Penn, R D; Kurtz, D

1977-03-01

The authors conducted quantitative analysis of computerized tomography (CT) scans to measure tumor size, cerebral edema, and regional blood volume in man. Mass lesions without edema caused a local reduction in blood volume. Cerebral edema also reduced blood volume in proportion to its severity. Consideration of the electrolyte changes and water shifts in white-matter edema suggested that the decrease in absorption coefficient seen in CT scans was due to the increase in water content. Thus, in cerebral edema separation of blood vessels as well as increased interstitial pressure decrease blood volume, and the regional differences in turn reflect pressure gradients within the brain.

Multimodal Registration of White Matter Brain Data via Optimal Mass Transport.

PubMed

Rehman, Tauseefur; Haber, Eldad; Pohl, Kilian M; Haker, Steven; Halle, Mike; Talos, Florin; Wald, Lawrence L; Kikinis, Ron; Tannenbaum, Allen

2008-09-01

The elastic registration of medical scans from different acquisition sequences is becoming an important topic for many research labs that would like to continue the post-processing of medical scans acquired via the new generation of high-field-strength scanners. In this note, we present a parameter-free registration algorithm that is well suited for this scenario as it requires no tuning to specific acquisition sequences. The algorithm encompasses a new numerical scheme for computing elastic registration maps based on the minimizing flow approach to optimal mass transport. The approach utilizes all of the gray-scale data in both images, and the optimal mapping from image A to image B is the inverse of the optimal mapping from B to A . Further, no landmarks need to be specified, and the minimizer of the distance functional involved is unique. We apply the algorithm to register the white matter folds of two different scans and use the results to parcellate the cortex of the target image. To the best of our knowledge, this is the first time that the optimal mass transport function has been applied to register large 3D multimodal data sets.

Multimodal Registration of White Matter Brain Data via Optimal Mass Transport

PubMed Central

Rehman, Tauseefur; Haber, Eldad; Pohl, Kilian M.; Haker, Steven; Halle, Mike; Talos, Florin; Wald, Lawrence L.; Kikinis, Ron; Tannenbaum, Allen

2017-01-01

The elastic registration of medical scans from different acquisition sequences is becoming an important topic for many research labs that would like to continue the post-processing of medical scans acquired via the new generation of high-field-strength scanners. In this note, we present a parameter-free registration algorithm that is well suited for this scenario as it requires no tuning to specific acquisition sequences. The algorithm encompasses a new numerical scheme for computing elastic registration maps based on the minimizing flow approach to optimal mass transport. The approach utilizes all of the gray-scale data in both images, and the optimal mapping from image A to image B is the inverse of the optimal mapping from B to A. Further, no landmarks need to be specified, and the minimizer of the distance functional involved is unique. We apply the algorithm to register the white matter folds of two different scans and use the results to parcellate the cortex of the target image. To the best of our knowledge, this is the first time that the optimal mass transport function has been applied to register large 3D multimodal data sets. PMID:28626844

Portable, Battery Operated Capillary Electrophoresis with Optical Isomer Resolution Integrated with Ionization Source for Mass Spectrometry

NASA Astrophysics Data System (ADS)

Moini, Mehdi; Rollman, Christopher M.

2016-03-01

We introduce a battery operated capillary electrophoresis electrospray ionization (CE/ESI) source for mass spectrometry with optical isomer separation capability. The source fits in front of low or high resolution mass spectrometers similar to a nanospray source with about the same weight and size. The source has two high voltage power supplies (±25 kV HVPS) capable of operating in forward or reverse polarity modes and powered by a 12 V rechargeable lithium ion battery with operation time of ~10 h. In ultrafast CE mode, in which short narrow capillaries (≤15 μm i.d., 15-25 cm long) and field gradients ≥1000 V/cm are used, peak widths at the base are <1 s wide. Under these conditions, the source provides high resolution separation, including optical isomer resolution in ~1 min. Using a low resolution mass spectrometer (LTQ Velos) with a scan time of 0.07 s/scan, baseline separation of amino acids and their optical isomers were achieved in ~1 min. Moreover, bovine serum albumin (BSA) was analyzed in ~1 min with 56% coverage using the data-dependent MS/MS. Using a high resolution mass spectrometer (Thermo Orbitrap Elite) with 15,000 resolution, the fastest scan time achieved was 0.15 s, which was adequate for CE-MS analysis when optical isomer separation is not required or when the optical isomers were well separated. Figures of merit including a detection limit of 2 fmol and linear dynamic range of two orders of magnitude were achieved for amino acids.

Protein/Arabinoxylans Gels: Effect of mass ratio on the rheological, microstructural and diffusional characteristics

USDA-ARS?s Scientific Manuscript database

Arabinoxylan (AX) gels entrapping standard model proteins at different mass ratios were formed. The distribution of protein through the network was investigated by confocal laser scanning microscopy (CLSM). In mixed gels, protein aggregates forming clusters were detected at protein/polysaccharide ra...

Highly reproducible laser beam scanning device for an internal source laser desorption microprobe Fourier transform mass spectrometer

NASA Astrophysics Data System (ADS)

Scott, Jill R.; Tremblay, Paul L.

2002-03-01

Traditionally, mass spectrometry has relied on manipulating the sample target to provide scanning capabilities for laser desorption microprobes. This has been problematic for an internal source laser desorption Fourier transform mass spectrometer (LD-FTMS) because of the high magnetic field (7 Tesla) and geometric constraints of the superconducting magnet bore. To overcome these limitations, we have implemented a unique external laser scanning mechanism for an internal source LD-FTMS. This mechanism provides adjustable resolution enhancement so that the spatial resolution at the target is not limited to that of the stepper motors at the light source (˜5 μm/step). The spatial resolution is now limited by the practical optical diffraction limit of the final focusing lens. The scanning mechanism employs a virtual source that is wavelength independent up to the final focusing lens, which can be controlled remotely to account for focal length dependence on wavelength. A binary index provides an automatic alignment feature. The virtual source is located ˜9 ft from the sample; therefore, it is completely outside of the vacuum system and beyond the 50 G line of the fringing magnetic field. To eliminate reproducibility problems associated with vacuum pump vibrations, we have taken advantage of the magnetic field inherent to the FTMS to utilize Lenz's law for vibrational dampening. The LD-FTMS microprobe has exceptional reproducibility, which enables successive mapping sequences for depth-profiling studies.

Diagnostic value of a pancreatic mass on computed tomography in patients undergoing pancreatoduodenectomy for presumed pancreatic cancer.

PubMed

Gerritsen, Arja; Bollen, Thomas L; Nio, C Yung; Molenaar, I Quintus; Dijkgraaf, Marcel G W; van Santvoort, Hjalmar C; Offerhaus, G Johan; Brosens, Lodewijk A; Biermann, Katharina; Sieders, Egbert; de Jong, Koert P; van Dam, Ronald M; van der Harst, Erwin; van Goor, Harry; van Ramshorst, Bert; Bonsing, Bert A; de Hingh, Ignace H; Gerhards, Michael F; van Eijck, Casper H; Gouma, Dirk J; Borel Rinkes, Inne H M; Busch, Olivier R C; Besselink, Marc G H

2015-07-01

Previous studies have shown that 5-14% of patients undergoing pancreatoduodenectomy for suspected malignancy ultimately are diagnosed with benign disease. A "pancreatic mass" on computed tomography (CT) is considered to be the strongest predictor of malignancy, but studies describing its diagnostic value are lacking. The aim of this study was to determine the diagnostic value of a pancreatic mass on CT in patients with presumed pancreatic cancer, as well as the interobserver agreement among radiologists and the additional value of reassessment by expert-radiologists. Reassessment of preoperative CT scans was performed within a previously described multicenter retrospective cohort study in 344 patients undergoing pancreatoduodenectomy for suspected malignancy (2003-2010). Preoperative CT scans were reassessed by 2 experienced abdominal radiologists separately and subsequently in a consensus meeting, after defining a pancreatic mass as "a measurable space occupying soft tissue density, except for an enlarged papilla or focal steatosis". CT scans of 86 patients with benign and 258 patients with (pre)malignant disease were reassessed. In 66% of patients a pancreatic mass was reported in the original CT report, versus 48% and 50% on reassessment by the 2 expert radiologists separately and 44% in consensus (P < .001 vs original report). Interobserver agreement between the original CT report and expert consensus was fair (kappa = 0.32, 95% confidence interval 0.23-0.42). Among both expert-radiologists agreement was moderate (kappa = 0.47, 95% confidence interval 0.38-0.56), with disagreement on the presence of a pancreatic mass in 29% of cases. The specificity for malignancy of pancreatic masses identified in expert consensus was twice as high compared with the original CT report (87% vs 42%, respectively). Positive predictive value increased to 98% after expert consensus, but negative predictive value was low (12%). Clinicians need to be aware of potential considerable disagreement among radiologists about the presence of a pancreatic mass. The specificity for malignancy doubled by expert radiologist reassessment when a uniform definition of "pancreatic mass" was used. Copyright © 2015 Elsevier Inc. All rights reserved.

SU-E-J-76: CBCT Reconstruction of a Full Couch Using Rigid Registration and Pre-Scanned Couch Image and Its Clinical Application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, E; Lasio, G; Lee, M

Purpose: Only a part of a treatment couch is reconstructed in CBCT due to the limited field of view (FOV). This often generates inaccurate results in the delivered dose evaluation with CBCT and more noise in the CBCT reconstruction. Full reconstruction of the couch at treatment setup can be used for more accurate exit beam dosimetry. The goal of this study is to develop a method to reconstruct a full treatment couch using a pre-scanned couch image and rigid registration. Methods: A full couch (Exact Couch, Varian) model image was reconstructed by rigidly registering and combining two sets of partialmore » CBCT images. The full couch model includes three parts: two side rails and a couch top. A patient CBCT was reconstructed with reconstruction grid size larger than the physical field of view to include the full couch. The image quality of the couch is not good due to data truncation, but good enough to allow rigid registration of the couch. A composite CBCT image of the patient plus couch has been generated from the original reconstruction by replacing couch portion with the pre-acquired model couch, rigidly registered to the original scan. We evaluated the clinical usefulness of this method by comparing treatment plans generated on the original and on the modified scans. Results: The full couch model could be attached to a patient CBCT image set via rigid image registration. Plan DVHs showed 1∼2% difference between plans with and without full couch modeling. Conclusion: The proposed method generated a full treatment couch CBCT model, which can be successfully registered to the original patient image. This method was also shown to be useful in generating more accurate dose distributions, by lowering 1∼2% dose in PTV and a few other critical organs. Part of this study is supported by NIH R01CA133539.« less

Discovery and Identification of Dimethylsilanediol as a Contaminant in ISS Potable Water

NASA Technical Reports Server (NTRS)

Rutz, Jeffrey A.; Schultz, John R.; Kuo, C. Mike; Cole, Hraold E.; Manuel, Sam; Curtis, Matthew; Jones, Patrick R.; Sparkman, O. David; McCoy, J. Torin

2010-01-01

In September of 2010, analysis of ISS potable water samples was undertaken to determine the contaminant responsible for a rise in total organic carbon (TOC). As analysis of the routine target list of organic compounds did not reveal the contaminant, efforts to look for unknown compounds was initiated, resulting in an unknown peak being discovered in the gas chromatography/mass spectrometry (GC/MS) analysis for glycols. A mass spectrum of the contaminant was then generated by concentrating one of the samples by evaporation and analyzing by GC/MS in full-scan mode. Although a computer match of the compound s identity could not be obtained with the instrument s database, a search with a more up to date mass spectral library yielded a good match with dimethylsilanediol (DMSD). Inductively Coupled Plasma/Mass Spectrometry (ICP/MS) analyses showed abnormally high silicon levels in the samples, confirming that the unknown contained silicon. DMSD was then synthesized to confirm the identification and provide a standard to develop a calibration curve. Further confirmation was provided by external Direct Analysis in Real Time (DART) GC/MS analysis. A preliminary GC/MS method was then developed and archived samples from various locations on ISS were analyzed to determine the extent of the contamination and provide data for troubleshooting. This paper describes these events in more detail as well as problems encountered in routine GC/MS analyses and the subsequent development of high performance liquid chromatography and LC/MS/MS methods for quantitation of DMSD.

Degradation of the Neonicotinoid Pesticides in the Atmospheric Pressure Ionization Source

NASA Astrophysics Data System (ADS)

Chai, Yunfeng; Chen, Hongping; Liu, Xin; Lu, Chengyin

2018-02-01

During the analysis of neonicotinoid pesticide standards (thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid) by mass spectrometry, the degradation of these pesticides (M-C=N-R is degraded into M-C=O, M is the skeleton moiety, and R is NO2 or CN) was observed in the atmospheric pressure ionization interfaces (ESI and APCI). In APCI, the degradation of all the five neonicotinoid pesticides studied took place, and the primary mechanism was in-source ion/molecule reaction, in which a molecule of water (confirmed by use of H2 18O) attacked the carbon of the imine group accompanying with loss of NH2R (R=NO2, CN). For the nitroguanidine neonicotinoid pesticides (R=NO2, including thiamethoxam, clothianidin, and imidacloprid), higher auxiliary gas heater temperature also contributed to their degradation in APCI due to in-source pyrolysis. The degradation of the five neonicotinoid pesticides studied in ESI was not significant. In ESI, only the nitroguanidine neonicotinoid pesticides could generate the degradation products through in-source fragmentation mechanism. The degradation of cyanoamidine neonicotinoid pesticides (R=CN, including acetamiprid and thiacloprid) in ESI was not observed. The degradation of neonicotinoid pesticides in the ion source of mass spectrometer renders some adverse consequences, such as difficulty interpreting the full-scan mass spectrum, reducing the sensitivity and accuracy of quantitative analysis, and misleading whether these pesticides have degraded in the real samples. Therefore, a clear understanding of these unusual degradation reactions should facilitate the analysis of neonicotinoid pesticides by atmospheric pressure ionization mass spectrometry.

A Novel Method for Profiling and Quantifying Short- and Medium-Chain Chlorinated Paraffins in Environmental Samples Using Comprehensive Two-Dimensional Gas Chromatography-Electron Capture Negative Ionization High-Resolution Time-of-Flight Mass Spectrometry.

PubMed

Xia, Dan; Gao, Lirong; Zheng, Minghui; Tian, Qichang; Huang, Huiting; Qiao, Lin

2016-07-19

Chlorinated paraffins (CPs) are complex technical mixtures containing thousands of isomers. Analyzing CPs in environmental matrices is extremely challenging. CPs have broad, unresolved profiles when analyzed by one-dimensional gas chromatography (GC). Comprehensive two-dimensional GC (GC×GC) can separate CPs with a high degree of orthogonality. A novel method for simultaneously profiling and quantifying short- and medium-chain CPs, using GC×GC coupled with electron capture negative ionization high-resolution time-of-flight mass spectrometry, was developed. The method allowed 48 CP formula congener groups to be analyzed highly selectively in one injection through accurate mass measurements of the [M - Cl](-) ions in full scan mode. The correlation coefficients (R(2)) for the linear calibration curves for different chlorine contents were 0.982 for short-chain CPs and 0.945 for medium-chain CPs. The method was successfully used to determine CPs in sediment and fish samples. By using this method, with enhanced chromatographic separation and high mass resolution, interferences between CP congeners and other organohalogen compounds, such as toxaphene, are minimized. New compounds, with the formulas C9H14Cl6 and C9H13Cl7, were found in sediment and biological samples for the first time. The method was shown to be a powerful tool for the analysis of CPs in environmental samples.

Paper spray mass spectrometry and PLS-DA improved by variable selection for the forensic discrimination of beers.

PubMed

Pereira, Hebert Vinicius; Amador, Victória Silva; Sena, Marcelo Martins; Augusti, Rodinei; Piccin, Evandro

2016-10-12

Paper spray mass spectrometry (PS-MS) combined with partial least squares discriminant analysis (PLS-DA) was applied for the first time in a forensic context to a fast and effective differentiation of beers. Eight different brands of American standard lager beers produced by four different breweries (141 samples from 55 batches) were studied with the aim at performing a differentiation according to their market prices. The three leader brands in the Brazilian beer market, which have been subject to fraud, were modeled as the higher-price class, while the five brands most used for counterfeiting were modeled as the lower-price class. Parameters affecting the paper spray ionization were examined and optimized. The best MS signal stability and intensity was obtained while using the positive ion mode, with PS(+) mass spectra characterized by intense pairs of signals corresponding to sodium and potassium adducts of malto-oligosaccharides. Discrimination was not apparent neither by using visual inspection nor principal component analysis (PCA). However, supervised classification models provided high rates of sensitivity and specificity. A PLS-DA model using full scan mass spectra were improved by variable selection with ordered predictors selection (OPS), providing 100% of reliability rate and reducing the number of variables from 1701 to 60. This model was interpreted by detecting fifteen variables as the most significant VIP (variable importance in projection) scores, which were therefore considered diagnostic ions for this type of beer counterfeit. Copyright © 2016 Elsevier B.V. All rights reserved.

Graded-threshold parametric response maps: towards a strategy for adaptive dose painting

NASA Astrophysics Data System (ADS)

Lausch, A.; Jensen, N.; Chen, J.; Lee, T. Y.; Lock, M.; Wong, E.

2014-03-01

Purpose: To modify the single-threshold parametric response map (ST-PRM) method for predicting treatment outcomes in order to facilitate its use for guidance of adaptive dose painting in intensity-modulated radiotherapy. Methods: Multiple graded thresholds were used to extend the ST-PRM method (Nat. Med. 2009;15(5):572-576) such that the full functional change distribution within tumours could be represented with respect to multiple confidence interval estimates for functional changes in similar healthy tissue. The ST-PRM and graded-threshold PRM (GT-PRM) methods were applied to functional imaging scans of 5 patients treated for hepatocellular carcinoma. Pre and post-radiotherapy arterial blood flow maps (ABF) were generated from CT-perfusion scans of each patient. ABF maps were rigidly registered based on aligning tumour centres of mass. ST-PRM and GT-PRM analyses were then performed on overlapping tumour regions within the registered ABF maps. Main findings: The ST-PRMs contained many disconnected clusters of voxels classified as having a significant change in function. While this may be useful to predict treatment response, it may pose challenges for identifying boost volumes or for informing dose-painting by numbers strategies. The GT-PRMs included all of the same information as ST-PRMs but also visualized the full tumour functional change distribution. Heterogeneous clusters in the ST-PRMs often became more connected in the GT-PRMs by voxels with similar functional changes. Conclusions: GT-PRMs provided additional information which helped to visualize relationships between significant functional changes identified by ST-PRMs. This may enhance ST-PRM utility for guiding adaptive dose painting.

Dynamic electronic collimation method for 3-D catheter tracking on a scanning-beam digital x-ray system

PubMed Central

Dunkerley, David A. P.; Slagowski, Jordan M.; Funk, Tobias; Speidel, Michael A.

2017-01-01

Abstract. Scanning-beam digital x-ray (SBDX) is an inverse geometry x-ray fluoroscopy system capable of tomosynthesis-based 3-D catheter tracking. This work proposes a method of dose-reduced 3-D catheter tracking using dynamic electronic collimation (DEC) of the SBDX scanning x-ray tube. This is achieved through the selective deactivation of focal spot positions not needed for the catheter tracking task. The technique was retrospectively evaluated with SBDX detector data recorded during a phantom study. DEC imaging of a catheter tip at isocenter required 340 active focal spots per frame versus 4473 spots in full field-of-view (FOV) mode. The dose-area product (DAP) and peak skin dose (PSD) for DEC versus full FOV scanning were calculated using an SBDX Monte Carlo simulation code. The average DAP was reduced to 7.8% of the full FOV value, consistent with the relative number of active focal spots (7.6%). For image sequences with a moving catheter, PSD was 33.6% to 34.8% of the full FOV value. The root-mean-squared-deviation between DEC-based 3-D tracking coordinates and full FOV 3-D tracking coordinates was less than 0.1 mm. The 3-D distance between the tracked tip and the sheath centerline averaged 0.75 mm. DEC is a feasible method for dose reduction during SBDX 3-D catheter tracking. PMID:28439521

Generic sample preparation combined with high-resolution liquid chromatography-time-of-flight mass spectrometry for unification of urine screening in doping-control laboratories.

PubMed

Peters, R J B; Oosterink, J E; Stolker, A A M; Georgakopoulos, C; Nielen, M W F

2010-04-01

A unification of doping-control screening procedures of prohibited small molecule substances--including stimulants, narcotics, steroids, beta2-agonists and diuretics--is highly urgent in order to free resources for new classes such as banned proteins. Conceptually this may be achieved by the use of a combination of one gas chromatography-time-of-flight mass spectrometry method and one liquid chromatography-time-of-flight mass spectrometry method. In this work a quantitative screening method using high-resolution liquid chromatography in combination with accurate-mass time-of-flight mass spectrometry was developed and validated for determination of glucocorticosteroids, beta2-agonists, thiazide diuretics, and narcotics and stimulants in urine. To enable the simultaneous isolation of all the compounds of interest and the necessary purification of the resulting extracts, a generic extraction and hydrolysis procedure was combined with a solid-phase extraction modified for these groups of compounds. All 56 compounds are determined using positive electrospray ionisation with the exception of the thiazide diuretics for which the best sensitivity was obtained by using negative electrospray ionisation. The results show that, with the exception of clenhexyl, procaterol, and reproterol, all compounds can be detected below the respective minimum required performance level and the results for linearity, repeatability, within-lab reproducibility, and accuracy show that the method can be used for quantitative screening. If qualitative screening is sufficient the instrumental analysis may be limited to positive ionisation, because all analytes including the thiazides can be detected at the respective minimum required levels in the positive mode. The results show that the application of accurate-mass time-of-flight mass spectrometry in combination with generic extraction and purification procedures is suitable for unification and expansion of the window of screening methods of doping laboratories. Moreover, the full-scan accurate-mass data sets obtained still allow retrospective examination for emerging doping agents, without re-analyzing the samples.

Mass loss in red giants and supergiants

NASA Technical Reports Server (NTRS)

Sanner, F.

1976-01-01

The circumstellar envelopes surrounding 13 late-type giants and supergiants have been studied using a homogeneous collection of high-resolution, photoelectric scans of strong optical resonance lines. Various properties of the envelopes, including the mass loss rate, dilution factor, hydrogen density, and degree of ionization, have been determined quantitatively.

Concepts for laser beam parameter monitoring during industrial mass production

NASA Astrophysics Data System (ADS)

Harrop, Nicholas J.; Maerten, Otto; Wolf, Stefan; Kramer, Reinhard

2017-02-01

In today's industrial mass production, lasers have become an established tool for a variety of processes. As with any other tool, mechanical or otherwise, the laser and its ancillary components are prone to wear and ageing. Monitoring of these ageing processes at full operating power of an industrial laser is challenging for a range of reasons. Not only the damage threshold of the measurement device itself, but also cycle time constraints in industrial processing are just two of these challenges. Power measurement, focus spot size or full beam caustic measurements are being implemented in industrial laser systems. The scope of the measurement and the amount of data collected is limited by the above mentioned cycle time, which in some cases can only be a few seconds. For successful integration of these measurement systems into automated production lines, the devices must be equipped with standardized communication interfaces, enabling a feedback loop from the measurement device to the laser processing systems. If necessary these measurements can be performed before each cycle. Power is determined with either static or dynamic calorimetry while camera and scanning systems are used for beam profile analysis. Power levels can be measured from 25W up to 20 kW, with focus spot sizes between 10μm and several millimeters. We will show, backed by relevant statistical data, that defects or contamination of the laser beam path can be detected with applied measurement systems, enabling a quality control chain to prevent process defects.

Pupil engineering for a confocal reflectance line-scanning microscope

NASA Astrophysics Data System (ADS)

Patel, Yogesh G.; Rajadhyaksha, Milind; DiMarzio, Charles A.

2011-03-01

Confocal reflectance microscopy may enable screening and diagnosis of skin cancers noninvasively and in real-time, as an adjunct to biopsy and pathology. Current confocal point-scanning systems are large, complex, and expensive. A confocal line-scanning microscope, utilizing a of linear array detector can be simpler, smaller, less expensive, and may accelerate the translation of confocal microscopy in clinical and surgical dermatology. A line scanner may be implemented with a divided-pupil, half used for transmission and half for detection, or with a full-pupil using a beamsplitter. The premise is that a confocal line-scanner with either a divided-pupil or a full-pupil will provide high resolution and optical sectioning that would be competitive to that of the standard confocal point-scanner. We have developed a confocal line-scanner that combines both divided-pupil and full-pupil configurations. This combined-pupil prototype is being evaluated to determine the advantages and limitations of each configuration for imaging skin, and comparison of performance to that of commercially available standard confocal point-scanning microscopes. With the combined configuration, experimental evaluation of line spread functions (LSFs), contrast, signal-to-noise ratio, and imaging performance is in progress under identical optical and skin conditions. Experimental comparisons between divided-pupil and full-pupil LSFs will be used to determine imaging performance. Both results will be compared to theoretical calculations using our previously reported Fourier analysis model and to the confocal point spread function (PSF). These results may lead to a simpler class of confocal reflectance scanning microscopes for clinical and surgical dermatology.

Spindle epithelial tumor with thymus-like differentiation of the thyroid in a 70-year-old man.

PubMed

Lee, Sunhye; Kim, Yon Seon; Lee, Jeong Hyeon; Hwang, Sung Ho; Oh, Yu-Hwan; Ko, Byung Kyun; Ham, Soo-Youn

2018-06-01

Spindle epithelial tumor with thymus-like differentiation (SETTLE) is a very rare tumor of the thyroid gland mostly occurring in young patients. The imaging findings of SETTLE tumors are yet to be defined. However, they are usually described as well-defined heterogeneously enhanced masses on CT scan. The current case has the potential growth as compared with a 2009 chest radiography. We took into account the possibility of SETTLE in the case of a bulky mass in patients over 70 years old, particularly in the lower neck. Herein, we report a case of the oldest patient so far. The patient underwent a right lobectomy of the thyroid and mass excision. Follow-up CT scans after 6 months revealed no local recurrence. Surgery is the gold standard treatment for SETTLE. Chemotherapy and radiotherapy could be another possible option for patients with advanced stage SETTLE.

[Mesenteric volvulus associated with mesenteric lipoma: about a case].

PubMed

Dème, Hamidou; Badji, Nfally; Akpo, Léra Géraud; Touré, Mouhamed Hamine; Draha, Ronald; Niang, Fallou Gallas; Diop, Abdoulaye Dione; Niang, El Hadj

2016-01-01

We report the case of a 7-year old patient presenting for acute paroxysmal abdominal pain at the level of epigastrium associated with vomiting without involving blockage of materials and gas. Clinical examination and laboratory tests were unremarkable. Abdominal ultrasound was requested as a first line investigationa and showed a right echogenic homogeneous flank and iliac fossa mass with regular contours without vascular Doppler signal and associated with "whirl sign" of mesenteric vessels. On CT scan this mass was seen as a well-defined lipoma formation, exerting a mass effect on the cecum, which was in direct contact with mesenteric volvulus. Arrangement of the mesenteric vessels at their origin was normal. The diagnosis of mesenteric volvulus associated with lipoma was retained. Surgical management and histological analysis of the surgical specimen confirmed the diagnosis. This clinical case aims to highlight the contribution of ultrasound and CT scan in the diagnosis of midgut volvulus.

Quadrupole mass filter: design and performance for operation in stability zone 3.

PubMed

Syed, Sarfaraz U A H; Hogan, Thomas J; Antony Joseph, Mariya J; Maher, Simon; Taylor, Stephen

2013-10-01

The predicted performance of a quadrupole mass filter (QMF) operating in Mathieu stability zone 3 is described in detail using computer simulations. The investigation considers the factors that limit the ultimate maximum resolution (Rmax) and percentage transmission (%Tx), which can be obtained for a given QMF for a particular scan line of operation. The performance curve (i.e., the resolution (R) versus number (N) of radio frequency (rf) cycles experienced by the ions in the mass filter) has been modeled for the upper and lower tip of stability zone 3. The saturation behavior of the performance curve observed in practice for zone 3 is explained. Furthermore, new design equations are presented by examining the intersection of the scan line with stability zone 3. Resolution versus transmission characteristics of stability zones 1 and 3 are compared and the dependence of performance for zones 1 and 3 is related to particular instrument operating parameters.

APT mass spectrometry and SEM data for CdTe solar cells

DOE PAGES

Li, Chen; Paudel, Naba R.; Yan, Yanfa; ...

2016-03-16

Atom probe tomography (APT) data acquired from a CAMECA LEAP 4000 XHR for the CdS/CdTe interface for a non-CdCl 2 treated CdTe solar cell as well as the mass spectrum of an APT data set including a GB in a CdCl 2-treated CdTe solar cell are presented. Scanning electron microscopy (SEM) data showing the evolution of sample preparation for APT and scanning transmission electron microscopy (STEM) electron beam induced current (EBIC) are also presented. As a result, these data show mass spectrometry peak decomposition of Cu and Te within an APT dataset, the CdS/CdTe interface of an untreated CdTe solarmore » cell, preparation of APT needles from the CdS/CdTe interface in superstrate grown CdTe solar cells, and the preparation of a cross-sectional STEM EBIC sample.« less

Investigation of cone-beam CT image quality trade-off for image-guided radiation therapy

NASA Astrophysics Data System (ADS)

Bian, Junguo; Sharp, Gregory C.; Park, Yang-Kyun; Ouyang, Jinsong; Bortfeld, Thomas; El Fakhri, Georges

2016-05-01

It is well-known that projections acquired over an angular range slightly over 180° (so-called short scan) are sufficient for fan-beam reconstruction. However, due to practical imaging conditions (projection data and reconstruction image discretization, physical factors, and data noise), the short-scan reconstructions may have different appearances and properties from the full-scan (scans over 360°) reconstructions. Nevertheless, short-scan configurations have been used in applications such as cone-beam CT (CBCT) for head-neck-cancer image-guided radiation therapy (IGRT) that only requires a small field of view due to the potential reduced imaging time and dose. In this work, we studied the image quality trade-off for full, short, and full/short scan configurations with both conventional filtered-backprojection (FBP) reconstruction and iterative reconstruction algorithms based on total-variation (TV) minimization for head-neck-cancer IGRT. Anthropomorphic and Catphan phantoms were scanned at different exposure levels with a clinical scanner used in IGRT. Both visualization- and numerical-metric-based evaluation studies were performed. The results indicate that the optimal exposure level and number of views are in the middle range for both FBP and TV-based iterative algorithms and the optimization is object-dependent and task-dependent. The optimal view numbers decrease with the total exposure levels for both FBP and TV-based algorithms. The results also indicate there are slight differences between FBP and TV-based iterative algorithms for the image quality trade-off: FBP seems to be more in favor of larger number of views while the TV-based algorithm is more robust to different data conditions (number of views and exposure levels) than the FBP algorithm. The studies can provide a general guideline for image-quality optimization for CBCT used in IGRT and other applications.

Investigation of cone-beam CT image quality trade-off for image-guided radiation therapy.

PubMed

Bian, Junguo; Sharp, Gregory C; Park, Yang-Kyun; Ouyang, Jinsong; Bortfeld, Thomas; El Fakhri, Georges

2016-05-07

It is well-known that projections acquired over an angular range slightly over 180° (so-called short scan) are sufficient for fan-beam reconstruction. However, due to practical imaging conditions (projection data and reconstruction image discretization, physical factors, and data noise), the short-scan reconstructions may have different appearances and properties from the full-scan (scans over 360°) reconstructions. Nevertheless, short-scan configurations have been used in applications such as cone-beam CT (CBCT) for head-neck-cancer image-guided radiation therapy (IGRT) that only requires a small field of view due to the potential reduced imaging time and dose. In this work, we studied the image quality trade-off for full, short, and full/short scan configurations with both conventional filtered-backprojection (FBP) reconstruction and iterative reconstruction algorithms based on total-variation (TV) minimization for head-neck-cancer IGRT. Anthropomorphic and Catphan phantoms were scanned at different exposure levels with a clinical scanner used in IGRT. Both visualization- and numerical-metric-based evaluation studies were performed. The results indicate that the optimal exposure level and number of views are in the middle range for both FBP and TV-based iterative algorithms and the optimization is object-dependent and task-dependent. The optimal view numbers decrease with the total exposure levels for both FBP and TV-based algorithms. The results also indicate there are slight differences between FBP and TV-based iterative algorithms for the image quality trade-off: FBP seems to be more in favor of larger number of views while the TV-based algorithm is more robust to different data conditions (number of views and exposure levels) than the FBP algorithm. The studies can provide a general guideline for image-quality optimization for CBCT used in IGRT and other applications.

Radiation Internal Monitoring by In Vivo Scanning in Operation Tomodachi

DTIC Science & Technology

2013-08-01

2 cubic meter (m3) Mass /Density pound (lb) 4.535 924 × 10–1 kilogram (kg) atomic mass unit (AMU) 1.660 539 × 10–27 kilogram (kg) pound- mass per...40 2.2.5. Critical Level and Minimum Detectable Activity ............................... 42 ii Section 3. Radiological Properties...operation quality assurance program. x Operation Tomodachi Dose Assessment and Recording Working Group members, who provided critical information

Mirion--a software package for automatic processing of mass spectrometric images.

PubMed

Paschke, C; Leisner, A; Hester, A; Maass, K; Guenther, S; Bouschen, W; Spengler, B

2013-08-01

Mass spectrometric imaging (MSI) techniques are of growing interest for the Life Sciences. In recent years, the development of new instruments employing ion sources that are tailored for spatial scanning allowed the acquisition of large data sets. A subsequent data processing, however, is still a bottleneck in the analytical process, as a manual data interpretation is impossible within a reasonable time frame. The transformation of mass spectrometric data into spatial distribution images of detected compounds turned out to be the most appropriate method to visualize the results of such scans, as humans are able to interpret images faster and easier than plain numbers. Image generation, thus, is a time-consuming and complex yet very efficient task. The free software package "Mirion," presented in this paper, allows the handling and analysis of data sets acquired by mass spectrometry imaging. Mirion can be used for image processing of MSI data obtained from many different sources, as it uses the HUPO-PSI-based standard data format imzML, which is implemented in the proprietary software of most of the mass spectrometer companies. Different graphical representations of the recorded data are available. Furthermore, automatic calculation and overlay of mass spectrometric images promotes direct comparison of different analytes for data evaluation. The program also includes tools for image processing and image analysis.

Studies on drug metabolism by fungi colonizing decomposing human cadavers. Part II: biotransformation of five model drugs by fungi isolated from post-mortem material.

PubMed

Martínez-Ramírez, Jorge A; Walther, Grit; Peters, Frank T

2015-04-01

The present study investigated the in vitro metabolic capacity of 28 fungal strains isolated from post-mortem material towards five model drugs: amitriptyline, metoprolol, mirtazapine, promethazine, and zolpidem. Each fungal strain was incubated at 25 °C for up to 120 h with each of the five models drugs. Cunninghamella elegans was used as positive control. Aliquots of the incubation mixture were centrifuged and 50 μL of the supernatants were diluted and directly analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with product ion scanning. The remaining mixture was analyzed by full scan gas chromatography-mass spectrometry (GC-MS) after liquid-liquid extraction and acetylation. The metabolic activity was evaluated through the total number of detected metabolites (NDM) produced in each model and fungal strains and the percentage of parent drug remaining (%RPD) after up to five days of incubation. All the tested fungal strains were capable of forming mammalian phase I metabolites. Fungi from the normal fungal flora of the human body such as Candida sp., Geotrichum candidum, and Trichosporon asahii) formed up to seven metabolites at %RPD values greater than 52% but no new fungal metabolites (NFM). In contrast, some airborne fungal strains like Bjerkandera adusta, Chaetomium sp, Coriolopsis sp., Fusarium solani and Mucor plumbeus showed NDM values exceeding those of the positive control, complete metabolism of the parent drug in some models and formation of NFM. NFM (numbers in brackets) were detected in four of the five model drugs: amitriptyline (18), metoprolol (4), mirtazapine (8), and zolpidem (2). The latter NFM are potential candidates for marker substances indicating post-mortem fungal metabolism. Copyright © 2014 John Wiley & Sons, Ltd.

Beam energy scan with asymmetric collision at RHIC

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, C.; Alessi, J.; Beebe, E.

A beam energy scan of deuteron-gold collision, with center-of-mass energy at 19.6, 39, 62.4 and 200.7 GeV/n, was performed at the Relativistic Heavy Ion Collider in 2016 to study the threshold for quark-gluon plasma (QGP) production. The lattice, RF, stochastic cooling and other subsystems were in different configurations for the various energies. The operational challenges changed with every new energy. The operational experience at each energy, the operation performance, highlights and lessons of the beam energy scan are reviewed in this report.

Inadequate increase in the volume of major epicardial coronary arteries compared with that in left ventricular mass. Novel concept for characterization of coronary arteries using 64-slice computed tomography.

PubMed

Ehara, Shoichi; Okuyama, Takuhiro; Shirai, Nobuyuki; Sugioka, Kenichi; Oe, Hiroki; Itoh, Toshihide; Matsuoka, Toshiyuki; Ikura, Yoshihiro; Ueda, Makiko; Naruko, Takahiko; Hozumi, Takeshi; Yoshiyama, Minoru

2009-08-01

Previous studies have shown a correlation between coronary artery cross-sectional diameter and left ventricular (LV) mass. However, no studies have examined the correlation between actual coronary artery volume (CAV) and LV mass. In the present study, measurements of CAV by 64-multislice computed tomography (MSCT) were validated and the relationship between CAV and LV mass was investigated. First, coronary artery phantoms consisting of syringes filled with solutions of contrast medium moving at simulated heart rates were scanned by 64-MSCT. Display window settings permitting accurate calculation of small volumes were optimized by evaluating volume-rendered images of the segmented contrast medium at different window settings. Next, 61 patients without significant coronary artery stenosis were scanned by 64-MSCT with the same protocol as for the phantoms. Coronary arteries were segmented on a workstation and the same window settings were applied to the volume-rendered images to calculate total CAV. Significant correlations between total CAV and LV mass (r=0.660, P<0.0001) were found, whereas an inverse relation was present between total CAV per 100 g of LV mass and LV mass. The novel concept of "CAV" for the characterization of coronary arteries may prove useful for future research, particularly on the causes of LV hypertrophy.

Conically scanned lidar telescope using holographic optical elements

NASA Technical Reports Server (NTRS)

Schwemmer, Geary K.; Wilkerson, Thomas D.

1992-01-01

Holographic optical elements (HOE) using volume phase holograms make possible a new class of lightweight scanning telescopes having advantages for lidar remote sensing instruments. So far, the only application of HOE's to lidar has been a non-scanning receiver for a laser range finder. We introduce a large aperture, narrow field of view (FOV) telescope used in a conical scanning configuration, having a much smaller rotating mass than in conventional designs. Typically, lidars employ a large aperture collector and require a narrow FOV to limit the amount of skylight background. Focal plane techniques are not good approaches to scanning because they require a large FOV within which to scan a smaller FOV mirror or detector array. Thus, scanning lidar systems have either used a large flat scanning mirror at which the receiver telescope is pointed, or the entire telescope is steered. We present a concept for a conically scanned lidar telescope in which the only moving part is the HOE which serves as the primary collecting optic. We also describe methods by which a multiplexed HOE can be used simultaneously as a dichroic beamsplitter.

Chest CT scanning for clinical suspected thoracic aortic dissection: beware the alternate diagnosis.

PubMed

Thoongsuwan, Nisa; Stern, Eric J

2002-11-01

The aim of the study was retrospectively to evaluate the spectrum of chest diseases in patients presenting with clinical suspicion of thoracic aortic dissection in the emergency department. We performed a retrospective medical records review of 86 men and 44 women (ages ranging between 23 and 106 years) with clinically suspected aortic dissection, for CT scan findings and final clinical diagnoses dating between January 1996 and September 2001. All images were obtained by using a standard protocol for aortic dissection. We found aortic dissection in 32 patients (24.6%), 22 of which were Stanford classification type A and 10 Stanford type B. In 70 patients (53.9%), chest pain could not be explained by the CT scan findings. However, in 28 patients (21.5%), CT scanning did reveal an alternate diagnosis that, along with the clinical impression, probably explained the patients' presenting symptoms, including: hiatal hernia (7), pneumonia (5), intrathoracic mass (4), pericardial effusion/hemopericardium (3), esophageal mass/rupture (2), aortic aneurysm without dissection (2), pulmonary embolism (2), pleural effusion (1), aortic rupture (1), and pancreatitis (1). In cases where there is clinical suspicion of aortic dissection, CT scan findings of an alternate diagnosis for the presenting symptoms are only slightly less common than the finding of aortic dissection itself. Although the spectrum of findings will vary depending upon your patient population, beware the alternate diagnosis.

Vector generator scan converter

DOEpatents

Moore, James M.; Leighton, James F.

1990-01-01

High printing speeds for graphics data are achieved with a laser printer by transmitting compressed graphics data from a main processor over an I/O (input/output) channel to a vector generator scan converter which reconstructs a full graphics image for input to the laser printer through a raster data input port. The vector generator scan converter includes a microprocessor with associated microcode memory containing a microcode instruction set, a working memory for storing compressed data, vector generator hardward for drawing a full graphic image from vector parameters calculated by the microprocessor, image buffer memory for storing the reconstructed graphics image and an output scanner for reading the graphics image data and inputting the data to the printer. The vector generator scan converter eliminates the bottleneck created by the I/O channel for transmitting graphics data from the main processor to the laser printer, and increases printer speed up to thirty fold.

Vector generator scan converter

DOEpatents

Moore, J.M.; Leighton, J.F.

1988-02-05

High printing speeds for graphics data are achieved with a laser printer by transmitting compressed graphics data from a main processor over an I/O channel to a vector generator scan converter which reconstructs a full graphics image for input to the laser printer through a raster data input port. The vector generator scan converter includes a microprocessor with associated microcode memory containing a microcode instruction set, a working memory for storing compressed data, vector generator hardware for drawing a full graphic image from vector parameters calculated by the microprocessor, image buffer memory for storing the reconstructed graphics image and an output scanner for reading the graphics image data and inputting the data to the printer. The vector generator scan converter eliminates the bottleneck created by the I/O channel for transmitting graphics data from the main processor to the laser printer, and increases printer speed up to thirty fold. 7 figs.

Intra-tumoral heterogeneity of gemcitabine delivery and mass transport in human pancreatic cancer

NASA Astrophysics Data System (ADS)

Koay, Eugene J.; Baio, Flavio E.; Ondari, Alexander; Truty, Mark J.; Cristini, Vittorio; Thomas, Ryan M.; Chen, Rong; Chatterjee, Deyali; Kang, Ya'an; Zhang, Joy; Court, Laurence; Bhosale, Priya R.; Tamm, Eric P.; Qayyum, Aliya; Crane, Christopher H.; Javle, Milind; Katz, Matthew H.; Gottumukkala, Vijaya N.; Rozner, Marc A.; Shen, Haifa; Lee, Jeffrey E.; Wang, Huamin; Chen, Yuling; Plunkett, William; Abbruzzese, James L.; Wolff, Robert A.; Maitra, Anirban; Ferrari, Mauro; Varadhachary, Gauri R.; Fleming, Jason B.

2014-12-01

There is substantial heterogeneity in the clinical behavior of pancreatic cancer and in its response to therapy. Some of this variation may be due to differences in delivery of cytotoxic therapies between patients and within individual tumors. Indeed, in 12 patients with resectable pancreatic cancer, we previously demonstrated wide inter-patient variability in the delivery of gemcitabine as well as in the mass transport properties of tumors as measured by computed tomography (CT) scans. However, the variability of drug delivery and transport properties within pancreatic tumors is currently unknown. Here, we analyzed regional measurements of gemcitabine DNA incorporation in the tumors of the same 12 patients to understand the degree of intra-tumoral heterogeneity of drug delivery. We also developed a volumetric segmentation approach to measure mass transport properties from the CT scans of these patients and tested inter-observer agreement with this new methodology. Our results demonstrate significant heterogeneity of gemcitabine delivery within individual pancreatic tumors and across the patient cohort, with gemcitabine DNA incorporation in the inner portion of the tumors ranging from 38 to 74% of the total. Similarly, the CT-derived mass transport properties of the tumors had a high degree of heterogeneity, ranging from minimal difference to almost 200% difference between inner and outer portions of the tumor. Our quantitative method to derive transport properties from CT scans demonstrated less than 5% difference in gemcitabine prediction at the average CT-derived transport value across observers. These data illustrate significant inter-patient and intra-tumoral heterogeneity in the delivery of gemcitabine, and highlight how this variability can be reproducibly accounted for using principles of mass transport. With further validation as a biophysical marker, transport properties of tumors may be useful in patient selection for therapy and prediction of therapeutic outcome.

Corporate psychopathy and the full-range leadership model.

PubMed

Mathieu, Cynthia; Neumann, Craig; Babiak, Paul; Hare, Robert D

2015-06-01

The B-Scan 360 is a relatively new, purpose-built measure of corporate psychopathy that addresses many of the issues inherent in studying psychopathy in organizations. The primary goal of the present study was to measure the relationship between employees' perception of psychopathic features in their supervisor and their rating of their supervisor on the Full-Range Model of Leadership. The second goal of the study was to test the B-Scan 360's factor structure and test its interrater reliability in an organizational sample. A total of 491 civic employees and 116 employees from a branch of a large financial company completed the B-Scan 360 as well as the Multifactor Leadership Questionnaire on their direct supervisor. The B-Scan 360 and all of its four factors were positively correlated with passive leadership (Laissez-Faire leadership) and negatively correlated with positive leadership (both Transactional and Transformational leadership). Furthermore, results revealed the same four-factor structure and good interrater reliability for the B-Scan 360 in this business sample as previously reported for a general population. Overall, the results provide additional support for the B-Scan 360 as a measure of psychopathic traits in corporate settings. © The Author(s) 2014.

A simultaneous screening and quantitative method for the multiresidue analysis of pesticides in spices using ultra-high performance liquid chromatography-high resolution (Orbitrap) mass spectrometry.

PubMed

Goon, Arnab; Khan, Zareen; Oulkar, Dasharath; Shinde, Raviraj; Gaikwad, Suresh; Banerjee, Kaushik

2018-01-12

A novel screening and quantitation method is reported for non-target multiresidue analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70-120%, and precision-RSDs <20%. Furthermore, the method allowed the identification of suspected non-target analytes through retrospective search of the accurate mass of the compound-specific precursor and product ions. Compared to LC-MS/MS, the quantitative performance of this Orbitrap-MS method had agreements in residue values between 78-100%. Copyright © 2017 Elsevier B.V. All rights reserved.

High-throughput and cost-effective global DNA methylation assay by liquid chromatography-mass spectrometry

PubMed Central

Li, Xingnan; Franke, Adrian A.

2015-01-01

An affordable and fast liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the accurate and precise determination of global DNA methylation levels in peripheral blood. Global DNA methylation extent was expressed as the ratio of methylated 2′-deoxycytidine (5MedC) to 2′-deoxyguanosine (dG), which were obtained after DNA extraction and hydrolysis and determined by positive electrospray LC–ESI-MS/MS. The cost-effective internal standards 15N3-dC and 15N5-dG were incorporated for the accurate quantification of 5MedC and dG, respectively. The desired nucleoside analytes were separated and eluted by LC within 2.5 min on a reverse phase column with a limit of detection of 1.4 femtomole on column for 5MedC. Sample preparation in 96-well format has significantly increased the assay throughput and filtration was found to be a necessary step to assure precision. Precision was performed with repeated analysis of four DNA QC sample over 12 days, with mean intra- and inter-day CVs of 6% and 11%, respectively. Accuracy was evaluated by comparison with a previously reported method showing a mean CV of 4% for 5 subjects analyzed. Furthermore, application of the assay using a benchtop orbitrap LCMS in exact mass full scan mode showed comparable sensitivity to tandem LCMS using multiple reaction monitoring. PMID:21843675

Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry.

PubMed

Domènech, Albert; Cortés-Francisco, Nuria; Palacios, Oscar; Franco, José M; Riobó, Pilar; Llerena, José J; Vichi, Stefania; Caixach, Josep

2014-02-07

A multitoxin method has been developed for quantification and confirmation of lipophilic marine biotoxins in mussels by liquid chromatography coupled to high resolution mass spectrometry (HRMS), using an Orbitrap-Exactive HCD mass spectrometer. Okadaic acid (OA), yessotoxin, azaspiracid-1, gymnodimine, 13-desmethyl spirolide C, pectenotoxin-2 and Brevetoxin B were analyzed as representative compounds of each lipophilic toxin group. HRMS identification and confirmation criteria were established. Fragment and isotope ions and ion ratios were studied and evaluated for confirmation purpose. In depth characterization of full scan and fragmentation spectrum of the main toxins were carried out. Accuracy (trueness and precision), linearity, calibration curve check, limit of quantification (LOQ) and specificity were the parameters established for the method validation. The validation was performed at 0.5 times the current European Union permitted levels. The method performed very well for the parameters investigated. The trueness, expressed as recovery, ranged from 80% to 94%, the precision, expressed as intralaboratory reproducibility, ranged from 5% to 22% and the LOQs range from 0.9 to 4.8pg on column. Uncertainty of the method was also estimated for OA, using a certified reference material. A top-down approach considering two main contributions: those arising from the trueness studies and those coming from the precision's determination, was used. An overall expanded uncertainty of 38% was obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

Liquid chromatography with mass spectrometry method based two-step precursor ion scanning for the structural elucidation of flavonoids.

PubMed

Li, Yong; Pang, Tao; Shi, Junli; Lu, Xiuping; Deng, Jianhua; Lin, Qian

2014-11-01

Plant flavonoids are very important secondary metabolites for insect and virus control of their host plant and are potent nutrients for humans. To be able to understand the bioavailability and functions of plant flavonoids, it is necessary to reveal their exact chemical structures. Liquid chromatography with tandem mass spectrometry is a powerful approach for structural elucidation of metabolites. In this report, a two-step precursor ion scanning based liquid chromatography with tandem mass spectrometry method was developed for the structural elucidation of plant flavonoids. The established method consists of the two-step precursor ions scanning for possible flavonoids extraction, MS(2) fragment spectra acquisition and comparison with an online database, liquid chromatography retention rules correction, and commercial standards verification. The developed method was used for the structure elucidation of flavonoids in flowers and leaves of tobacco (Nicotiana tabacum), and 17 flavonoids were identified in the tobacco variety Yunyan 97. Nine of the 17 identified flavonoids were considered to be found in tobacco flowers or/and leaves for the first time based on the available references. This method was proved to be very effective and can be used for the identification of flavonoids in other plants. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Impact of the Rock Mass Deformation on Geometric Changes of a Historical Chimney in the Salt Mine of Bochnia

NASA Astrophysics Data System (ADS)

Szafarczyk, Anna; Gawałkiewicz, Rafał

2018-03-01

There are many ways of the geometry measurement of slim objects, with the application of geodetic and photogrammetric methods. A modern solution in the diagnostics of slim objects is the application of laser scanning, with the use of a scanner of a scanning total station. The point cloud, obtained from the surface of the scanned object gives the possibility of generating not only information on structural surface deformations, but also facilitates obtaining the data on the geometry of the axis of the building, as a basic indicator of the characteristics of its deformation. The cause of the change in the geometry of slim objects is the impact of many external and internal factors. These objects are located in the areas of working or closed underground mines. They can be impacted by the ground and they can face the results of the convergence of cavities. A specific structure of the salt rock mass causes subsequent convergence of the post-exploitation cavities, which has the influence on the behaviour of the terrain surface and the related objects. The authors analysed the impact of the changes in the rock mass and the surface on the changes of the industrial chimney in the Bochnia Salt Mine.

Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

PubMed

Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

2005-03-04

Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

Hierarchical parsing and semantic navigation of full body CT data

NASA Astrophysics Data System (ADS)

Seifert, Sascha; Barbu, Adrian; Zhou, S. Kevin; Liu, David; Feulner, Johannes; Huber, Martin; Suehling, Michael; Cavallaro, Alexander; Comaniciu, Dorin

2009-02-01

Whole body CT scanning is a common diagnosis technique for discovering early signs of metastasis or for differential diagnosis. Automatic parsing and segmentation of multiple organs and semantic navigation inside the body can help the clinician in efficiently obtaining accurate diagnosis. However, dealing with the large amount of data of a full body scan is challenging and techniques are needed for the fast detection and segmentation of organs, e.g., heart, liver, kidneys, bladder, prostate, and spleen, and body landmarks, e.g., bronchial bifurcation, coccyx tip, sternum, lung tips. Solving the problem becomes even more challenging if partial body scans are used, where not all organs are present. We propose a new approach to this problem, in which a network of 1D and 3D landmarks is trained to quickly parse the 3D CT data and estimate which organs and landmarks are present as well as their most probable locations and boundaries. Using this approach, the segmentation of seven organs and detection of 19 body landmarks can be obtained in about 20 seconds with state-of-the-art accuracy and has been validated on 80 CT full or partial body scans.

TU-H-207A-09: An Automated Technique for Estimating Patient-Specific Regional Imparted Energy and Dose From TCM CT Exams Across 13 Protocols

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sanders, J; Tian, X; Segars, P

2016-06-15

Purpose: To develop an automated technique for estimating patient-specific regional imparted energy and dose from tube current modulated (TCM) computed tomography (CT) exams across a diverse set of head and body protocols. Methods: A library of 58 adult computational anthropomorphic extended cardiac-torso (XCAT) phantoms were used to model a patient population. A validated Monte Carlo program was used to simulate TCM CT exams on the entire library of phantoms for three head and 10 body protocols. The net imparted energy to the phantoms, normalized by dose length product (DLP), and the net tissue mass in each of the scan regionsmore » were computed. A knowledgebase containing relationships between normalized imparted energy and scanned mass was established. An automated computer algorithm was written to estimate the scanned mass from actual clinical CT exams. The scanned mass estimate, DLP of the exam, and knowledgebase were used to estimate the imparted energy to the patient. The algorithm was tested on 20 chest and 20 abdominopelvic TCM CT exams. Results: The normalized imparted energy increased with increasing kV for all protocols. However, the normalized imparted energy was relatively unaffected by the strength of the TCM. The average imparted energy was 681 ± 376 mJ for abdominopelvic exams and 274 ± 141 mJ for chest exams. Overall, the method was successful in providing patientspecific estimates of imparted energy for 98% of the cases tested. Conclusion: Imparted energy normalized by DLP increased with increasing tube potential. However, the strength of the TCM did not have a significant effect on the net amount of energy deposited to tissue. The automated program can be implemented into the clinical workflow to provide estimates of regional imparted energy and dose across a diverse set of clinical protocols.« less

Discovery and Identification of Dimethylsilanediol as a Contaminant in ISS Potable Water

NASA Technical Reports Server (NTRS)

Rutz, Jeffrey A.; Schultz, John R.; Kuo, C. Mike; Curtis, Matthew; Jones, Patrick R.; Sparkman, O. David; McCoy, J. Torin

2011-01-01

In September 2010, analysis of ISS potable water samples was undertaken to determine the contaminant(s) responsible for a rise of total organic carbon (TOC) in the Water Processor Assembly (WPA) product water. As analysis of the routine target list of organic compounds did not reveal the contaminant, efforts to look for unknown compounds were initiated, resulting in discovery of an unknown peak in the gas chromatography/mass spectrometry (GC/MS) analysis for glycols. A mass spectrum of the contaminant was then generated by concentrating one of the samples and analyzing it by GC/MS in full-scan mode. Although a computer match of the compound identity could not be obtained with the instrument database, a search with a more up-to-date mass spectral library yielded a good match with dimethylsilanediol (DMSD). Inductively coupled plasma/mass spectrometry (ICP/MS) analyses showed abnormally high silicon levels in the samples, confirming that the unknown compound(s) contained silicon. DMSD was then synthesized to confirm the identification and provide a standard to develop a calibration curve. Further confirmation was provided by external direct analysis in real time time of flight (DART TOF) mass spectrometry. To routinely test for DMSD in the future, a quantitative method was needed. A preliminary GC/MS method was developed and archived samples from various locations on ISS were analyzed to determine the extent of the contamination and provide data for troubleshooting. This paper describes these events in more detail as well as problems encountered in routine GC/MS analyses and the subsequent development of high performance liquid chromatography and LC/MS/MS methods for measuring DMSD.

Simultaneous screening of targeted and non-targeted contaminants using an LC-QTOF-MS system and automated MS/MS library searching.

PubMed

Herrera-Lopez, S; Hernando, M D; García-Calvo, E; Fernández-Alba, A R; Ulaszewska, M M

2014-09-01

Simultaneous high-resolution full-scan and tandem mass spectrometry (MS/MS) analysis using time of flight mass spectrometry brings an answer for increasing demand of retrospective and non-targeted data analysis. Such analysis combined with spectral library searching is a promising tool for targeted and untargeted screening of small molecules. Despite considerable extension of the panel of compounds of tandem mass spectral libraries, the heterogeneity of spectral data poses a major challenge against the effective usage of spectral libraries. Performance evaluation of available LC-MS/MS libraries will significantly increase credibility in the search results. The present work was aimed to evaluate fluctuation of MS/MS pattern, in the peak intensities distribution together with mass accuracy measurements, and in consequence, performance compliant with ion ratio and mass error criteria as principles in identification processes for targeted and untargeted contaminants at trace levels. Matrix effect and ultra-trace levels of concentration (from 50 ng l(-1) to 1000 ng l(-1) were evaluated as potential source of inaccuracy in the performance of spectral matching. Matrix-matched samples and real samples were screened for proof of applicability. By manual review of data and application of ion ratio and ppm error criteria, false negatives were obtained; this number diminished when in-house library was used, while with on-line MS/MS databases 100% of positive samples were found. In our experience, intensity of peaks across spectra was highly correlated to the concentration effect and matrix complexity. In turn, analysis of spectra acquired at trace concentrations and in different matrices results in better performance in providing correct and reliable identification. Copyright © 2014 John Wiley & Sons, Ltd.

Street-Like Synthesis of Krokodil Results in the Formation of an Enlarged Cluster of Known and New Morphinans.

PubMed

Soares, José Xavier; Alves, Emanuele Amorim; Silva, André M N; de Figueiredo, Natália Guimarães; Neves, João F; Cravo, Sara Manuela; Rangel, Maria; Netto, Annibal Duarte Pereira; Carvalho, Félix; Dinis-Oliveira, Ricardo Jorge; Afonso, Carlos Manuel

2017-08-21

"Krokodil" is the street name for a homemade injectable drug that has been used as a cheap substitute for heroin. Codeine is the opioid starting material for krokodil synthesis, and desomorphine is claimed to be the main opioid of krokodil and the main component responsible for its addictive and psychoactive characteristics. However, due to its peculiar manufacture, using cheap raw materials, krokodil is composed of a large and complex mixture of different substances. In order to shed some light upon the chemical complexity of krokodil, its profiling was conducted by reverse phase high performance liquid chromatography coupled to a photodiode array detector (RP-HPLC-DAD) and by liquid chromatography coupled to high resolution tandem mass spectrometry (LC-ESI-IT-Orbitrap-MS). Besides desomorphine, codeine, and morphine, profiting from the high resolution mass spectrometry (HRMS) data, an endeavor to study the morphinans content in krokodil was set for the first time. Considering codeine as the only morphinan precursor and the possible chemical transformations that can occur during krokodil synthesis, the morphinan chemical space was designed, and 95 compounds were defined. By making use of the morphinan chemical space in krokodil, the exact masses featured by HRMS, and the morphinan mass fragmentations patterns, a targeted identification approach was designed and implemented.The proposed 95 morphinans were searched using the full scan chromatogram of krokodil, and findings were validated by mass fragmentation of the correspondent precursor ions (MS 2 spectra). Following this effort, a total of 54 morphinans were detected, highlighting the fact that these additional morphinans may contribute to the psychotropic effects of krokodil.

Reversed-phase ultra-high-performance liquid chromatography coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry as a powerful tool for metabolic profiling of vegetables: Lactuca sativa as an example of its application.

PubMed

Abu-Reidah, I M; Contreras, M M; Arráez-Román, D; Segura-Carretero, A; Fernández-Gutiérrez, A

2013-10-25

Lettuce (Lactuca sativa), a leafy vegetal widely consumed worldwide, fresh cut or minimally processed, constitutes a major dietary source of natural antioxidants and bioactive compounds. In this study, reversed-phase ultra-high-performance liquid chromatography (RP-UHPLC) coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry (ESI-QTOF-MS) was applied for the comprehensive profiling of polar and semi-polar metabolites from three lettuce cultivars (baby, romaine, and iceberg). The UHPLC systems allowed the use of a small-particle-size C18 column (1.8 μm), with very fine resolution for the separation of up to seven isomers, and the QTOF mass analyzer enabled sensitive detection with high mass resolution and accuracy in full scan. Thus, a total of 171 compounds were tentatively identified by matching their accurate mass signals and suggested molecular formula with those previously reported in family Asteraceae. Afterwards, their structures were also corroborated by the MS/MS data provided by the QTOF analyzer. Well-known amino acids, organic acids, sesquiterpene lactones, phenolic acids and flavonoids were characterized, e.g. lactucin, lactucopicrin, caftaric acid, chlorogenic acid, caffeoylmalic acid, chicoric acid, isochlorogenic acid A, luteolin, and quercetin glycosides. For this plant species, this is the first available report of several isomeric forms of the latter polyphenols and other types of components such as nucleosides, peptides, and tryptophan-derived alkaloids. Remarkably, 10 novel structures formed by the conjugation of known amino acids and sesquiterpene lactones were also proposed. Thus, the methodology applied is a useful option to develop an exhaustive metabolic profiling of plants that helps to explain their potential biological activities and folk uses. Copyright © 2013 Elsevier B.V. All rights reserved.

Anthropometric and Three-Compartment Body Composition Differences between Super League and Championship Rugby League Players: Considerations for the 2015 Season and Beyond

PubMed Central

Jones, Ben; Till, Kevin; Barlow, Matthew; Lees, Matthew; O’Hara, John Paul; Hind, Karen

2015-01-01

Super League (SL) and Championship (RLC) rugby league players will compete against each other in 2015 and beyond. To identify possible discrepancies, this study compared the anthropometric profile and body composition of current SL (full-time professional) and RLC (part-time semi-professional) players using dual-energy X-ray absorptiometry (DXA). A cross-sectional design involved DXA scans on 67 SL (n=29 backs, n=38 forwards) and 46 RLC (n=20 backs, n=26 forwards) players during preseason. A one-way ANOVA was used to compare age, stature, body mass, soft tissue fat percentage, bone mineral content (BMC), total and regional (i.e., arms, legs and trunk) fat and lean mass between SL forwards, SL backs, RLC forwards and RLC backs. No significant differences in age, stature or body mass were observed. SL forwards and backs had relatively less soft tissue fat (17.5 ± 3.7 and 14.8 ± 3.6 vs. 21.4 ± 4.3 and 20.8 ± 3.8%), greater BMC (4,528 ± 443 and 4,230 ± 447 vs. 4,302 ± 393 and 3,971 ± 280 g), greater trunk lean mass (37.3 ± 3.0 and 35.3 ± 3.8 vs. 34.9 ± 32.3 and 32.3 ± 2.6 kg) and less trunk fat mass (8.5 ± 2.7 and 6.2 ± 2.1 vs. 10.7 ± 2.8 and 9.5 ± 2.9 kg) than RLC forwards and backs. Observed differences may reflect selection based on favourable physical attributes, or training adaptations. To reduce this discrepancy, some RLC players should reduce fat mass and increase lean mass, which may be of benefit for the 2015 season and beyond. PMID:26221720

Induced in-source fragmentation pattern of certain novel (1Z,2E)-N-(aryl)propanehydrazonoyl chlorides by electrospray mass spectrometry (ESI-MS/MS)

PubMed Central

2013-01-01

Background Collision induced dissociation (CID) in the triple quadrupole mass spectrometer system (QQQ) typically yields more abundant fragment ions than those produced with resonance excitation in the presence of helium gas in the ion trap mass spectrometer system (IT). Detailed product ion spectra can be obtained from one stage MS2 scan using the QQQ. In contrast, generating the same number of fragment ions in the ion trap requires multiple stages of fragmentation (MSn) using CID via in-trap resonance excitation with the associated time penalties and drop in sensitivity. Results The use of in-source fragmentation with electrospray ionization (ESI) followed by product ion scan (MS2) in a triple quadrupole mass spectrometer system, was demonstrated. This process enhances the qualitative power of tandem mass spectrometry to simulate the MS3 of ion trap for a comprehensive study of fragmentation mechanisms. A five pharmacologically significant (1Z, 2E)-N-arylpropanehydrazonoyl chlorides (3a-e) were chosen as model compounds for this study. In this work, detailed fragmentation pathways were elucidated by further dissociation of each fragment ion in the ion spectrum, essentially, by incorporating fragmentor voltage induced dissociation (in-source fragmentation) and isolation of fragments in a quadrupole cell Q1. Subsequently, CID occurs in cell, Q2, and fragment ions are analyzed in Q3 operated in product ion mode this process can be referred to as pseudo-MS3 scan mode. Conclusions This approach allowed unambiguous assignment of all fragment ions using tandem mass spectrometer and provided adequate sensitivity and selectivity. It is beneficial for structure determination of unknown trace components. The data presented in this paper provide useful information on the effect of different substituents on the ionization/fragmentation processes and can be used in the characterization of this important class of compounds. PMID:23351484

Three-dimensional computational model of a blood oxygenator reconstructed from micro-CT scans.

PubMed

D'Onofrio, C; van Loon, R; Rolland, S; Johnston, R; North, L; Brown, S; Phillips, R; Sienz, J

2017-09-01

Cardiopulmonary bypass procedures are one of the most common operations and blood oxygenators are the centre piece for the heart-lung machines. Blood oxygenators have been tested as entire devices but intricate details on the flow field inside the oxygenators remain unknown. In this study, a novel method is presented to analyse the flow field inside oxygenators based on micro Computed Tomography (μCT) scans. Two Hollow Fibre Membrane (HFM) oxygenator prototypes were scanned and three-dimensional full scale models that capture the device-specific fibre distributions are set up for computational fluid dynamics analysis. The blood flow through the oxygenator is modelled as a non-Newtonian fluid. The results were compared against the flow solution through an ideal fibre distribution and show the importance of a uniform distribution of fibres and that the oxygenators analysed are not susceptible to flow directionality as mass flow versus area remain the same. However the pressure drop across the oxygenator is dependent on flow rate and direction. By comparing residence time of blood against the time frame to fully saturate blood with oxygen we highlight the potential of this method as design optimisation tool. In conclusion, image-based reconstruction is found to be a feasible route to assess oxygenator performance through flow modelling. It offers the possibility to review a product as manufactured rather than as designed, which is a valuable insight as a precursor to the approval processes. Finally, the flow analysis presented may be extended, at computational cost, to include species transport in further studies. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

An Intercomparison of Research Scanning Polarimeter Cloud Droplet Number Concentrations with Aerosol Properties over the Atlantic Ocean

NASA Astrophysics Data System (ADS)

Sinclair, K.; van Diedenhoven, B.; Cairns, B.; Alexandrov, M. D.; Ziemba, L. D.; Moore, R.; Crosbie, E.; Hostetler, C. A.

2016-12-01

Cloud droplet number concentration (CDNC) is a key parameter of of liquid clouds and is essential for the understanding of aerosol-cloud interaction. It couples surface aerosol composition and chemistry on the one hand and cloud reflectivity on the other. It impacts radiative forcing, cloud evolution, precipitation, global climate and, through observation, can be used to monitor the cloud albedo effect, or the first indirect effect. The North Atlantic and Marine Ecosystems Study (NAAMES), which is a NASA-led ship and air campaign that takes place off the east coast of Newfoundland, observed many low cloud decks and aerosols over a marine environment. This campaign has completed two of four deployments and provides an excellent opportunity for the Research Scanning Polarimeter (RSP) to cross-validate its approach of sensing CDNC with the Langley Aerosol Research Group Experiment's (LARGE's) Cloud Droplet Probe (CDP). The RSP is an airborne scanning sensor that provides high-precision measurements of polarized and full-intensity radiances at multiple angles over a wide spectral range. Each of the four NAAMES deployments are aligned to a specific annual event in the plankton cycle, along with other variations in environmental conditions. The Fall 2015 and spring 2016 deployments allow us to demonstrate and characterize the RSP's performance over a range of CDNCs and cloud types. We also assess correlations between the RSP CDNC measurements and atmospheric aerosol load. Using the LARGE Cloud Particle Counter (CPC) and Aerosol Mass Spectrometer (AMS), links between the size and type of aerosols and the RSP CDNC retrievals are explored.

Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

USGS Publications Warehouse

Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

2000-01-01

A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

Determining concentrations of 2-bromoallyl alcohol and dibromopropene in ground water using quantitative methods

USGS Publications Warehouse

Panshin, Sandra Y.

1997-01-01

A method for determining levels of 2-bromoallyl alcohol and 2,3-dibromopropene from ground-water samples using liquid/liquid extraction followed by gas chromatography/mass spectrometry is described. Analytes were extracted from the water using three aliquots of dichloromethane. The aliquots were combined and reduced in volume by rotary evaporation followed by evaporation using a nitrogen stream. The extracts were analyzed by capillary-column gas chromatography/mass spectrometry in the full-scan mode. Estimated method detection limits were 30 nanograms per liter for 2-bromoallyl alcohol and 10 nanograms per liter for 2,3-dibromopropene. Recoveries were determined by spiking three matrices at two concentration levels (0.540 and 5.40 micrograms per liter for 2-bromoallyl alcohol; and 0.534 and 5.34micro-grams per liter for dibromopropene). For seven replicates of each matrix at the high concentration level, the mean percent recoveries ranged from 43.9 to 64.9 percent for 2-bromoallyl alcohol, and from 87.5 to 99.3 percent for dibromopropene. At the low concentration level, the mean percent recoveries ranged from 43.8 to 95.2 percent for 2-bromoallyl alcohol, and from 71.3 to 84.9 percent for dibromopropene.

In Vitro Metabolic Studies of REV-ERB Agonists SR9009 and SR9011.

PubMed

Geldof, Lore; Deventer, Koen; Roels, Kris; Tudela, Eva; Van Eeno, Peter

2016-10-03

SR9009 and SR9011 are attractive as performance-enhancing substances due to their REV-ERB agonist effects and thus circadian rhythm modulation activity. Although no pharmaceutical preparations are available yet, illicit use of SR9009 and SR9011 for doping purposes can be anticipated, especially since SR9009 is marketed in illicit products. Therefore, the aim was to identify potential diagnostic metabolites via in vitro metabolic studies to ensure effective (doping) control. The presence of SR9009 could be demonstrated in a black market product purchased over the Internet. Via human liver microsomal metabolic assays, eight metabolites were detected for SR9009 and fourteen metabolites for SR9011 by liquid chromatography-high resolution mass spectrometry (LC-HRMS). Structure elucidation was performed for all metabolites by LC-HRMS product ion scans in both positive and negative ionization mode. Retrospective data analysis was applied to 1511 doping control samples previously analyzed by a full-scan LC-HRMS screening method to verify the presence of SR9009, SR9011 and their metabolites. So far, the presence of neither the parent compound nor the metabolites could be detected in routine urine samples. However, to further discourage use of these potentially harmful compounds, incorporation of SR9009 and SR9011 into screening methods is highly recommended.

Design Spectrum Analysis in NASTRAN

NASA Technical Reports Server (NTRS)

Butler, T. G.

1984-01-01

The utility of Design Spectrum Analysis is to give a mode by mode characterization of the behavior of a design under a given loading. The theory of design spectrum is discussed after operations are explained. User instructions are taken up here in three parts: Transient Preface, Maximum Envelope Spectrum, and RMS Average Spectrum followed by a Summary Table. A single DMAP ALTER packet will provide for all parts of the design spectrum operations. The starting point for getting a modal break-down of the response to acceleration loading is the Modal Transient rigid format. After eigenvalue extraction, modal vectors need to be isolated in the full set of physical coordinates (P-sized as opposed to the D-sized vectors in RF 12). After integration for transient response the results are scanned over the solution time interval for the peak values and for the times that they occur. A module called SCAN was written to do this job, that organizes these maxima into a diagonal output matrix. The maximum amplifier in each mode is applied to the eigenvector of each mode which then reveals the maximum displacements, stresses, forces and boundary reactions that the structure will experience for a load history, mode by mode. The standard NASTRAN output processors have been modified for this task. It is required that modes be normalized to mass.

In Vitro Metabolic Studies of REV-ERB Agonists SR9009 and SR9011

PubMed Central

Geldof, Lore; Deventer, Koen; Roels, Kris; Tudela, Eva; Van Eenoo, Peter

2016-01-01

SR9009 and SR9011 are attractive as performance-enhancing substances due to their REV-ERB agonist effects and thus circadian rhythm modulation activity. Although no pharmaceutical preparations are available yet, illicit use of SR9009 and SR9011 for doping purposes can be anticipated, especially since SR9009 is marketed in illicit products. Therefore, the aim was to identify potential diagnostic metabolites via in vitro metabolic studies to ensure effective (doping) control. The presence of SR9009 could be demonstrated in a black market product purchased over the Internet. Via human liver microsomal metabolic assays, eight metabolites were detected for SR9009 and fourteen metabolites for SR9011 by liquid chromatography–high resolution mass spectrometry (LC–HRMS). Structure elucidation was performed for all metabolites by LC–HRMS product ion scans in both positive and negative ionization mode. Retrospective data analysis was applied to 1511 doping control samples previously analyzed by a full-scan LC–HRMS screening method to verify the presence of SR9009, SR9011 and their metabolites. So far, the presence of neither the parent compound nor the metabolites could be detected in routine urine samples. However, to further discourage use of these potentially harmful compounds, incorporation of SR9009 and SR9011 into screening methods is highly recommended. PMID:27706103

The Large Quasar Reference Frame (LQRF). An Optical Representation of the ICRS

DTIC Science & Technology

2009-10-01

faint regimes, both the 2MASS and the preliminary northernmost UCAC2 positions are shown of astrometry consistent with the UCAC2 main catalog, and the...is used. 2.7. 2MASS The Two Micron All-Sky Survey point source catalog (Cutri et al. 2003), hereafter 2MASS , derives from an uniform scan of the...17.1, H = 16.4, and K = 15.3. The 2MASS contains the position of 470 992 970 sources, but no proper motions. The astrometry is referred to the

Unicentric Castleman's Disease Revealed by 18F-FDG PET/CT and Somatostatin Receptor Scintigraphy With 99mTc-HYNIC-TOC.

PubMed

Luo, Yaping; Wang, Ling; Pan, Qingqing; Ma, Yanru; Li, Fang

2018-07-01

A 51-year-old woman with a history of hypertension and abdominal pain was found with a retroperitoneal mass. The mass had intense enhancement in contrast-enhanced CT, and it showed a moderate degree of increased FDG uptake in PET/CT. The mass was also positive in somatostatin receptor scintigraphy with Tc-HYNIC-TOC, but it was negative in I-MIBG scan. The histopathological result after surgical resection of the mass confirmed the diagnosis of Castleman's disease, the hyaline vascular variant.

Castleman Disease Presenting as an Abdominal Mass.

PubMed

Shariati, Farnaz; Verter, Elizabeth; Chang, Wendy; Huang, Li; Joshi, Virendra

2017-01-01

Unicentric Castleman disease is a rare condition of lymphoid hyperplasia, of which only 15% of cases occur in the abdomen. We report a 66-year-old man who presented with complaints of abdominal pain. Computed tomography scans revealed nephrolithiasis and a homogeneous calcified mass between the pancreas and stomach and several para-pancreatic nodes. Direct visualization during exploratory laparotomy revealed a mass on the lesser curvature of the stomach. Pyloromyotomy and mass resection were performed. Biopsy showed reactive lymphoid hyperplasia consistent with the hyaline vascular variant of Castleman disease.

Castleman Disease Presenting as an Abdominal Mass

PubMed Central

Verter, Elizabeth; Chang, Wendy; Huang, Li; Joshi, Virendra

2017-01-01

Unicentric Castleman disease is a rare condition of lymphoid hyperplasia, of which only 15% of cases occur in the abdomen. We report a 66-year-old man who presented with complaints of abdominal pain. Computed tomography scans revealed nephrolithiasis and a homogeneous calcified mass between the pancreas and stomach and several para-pancreatic nodes. Direct visualization during exploratory laparotomy revealed a mass on the lesser curvature of the stomach. Pyloromyotomy and mass resection were performed. Biopsy showed reactive lymphoid hyperplasia consistent with the hyaline vascular variant of Castleman disease. PMID:28584844

An intelligent detection method for high-field asymmetric waveform ion mobility spectrometry.

PubMed

Li, Yue; Yu, Jianwen; Ruan, Zhiming; Chen, Chilai; Chen, Ran; Wang, Han; Liu, Youjiang; Wang, Xiaozhi; Li, Shan

2018-04-01

In conventional high-field asymmetric waveform ion mobility spectrometry signal acquisition, multi-cycle detection is time consuming and limits somewhat the technique's scope for rapid field detection. In this study, a novel intelligent detection approach has been developed in which a threshold was set on the relative error of α parameters, which can eliminate unnecessary time spent on detection. In this method, two full-spectrum scans were made in advance to obtain the estimated compensation voltage at different dispersion voltages, resulting in a narrowing down of the whole scan area to just the peak area(s) of interest. This intelligent detection method can reduce the detection time to 5-10% of that of the original full-spectrum scan in a single cycle.

Novel LC-ESI/MS/MSn Method for the Characterization and Quantification of 2′-Deoxyguanosine Adducts of the Dietary Carcinogen 2-Amino-1-methyl-6-phenylimidazo[4,5-b]pyridine by 2-D Linear Quadrupole Ion Trap Mass Spectrometry

PubMed Central

Goodenough, Angela K.; Schut, Herman A. J.; Turesky, Robert J.

2008-01-01

An accurate and sensitive liquid chromatography-electrospray ionization/multi-stage mass spectrometry (LC-ESI/MS/MSn) technique has been developed for the characterization and quantification of 2′-deoxyguanosine (dG) adducts of the dietary mutagen, 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP). PhIP is an animal and potential human carcinogen that occurs in grilled meats. Following enzymatic digestion and adduct enrichment by solid-phase extraction (SPE), PhIP—DNA adducts were analyzed by MS/MS and MSn scan modes on a 2-D linear quadrupole ion trap mass spectrometer (QIT/MS). The major DNA adduct, N-(deoxyguanosin-8-yl)-2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (dG-C8-PhIP), was detected in calf thymus (CT) DNA modified in vitro with a bioactivated form of PhIP and in the colon and liver of rats given PhIP as part of the diet. The lower limit of detection (LOD) was 1 adduct per 108 DNA bases, and the limit of quantification (LOQ) was 3 adducts per 108 DNA bases in both MS/MS and MS3 scan modes, using 27 μg of DNA for analysis. Measurements were based on isotope dilution with the internal standard, N-(deoxyguanosin-8-yl)-2-amino-1-(trideutero)methyl-6-phenylimidazo[4,5-b]pyridine (dG-C8-[2H3C]-PhIP). The selected reaction monitoring (SRM) scan mode in MS/MS was employed to monitor the loss of deoxyribose (dR) from the protonated molecules of the adducts ([M + H - 116]+). The consecutive reaction monitoring (CRM) scan modes in MS3 and MS4 were used to measure and further characterize product ions of the aglycone ion (BH2+) (Guanyl-PhIP). The MS3 scan mode was effective in eliminating isobaric interferences observed in the MS/MS scan mode and resulted in an improved signal-to-noise (S/N) ratio. Moreover, the product ion spectra obtained by the MSn scan modes provided rich structural information about the adduct and were used to corroborate the identity of dG-C8-PhIP. In addition, an isomeric dG-PhIP adduct was detected in vivo. This LCESI/MS/MSn method is the first reported application on the use of the MS3 scan mode for the analysis of DNA adducts in vivo. PMID:17305409

The effective dose of different scanning protocols using the Sirona GALILEOS® comfort CBCT scanner

PubMed Central

Bohay, R; Kaci, L; Barnett, R; Battista, J

2015-01-01

Objectives: To determine the effective dose and CT dose index (CTDI) for a range of imaging protocols using the Sirona GALILEOS® Comfort CBCT scanner (Sirona Dental Systems GmbH, Bensheim, Germany). Methods: Calibrated optically stimulated luminescence dosemeters were placed at 26 sites in the head and neck of a modified RANDO® phantom (The Phantom Laboratory, Greenwich, NY). Effective dose was calculated for 12 different scanning protocols. CTDI measurements were also performed to determine the dose–length product (DLP) and the ratio of effective dose to DLP for each scanning protocol. Results: The effective dose for a full maxillomandibular scan at 42 mAs was 102 ± 1 μSv and remained unchanged with varying contrast and resolution settings. This compares with 71 μSv for a maxillary scan and 76 μSv for a mandibular scan with identical milliampere-seconds (mAs) at high contrast and resolution settings. Conclusions: Changes to mAs and beam collimation have a significant influence on effective dose. Effective dose and DLP vary linearly with mAs. A collimated maxillary or mandibular scan decreases effective dose by approximately 29% and 24%, respectively, as compared with a full maxillomandibular scan. Changes to contrast and resolution settings have little influence on effective dose. This study provides data for setting individualized patient exposure protocols to minimize patient dose from ionizing radiation used for diagnostic or treatment planning tasks in dentistry. PMID:25358865

Appendicular and whole body lean mass outcomes are associated with finite element analysis-derived bone strength at the distal radius and tibia in adults aged 40years and older.

PubMed

Gibbs, Jenna C; Giangregorio, Lora M; Wong, Andy K O; Josse, Robert G; Cheung, Angela M

2017-10-01

The purpose of this cross-sectional study was to determine how appendicular lean mass index (ALMI), and whole body lean (LMI) and fat mass indices (FMI) associate with estimated bone strength outcomes at the distal radius and tibia in adults aged 40 years and older. Dual energy X-ray absorptiometry (DXA) scans were performed to determine body composition, including whole body lean and fat mass, and appendicular lean mass. ALMI (appendicular lean mass/height 2 ), LMI (lean tissue mass/height 2 ) and FMI (fat mass/height 2 ) were calculated. High-resolution peripheral quantitative computed tomography (HRpQCT) scans were performed to assess bone structural properties at the distal radius and tibia. Using finite element analysis, failure load (N), stiffness (N/mm), ultimate stress (MPa), and cortical-to-trabecular load ratio were estimated from HRpQCT scans. The associations between body composition (ALMI, LMI, FMI) and estimated bone strength were examined using bivariate and multivariable linear regression analyses adjusting for age, sex, and other confounding variables. In 197 participants (127 women; mean±SD, age: 69.5±10.3y, body mass index: 27.95±4.95kg/m 2 , ALMI: 7.31±1.31kg/m 2 ), ALMI and LMI were significantly associated with failure load at the distal radius and tibia (explained 39%-48% of the variance) and remained significant after adjusting for confounding variables and multiple testing (R 2 =0.586-0.645, p<0.001). ALMI, LMI, and FMI did not have significant associations with ultimate stress in our multivariable models. FMI was significantly associated with cortical-to-trabecular load ratio at the distal radius and tibia (explained 6%-12% of the variance) and remained significant after adjusting for confounders and multiple testing (R 2 =0.208-0.243, p<0.001). FMI was no longer significantly associated with failure load after adjusting for confounders. These findings suggest that ALMI and LMI are important determinants of estimated bone strength, particularly failure load, at the distal radius and tibia, and may contribute to preservation of bone strength in middle-to-late adulthood. Copyright © 2017 Elsevier Inc. All rights reserved.

In silico comparison of the reproducibility of full-arch implant provisional restorations to final restoration between a 3D Scan/CAD/CAM technique and the conventional method.

PubMed

Mino, Takuya; Maekawa, Kenji; Ueda, Akihiro; Higuchi, Shizuo; Sejima, Junichi; Takeuchi, Tetsuo; Hara, Emilio Satoshi; Kimura-Ono, Aya; Sonoyama, Wataru; Kuboki, Takuo

2015-04-01

The aim of this article was to investigate the accuracy in the reproducibility of full-arch implant provisional restorations to final restorations between a 3D Scan/CAD/CAM technique and the conventional method. We fabricated two final restorations for rehabilitation of maxillary and mandibular complete edentulous area and performed a computer-based comparative analysis of the accuracy in the reproducibility of the provisional restoration to final restoration between a 3D scanning and CAD/CAM (Scan/CAD/CAM) technique and the conventional silicone-mold transfer technique. Final restorations fabricated either by the conventional or Scan/CAD/CAM method were successfully installed in the patient. The total concave/convex volume discrepancy observed with the Scan/CAD/CAM technique was 503.50mm(3) and 338.15 mm(3) for maxillary and mandibular implant-supported prostheses (ISPs), respectively. On the other hand, total concave/convex volume discrepancy observed with the conventional method was markedly high (1106.84 mm(3) and 771.23 mm(3) for maxillary and mandibular ISPs, respectively). The results of the present report suggest that Scan/CAD/CAM method enables a more precise and accurate transfer of provisional restorations to final restorations compared to the conventional method. Copyright © 2014 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

Pituitary Magnetic Resonance Imaging for Sellar and Parasellar Masses: Ten-Year Experience in 2598 Patients

PubMed Central

Famini, Pouyan; Maya, Marcel M.

2011-01-01

Context: Sellar and parasellar masses present with overlapping clinical and radiological features ranging from asymptomatic incidental presentations and hormonal effects to compressive local mass effects. Pituitary masses are diagnosed with increased frequency with magnetic resonance imaging (MRI) advancements and availability, but indications and diagnostic outcomes of MRI screening for sellar lesions are not defined. Although pituitary adenomas are the most frequently encountered sellar mass lesions, other etiologies should be considered in the differential diagnosis of a sellar mass. Setting: The study was conducted at a tertiary pituitary center. Patients: This study was a retrospective review of 2598 subjects undergoing at least one pituitary MRI scan from 1999 to 2009. Main Outcome Measure: Prevalence and diagnosis of specific sellar and parasellar masses as screened by pituitary MRI. Results: The most common indications for pituitary imaging, excluding known mass follow-up, were for evaluation of hyperprolactinemia or hypogonadism. A normal pituitary gland was reported in 47% of subjects undergoing pituitary MRI. The most common pituitary adenomas initially identified by MRI included prolactinoma (40%), nonfunctioning adenoma (37%), and GH adenoma (13%). Nonadenomatous sellar masses accounted for 18% of visible lesions, of which the most common were Rathke's cleft cyst (19%), craniopharyngioma (15%), and meningioma (15%). Metastases accounted for 5% of nonpituitary lesions and breast cancer was the most common primary source. Conclusions: Half of all pituitary MRI scans performed in a large patient population yielded no visible lesion. Nonadenomatous pituitary lesions should be considered in the diagnosis of sellar masses observed on MRI, and a high clinical suspicion is required to exclude the presence of a nonfunctioning pituitary adenoma. PMID:21470998

Simultaneous determination of 40 novel psychoactive stimulants in urine by liquid chromatography-high resolution mass spectrometry and library matching

PubMed Central

Concheiro, Marta; Castaneto, Marisol; Kronstrand, Robert; Huestis, Marilyn A.

2015-01-01

The emergence of novel psychoactive substances is an ongoing challenge for analytical toxicologists. Different analogs are continuously introduced in the market to circumvent legislation and to enhance their pharmacological activity. Although detection of drugs in blood indicates recent exposure and link intoxication to the causative agent, urine is still the most preferred testing matrix in clinical and forensic settings. We developed a method for the simultaneous quantification of 8 piperazines, 4 designer amphetamines and 28 synthetic cathinones and 4 metabolites, in urine by liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS). Data were acquired in full scan and data dependent MS2 mode. Compounds were quantified by precursor ion exact mass, and confirmed by product ion spectra library matching, taking into account product ions’ exact mass and intensities. One-hundred μL urine was subjected to solid phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase separation was achieved with gradient mobile phase of 0.1% formic acid in water and in acetonitrile in 20 min. The assay was linear from 2.5 or 5 to 500μg/L. Imprecision (n=15) was <15.4%, and accuracy (n=15) 84.2-118.5%. Extraction efficiency was 51.2-111.2%, process efficiency 57.7-104.9% and matrix effect ranged from -41.9 to 238.5% (CV<23.3%, except MDBZP CV<34%). Authentic urine specimens (n=62) were analyzed with the method that provides a comprehensive confirmation for 40 new stimulant drugs with specificity and sensitivity. PMID:25931378

Assessment of meat authenticity using bioinformatics, targeted peptide biomarkers and high-resolution mass spectrometry.

PubMed

Ruiz Orduna, Alberto; Husby, Erik; Yang, Charles T; Ghosh, Dipankar; Beaudry, Francis

2015-01-01

In recent years a significant increase of food fraud has been observed, ranging from false label claims to the use of additives and fillers to increase profitability. Recently in 2013 horse and pig DNAs were detected in beef products sold from several retailers. Mass spectrometry (MS) has become the workhorse in protein research, and the detection of marker proteins could serve for both animal species and tissue authentication. Meat species authenticity is performed in this paper using a well-defined proteogenomic annotation, carefully chosen surrogate tryptic peptides and analysis using a hybrid quadrupole-Orbitrap MS. Selected mammalian meat samples were homogenised and proteins were extracted and digested with trypsin. The samples were analysed using a high-resolution MS. Chromatography was achieved using a 30-min linear gradient along with a BioBasic C8 100 × 1 mm column at a flow rate of 75 µl min(-1). The MS was operated in full-scan high resolution and accurate mass. MS/MS spectra were collected for selected proteotypic peptides. Muscular proteins were methodically analysed in silico in order to generate tryptic peptide mass lists and theoretical MS/MS spectra. Following a comprehensive bottom-up proteomic analysis, we detected and identified a proteotypic myoglobin tryptic peptide (120-134) for each species with observed m/z below 1.3 ppm compared with theoretical values. Moreover, proteotypic peptides from myosin-1, myosin-2 and β-haemoglobin were also identified. This targeted method allowed comprehensive meat speciation down to 1% (w/w) of undesired product.

Degradation of the Neonicotinoid Pesticides in the Atmospheric Pressure Ionization Source.

PubMed

Chai, Yunfeng; Chen, Hongping; Liu, Xin; Lu, Chengyin

2018-02-01

During the analysis of neonicotinoid pesticide standards (thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid) by mass spectrometry, the degradation of these pesticides (M-C=N-R is degraded into M-C=O, M is the skeleton moiety, and R is NO 2 or CN) was observed in the atmospheric pressure ionization interfaces (ESI and APCI). In APCI, the degradation of all the five neonicotinoid pesticides studied took place, and the primary mechanism was in-source ion/molecule reaction, in which a molecule of water (confirmed by use of H 2 18 O) attacked the carbon of the imine group accompanying with loss of NH 2 R (R=NO 2 , CN). For the nitroguanidine neonicotinoid pesticides (R=NO 2 , including thiamethoxam, clothianidin, and imidacloprid), higher auxiliary gas heater temperature also contributed to their degradation in APCI due to in-source pyrolysis. The degradation of the five neonicotinoid pesticides studied in ESI was not significant. In ESI, only the nitroguanidine neonicotinoid pesticides could generate the degradation products through in-source fragmentation mechanism. The degradation of cyanoamidine neonicotinoid pesticides (R=CN, including acetamiprid and thiacloprid) in ESI was not observed. The degradation of neonicotinoid pesticides in the ion source of mass spectrometer renders some adverse consequences, such as difficulty interpreting the full-scan mass spectrum, reducing the sensitivity and accuracy of quantitative analysis, and misleading whether these pesticides have degraded in the real samples. Therefore, a clear understanding of these unusual degradation reactions should facilitate the analysis of neonicotinoid pesticides by atmospheric pressure ionization mass spectrometry. Graphical Abstract.

Metastatic Neuroblastoma in Adult Patient, Presenting as a Super Scan on 68Ga-DOTANOC PET/CT Imaging.

PubMed

Malik, Dharmender; Jois, Abhiram; Singh, Harmandeep; Bora, Girdhar S; Basher, Rajender Kumar; Mittal, Bhagwant Rai

2017-09-01

We report a case of 23-year-old man who presented with complaints of progressive abdominal distension for the past 3 months along with the loss of appetite and weight and had a large solid cystic mass in the left half of the abdominal cavity revealed on ultrasonography and contrast-enhanced CT of the abdomen. Subsequent biopsy and histopathology revealed it to be neuroblastoma. Ga-DOTANOC PET/CT scan performed to rule out distant metastasis showed intense radiotracer uptake distributed throughout the skeleton, mimicking a super scan.

Identification of glyceollin metabolites derived from conjugation with glutathione and glucuronic acid in rats by on-line liquid chromatography-electrospray ionization tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

Glyceollin-related metabolites produced in rats following oral glyceollin administration were screened and identified by precursor and product ion scanning using liquid chromatography, coupled on-line with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS), to identify all glyceollin me...

Gibberellin A3 Is Biosynthesized from Gibberellin A20 via Gibberellin A5 in Shoots of Zea mays L. 1

PubMed Central

Fujioka, Shozo; Yamane, Hisakazu; Spray, Clive R.; Phinney, Bernard O.; Gaskin, Paul; MacMillan, Jake; Takahashi, Nobutaka

1990-01-01

[17-13C,3H]-Labeled gibberellin A20 (GA20), GA5, and GA1 were fed to homozygous normal (+/+), heterozygous dominant dwarf (D8/+), and homozygous dominant dwarf (D8/D8) seedlings of Zea mays L. (maize). 13C-Labeled GA29, GA8, GA5, GA1, and 3-epi-GA1, as well as unmetabolized [13C]GA20, were identified by gas chromatography-selected ion monitoring (GC-SIM) from feeds of [17-13C, 3H]GA20 to all three genotypes. 13C-Labeled GA8 and 3-epi-G1, as well as unmetabolized [13C]GA1, were identified by GC-SIM from feeds of [17-13C, 3H]GA1 to all three genotypes. From feeds of [17-13C, 3H]GA5, 13C-labeled GA3 and the GA3-isolactone, as well as unmetabolized [13C]GA5, were identified by GC-SIM from +/+ and D8/D8, and by full scan GC-MS from D8/+. No evidence was found for the metabolism of [17-13C, 3H]GA5 to [13C]GA1, either by full scan GC-mass spectrometry or by GC-SIM. The results demonstrate the presence in maize seedlings of three separate branches from GA20, as follows: (a) GA20 → GA1 → GA8; (b) GA20 → GA5 → GA3; and (c) GA20 → GA29. The in vivo biogenesis of GA3 from GA5, as well as the origin of GA5 from GA20, are conclusively established for the first time in a higher plant (maize shoots). PMID:16667678

Measuring the Autocorrelation Function of Nanoscale Three-Dimensional Density Distribution in Individual Cells Using Scanning Transmission Electron Microscopy, Atomic Force Microscopy, and a New Deconvolution Algorithm.

PubMed

Li, Yue; Zhang, Di; Capoglu, Ilker; Hujsak, Karl A; Damania, Dhwanil; Cherkezyan, Lusik; Roth, Eric; Bleher, Reiner; Wu, Jinsong S; Subramanian, Hariharan; Dravid, Vinayak P; Backman, Vadim

2017-06-01

Essentially all biological processes are highly dependent on the nanoscale architecture of the cellular components where these processes take place. Statistical measures, such as the autocorrelation function (ACF) of the three-dimensional (3D) mass-density distribution, are widely used to characterize cellular nanostructure. However, conventional methods of reconstruction of the deterministic 3D mass-density distribution, from which these statistical measures can be calculated, have been inadequate for thick biological structures, such as whole cells, due to the conflict between the need for nanoscale resolution and its inverse relationship with thickness after conventional tomographic reconstruction. To tackle the problem, we have developed a robust method to calculate the ACF of the 3D mass-density distribution without tomography. Assuming the biological mass distribution is isotropic, our method allows for accurate statistical characterization of the 3D mass-density distribution by ACF with two data sets: a single projection image by scanning transmission electron microscopy and a thickness map by atomic force microscopy. Here we present validation of the ACF reconstruction algorithm, as well as its application to calculate the statistics of the 3D distribution of mass-density in a region containing the nucleus of an entire mammalian cell. This method may provide important insights into architectural changes that accompany cellular processes.

Multiple Ewing Sarcoma/Primitive Neuroectodermal Tumors in the Mediastinum: A Case Report and Literature Review.

PubMed

Bae, Sung Hwan; Hwang, Jung Hwa; Da Nam, Bo; Kim, Hyun Jo; Kim, Ki-Up; Kim, Dong Won; Choi, In Ho

2016-02-01

Ewing sarcoma/primitive neuroectodermal tumors (ES/PNET) are high-grade malignant neoplasms. These malignancies present very rare tumors of thoracopulmonary area and even rarer in the mediastinum. In our knowledge, ES/PNET presented with multiple mediastinal masses has not been reported previously. We experienced a case of a 42-year-old man presented with gradual onset of left-side pleuritic chest pain. A contrast-enhanced chest computed tomography (CT) scan showed separate 2 large heterogeneously enhancing masses in each anterior and middle mediastinum of the left hemithorax. Positron emission tomography-computed tomography (PET-CT) scan revealed high fluorodeoxyglucose (FDG) uptake in the mediastinal masses. After surgical excision for the mediastinal masses, both of the masses were diagnosed as the ES/PNET group of tumors on the histopathologic examination. The patient refused postoperative adjuvant chemotherapy and came back with local tumor recurrence and distant metastasis on 4-month follow-up after surgical resection. We report this uncommon form of ES/PNET. We are to raise awareness that this rare malignancy should be considered as a differential diagnosis of the malignant mediastinal tumors and which can be manifested as multiple masses in a patient. Understanding this rare entity of extra-skeletal ES/PNET and characteristic imaging findings can help radiologists and clinicians to approach proper diagnosis and better management for this highly malignant tumor.

Multiple Ewing Sarcoma/Primitive Neuroectodermal Tumors in the Mediastinum

PubMed Central

Bae, Sung Hwan; Hwang, Jung Hwa; Da Nam, Bo; Kim, Hyun Jo; Kim, Ki-Up; Kim, Dong Won; Choi, In Ho

2016-01-01

Abstract Ewing sarcoma/primitive neuroectodermal tumors (ES/PNET) are high-grade malignant neoplasms. These malignancies present very rare tumors of thoracopulmonary area and even rarer in the mediastinum. In our knowledge, ES/PNET presented with multiple mediastinal masses has not been reported previously. We experienced a case of a 42-year-old man presented with gradual onset of left-side pleuritic chest pain. A contrast-enhanced chest computed tomography (CT) scan showed separate 2 large heterogeneously enhancing masses in each anterior and middle mediastinum of the left hemithorax. Positron emission tomography-computed tomography (PET-CT) scan revealed high fluorodeoxyglucose (FDG) uptake in the mediastinal masses. After surgical excision for the mediastinal masses, both of the masses were diagnosed as the ES/PNET group of tumors on the histopathologic examination. The patient refused postoperative adjuvant chemotherapy and came back with local tumor recurrence and distant metastasis on 4-month follow-up after surgical resection. We report this uncommon form of ES/PNET. We are to raise awareness that this rare malignancy should be considered as a differential diagnosis of the malignant mediastinal tumors and which can be manifested as multiple masses in a patient. Understanding this rare entity of extra-skeletal ES/PNET and characteristic imaging findings can help radiologists and clinicians to approach proper diagnosis and better management for this highly malignant tumor. PMID:26886614

A high-resolution full-field range imaging system

NASA Astrophysics Data System (ADS)

Carnegie, D. A.; Cree, M. J.; Dorrington, A. A.

2005-08-01

There exist a number of applications where the range to all objects in a field of view needs to be obtained. Specific examples include obstacle avoidance for autonomous mobile robots, process automation in assembly factories, surface profiling for shape analysis, and surveying. Ranging systems can be typically characterized as being either laser scanning systems where a laser point is sequentially scanned over a scene or a full-field acquisition where the range to every point in the image is simultaneously obtained. The former offers advantages in terms of range resolution, while the latter tend to be faster and involve no moving parts. We present a system for determining the range to any object within a camera's field of view, at the speed of a full-field system and the range resolution of some point laser scans. Initial results obtained have a centimeter range resolution for a 10 second acquisition time. Modifications to the existing system are discussed that should provide faster results with submillimeter resolution.

Validation of Bedside Ultrasound of Muscle Layer Thickness of the Quadriceps in the Critically Ill Patient (VALIDUM Study).

PubMed

Paris, Michael T; Mourtzakis, Marina; Day, Andrew; Leung, Roger; Watharkar, Snehal; Kozar, Rosemary; Earthman, Carrie; Kuchnia, Adam; Dhaliwal, Rupinder; Moisey, Lesley; Compher, Charlene; Martin, Niels; Nicolo, Michelle; White, Tom; Roosevelt, Hannah; Peterson, Sarah; Heyland, Daren K

2017-02-01

In critically ill patients, muscle atrophy is associated with long-term disability and mortality. Bedside ultrasound may quantify muscle mass, but it has not been validated in the intensive care unit (ICU). Here, we compared ultrasound-based quadriceps muscle layer thickness (QMLT) with precise quantifications of computed tomography (CT)-based muscle cross-sectional area (CSA). Patients ≥18 years old with abdominal CT scans performed for clinical reasons were recruited from 9 ICUs for an ultrasound assessment of the quadriceps. CT scans of the third lumbar vertebra, performed <24 hours before or <72 hours after ICU admission, were analyzed for CSA. Low muscularity was defined as 170 cm 2 for men and 110 cm 2 for women. The ultrasound probe was maximally compressed against the skin and QMLT was measured on 2 sites of each quadriceps <72 hours of the CT scan. Mean CT-derived muscle CSA was 109 ± 25 cm 2 for women and 168 ± 37 cm 2 for men, where 58% of patients exhibited low muscularity; only 2.7% patients were underweight according to body mass index. QMLT was positively correlated with CT CSA ( r = 0.45, P < .001). Based on logistic regression to predict low muscularity, QMLT independently generated a concordance index ( c) of 0.67 ( P < .002), which increased to 0.77 ( P < .001) when age, sex, body mass index, Charlson Comorbidity Index, and admission type (surgical vs medical) were added. Our results suggest that QMLT alone with our current protocol may not accurately identify patients with low muscle mass.

Quantitative thin-layer chromatography/mass spectrometry analysis of caffeine using a surface sampling probe electrospray ionization tandem mass spectrometry system.

PubMed

Ford, Michael J; Deibel, Michael A; Tomkins, Bruce A; Van Berkel, Gary J

2005-07-15

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 mum/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 muL) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by approximately 8% or more) than the literature values.

Development and verification of a novel device for dental intra-oral 3D scanning using chromatic confocal technology

NASA Astrophysics Data System (ADS)

Zint, M.; Stock, K.; Graser, R.; Ertl, T.; Brauer, E.; Heyninck, J.; Vanbiervliet, J.; Dhondt, S.; De Ceuninck, P.; Hibst, R.

2015-03-01

The presented work describes the development and verification of a novel optical, powder-free intra-oral scanner based on chromatic confocal technology combined with a multifocal approach. The proof of concept for a chromatic confocal area scanner for intra-oral scanning is given. Several prototype scanners passed a verification process showing an average accuracy (distance deviation on flat surfaces) of less than 31μm +/- 21μm and a reproducibility of less than 4μm +/- 3μm. Compared to a tactile measurement on a full jaw model fitted with 4mm ceramic spheres the measured average distance deviation between the spheres was 49μm +/- 12μm for scans of up to 8 teeth (3- unit bridge, single Quadrant) and 104μm +/- 82μm for larger scans and full jaws. The average deviation of the measured sphere diameter compared to the tactile measurement was 27μm +/- 14μm. Compared to μCT scans of plaster models equipped with human teeth the average standard deviation on up to 3 units was less than 55μm +/- 49μm whereas the reproducibility of the scans was better than 22μm +/- 10μm.

Military Interoperable Digital Hospital Testbed

DTIC Science & Technology

2012-07-01

Subject outcome measures include blood pressure, waist circumference, weight, body mass index (BMI), body fat, HDL cholesterol, triglycerides , glucose ...master patient index (MPI), 625 duplicate chest x-rays and CT scans of the head between sending and receiving institution (taken within 0-7 days) were... Index (MPI) software. The report included chest x-rays (CPT 71010 and 71020) and CT scans of the head (CPT 70450) for the stated time periods. The

Biological particle analysis by mass spectrometry

NASA Technical Reports Server (NTRS)

Vilker, V. L.; Platz, R. M.

1983-01-01

An instrument that analyzes the chemical composition of biological particles in aerosol or hydrosol form was developed. Efforts were directed toward the acquisition of mass spectra from aerosols of biomolecules and bacteria. The filament ion source was installed on the particle analysis by mass spectrometry system. Modifications of the vacuum system improved the sensitivity of the mass spectrometer. After the modifications were incorporated, detailed mass spectra of simple compounds from the three major classes of biomolecules, proteins, nucleic acids, and carbohydrates were obtained. A method of generating bacterial aerosols was developed. The aerosols generated were collected and examined in the scanning electron microscope to insure that the bacteria delivered to the mass spectrometer were intact and free from debris.

Formation of Copper Sulfide Precipitate in Solid Iron

NASA Astrophysics Data System (ADS)

Urata, Kentaro; Kobayashi, Yoshinao

The growth rate of copper sulfide precipitates has been measured in low carbon steel samples such as Fe-0.3mass%Cu-0.03mass%S-0.1mass%C and Fe-0.1mass%Cu-0.01mass%S- 0.1mass%C. Heat-treatment of the samples was conducted at 1273, 1423 and 1573 K for 100 s - 14.4 ks for precipitation of copper sulfides and then the samples were observed by a scanning electron microscope and a transmission electron microscope to measure the diameter of copper sulfides precipitated in the samples. The growth rate of copper sulfide has been found to be well described by the Ostwald growth model, as follows: R\

Radiation dose calculations for CT scans with tube current modulation using the approach to equilibrium function

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Xinhua; Zhang, Da; Liu, Bob, E-mail: bliu7@mgh.harvard.edu

2014-11-01

Purpose: The approach to equilibrium function has been used previously to calculate the radiation dose to a shift-invariant medium undergoing CT scans with constant tube current [Li, Zhang, and Liu, Med. Phys. 39, 5347–5352 (2012)]. The authors have adapted this method to CT scans with tube current modulation (TCM). Methods: For a scan with variable tube current, the scan range was divided into multiple subscan ranges, each with a nearly constant tube current. Then the dose calculation algorithm presented previously was applied. For a clinical CT scan series that presented tube current per slice, the authors adopted an efficient approachmore » that computed the longitudinal dose distribution for one scan length equal to the slice thickness, which center was at z = 0. The cumulative dose at a specific point was a summation of the contributions from all slices and the overscan. Results: The dose calculations performed for a total of four constant and variable tube current distributions agreed with the published results of Dixon and Boone [Med. Phys. 40, 111920 (14pp.) (2013)]. For an abdomen/pelvis scan of an anthropomorphic phantom (model ATOM 701-B, CIRS, Inc., VA) on a GE Lightspeed Pro 16 scanner with 120 kV, N × T = 20 mm, pitch = 1.375, z axis current modulation (auto mA), and angular current modulation (smart mA), dose measurements were performed using two lines of optically stimulated luminescence dosimeters, one of which was placed near the phantom center and the other on the surface. Dose calculations were performed on the central and peripheral axes of a cylinder containing water, whose cross-sectional mass was about equal to that of the ATOM phantom in its abdominal region, and the results agreed with the measurements within 28.4%. Conclusions: The described method provides an effective approach that takes into account subject size, scan length, and constant or variable tube current to evaluate CT dose to a shift-invariant medium. For a clinical CT scan, dose calculations may be performed with a water-containing cylinder whose cross-sectional mass is equal to that of the subject. This method has the potential to substantially improve evaluations of patient dose from clinical CT scans, compared to CTDI{sub vol}, size-specific dose estimate (SSDE), or the dose evaluated for a TCM scan with a constant tube current equal to the average tube current of the TCM scan.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Yuanyuan; Browning, Nigel D.

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelasticmore » scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. We demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Yuanyuan; Browning, Nigel D.

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelasticmore » scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. Furthermore, we demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.« less

Aerogel Track Morphology: Measurement, Three Dimensional Reconstruction and Particle Location using Confocal Laser Scanning Microscopy

NASA Technical Reports Server (NTRS)

Kearsley, A. T.; Ball, A. D.; Wozniakiewicz, P. A.; Graham, G. A.; Burchell, M. J.; Cole, M. J.; Horz, F.; See, T. H.

2007-01-01

The Stardust spacecraft returned the first undoubted samples of cometary dust, with many grains embedded in the silica aerogel collector . Although many tracks contain one or more large terminal particles of a wide range of mineral compositions , there is also abundant material along the track walls. To help interpret the full particle size, structure and mass, both experimental simulation of impact by shots and numerical modeling of the impact process have been attempted. However, all approaches require accurate and precise measurement of impact track size parameters such as length, width and volume of specific portions. To make such measurements is not easy, especially if extensive aerogel fracturing and discoloration has occurred. In this paper we describe the application and limitations of laser confocal imagery for determination of aerogel track parameters, and for the location of particle remains.

Nuclear recoil measurements with the ARIS experiment

NASA Astrophysics Data System (ADS)

Fan, Alden; ARIS Collaboration

2017-01-01

As direct dark matter searches become increasingly sensitive, it is important to fully characterize the target of the search. The goal of the Argon Recoil Ionization and Scintillation (ARIS) experiment is to quantify information related to the scintillation and ionization energy scale, quenching factor, ion recombination probability, and scintillation time response of nuclear recoils, as expected from WIMPs, in liquid argon. A time projection chamber with an active mass of 0.5 kg of liquid argon and capable of full 3D position reconstruction was exposed to an inverse kinematic neutron beam at the Institut de Physique Nucleaire d'Orsay in France. A scan of nuclear recoil energies was performed through coincidence with a set of neutron detectors to quantify properties of nuclear recoils in liquid argon at various electric fields. The difference in ionization and scintillation response with differing recoil track angle to the electric field was also studied. The preliminary results of the experiment will be presented.

High energy density supercapacitors from lignin derived submicron activated carbon fibers in aqueous electrolytes

NASA Astrophysics Data System (ADS)

Hu, Sixiao; Zhang, Sanliang; Pan, Ning; Hsieh, You-Lo

2014-12-01

Highly porous submicron activated carbon fibers (ACFs) were robustly generated from low sulfonated alkali lignin and fabricated into supercapacitors for capacitive energy storage. The hydrophilic and high specific surface ACFs exhibited large-size nanographites and good electrical conductivity to demonstrate outstanding electrochemical performance. ACFs from KOH activation, in particular, showed very high 344 F g-1 specific capacitance at low 1.8 mg cm-2 mass loading and 10 mV s-1 scan rate in aqueous electrolytes. Even at relatively high scan rate of 50 mV s-1 and mass loading of 10 mg cm-2, a decent specific capacitance of 196 F g-1 and a remarkable areal capacitance of 0.55 F cm-2 was obtained, leading to high energy density of 8.1 Wh kg-1 based on averaged electrodes mass. Furthermore, over 96% capacitance retention rates were achieved after 5000 charge/discharge cycles. Such excellent performance demonstrated great potential of lignin derived carbons for electrical energy storage.

Microstructure characterization of a food-grade U-type microemulsion system by differential scanning calorimetry and electrical conductivity techniques.

PubMed

Zhang, Hui; Taxipalati, Maierhaba; Que, Fei; Feng, Fengqin

2013-12-01

The microstructure transitions of a food-grade U-type microemulsion system containing glycerol monolaurate and propionic acid at a 1:1 mass ratio as oil phase and Tween 80 as surfactant were investigated along a water dilution line at a ratio of 80:20 mass% surfactant/oil phase, based on a previously studied phase diagram. From the water thermal behaviours detected by differential scanning calorimetry, three structural regions are identified along the dilution line. In the first region, all water molecules are confined to the water core of the reverse micelles, leading to the formation of w/o microemulsion. As the water content increases, the water gains mobility, transforms into bicontinuous in the second region, and finally the microemulsion become o/w in the third region. The thermal transition points coincide with the structural phase transitions by electrical conductivity measurements, indicating that the structural transitions occur at 35 and 65 mass% of water along the dilution line. Copyright © 2013 Elsevier Ltd. All rights reserved.

Pulmonary suture abscess with false-positive 18F-fluorodeoxyglucose positron emission scan mimicking lung cancer recurrence.

PubMed

Iwasaki, Teruo; Nakagawa, Katsuhiro; Katsura, Hiroshi; Nakane, Shigeru; Kawahara, Kunimitsu; Fukuda, Haruyuki

2006-08-01

We present the case of a 57-year-old woman with pulmonary suture abscess. She had undergone right S3 segmentectomy for early lung adenocarcinoma 7 years before and right breast-conserving surgery for invasive ductal carcinoma 5 months previously, followed by irradiation plus endocrine therapy. Chest radiography and computed tomography revealed an irregular mass (3.5 cm in diameter) between the residual S1 segment and the middle lobe, neighboring the staple line of the segmentectomy. 18F-fluorodeoxyglucose uptake into the mass increased, seen by positron emission scans. Therefore, we could not rule out the possibility of local recurrence of lung cancer and resected it. Pathologically and microbiologically, the mass was a suture abscess arising around the nylon suture of the previous segmentectomy. This lesion was the result of a foreign-body reaction, as confirmed by polarized microscopy. Moreover, titanium staples at the segmentectomy and breast-conserving surgery may also have contributed to this condition.

Measurement of effective detective quantum efficiency for a photon counting scanning mammography system and comparison with two flat panel full-field digital mammography systems

NASA Astrophysics Data System (ADS)

Wood, Tim J.; Moore, Craig S.; Saunderson, John R.; Beavis, Andrew W.

2018-01-01

Effective detective quantum efficiency (eDQE) describes the resolution and noise properties of an imaging system along with scatter and primary transmission, all measured under clinically appropriate conditions. Effective dose efficiency (eDE) is the eDQE normalised to mean glandular dose and has been proposed as a useful metric for the optimisation of clinical imaging systems. The aim of this study was to develop a methodology for measuring eDQE and eDE on a Philips microdose mammography (MDM) L30 photon counting scanning system, and to compare performance with two conventional flat panel systems. A custom made lead-blocker was manufactured to enable the accurate determination of dose measurements, and modulation transfer functions were determined free-in-air at heights of 2, 4 and 6 cm above the breast support platform. eDQE were calculated for a Philips MDM L30, Hologic Dimensions and Siemens Inspiration digital mammography system for 2, 4 and 6 cm thick poly(methyl methacrylate) (PMMA). The beam qualities (target/filter and kilovoltage) assessed were those selected by the automatic exposure control, and anti-scatter grids were used where available. Measurements of eDQE demonstrate significant differences in performance between the slit- and scan-directions for the photon counting imaging system. MTF has been shown to be the limiting factor in the scan-direction, which results in a rapid fall in eDQE at mid-to-high spatial frequencies. A comparison with two flat panel mammography systems demonstrates that this may limit image quality for small details, such as micro-calcifications, which correlates with a more conventional image quality assessment with the CDMAM phantom. eDE has shown the scanning photon counting system offers superior performance for low spatial frequencies, which will be important for the detection of large low contrast masses. Both eDQE and eDE are proposed as useful metrics that should enable optimisation of the Philips MDM L30.

Retinal Parameters as Compared with Head Circumference, Height, Weight, and Body Mass Index in Children in Kenya and Bhutan.

PubMed

Grundy, Sara J; Tshering, Lhab; Wanjala, Stanley W; Diamond, Megan B; Audi, Martin S; Prasad, Sashank; Shinohara, Russell T; Rogo, Debora; Wangmo, Dechen; Wangdi, Ugyen; Aarayang, Abi; Tshering, Thukten; Burke, Thomas F; Mateen, Farrah J

2018-06-11

The retina shares embryological derivation with the brain and may provide a new measurement of overall growth status, especially useful in resource-limited settings. Optical coherence tomography (OCT) provides detailed quantification of retinal structures. We enrolled community-dwelling children ages 3-11 years old in Siaya, Kenya and Thimphu, Bhutan in 2016. We measured head circumference (age < 5 years only), height, and weight, and standardized these by age and gender. Research staff performed OCT ( iScan ; Optovue, Inc., Fremont, CA), measuring the peripapillary retinal nerve fiber layer (RNFL) and macular ganglion cell complex (GCC) thicknesses. A neuro-ophthalmologist performed quality control for centration, motion artifact, and algorithm-derived quality scores. Generalized estimating equations were used to determine the relationship between anthropometric and retinal measurements. Two hundred and fifty-eight children (139 females, average age 6.4 years) successfully completed at least one retinal scan, totaling 1,048 scans. Nine hundred and twenty-two scans (88.0%) were deemed usable. Fifty-three of the 258 children (20.5%) were able to complete all six scans. Kenyan children had a thinner average GCC ( P < 0.001) than Bhutanese children after adjustment for age and gender, but not RNFL ( P = 0.70). In models adjusting for age, gender, and study location, none of standardized height, weight, and body mass index (BMI) were statistically significantly associated with RNFL or GCC. We determined that OCT is feasible in some children in resource-limited settings, particularly those > 4 years old, using the iScan device. We found no evidence for GCC or RNFL as a proxy for height-, weight-, or BMI-for-age. The variation in mean GCC thickness in Asian versus African children warrants further investigation.

Method of mechanical holding of cantilever chip for tip-scan high-speed atomic force microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fukuda, Shingo; Uchihashi, Takayuki; Ando, Toshio

In tip-scan atomic force microscopy (AFM) that scans a cantilever chip in the three dimensions, the chip body is held on the Z-scanner with a holder. However, this holding is not easy for high-speed (HS) AFM because the holder that should have a small mass has to be able to clamp the cantilever chip firmly without deteriorating the Z-scanner’s fast performance, and because repeated exchange of cantilever chips should not damage the Z-scanner. This is one of the reasons that tip-scan HS-AFM has not been established, despite its advantages over sample stage-scan HS-AFM. Here, we present a novel method ofmore » cantilever chip holding which meets all conditions required for tip-scan HS-AFM. The superior performance of this novel chip holding mechanism is demonstrated by imaging of the α{sub 3}β{sub 3} subcomplex of F{sub 1}-ATPase in dynamic action at ∼7 frames/s.« less

Copernicus ultraviolet spectra of OB supergiants with strong stellar winds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hutchings, J.B.

1976-03-01

Spectral scans at approximately 0.2 A resolution have been obtained in the far-ultraviolet of eight stars which have high mass-loss rates from stellar winds. The P Cygni characteristics of the line profiles appear to vary inversely as the mass flow rate, and in P Cygni itself the C III lambda 1175 line shows no velocity shift, or emission. It is suggested that higher mass flow rates occur through a denser, slower moving envelope in which collisional interactions are important. (auth)

Multiclass screening of >200 pharmaceutical and other residues in aquatic foods by ultrahigh-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry.

PubMed

Kong, Cong; Wang, Yang; Huang, Yuanfei; Yu, Huijuan

2018-05-11

A quick screening method of more than 200 pharmaceutical and other residues in aquatic foods based on ultrahigh-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry (UHPLC-Q/Orbitrap MS) was established. In this method, after the addition of 200 μL of 1 M EDTA-Na 2 , 2 g of each sample homogenate was extracted successively with 10 mL of acetonitrile and 10 mL of ethyl acetate. The extracts were combined, dried under nitrogen flow, and redissolved in 0.1% formic acid in acetonitrile/water (4:6, v/v) for analysis. The prepared samples were analyzed by UHPLC- Q/Orbitrap MS system in Full MS/ddMS 2 (full-scan data-dependent MS/MS) mode. Compound identification was performed through comparison of the sample data with the database for standard chemicals, including the retention time, precursor ion, product ions, and isotope pattern for all 206 compounds. Five different aquatic food matrices (carp, shrimp, crab, eel, and mussel) spiked with the analytes at 1, 10, and 50 ng/g were evaluated to assess recoveries, precision, matrix effects, stability, and detection limits using the method. UHPLC analyses required 25 min, and 178-200 analytes met identification criteria at 50 ng/g depending on the matrix. Furthermore, practical application of this method for real samples displayed strong screening capability. Graphical abstract A quick screening method of >200 pharmaceutical and other residues in aquatic foods based on ultrahighperformance liquid chromatography-quadrupole-Orbitrap mass spectrometer was established. Fivedifferent aquatic food matrices, including carp, shrimp, crab, eel and mussel, were studied to evaluatescreen limit at 1, 10 and 50 μg·kg-1 level. Results suggest the high reliability, high time-efficiency and goodsimplicity of the method.

A disappearing left-sided neck mass.

PubMed

Lutwak, Nancy; Dill, Curt

2012-07-04

The patient was a 48-year-old man who presented to the emergency department with complaints of a left-sided painful neck mass, which changed in size relative to ingestion of meals. He denied voice change, fever, chills, weight loss, dysphagia and hoarseness. Physical examination was unremarkable. CT scan demonstrated a 3.9 mm calculus of the submandibular gland duct. Therapeutic sialendocopy was successfully performed.

An evaluation: The potential of discarded tires as a source of fuel

NASA Technical Reports Server (NTRS)

Collins, L. W.; Downs, W. R.; Gibson, E. K.; Moore, G. W.

1974-01-01

The destructive distillation of rubber tire samples was studied by thermogravimetry, differential scanning calorimetry, combustion calorimetry, and mass spectroscopy. The decomposition reaction was found to be exothermic and produced a mass loss of 65 percent. The gas evolution curves that were obtained indicate that a variety of organic materials are evolved simultaneously during the decomposition of the rubber polymer.

Cellular Angiofibroma Presenting as an Inguinal Subcutaneous Mass: a Case Report and Review of the Literature.

PubMed

Schiebel, Frank; Cassim, R

2016-01-01

Cellular angiofibroma is a rare benign mesenchymal tumor that occurs in the inguinal and vulvovaginal region. We report a case of the tumor occurring in the right inguinal region of a 64 old male and a review of the current literature. A 64 year old male veteran was referred to our general surgery service with an incidentally discovered right inguinal mass on a computerized tomography scan. The scan was performed to follow a history of prostate cancer that had been treated with brachytherapy. Magnetic resonance imaging of the lesion helped confirm that the mass did not represent a hernia or an undescended testicle. Surgical resection revealed encapsulated, yellowish, pink tissue measuring 6.5 x 5 x 3.5 cm. Microscopically, the sections showed densely fibrous to loose and focally fibromyxoid background of oval to spindle-shaped cells with a few scattered plasma cells and mast cells. Based upon the clinical, histologic, and immunohistochemical findings, the lesion was classified as a cellular angiofibroma. Cellular angiofibroma of the inguinal region is a rare benign encapsulated tumor.It should be considered in the differential diagnosis of a male with an inguinal mass proven not to be a hernia or undescended testicle.

Surface area-volume ratios in insects.

PubMed

Kühsel, Sara; Brückner, Adrian; Schmelzle, Sebastian; Heethoff, Michael; Blüthgen, Nico

2017-10-01

Body mass, volume and surface area are important for many aspects of the physiology and performance of species. Whereas body mass scaling received a lot of attention in the literature, surface areas of animals have not been measured explicitly in this context. We quantified surface area-volume (SA/V) ratios for the first time using 3D surface models based on a structured light scanning method for 126 species of pollinating insects from 4 orders (Diptera, Hymenoptera, Lepidoptera, and Coleoptera). Water loss of 67 species was measured gravimetrically at very dry conditions for 2 h at 15 and 30 °C to demonstrate the applicability of the new 3D surface measurements and relevance for predicting the performance of insects. Quantified SA/V ratios significantly explained the variation in water loss across species, both directly or after accounting for isometric scaling (residuals of the SA/V ∼ mass 2/3 relationship). Small insects with a proportionally larger surface area had the highest water loss rates. Surface scans of insects to quantify allometric SA/V ratios thus provide a promising method to predict physiological responses, improving the potential of body mass isometry alone that assume geometric similarity. © 2016 Institute of Zoology, Chinese Academy of Sciences.

Construction and characterization of the detection modules for the Muon Portal Project

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blancato, A.A.; Bonanno, D.L.; La Rocca, P.

The Muon Portal Project is a joint initiative between research and industrial partners, aimed at the construction of a real size detector prototype (6 x 3 x 7 m{sup 3}) for the inspection of containers by the muon scattering technique, devised to search for hidden high-Z fissile materials and provide a full 3D tomography of the interior of the container in a scanning time of the order of minutes. The muon tracking detector is based on a set of 48 detection modules (size 1 m x 3 m), each built with 100 extruded scintillator strips, so as to provide fourmore » X-Y detection planes, two placed above and two below the container to be inspected. Two wavelength shifting (WLS) fibres embedded in each strip convey the emitted photons to Silicon Photomultipliers (SiPM) which act as photo-sensors. After a research and development phase, which led to the choice and test of the individual components, the construction of the full size detector has already started. The paper describes the results of the mass characterization of the photo-sensors and the construction and test measurements of the first detection modules of the Project. (authors)« less

The application of high-resolution mass spectrometry-based data-mining tools in tandem to metabolite profiling of a triple drug combination in humans.

PubMed

Xing, Jie; Zang, Meitong; Zhang, Haiying; Zhu, Mingshe

2015-10-15

Patients are usually exposed to multiple drugs, and metabolite profiling of each drug in complex biological matrices is a big challenge. This study presented a new application of an improved high resolution mass spectrometry (HRMS)-based data-mining tools in tandem to fast and comprehensive metabolite identification of combination drugs in human. The model drug combination was metronidazole-pantoprazole-clarithromycin (MET-PAN-CLAR), which is widely used in clinic to treat ulcers caused by Helicobacter pylori. First, mass defect filter (MDF), as a targeted data processing tool, was able to recover all relevant metabolites of MET-PAN-CLAR in human plasma and urine from the full-scan MS dataset when appropriate MDF templates for each drug were defined. Second, the accurate mass-based background subtraction (BS), as an untargeted data-mining tool, worked effectively except for several trace metabolites, which were buried in the remaining background signals. Third, an integrated strategy, i.e., untargeted BS followed by improved MDF, was effective for metabolite identification of MET-PAN-CLAR. Most metabolites except for trace ones were found in the first step of BS-processed datasets, and the results led to the setup of appropriate metabolite MDF template for the subsequent MDF data processing. Trace metabolites were further recovered by MDF, which used both common MDF templates and the novel metabolite-based MDF templates. As a result, a total of 44 metabolites or related components were found for MET-PAN-CLAR in human plasma and urine using the integrated strategy. New metabolic pathways such as N-glucuronidation of PAN and dehydrogenation of CLAR were found. This study demonstrated that the combination of accurate mass-based multiple data-mining techniques in tandem, i.e., untargeted background subtraction followed by targeted mass defect filtering, can be a valuable tool for rapid metabolite profiling of combination drugs in vivo. Copyright © 2015 Elsevier B.V. All rights reserved.

Targeted screening of pesticides, veterinary drugs and mycotoxins in bakery ingredients and food commodities by liquid chromatography-high-resolution single-stage Orbitrap mass spectrometry.

PubMed

De Dominicis, Emiliano; Commissati, Italo; Suman, Michele

2012-09-01

In the food industry, it is frequently necessary to check the quality of an ingredient to decide whether to use it in production and/or to have an idea of the final possible contamination of the finished product. The current need to quickly separate and identify relevant contaminants within different classes, often with legal residue limits on the order of 1-100 µg kg(-1), has led to the need for more effective analytical methods. With thousands of organic compounds present in complex food matrices, the development of new analytical solutions leaned towards simplified extraction/clean-up procedures and chromatography coupled with mass spectrometry. Efforts must also be made regarding the instrumental phase to overcome sensitivity/selectivity limits and interferences. For this purpose, high-resolution full scan analysis in mass spectrometry is an interesting alternative to the traditional tandem mass approach. A fast method for extracting and purifying bakery matrices was therefore developed and combined with the exploitation of ultra-high-pressure liquid chromatography (UHPLC) coupled to a Orbitrap Exactive™ high-resolution mass spectrometer (HRMS). Extracts of blank, naturally contaminated and fortified minicakes, prepared through a combined use of industrial and pilot plant production lines, were analyzed at different concentration levels (1-100 µg kg(-1)) of various contaminants: a limit of detection at 10 µg kg(-1) was possible for most of the analytes within all the categories analyzed, including pesticides, aflatoxins, trichothecene toxins and veterinary drugs. The application of accurate mass targeted screening described in this article demonstrates that current single-stage HRMS analytical instrumentation is well equipped to meet the challenges posed by chemical contaminants in the screening of both bakery raw materials and finished products. Copyright © 2012 John Wiley & Sons, Ltd.

Negative chemical ionization gas chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry and automated accurate mass data processing for determination of pesticides in fruit and vegetables.

PubMed

Besil, Natalia; Uclés, Samanta; Mezcúa, Milagros; Heinzen, Horacio; Fernández-Alba, Amadeo R

2015-08-01

Gas chromatography coupled to high resolution hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS), operating in negative chemical ionization (NCI) mode and combining full scan with MSMS experiments using accurate mass analysis, has been explored for the automated determination of pesticide residues in fruit and vegetables. Seventy compounds were included in this approach where 50 % of them are not approved by the EU legislation. A global 76 % of the analytes could be identified at 1 μg kg(-1). Recovery studies were developed at three concentration levels (1, 5, and 10 μg kg(-1)). Seventy-seven percent of the detected pesticides at the lowest level yielded recoveries within the 70 %-120 % range, whereas 94 % could be quantified at 5 μg kg(-1), and the 100 % were determined at 10 μg kg(-1). Good repeatability, expressed as relative standard deviation (RSD <20 %), was obtained for all compounds. The main drawback of the method was the limited dynamic range that was observed for some analytes that can be overcome either diluting the sample or lowering the injection volume. A home-made database was developed and applied to an automatic accurate mass data processing. Measured mass accuracies of the generated ions were mainly less than 5 ppm for at least one diagnostic ion. When only one ion was obtained in the single-stage NCI-MS, a representative product ion from MSMS experiments was used as identification criterion. A total of 30 real samples were analyzed and 67 % of the samples were positive for 12 different pesticides in the range 1.0-1321.3 μg kg(-1).

[Deconvolution of overlapped peaks in total ion chromatogram of essential oil from citri reticulatae pericarpium viride by automated mass spectral deconvolution & identification system].

PubMed

Wang, Jian; Chen, Hong-Ping; Liu, You-Ping; Wei, Zheng; Liu, Rong; Fan, Dan-Qing

2013-05-01

This experiment shows how to use the automated mass spectral deconvolution & identification system (AMDIS) to deconvolve the overlapped peaks in the total ion chromatogram (TIC) of volatile oil from Chineses materia medica (CMM). The essential oil was obtained by steam distillation. Its TIC was gotten by GC-MS, and the superimposed peaks in TIC were deconvolved by AMDIS. First, AMDIS can detect the number of components in TIC through the run function. Then, by analyzing the extracted spectrum of corresponding scan point of detected component and the original spectrum of this scan point, and their counterparts' spectra in the referred MS Library, researchers can ascertain the component's structure accurately or deny some compounds, which don't exist in nature. Furthermore, through examining the changeability of characteristic fragment ion peaks of identified compounds, the previous outcome can be affirmed again. The result demonstrated that AMDIS could efficiently deconvolve the overlapped peaks in TIC by taking out the spectrum of matching scan point of discerned component, which led to exact identification of the component's structure.

Unambiguous characterization of gunshot residue particles using scanning laser ablation and inductively coupled plasma-mass spectrometry.

PubMed

Abrego, Zuriñe; Ugarte, Ana; Unceta, Nora; Fernández-Isla, Alberto; Goicolea, M Aranzazu; Barrio, Ramón J

2012-03-06

A new method based on scanning laser ablation and inductively coupled plasma-mass spectrometry (LA-ICPMS) for the detection and identification of gunshot residue (GSR) particles from firearms discharges has been developed. Tape lifts were used to collect inorganic residues from skin surfaces. The laser ablation pattern and ICPMS conditions were optimized for the detection of metals present in GSR, such as (121)Sb, (137)Ba, and (208)Pb. Other isotopes ((27)Al, (29)Si, (31)P, (33)S, (35)Cl, (39)K, (44)Ca, (57)Fe, (60)Ni, (63)Cu, (66)Zn, and (118)Sn) were monitored during the ICPMS analyses to obtain additional information to possibly classify the GSR particles as either characteristic of GSR or consistent with GSR. In experiments with real samples, different firearms, calibers, and ammunitions were used. The performed method evaluation confirms that the developed methodology can be used as an alternative to the standard scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) technique, with the significant advantage of drastically reducing the analysis time to less than 66 min.

Differential scanning calorimetry of coal

NASA Technical Reports Server (NTRS)

Gold, P. I.

1978-01-01

Differential scanning calorimetry studies performed during the first year of this project demonstrated the occurrence of exothermic reactions associated with the production of volatile matter in or near the plastic region. The temperature and magnitude of the exothermic peak were observed to be strongly affected by the heating rate, sample mass and, to a lesser extent, by sample particle size. Thermal properties also were found to be influenced by oxidation of the coal sample due to weathering effects.

Empty calories and phantom fullness: a randomized trial studying the relative effects of energy density and viscosity on gastric emptying determined by MRI and satiety.

PubMed

Camps, Guido; Mars, Monica; de Graaf, Cees; Smeets, Paul Am

2016-07-01

Stomach fullness is a determinant of satiety. Although both the viscosity and energy content have been shown to delay gastric emptying, their relative importance is not well understood. We compared the relative effects of and interactions between the viscosity and energy density on gastric emptying and perceived satiety. A total of 15 healthy men [mean ± SD age: 22.6 ± 2.4 y; body mass index (in kg/m(2)): 22.6 ± 1.8] participated in an experiment with a randomized 2 × 2 crossover design. Participants received dairy-based shakes (500 mL; 50% carbohydrate, 20% protein, and 30% fat) that differed in viscosity (thin and thick) and energy density [100 kcal (corresponding to 0.2 kcal/mL) compared with 500 kcal (corresponding to 1 kcal/mL)]. After ingestion, participants entered an MRI scanner where abdominal scans and oral appetite ratings on a 100-point scale were obtained every 10 min until 90 min after ingestion. From the scans, gastric content volumes were determined. Overall, the gastric emptying half-time (GE t50) was 54.7 ± 3.8 min. The thin 100-kcal shake had the lowest GE t50 of 26.5 ± 3.0 min, followed by the thick 100-kcal shake with a GE t50 of 41 ± 3.9 min and the thin 500-kcal shake with a GE t50 of 69.5 ± 5.9 min, and the thick 500-kcal shake had the highest GE t50 of 81.9 ± 8.3 min. With respect to appetite, the thick 100-kcal shake led to higher fullness (58 points at 40 min) than the thin 500-kcal shake (48 points at 40 min). Our results show that increasing the viscosity is less effective than increasing the energy density in slowing gastric emptying. However, the viscosity is more important to increase the perceived fullness. These results underscore the lack of the satiating efficiency of empty calories in quickly ingested drinks such as sodas. The increase in perceived fullness that is due solely to the increased viscosity, which is a phenomenon that we refer to as phantom fullness, may be useful in lowering energy intake. This trial was registered at www.trialregister.nl as NTR4573. © 2016 American Society for Nutrition.

A new apparatus for electron tomography in the scanning electron microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morandi, V., E-mail: morandi@bo.imm.cnr.it; Maccagnani, P.; Masini, L.

2015-06-23

The three-dimensional reconstruction of a microscopic specimen has been obtained by applying the tomographic algorithm to a set of images acquired in a Scanning Electron Microscope. This result was achieved starting from a series of projections obtained by stepwise rotating the sample under the beam raster. The Scanning Electron Microscope was operated in the scanning-transmission imaging mode, where the intensity of the transmitted electron beam is a monotonic function of the local mass-density and thickness of the specimen. The detection strategy has been implemented and tailored in order to maintain the projection requirement over the large tilt range, as requiredmore » by the tomographic workflow. A Si-based electron detector and an eucentric-rotation specimen holder have been specifically developed for the purpose.« less

Sensitive quantification of apomorphine in human plasma using a LC-ESI-MS-MS method.

PubMed

Abe, Emuri; Alvarez, Jean-Claude

2006-06-01

An analytical method based on liquid chromatography coupled with ion trap mass spectrometry (MS) detection with electrospray ionization interface has been developed for the identification and quantification of apomorphine in human plasma. Apomorphine was isolated from 0.5 mL of plasma using a liquid-liquid extraction with diethyl ether and boldine as internal standard, with satisfactory extraction recoveries. Analytes were separated on a 5-microm C18 Highpurity (Thermohypersil) column (150 mm x 2.1 mm I.D.) maintained at 30 degrees C, coupled to a precolumn (C18, 5-microm, 10 mm x 2.0 mm I.D., Thermo). The elution was achieved isocratically with a mobile phase of 2 mM NH4COOH buffer pH 3.8/acetonitrile (50/50, vol/vol) at a flow rate of 200 microL per minute. Data were collected either in full-scan MS mode at m/z 150 to 500 or in full-scan tandem mass spectrometry mode, selecting the [M+H]ion at m/z 268.0 for apomorphine and m/z 328.0 for boldine. The most intense daughter ion of apomorphine (m/z 237.1) and boldine (m/z 297.0) were used for quantification. Retention times were 2.03 and 2.11 minutes for boldine and apomorphine, respectively. Calibration curves were linear in the 0.025 to 20 ng/mL range. The limits of detection and quantification were 0.010 ng/mL and 0.025 ng/mL, respectively. Accuracy and precision of the assay were measured by analyzing 54 quality control samples for 3 days. At concentrations of 0.075, 1.5, and 15 ng/mL, intraday precisions were less than 10.1%, 5.3%, and 3.8%, and interday precisions were less than 4.8%, 6.6%, and 6.5%, respectively. Accuracies were in the 99.5 to 104.2% range. An example of a patient who was given 6 mg of apomorphine subcutaneously is shown, with concentrations of 14.1 ng/mL after 30 minutes and 0.20 ng/mL after 6 hours. The method described enables the unambiguous identification and quantification of apomorphine with very good sensitivity using only 0.5 mL of sample, and is very convenient for therapeutic drug monitoring and pharmacokinetic studies.

Metabolomic spectral libraries for data-independent SWATH liquid chromatography mass spectrometry acquisition.

PubMed

Bruderer, Tobias; Varesio, Emmanuel; Hidasi, Anita O; Duchoslav, Eva; Burton, Lyle; Bonner, Ron; Hopfgartner, Gérard

2018-03-01

High-quality mass spectral libraries have become crucial in mass spectrometry-based metabolomics. Here, we investigate a workflow to generate accurate mass discrete and composite spectral libraries for metabolite identification and for SWATH mass spectrometry data processing. Discrete collision energy (5-100 eV) accurate mass spectra were collected for 532 metabolites from the human metabolome database (HMDB) by flow injection analysis and compiled into composite spectra over a large collision energy range (e.g., 10-70 eV). Full scan response factors were also calculated. Software tools based on accurate mass and predictive fragmentation were specially developed and found to be essential for construction and quality control of the spectral library. First, elemental compositions constrained by the elemental composition of the precursor ion were calculated for all fragments. Secondly, all possible fragments were generated from the compound structure and were filtered based on their elemental compositions. From the discrete spectra, it was possible to analyze the specific fragment form at each collision energy and it was found that a relatively large collision energy range (10-70 eV) gives informative MS/MS spectra for library searches. From the composite spectra, it was possible to characterize specific neutral losses as radical losses using in silico fragmentation. Radical losses (generating radical cations) were found to be more prominent than expected. From 532 metabolites, 489 provided a signal in positive mode [M+H] + and 483 in negative mode [M-H] - . MS/MS spectra were obtained for 399 compounds in positive mode and for 462 in negative mode; 329 metabolites generated suitable spectra in both modes. Using the spectral library, LC retention time, response factors to analyze data-independent LC-SWATH-MS data allowed the identification of 39 (positive mode) and 72 (negative mode) metabolites in a plasma pool sample (total 92 metabolites) where 81 previously were reported in HMDB to be found in plasma. Graphical abstract Library generation workflow for LC-SWATH MS, using collision energy spread, accurate mass, and fragment annotation.

Estimating the effective radiation dose imparted to patients by intraoperative cone-beam computed tomography in thoracolumbar spinal surgery.

PubMed

Lange, Jeffrey; Karellas, Andrew; Street, John; Eck, Jason C; Lapinsky, Anthony; Connolly, Patrick J; Dipaola, Christian P

2013-03-01

Observational. To estimate the radiation dose imparted to patients during typical thoracolumbar spinal surgical scenarios. Minimally invasive techniques continue to become more common in spine surgery. Computer-assisted navigation systems coupled with intraoperative cone-beam computed tomography (CT) represent one such method used to aid in instrumented spinal procedures. Some studies indicate that cone-beam CT technology delivers a relatively low dose of radiation to patients compared with other x-ray-based imaging modalities. The goal of this study was to estimate the radiation exposure to the patient imparted during typical posterior thoracolumbar instrumented spinal procedures, using intraoperative cone-beam CT and to place these values in the context of standard CT doses. Cone-beam CT scans were obtained using Medtronic O-arm (Medtronic, Minneapolis, MN). Thermoluminescence dosimeters were placed in a linear array on a foam-plastic thoracolumbar spine model centered above the radiation source for O-arm presets of lumbar scans for small or large patients. In-air dosimeter measurements were converted to skin surface measurements, using published conversion factors. Dose-length product was calculated from these values. Effective dose was estimated using published effective dose to dose-length product conversion factors. Calculated dosages for many full-length procedures using the small-patient setting fell within the range of published effective doses of abdominal CT scans (1-31 mSv). Calculated dosages for many full-length procedures using the large-patient setting fell within the range of published effective doses of abdominal CT scans when the number of scans did not exceed 3. We have demonstrated that single cone-beam CT scans and most full-length posterior instrumented spinal procedures using O-arm in standard mode would likely impart a radiation dose within the range of those imparted by a single standard CT scan of the abdomen. Radiation dose increases with patient size, and the radiation dose received by larger patients as a result of more than 3 O-arm scans in standard mode may exceed the dose received during standard CT of the abdomen. Understanding radiation imparted to patients by cone-beam CT is important for assessing risks and benefits of this technology, especially when spinal surgical procedures require multiple intraoperative scans.

Amino Acid Contents of Meteorite Mineral Separates

NASA Astrophysics Data System (ADS)

Berger, E. L.; Burton, A. S.; Locke, D.

2017-07-01

We investigate the relationship between parent body conditions, mineralogy, and amino acid composition, by analyzing meteoric mineral separates using liquid chromatography-mass spectrometry, scanning electron microscopy, and x-ray diffraction.

Osteoid osteoma of the foot: presentation following trauma.

PubMed

Ambrosia, J M; Kernek, C B

1985-05-01

A 15 year old black boy presented with a seven-month history of apparent post traumatic foot pain. Radiologic workup including bone scan, tomograms, and CT scan showed osteoid osteoma, which was treated by surgical excision. This treatment resulted in complete pain relief and return to full activities.

Quantitative Multiclass Pesticide Residue Analysis in Apple, Pear, and Grape by Modified QuEChERS and Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

PubMed

Munaretto, Juliana S; Viera, Mariela de S; Martins, Manoel L; Adaime, Martha B; Zanella, Renato

2016-11-01

Most of the analytical methods currently applied in food control laboratories are focused on the determination of target compounds using LC coupled to tandem MS, which is an effective technique, but low-resolution MS is limited. Thus, a method for determination of pesticide multiresidues in fruits (pear, apple, and grape) using a modified quick, easy, cheap, effective, rugged, and safe method and LC coupled to quadrupole time-of-flight (Q-TOF) MS was developed and validated. The proposed method showed good linearity (r2 > 0.99) from 1 to 100 μg/L. Recoveries for blank samples spiked at 0.01, 0.04, and 0.10 mg/kg were between 66 and 122%, with RSDs <28%. Respective LOQs for apple, pear, and grape matrixes were 0.01 mg/kg for 112, 120, and 118 compounds, and 0.04 mg/kg for 22, 12, and 17 compounds, and average mass accuracy error was 3.2 ppm. LC with Q-TOF MS detection using protonated molecular ion and/or adducts and mass accuracy provided reliability for the method. The proposed method is effective for pesticide residue determination in apple, pear, and grape samples, proving that high-resolution MS using full scan mode can be a powerful and reliable technique for quantification purposes, being adequate for application in the surveillance of maximum residue limits set by different legislations.

Extract-filter-shoot liquid chromatography with mass spectrometry for the analysis of vitamin D2 in a powdered supplement capsule and standard reference material 3280.

PubMed

Byrdwell, William Craig

2014-08-01

An "extract-filter-shoot" method for the analysis of vitamin D2, ergocalciferol, in a dry powdered dietary supplement capsule containing rice flour excipient and in a National Institute of Standards and Technology standard reference material 3280 is reported. Quantification of vitamin D2 was done by atmospheric pressure chemical ionization mass spectrometry using selected ion monitoring, two transitions of selected reaction monitoring, and extracted ion chromatograms from full scans. UV detection was used for the quantification of Vitamin D2 in the dry powder capsule, whereas interfering species rendered UV detection unreliable for standard reference material 3280. Average values for standard reference material 3280 ranged from 8.27 ± 0.58 to 8.33 ± 0.57 μg/g using internal standard calibration and response factor approaches, compared to the previous National Institute of Standards and Technology internal value for vitamin D2 of 8.78 ± 0.11 μg/g, and the recently updated reference value of 8.6 ± 2.6 μg/g. The powdered supplement capsule was found to contain 28.19 ± 0.35 to 28.67 ± 0.90 μg/capsule for a capsule labeled to contain 25.00 μg. The triacylglycerol composition of the rice flour excipient in the powdered supplement capsule determined by atmospheric pressure chemical ionization mass spectrometry is also reported. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Terrestrial Laser Scanning for Coastal Geomorphologic Research in Western Greece

NASA Astrophysics Data System (ADS)

Hoffmeister, D.; Tilly, N.; Curdt, C.; Aasen, H.; Ntageretzis, K.; Hadler, H.; Willershäuser, T.; Vött, A.; Bareth, G.

2012-07-01

We used terrestrial laser scanning (TLS) for (i) accurate volume estimations of dislocated boulders moved by high-energy impacts and for (ii) monitoring of annual coastal changes. In this contribution, we present three selected sites in Western Greece that were surveyed during a time span of four years (2008-2011). The Riegl LMS-Z420i laser scanner was used in combination with a precise DGPS system (Topcon HiPer Pro). Each scan position and a further target were recorded for georeferencing and merging of the point clouds. For the annual detection of changes, reference points for the base station of the DGPS system were marked. Our studies show that TLS is capable to accurately estimate volumes of boulders, which were dislocated and deposited inland from the littoral zone. The mass of each boulder was calculated from this 3D-reconstructed volume and according density data. The masses turned out to be considerably smaller than common estimated masses based on tape-measurements and according density approximations. The accurate mass data was incorporated into wave transport equations, which estimate wave velocities of high-energy impacts. As expected, these show smaller wave velocities, due to the incorporated smaller mass. Furthermore, TLS is capable to monitor annual changes on coastal areas. The changes are detected by comparing high resolution digital elevation models from every year. On a beach site, larger areas of sea-weed and sandy sediments are eroded. In contrast, bigger gravel with 30-50 cm diameter was accumulated. At the other area with bigger boulders and a different coastal configuration only slightly differences were detectable. In low-lying coastal areas and along recent beaches, post-processing of point clouds turned out to be more difficult, due to noise effects by water and shadowing effects. However, our studies show that the application of TLS in different littoral settings is an appropriate and promising tool. The combination of both instruments worked well and the annual positioning procedure with own survey point is precose for this purpose.

Reproducibility of lung tumor position and reduction of lung mass within the planning target volume using active breathing control (ABC).

PubMed

Cheung, Patrick C F; Sixel, Katharina E; Tirona, Romeo; Ung, Yee C

2003-12-01

The active breathing control (ABC) device allows for temporary immobilization of respiratory motion by implementing a breath hold at a predefined relative lung volume and air flow direction. The purpose of this study was to quantitatively evaluate the ability of the ABC device to immobilize peripheral lung tumors at a reproducible position, increase total lung volume, and thereby reduce lung mass within the planning target volume (PTV). Ten patients with peripheral non-small-cell lung cancer tumors undergoing radiotherapy had CT scans of their thorax with and without ABC inspiration breath hold during the first 5 days of treatment. Total lung volumes were determined from the CT data sets. Each peripheral lung tumor was contoured by one physician on all CT scans to generate gross tumor volumes (GTVs). The lung density and mass contained within a 1.5-cm PTV margin around each peripheral tumor was calculated using CT numbers. Using the center of the GTV from the Day 1 ABC scan as the reference, the displacement of subsequent GTV centers on Days 2 to 5 for each patient with ABC applied was calculated in three dimensions. With the use of ABC inspiration breath hold, total lung volumes increased by an average of 42%. This resulted in an average decrease in lung mass of 18% within a standard 1.5-cm PTV margin around the GTV. The average (+/- standard deviation) displacement of GTV centers with ABC breath hold applied was 0.3 mm (+/- 1.8 mm), 1.2 mm (+/- 2.3 mm), and 1.1 mm (+/- 3.5 mm) in the lateral direction, anterior-posterior direction, and superior-inferior direction, respectively. Results from this study indicate that there remains some inter-breath hold variability in peripheral lung tumor position with the use of ABC inspiration breath hold, which prevents significant PTV margin reduction. However, lung volumes can significantly increase, thereby decreasing the mass of lung within a standard PTV.

Segmental Musculoskeletal Examinations using Dual-Energy X-Ray Absorptiometry (DXA): Positioning and Analysis Considerations

PubMed Central

Hart, Nicolas H.; Nimphius, Sophia; Spiteri, Tania; Cochrane, Jodie L.; Newton, Robert U.

2015-01-01

Musculoskeletal examinations provide informative and valuable quantitative insight into muscle and bone health. DXA is one mainstream tool used to accurately and reliably determine body composition components and bone mass characteristics in-vivo. Presently, whole body scan models separate the body into axial and appendicular regions, however there is a need for localised appendicular segmentation models to further examine regions of interest within the upper and lower extremities. Similarly, inconsistencies pertaining to patient positioning exist in the literature which influence measurement precision and analysis outcomes highlighting a need for standardised procedure. This paper provides standardised and reproducible: 1) positioning and analysis procedures using DXA and 2) reliable segmental examinations through descriptive appendicular boundaries. Whole-body scans were performed on forty-six (n = 46) football athletes (age: 22.9 ± 4.3 yrs; height: 1.85 ± 0.07 cm; weight: 87.4 ± 10.3 kg; body fat: 11.4 ± 4.5 %) using DXA. All segments across all scans were analysed three times by the main investigator on three separate days, and by three independent investigators a week following the original analysis. To examine intra-rater and inter-rater, between day and researcher reliability, coefficients of variation (CV) and intraclass correlation coefficients (ICC) were determined. Positioning and segmental analysis procedures presented in this study produced very high, nearly perfect intra-tester (CV ≤ 2.0%; ICC ≥ 0.988) and inter-tester (CV ≤ 2.4%; ICC ≥ 0.980) reliability, demonstrating excellent reproducibility within and between practitioners. Standardised examinations of axial and appendicular segments are necessary. Future studies aiming to quantify and report segmental analyses of the upper- and lower-body musculoskeletal properties using whole-body DXA scans are encouraged to use the patient positioning and image analysis procedures outlined in this paper. Key points Musculoskeletal examinations using DXA technology require highly standardised and reproducible patient positioning and image analysis procedures to accurately measure and monitor axial, appendicular and segmental regions of interest. Internal rotation and fixation of the lower-limbs is strongly recommended during whole-body DXA scans to prevent undesired movement, improve frontal mass accessibility and enhance ankle joint visibility during scan performance and analysis. Appendicular segmental analyses using whole-body DXA scans are highly reliable for all regional upper-body and lower-body segmentations, with hard-tissue (CV ≤ 1.5%; R ≥ 0.990) achieving greater reliability and lower error than soft-tissue (CV ≤ 2.4%; R ≥ 0.980) masses when using our appendicular segmental boundaries. PMID:26336349

The Star Formation History of Orion and its Environs

NASA Technical Reports Server (NTRS)

Calvet, Nuria

2002-01-01

During the Winter and Fall 2001 observing campaigns, we obtained multifilter photometry using the Quest camera on the 1mt Schmidt of the Venezuelan National Observatory, to continue the survey of the Orion clouds. In the Winter 2001 season, we obtained photometry for 9 scans at DEC=+5, 3 scans at DEC=-5, and 2 scans at DEC=-3, while 2 additional scans at DEC=-3 were obtained during the Fall 2001 observing campaign (the width of each scan is 2.3 arc minutes). The photometric survey has not been completed this season because the instrument was damaged by lightening on Sep 2001 and operations were suspended until Dec 2001. Observations are still under way. Nonetheless, we have enough scans at -3 and +5 to start selecting candidates for spectroscopic follow up on the next season. Spectra of more than 300 objects was obtained with the FAST spectrograph on the Mt Hopkins 48 inch telescope during observing campaigns Jan-March 2001, and Oct-Dec 2001. Bad weather prevented observations with Hydra on the WIYN telescope on KPNO in Jan 2001. The FAST spectra are been analyzed to select the young population of the regions. Observations in the JHKL bands were obtained for a sample of 20-30 objects in Ori Ia and Ib from scan centered at DEC=-l, with the StellIRCam on the Mt Hopkins 48 inch telescope on Nov 2001. L band observations will be effective for picking up objects surrounded by accretion disks, in which inner disk holes prevent having any excess at shorter wavelength bands. Observations at 10 micrometers and 18 micrometers were obtained in que mode for a sample of 20 objects in Ori Ia and Ib in the same regions as the near IR photometry with the Gemini-South telescope. These new data is presently been reduced and analyzed, together with data from the observing campaigns of 2000. Analysis of Hydra fields at strips centered at DEC=-1 and +1 have confirmed 105 more candidates as low mass pre-main sequence objects. In addition, every target was detected at 10 micrometers and a few at 18 micrometers. With these data, combined with our optical and JHKL photometry, we will construct spectral energy distributions. This will allow us to begin studying the structure of disks around low mass T Tauri stars in the distributed population of the Orion clouds, for direct comparison with that of Taurus. Ours is the first determination of the infrared emission of protoplanetary disks around low mass stars in the Orion region.

Quantitative Thin-Layer Chromatography/Mass Spectrometry Analysis of Caffeine Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methodsmore » determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.« less

Quantitative Caffeine Analysis Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methodsmore » determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.« less

Body Fat Composition: A Predictive Factor for Sleep Related Breathing Disorder in Obese Children.

PubMed

Bhatia, Rajeev; Lesser, Daniel J; Oliveira, Flavia G S A; Tran, Winston H; Keens, Thomas G; Khoo, Michael C K; Davidson Ward, Sally L

2015-09-15

The association between body fat composition as measured by dual energy x-ray absorptiometry (DEXA) scanning and pediatric sleep related breathing disorder (SRBD) is not well established. We investigated the relationship between body mass index (BMI) and DEXA parameters and their association with SRBD in obese children. Overnight polysomnography was performed on obese/overweight children (10-17 years) with habitual snoring. Total body fat mass (g), trunk fat mass (g), total body % fat, and trunk % fat were determined by DEXA. Forty-one subjects were studied. Logarithm (Log) total arousal index correlated with BMI (p < 0.01, r = 0.473), total body fat mass (p < 0.05, r = 0.331), and trunk fat mass (p < 0.05, r = 0.319). Log desaturation index correlated with BMI (p < 0.05, r = 0.313), total body fat mass (p < 0.05, r = 0.375), and trunk fat mass (p < 0.05, r = 0.391), whereas obstructive apnea hypopnea index (OAHI) did not. In males 10-12 years, there was a significant correlation between Log total arousal index and obesity parameters, but not for males aged 13-17 years. BMI correlated with DEXA parameters in all subjects: total body fat mass (p < 0.001, r = 0.850); total body % fat (p < 0.01, r = 0.425); trunk fat mass (p < 0.001, r = 0.792) and trunk % fat (p < 0.05, r = 0.318) and in 10-12 year old males. This relationship was not significant in males aged 13-17 years. Total body fat mass and trunk fat mass as well as BMI correlated with total arousal index and desaturation index. BMI correlated with DEXA parameters in 10-12 year old males but not in 13-17 year old males. The value of using DEXA scanning to study the relationship between obesity and SRBD may depend on age and pubertal stage. © 2015 American Academy of Sleep Medicine.

The Selection of Computed Tomography Scanning Schemes for Lengthy Symmetric Objects

NASA Astrophysics Data System (ADS)

Trinh, V. B.; Zhong, Y.; Osipov, S. P.

2017-04-01

. The article describes the basic computed tomography scan schemes for lengthy symmetric objects: continuous (discrete) rotation with a discrete linear movement; continuous (discrete) rotation with discrete linear movement to acquire 2D projection; continuous (discrete) linear movement with discrete rotation to acquire one-dimensional projection and continuous (discrete) rotation to acquire of 2D projection. The general method to calculate the scanning time is discussed in detail. It should be extracted the comparison principle to select a scanning scheme. This is because data are the same for all scanning schemes: the maximum energy of the X-ray radiation; the power of X-ray radiation source; the angle of the X-ray cone beam; the transverse dimension of a single detector; specified resolution and the maximum time, which is need to form one point of the original image and complies the number of registered photons). It demonstrates the possibilities of the above proposed method to compare the scanning schemes. Scanning object was a cylindrical object with the mass thickness is 4 g/cm2, the effective atomic number is 15 and length is 1300 mm. It analyzes data of scanning time and concludes about the efficiency of scanning schemes. It examines the productivity of all schemes and selects the effective one.

Improved Differential Ion Mobility Separations Using Linked Scans of Carrier Gas Composition and Compensation Field

NASA Astrophysics Data System (ADS)

Santiago, Brandon G.; Harris, Rachel A.; Isenberg, Samantha L.; Ridgeway, Mark E.; Pilo, Alice L.; Kaplan, Desmond A.; Glish, Gary L.

2015-07-01

Differential ion mobility spectrometry (DIMS) separates ions based on differences in their mobilities in low and high electric fields. When coupled to mass spectrometric analyses, DIMS has the ability to improve signal-to-background by eliminating isobaric and isomeric compounds for analytes in complex mixtures. DIMS separation power, often measured by resolution and peak capacity, can be improved through increasing the fraction of helium in the nitrogen carrier gas. However, because the mobility of ions is higher in helium, a greater number of ions collide with the DIMS electrodes or housing, yielding losses in signal intensity. To take advantage of the benefits of helium addition on DIMS separations and reduce ion losses, linked scans were developed. In a linked scan the helium content of the carrier gas is reduced as the compensation field is increased. Linked scans were compared with conventional compensation field scans with constant helium content for the protein ubiquitin and a tryptic digest of bovine serum albumin (BSA). Linked scans yield better separation of ubiquitin charge states and enhanced peak capacities for the analysis of BSA compared with compensation field scans with constant helium carrier gas percentages. Linked scans also offer improved signal intensity retention in comparison to compensation field scans with constant helium percentages in the carrier gas.

Hard x-ray phase contrastmicroscopy - techniques and applications

NASA Astrophysics Data System (ADS)

Holzner, Christian

In 1918, Einstein provided the first description of the nature of the refractive index for X-rays, showing that phase contrast effects are significant. A century later, most x-ray microscopy and nearly all medical imaging remains based on absorption contrast, even though phase contrast offers orders of magnitude improvements in contrast and reduced radiation exposure at multi-keV x-ray energies. The work presented is concerned with developing practical and quantitative methods of phase contrast for x-ray microscopy. A theoretical framework for imaging in phase contrast is put forward; this is used to obtain quantitative images in a scanning microscope using a segmented detector, and to correct for artifacts in a commercial phase contrast x-ray nano-tomography system. The principle of reciprocity between scanning and full-field microscopes is then used to arrive at a novel solution: Zernike contrast in a scanning microscope. These approaches are compared on a theoretical and experimental basis in direct connection with applications using multi-keV x-ray microscopes at the Advanced Photon Source at Argonne National Laboratory. Phase contrast provides the best means to image mass and ultrastructure of light elements that mainly constitute biological matter, while stimulated x-ray fluorescence provides high sensitivity for studies of the distribution of heavier trace elements, such as metals. These approaches are combined in a complementary way to yield quantitative maps of elemental concentration from 2D images, with elements placed in their ultrastructural context. The combination of x-ray fluorescence and phase contrast poses an ideal match for routine, high resolution tomographic imaging of biological samples in the future. The presented techniques and demonstration experiments will help pave the way for this development.

Scanning fiber endoscopy with highly flexible, 1-mm catheterscopes for wide-field, full-color imaging

PubMed Central

Lee, Cameron M.; Engelbrecht, Christoph J.; Soper, Timothy D.; Helmchen, Fritjof; Seibel, Eric J.

2011-01-01

In modern endoscopy, wide field of view and full color are considered necessary for navigating inside the body, inspecting tissue for disease and guiding interventions such as biopsy or surgery. Current flexible endoscope technologies suffer from reduced resolution when device diameter shrinks. Endoscopic procedures today using coherent fiber bundle technology, on the scale of 1 mm, are performed with such poor image quality that the clinician’s vision meets the criteria for legal blindness. Here, we review a new and versatile scanning fiber imaging technology and describe its implementation for ultrathin and flexible endoscopy. This scanning fiber endoscope (SFE) or catheterscope enables high quality, laser-based, video imaging for ultrathin clinical applications while also providing new options for in vivo biological research of subsurface tissue and high resolution fluorescence imaging. PMID:20336702

Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC-ESI-MS/MS approach based on advanced mass spectrometric techniques.

PubMed

Dasenaki, Marilena E; Thomaidis, Nikolaos S

2010-07-05

A strategy was newly developed to rapidly screen seventeen sulfonamides and five tetracyclines in a single run from fish tissues using ultra-high performance liquid chromatography (UHPLC) coupled with comprehensive mass spectrometric approaches, including precursor-ion scan and data dependent scan. The product ions for precursor-ion scanning were selected by studying the MS/MS fragmentation of the analytes. All sulfonamides share the same diagnostic product ion at m/z 156 in positive MS/MS scan, while for tetracycline antibiotics the diagnostic product ion was proved to be at m/z 153.8. Further characterization of each compound was performed using a data dependent scan. Separation was performed on a Zorbax Eclipse Plus C18 column with a gradient elution using acetonitrile - 0.1% formic acid mobile phase at a flow rate of 0.1 mL min(-1). This approach has proven to be a powerful, highly selective, and sensitive tool for rapid screening and detection of non-targeted components in fish tissue and requires a minimum sample preparation such as one generic extraction step with MeOH:ACN 50:50 (v/v) acidified with 0.05% formic acid. The method has also been applied successfully to porcine and poultry meat. The validation of such a screening method was performed for the first time according to Commission Decision 2002/657/EC and satisfactory method performance characteristics were achieved. Copyright 2010 Elsevier B.V. All rights reserved.

A disappearing left-sided neck mass

PubMed Central

Lutwak, Nancy; Dill, Curt

2012-01-01

The patient was a 48-year-old man who presented to the emergency department with complaints of a left-sided painful neck mass, which changed in size relative to ingestion of meals. He denied voice change, fever, chills, weight loss, dysphagia and hoarseness. Physical examination was unremarkable. CT scan demonstrated a 3.9 mm calculus of the submandibular gland duct. Therapeutic sialendocopy was successfully performed. PMID:22764156

Mass spectrometric measurements of atmospheric composition

NASA Technical Reports Server (NTRS)

Hoffman, J. H.

1974-01-01

The development of a magnetic sector field analyzer for continuous sampling and measurement of outer planetary atmospheres is discussed. Special features of the analyzer include a dynamic range of 10 to the minus 7th power, a mass range from 1 to 48 AMU, two ion sensitivities, a special scan time of 35 sec at 14 BPS, and the use of ion counting techniques for analysis.

A flexible 3D laser scanning system using a robotic arm

NASA Astrophysics Data System (ADS)

Fei, Zixuan; Zhou, Xiang; Gao, Xiaofei; Zhang, Guanliang

2017-06-01

In this paper, we present a flexible 3D scanning system based on a MEMS scanner mounted on an industrial arm with a turntable. This system has 7-degrees of freedom and is able to conduct a full field scan from any angle, suitable for scanning object with the complex shape. The existing non-contact 3D scanning system usually uses laser scanner that projects fixed stripe mounted on the Coordinate Measuring Machine (CMM) or industrial robot. These existing systems can't perform path planning without CAD models. The 3D scanning system presented in this paper can scan the object without CAD models, and we introduced this path planning method in the paper. We also propose a practical approach to calibrating the hand-in-eye system based on binocular stereo vision and analyzes the errors of the hand-eye calibration.

Design and analysis of a sub-aperture scanning machine for the transmittance measurements of large-aperture optical system

NASA Astrophysics Data System (ADS)

He, Yingwei; Li, Ping; Feng, Guojin; Cheng, Li; Wang, Yu; Wu, Houping; Liu, Zilong; Zheng, Chundi; Sha, Dingguo

2010-11-01

For measuring large-aperture optical system transmittance, a novel sub-aperture scanning machine with double-rotating arms (SSMDA) was designed to obtain sub-aperture beam spot. Optical system full-aperture transmittance measurements can be achieved by applying sub-aperture beam spot scanning technology. The mathematical model of the SSMDA based on a homogeneous coordinate transformation matrix is established to develop a detailed methodology for analyzing the beam spot scanning errors. The error analysis methodology considers two fundamental sources of scanning errors, namely (1) the length systematic errors and (2) the rotational systematic errors. As the systematic errors of the parameters are given beforehand, computational results of scanning errors are between -0.007~0.028mm while scanning radius is not lager than 400.000mm. The results offer theoretical and data basis to the research on transmission characteristics of large optical system.

Mass and molecular composition of vesicular stomatitis virus: a scanning transmission electron microscopy analysis.

PubMed

Thomas, D; Newcomb, W W; Brown, J C; Wall, J S; Hainfeld, J F; Trus, B L; Steven, A C

1985-05-01

Dark-field scanning transmission electron microscopy was used to perform mass analyses of purified vesicular stomatitis virions, pronase-treated virions, and nucleocapsids, leading to a complete self-consistent account of the molecular composition of vesicular stomatitis virus. The masses obtained were 265.6 +/- 13.3 megadaltons (MDa) for the native virion, 197.5 +/- 8.4 MDa for the pronase-treated virion, and 69.4 +/- 4.9 MDa for the nucleocapsid. The reduction in mass effected by pronase treatment, which corresponds to excision of the external domains (spikes) of G protein, leads to an average of 1,205 molecules of G protein per virion. The nucleocapsid mass, after compensation for the RNA (3.7 MDa) and residual amounts of other proteins, yielded a complement of 1,258 copies of N protein. Calibration of the amounts of M, NS, and L proteins relative to N protein by biochemical quantitation yielded values of 1,826, 466, and 50 molecules, respectively, per virion. Assuming that the remaining virion mass is contributed by lipids in the viral envelope, we obtained a value of 56.1 MDa for its lipid content. In addition, four different electron microscopy procedures were applied to determine the nucleocapsid length, which we conclude to be 3.5 to 3.7 micron. The nucleocapsid comprises a strand of repeating units which have a center-to-center spacing of 3.3 nm as measured along the middle of the strand. We show that these repeating units represent monomers of N protein, each of which is associated with 9 +/- 1 bases of single-stranded RNA. From scanning transmission electron microscopy images of negatively stained nucleocapsids, we inferred that N protein has a wedge-shaped, bilobed structure with dimensions of approximately 9.0 nm (length), approximately 5.0 nm (depth), and approximately 3.3 nm (width, at the midpoint of its long axis). In the coiled configuration of the in situ nucleocapsid, the long axis of N protein is directed radially, and its depth corresponds to the pitch of the nucleocapsid helix.

Mass and molecular composition of vesicular stomatitis virus: a scanning transmission electron microscopy analysis.

PubMed Central

Thomas, D; Newcomb, W W; Brown, J C; Wall, J S; Hainfeld, J F; Trus, B L; Steven, A C

1985-01-01

Dark-field scanning transmission electron microscopy was used to perform mass analyses of purified vesicular stomatitis virions, pronase-treated virions, and nucleocapsids, leading to a complete self-consistent account of the molecular composition of vesicular stomatitis virus. The masses obtained were 265.6 +/- 13.3 megadaltons (MDa) for the native virion, 197.5 +/- 8.4 MDa for the pronase-treated virion, and 69.4 +/- 4.9 MDa for the nucleocapsid. The reduction in mass effected by pronase treatment, which corresponds to excision of the external domains (spikes) of G protein, leads to an average of 1,205 molecules of G protein per virion. The nucleocapsid mass, after compensation for the RNA (3.7 MDa) and residual amounts of other proteins, yielded a complement of 1,258 copies of N protein. Calibration of the amounts of M, NS, and L proteins relative to N protein by biochemical quantitation yielded values of 1,826, 466, and 50 molecules, respectively, per virion. Assuming that the remaining virion mass is contributed by lipids in the viral envelope, we obtained a value of 56.1 MDa for its lipid content. In addition, four different electron microscopy procedures were applied to determine the nucleocapsid length, which we conclude to be 3.5 to 3.7 micron. The nucleocapsid comprises a strand of repeating units which have a center-to-center spacing of 3.3 nm as measured along the middle of the strand. We show that these repeating units represent monomers of N protein, each of which is associated with 9 +/- 1 bases of single-stranded RNA. From scanning transmission electron microscopy images of negatively stained nucleocapsids, we inferred that N protein has a wedge-shaped, bilobed structure with dimensions of approximately 9.0 nm (length), approximately 5.0 nm (depth), and approximately 3.3 nm (width, at the midpoint of its long axis). In the coiled configuration of the in situ nucleocapsid, the long axis of N protein is directed radially, and its depth corresponds to the pitch of the nucleocapsid helix. Images PMID:2985822

MacMS: A Mass Spectrometer Simulator: Abstract of Issue 9906M

NASA Astrophysics Data System (ADS)

Bigger, Stephen W.; Craig, Robert A.

1999-10-01

MacMS is a program for Mac-OS compatible computers that simulates a magnetic sector mass spectrometer (1-4) designed to operate in the mass-to-charge (m/z) ratio range of 1-200 amu. MacMS has two operational modules. The first module (see Figure 1) is called the "Path" module and enables the user to quantitatively examine the trajectory of an ion of given m/z ratio in the electric and magnetic fields of the simulated "instrument". By systematically measuring a series of trajectories of different ions under different electric and magnetic field conditions, the user can determine how the resolution of the "instrument" is affected by these experimentally variable parameters. The user can thus choose suitable instrumental conditions for scanning a given m/z ratio range with good separation between the peaks. The second module (see Figure 2) is called as the "Spectrometer" module and enables the user to record, under any chosen instrumental conditions, the mass spectrum of (i) the instrumental background, (ii) neon, (iii) methane, or (iv) the parent ion of carbon tetrachloride. Both voltage scanning and magnetic scanning are possible (5). A hard copy of any mass spectrum that has been recorded can also be obtained. MacMS can read ASCII data files containing mass spectral information of compounds other than those that are "built-in" to the simulator. The appropriate format for creating such data files is described in the program documentation. There are a number of instructional exercises that can be conducted using the mass spectral information contained within the simulator. These are included in the program documentation. For example, the intensities of the 20Ne+, 21Ne+, and 22Ne+ species can be determined from hard copies of mass spectra of neon that are obtained under different instrumental sensitivities. The relative abundances of the three isotopes of neon can thus be calculated and compared with the literature values (6). The simulator also includes adjustable, fixed-value range and gain settings, which can be used to enhance the resolution and sensitivity of the instrument respectively.

1. Kiser, R. N. Introduction to Mass Spectrometry and its Applications; Prentice-Hall: Englewood Cliffs, N. J., 1965; pp 1-3; pp 32-65.
2. Johnstone, R. A. W.; Rose, M. E. Mass Spectrometry for Chemists and Biochemists, 2nd ed.; Cambridge University Press: Cambridge, 1996.
3. Hill, H. C.; Loudon, A. G. Introduction to Mass Spectrometry; 2nd ed.; Heyden: London, 1972; p 5.
4. Farmer, J. B. In Mass Spectrometry, McDowell, C. A., Ed.; McGraw-Hill: New York, 1963; pp 10-11.
5. Message, G. M. Practical Aspects of Gas Chromatography-Mass Spectrometry, Wiley: New York, 1984; Chapter 3.
6. CRC Handbook of Chemistry and Physics, 55th ed.; CRC: Cleveland, 1974.

Does C₁ fracture displacement correlate with transverse ligament integrity?

PubMed

Radcliff, Kristen E; Sonagli, Marcos A; Rodrigues, Luciano M; Sidhu, Gursukhman S; Albert, Todd J; Vaccaro, Alexander R

2013-05-01

The Rule of Spence states that displacement of the C₁ lateral masses by >6.9-8.1 mm suggests loss of transverse ligament integrity. The purpose of this study was to establish the thresholds of C₁ displacement on CT scans that correspond to transverse ligament disruption. Over four years, consecutive patients with acute C₁ fractures with at least three fracture lines were analyzed. CT measurements and MRI were assessed by blinded observers for bony displacement in the axial (internal and external lateral mass separation), coronal and sagittal planes and transverse ligament integrity. Eighteen patients were studied. Mean CT bony measurements were as follows: internal border lateral mass separation (ILM) 23.3 ± 3.4 mm, external border lateral mass separation (ELM) 50.3 ± 4.3 mm, total C₁ lateral mass overhang over the C₂ superior process (LMO) 5.4 ± 1.3 mm. Twelve patients were identified as having intact transverse ligament and six had transverse ligament disruption. There was no difference in mean normalized ILM, ELM, or LMO between patients with or without transverse ligament integrity (P > 0.05). There was no correlation between bony displacement and transverse ligament integrity. CT scans post-injury may not show the position of maximal displacement. If there is clinical concern about a possible transverse ligament injury, MRI should be performed. © 2013 Chinese Orthopaedic Association and Wiley Publishing Asia Pty Ltd.

Nanoporous-carbon as a potential host material for reversible Mg ion intercalation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siegal, Michael P.; Yelton, W. Graham; Perdue, Brian R.

Here, we study nanoporous-carbon (NPC) grown via pulsed laser deposition (PLD) as an electrically conductive anode host material for Mg 2+ intercalation. NPC has high surface area, and an open, accessible pore structure tunable via mass density that can improve diffusion. We fabricate 2032 coin cells using NPC coated stainless-steel disk anodes, metallic Mg cathodes, and a Grignard-based electrolyte. NPC mass density is controlled during growth, ranging from 0.06–1.3 g/cm 3. The specific surface area of NPC increases linearly from 1,000 to 1,700 m 2/g as mass density decreases from 1.3 to 0.26 g/cm 3, however, the surface area fallsmore » off dramatically at lower mass densities, implying a lack of mechanical integrity in such nanostructures. These structural characterizations correlate directly with coin cell electrochemical measurements. In particular, cyclic voltammetry (CV) scans for NPC with density ~0.5 g/cm 3 and BET surface area ~1500 m 2/g infer the possibility of reversible Mg-ion intercalation. Higher density NPC yields capacitive behavior, most likely resulting from the smaller interplanar spacings between graphene sheet fragments and tighter domain boundaries; lower density NPC results in asymmetrical CV scans, consistent with the likely structural degradation resulting from mass transport through soft, low-density carbon materials.« less

Two-Dimensional Echocardiography Estimates of Fetal Ventricular Mass throughout Gestation.

PubMed

Aye, Christina Y L; Lewandowski, Adam James; Ohuma, Eric O; Upton, Ross; Packham, Alice; Kenworthy, Yvonne; Roseman, Fenella; Norris, Tess; Molloholli, Malid; Wanyonyi, Sikolia; Papageorghiou, Aris T; Leeson, Paul

2017-08-12

Two-dimensional (2D) ultrasound quality has improved in recent years. Quantification of cardiac dimensions is important to screen and monitor certain fetal conditions. We assessed the feasibility and reproducibility of fetal ventricular measures using 2D echocardiography, reported normal ranges in our cohort, and compared estimates to other modalities. Mass and end-diastolic volume were estimated by manual contouring in the four-chamber view using TomTec Image Arena 4.6 in end diastole. Nomograms were created from smoothed centiles of measures, constructed using fractional polynomials after log transformation. The results were compared to those of previous studies using other modalities. A total of 294 scans from 146 fetuses from 15+0 to 41+6 weeks of gestation were included. Seven percent of scans were unanalysable and intraobserver variability was good (intraclass correlation coefficients for left and right ventricular mass 0.97 [0.87-0.99] and 0.99 [0.95-1.0], respectively). Mass and volume increased exponentially, showing good agreement with 3D mass estimates up to 28 weeks of gestation, after which our measurements were in better agreement with neonatal cardiac magnetic resonance imaging. There was good agreement with 4D volume estimates for the left ventricle. Current state-of-the-art 2D echocardiography platforms provide accurate, feasible, and reproducible fetal ventricular measures across gestation, and in certain circumstances may be the modality of choice. © 2017 S. Karger AG, Basel.

Nanoporous-carbon as a potential host material for reversible Mg ion intercalation

DOE PAGES

Siegal, Michael P.; Yelton, W. Graham; Perdue, Brian R.; ...

2016-03-25

Here, we study nanoporous-carbon (NPC) grown via pulsed laser deposition (PLD) as an electrically conductive anode host material for Mg 2+ intercalation. NPC has high surface area, and an open, accessible pore structure tunable via mass density that can improve diffusion. We fabricate 2032 coin cells using NPC coated stainless-steel disk anodes, metallic Mg cathodes, and a Grignard-based electrolyte. NPC mass density is controlled during growth, ranging from 0.06–1.3 g/cm 3. The specific surface area of NPC increases linearly from 1,000 to 1,700 m 2/g as mass density decreases from 1.3 to 0.26 g/cm 3, however, the surface area fallsmore » off dramatically at lower mass densities, implying a lack of mechanical integrity in such nanostructures. These structural characterizations correlate directly with coin cell electrochemical measurements. In particular, cyclic voltammetry (CV) scans for NPC with density ~0.5 g/cm 3 and BET surface area ~1500 m 2/g infer the possibility of reversible Mg-ion intercalation. Higher density NPC yields capacitive behavior, most likely resulting from the smaller interplanar spacings between graphene sheet fragments and tighter domain boundaries; lower density NPC results in asymmetrical CV scans, consistent with the likely structural degradation resulting from mass transport through soft, low-density carbon materials.« less

VizieR Online Data Catalog: Herschel-PACS and -SPIRE spectroscopy of 70 objects (Green+, 2016)

NASA Astrophysics Data System (ADS)

Green, J. D.; Yang, Y.-L.; Evans, N. J., II; Karska, A.; Herczeg, G.; van Dishoeck, E. F.; Lee, J.-E.; Larson, R. L.; Bouwman, J.

2016-10-01

We present the CDF (COPS-DIGIT-FOOSH) archive, with Herschel spectroscopic observations of 70 objects (protostars, young stellar objects, and FU Orionis objects) from the "Dust, Ice, and Gas in Time" (DIGIT) Key Project, FU Orionis Objects Surveyed with Herschel" Open Time Program (FOOSH OT1), and "CO in Protostars" Open Time Program (COPS OT2) Herschel programs. These have been delivered to the Herschel archive and are available. The full source list is shown in Table1. The full DIGIT spectroscopic sample consists of 63 sources: 24 Herbig Ae/Be stars (intermediate mass sources with circumstellar disks), 9 T Tauri stars (low mass young stars with circumstellar disks), and 30 protostars (young stars with significant envelope emission) observed with Photodetector Array Camera and Spectrometer (PACS) spectroscopy. DIGIT also included an additional wTTS (weak-line T Tauri star) sample that was observed photometrically and delivered separately. The wTTS sample is fully described by Cieza et al. 2013ApJ...762..100C. The full DIGIT embedded protostellar sample consisted of 30 Class 0/I targets, drawn from previous studies, focusing on protostars with high-quality Spitzer-IRS 5-40μm spectroscopy (summarized by Lahuis et al. 2006 c2d Spectroscopy Explanatory Supplement; Pasadena, CA: Spitzer Science Center), and UV, optical, infrared, and submillimeter complementary data. These objects are selected from some of the nearest and best-studied molecular clouds: Taurus (140pc; 6 targets), Ophiuchus (125pc; 7 targets), Perseus (230-250pc; 7 targets), R Corona Australis (130pc; 3 targets), Serpens (429pc; 2 targets), Chamaeleon (178pc, 1 target), and 4 additional isolated cores. PACS is a 5*5 array of 9.4''*9.4'' spatial pixels (spaxels) covering the spectral range from 50 to 210μm with λ/Δλ~1000-3000, divided into four segments, covering λ~50-75, 70-105, 100-145, and 140-210μm. The PACS spatial resolution ranges from ~9'' at the shortest wavelengths (50μm) to ~18'' at the longest (210μm), corresponding to 1000-4500AU at the distances of most sources. The nominal pointing rms of the telescope is 2''. For the DIGIT embedded protostars sample we utilized the full range of PACS (50-210μm) in two linked, pointed, chop/nod rangescans: a blue scan covering 50-75 and 100-150μm (SED B2A+short R1); and a red scan covering 70-105 and 140-210μm (SED B2B+long R1). We used 6 and 4 range repetitions respectively, for integration times of 6853 and 9088s (a total of ~16000s per target for the entire 50-210μm scan). Excluding overhead, 50% of the integration time is spent on source and 50% on sky. Thus the effective on-source integration times are 3088 and 4180s, for the blue and red scans, respectively. The total on-source integration time to achieve the entire 50-210μm scan is then 7268s. Most (21 of 33) disk sources were observed with the same procedure as the embedded objects. The other 12 sources have only partial spectral coverage: 8 Herbig Ae/Be sources (HD35187, HD203024, HD245906, HD142666, HD144432, HD141569, HD98922, and HD150193) and 4 T Tauri sources (HT Lup, RU Lup, RY Lup, and RNO90) were observed using only the blue scans (i.e., achieving a wavelength coverage only from SED B2A+short R1, 100-150μm). 9 of these 12 sources (all except HD35187, HD203024, and HD245906) were observed in a further limited wavelength range (60-72+120-134μm; referred to as "forsterite only" scans for their focus on the 69μm forsterite dust feature). The FU Orionis Objects Surveyed with Herschel (FOOSH) program consisted of 21hrs of Herschel observing time: V1057Cyg, V1331Cyg, V1515Cyg, V1735Cyg, and FUOri were observed as part of FOOSH. For the FOOSH sample we again utilized the full range of PACS (50-210μm) in two linked, pointed, chop/nod rangescans: a blue scan covering 50-75 and 100-150μm (SED B2A+short R1); and a red scan covering 70-105 and 140-210μm (SED B2B+long R1). We used 6 and 4 range repetitions respectively, for integration times of 3530 and 4620s (a total of ~8000s per target and off-positions combined, for the entire 50-210μm scan; the on-source integration time is ~3000s). The telescope sky background was subtracted using two nod positions 6' from the source. The Spectral and Photometric Imaging REceiver (SPIRE; 194-670μm)/Fourier Transform Spectrometer (FTS) data were taken in a single pointing with sparse image sampling, high spectral resolution mode, over 1hr of integration time. The spectrum is divided into two orders covering the spectral ranges 194-325μm ("SSW"; Spectrograph Short Wavelengths) and 320-690μm ("SLW"; Spectrograph Long Wavelengths), with a resolution, Δv of 1.44GHz and resolving power, λ/Δλ~300-800, increasing at shorter wavelengths. The sample of 31 COPS (CO in ProtoStars) protostars observed with SPIRE-FTS includes 25 sources from the DIGIT and 6 from the WISH (Water in Star-forming regions with Herschel, PI: E. van Dischoek; van Dishoeck et al. 2011PASP..123..138V; see also Nisini et al. 2010A&A...518L.120N; Kristensen et al. 2012A&A...542A...8K; Karska et al. 2013A&A...552A.141K; Wampfler et al. 2013A&A...552A..56W) key programs. A nearly identical sample was observed in COJ=16->15 with HIFI (PI: L. Kristensen) and is presented in L. Kristensen et al. 2016, (in preparation). This data set (COPS: SPIRE-FTS) is analyzed in a forthcoming paper (J. Green et al. 2016, in preparation). The SPIRE beamsize ranges from 17'' to 40'', equivalent to physical sizes of ~2000-10000AU at the distances of the COPS sources. The COPS SPIRE-FTS data were observed identically to the FOOSH SPIRE data, in a single pointing with sparse image sampling, high spectral resolution, in 1hr of integration time per source, with one exception: the IRS 44/46 data were observed in medium image sampling (e.g., complete spatial coverage within the inner 2 rings of spaxels), in 1.5hr, in order to better distinguish IRS44 (the comparatively brighter IR source; Green et al. 2013ApJ...770..123G, J. Green et al. 2016, in preparation) from IRS46. (2 data files).

The EXIST Mission Concept Study

NASA Technical Reports Server (NTRS)

Fishman, Gerald J.; Grindlay, J.; Hong, J.

2008-01-01

EXIST is a mission designed to find and study black holes (BHs) over a wide range of environments and masses, including: 1) BHs accreting from binary companions or dense molecular clouds throughout our Galaxy and the Local Group, 2) supermassive black holes (SMBHs) lying dormant in galaxies that reveal their existence by disrupting passing stars, and 3) SMBHs that are hidden from our view at lower energies due to obscuration by the gas that they accrete. 4) the birth of stellar mass BHs which is accompanied by long cosmic gamma-ray bursts (GRBs) which are seen several times a day and may be associated with the earliest stars to form in the Universe. EXIST will provide an order of magnitude increase in sensitivity and angular resolution as well as greater spectral resolution and bandwidth compared with earlier hard X-ray survey telescopes. With an onboard optical-infra red (IR) telescope, EXIST will measure the spectra and redshifts of GRBs and their utility as cosmological probes of the highest z universe and epoch of reionization. The mission would retain its primary goal of being the Black Hole Finder Probe in the Beyond Einstein Program. However, the new design for EXIST proposed to be studied here represents a significant advance from its previous incarnation as presented to BEPAC. The mission is now less than half the total mass, would be launched on the smallest EELV available (Atlas V-401) for a Medium Class mission, and most importantly includes a two-telescope complement that is ideally suited for the study of both obscured and very distant BHs. EXIST retains its very wide field hard X-ray imaging High Energy Telescope (HET) as the primary instrument, now with improved angular and spectral resolution, and in a more compact payload that allows occasional rapid slews for immediate optical/IR imaging and spectra of GRBs and AGN as well as enhanced hard X-ray spectra and timing with pointed observations. The mission would conduct a 2 year full sky survey in scanning mode, interrupted for several orbits per day by GRB follow-ups, followed by a combined pointing-scanning mission phase for optical/IR spectroscopy and redshifts for the large AGN sample found in the survey as well as GRBs and LSST transients. A Team of university, NASA, and industry investigators will conduct the study to determine the full sensitivity and capabilities of this new configuration for EXIST. It will build on the extensive studies of the prior design for the mission and the HET and will incorporate the optical/IR telescope (hereafter IRT) now fully developed by our ITT partner for the NextView Commercial Remote Sensing mission (early 2008 launch) with a focal plane to be developed at GSFC based in part on JWST/NIRSPEC designs. No new technology is needed for either the IRT or HET instruments. The study will pay close attention to full mission cost and present a design for the Decadal Survey Workshop to ensure this even more capable EXIST mission is once again part of the next Decadal Survey.

Design and development of an optical scanning mechanism (OSMA) with minimum momentum transfer

NASA Technical Reports Server (NTRS)

Sainz, L. B. F.; Herrera, E.; Bajo, J. M.; Mallard, H. J.

1981-01-01

The development model for an optical scanning mechanism assembly is described as being two equal inertial masses which collide with each other to minimize the momentum transfer to the satellite and other mounted instruments. The design criteria for the mirror, the compensating inertia structure and other components are given. The details of the design are discussed and related test results are presented, which show the validity of the design concept for momentum compensation.

Nano-Se: Cheap and easy-to-obtain novel material for all-dielectric nano-photonics

NASA Astrophysics Data System (ADS)

Ivanova, A. K.; Ionin, A. A.; Khmel'nitskii, R. A.; Klevkov, Yu. K.; Kudryashov, S. I.; Levchenko, A. O.; Mel'nik, N. N.; Nastulyavichus, A. A.; Rudenko, A. A.; Saraeva, I. N.; Smirnov, N. A.; Zayarny, D. A.; Gonchukov, S. A.; Tolordava, E. R.; Baranov, A. N.

2017-09-01

Milligram-per-second production of selenium nanoparticles in water sols was realized through few W, kHz-rate nanosecond laser ablation of a solid selenium pellet. High-yield particle formation mechanism and ultimate mass-removal yield were elucidated by optical profilometry and scanning electron microscopy characterization of crater depths and topographies. Deposited particles were inspected by scanning electron microscopy, while optical transmission Raman and dynamic light scattering spectroscopy characterized their hydrosols.

Selenomethionine Se 75 thymus scans in myasthenia gravis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Toole, J.F.; Cowan, R.; Maynard, D.

1975-01-01

In 1966, Toole and Witcofski introduced selenomethionine Se 75 mediastinal scanning as a diagnostic test for thymomas. Since then we have performed such scans on patients with myasthenic syndrome. Because the technique is atraumatic, safe, and accurate, it can be performed on critically ill myasthenics. Two hundred and fifty microcuries of selenomethionine Se 75 is injected intravenously. Within 1 hour the mediastinum from the suprasternal notch to the ziphoid process is scanned, using a 2 x 3 inch scanner. Delayed scans have been made in a few instances but they have not increased the number of positive cases. Selenomethionine Semore » 75 is incorporated into tissues undergoing rapid protein synthesis such as thyroid, pancreas, liver, and lymphomas. Of the 34 mediastinal scans performed on myasthenics between 1966 and December 31, 1974, 4 were positive for thymoma. In addition, there was a positive scan with uptake in an area of atelectasis of the lung adjacent to the mediastinum. Of interest is the fact that 1 patient with carcinoma of the lung had a positive scan over the lesion. In 13 patients with chronic lymphatic leukemia the mediastinal scans were negative. In another patient with a mediastinal mass noted on chest x-ray, a variety of differential diagnostic possibilities were considered, such as pericardial cyst, dermoid, and aneurysm. A selenomethionine scan was strongly positive, suggesting a thymoma which subsequent surgery confirmed.« less

Retention behavior of lipids in reversed-phase ultrahigh-performance liquid chromatography-electrospray ionization mass spectrometry.

PubMed

Ovčačíková, Magdaléna; Lísa, Miroslav; Cífková, Eva; Holčapek, Michal

2016-06-10

Reversed-phase ultrahigh-performance liquid chromatography (RP-UHPLC) method using two 15cm sub-2μm particles octadecylsilica gel columns is developed with the goal to separate and unambiguously identify a large number of lipid species in biological samples. The identification is performed by the coupling with high-resolution tandem mass spectrometry (MS/MS) using quadrupole - time-of-flight (QTOF) instrument. Electrospray ionization (ESI) full scan and tandem mass spectra are measured in both polarity modes with the mass accuracy better than 5ppm, which provides a high confidence of lipid identification. Over 400 lipid species covering 14 polar and nonpolar lipid classes from 5 lipid categories are identified in total lipid extracts of human plasma, human urine and porcine brain. The general dependences of relative retention times on relative carbon number or relative double bond number are constructed and fit with the second degree polynomial regression. The regular retention patterns in homologous lipid series provide additional identification point for UHPLC/MS lipidomic analysis, which increases the confidence of lipid identification. The reprocessing of previously published data by our and other groups measured in the RP mode and ultrahigh-performance supercritical fluid chromatography on the silica column shows more generic applicability of the polynomial regression for the description of retention behavior and the prediction of retention times. The novelty of this work is the characterization of general trends in the retention behavior of lipids within logical series with constant fatty acyl length or double bond number, which may be used as an additional criterion to increase the confidence of lipid identification. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid discrimination of bergamot essential oil by paper spray mass spectrometry and chemometric analysis.

PubMed

Taverna, Domenico; Di Donna, Leonardo; Mazzotti, Fabio; Tagarelli, Antonio; Napoli, Anna; Furia, Emilia; Sindona, Giovanni

2016-09-01

A novel approach for the rapid discrimination of bergamot essential oil from other citrus fruits oils is presented. The method was developed using paper spray mass spectrometry (PS-MS) allowing for a rapid molecular profiling coupled with a statistic tool for a precise and reliable discrimination between the bergamot complex matrix and other similar matrices, commonly used for its reconstitution. Ambient mass spectrometry possesses the ability to record mass spectra of ordinary samples, in their native environment, without sample preparation or pre-separation by creating ions outside the instrument. The present study reports a PS-MS method for the determination of oxygen heterocyclic compounds such as furocoumarins, psoralens and flavonoids present in the non-volatile fraction of citrus fruits essential oils followed by chemometric analysis. The volatile fraction of Bergamot is one of the most known and fashionable natural products, which found applications in flavoring industry as ingredient in beverages and flavored foodstuff. The development of the presented method employed bergamot, sweet orange, orange, cedar, grapefruit and mandarin essential oils. PS-MS measurements were carried out in full scan mode for a total run time of 2 min. The capability of PS-MS profiling to act as marker for the classification of bergamot essential oils was evaluated by using multivariate statistical analysis. Two pattern recognition techniques, linear discriminant analysis and soft independent modeling of class analogy, were applied to MS data. The cross-validation procedure has shown excellent results in terms of the prediction ability because both models have correctly classified all samples for each category. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Screening of 485 Pesticide Residues in Fruits and Vegetables by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and QTOF Spectrum Library.

PubMed

Pang, Guo-Fang; Fan, Chun-Lin; Chang, Qiao-Ying; Li, Jian-Xun; Kang, Jian; Lu, Mei-Ling

2018-03-22

This paper uses the LC-quadrupole-time-of-flight MS technique to evaluate the behavioral characteristics of MSof 485 pesticides under different conditions and has developed an accurate mass database and spectra library. A high-throughput screening and confirmation method has been developed for the 485 pesticides in fruits and vegetables. Through the optimization of parameters such as accurate mass number, time of retention window, ionization forms, etc., the method has improved the accuracy of pesticide screening, thus avoiding the occurrence of false-positive and false-negative results. The method features a full scan of fragments, with 80% of pesticide qualitative points over 10, which helps increase pesticide qualitative accuracy. The abundant differences of fragment categories help realize the effective separation and qualitative identification of isomer pesticides. Four different fruits and vegetables-apples, grapes, celery, and tomatoes-were chosen to evaluate the efficiency of the method at three fortification levels of 5, 10, and 20 μg/kg, and satisfactory results were obtained. With this method, a national survey of pesticide residues was conducted between 2012 and 2015 for 12 551 samples of 146 different fruits and vegetables collected from 638 sampling points in 284 counties across 31 provincial capitals/cities directly under the central government, which provided scientific data backup for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public. Meanwhile, the big data statistical analysis of the new technique also further proves it to be of high speed, high throughput, high accuracy, high reliability, and high informatization.

1300931

NASA Image and Video Library

2013-08-15

OVERVIEW OF THE MATERIALS DIAGNOSTIC LABORATORY. THE NEAR END SHOWS THE SURFACE ANALYSIS INSTRUMENTS SUCH AS THE SECONDARY ION MASS SPECTROSCOPE (CLOSEST) AND THE TWO ELECTRON SPECTROSCOPY INSTRUMENTS, WHILE THE FAR END SHOWS THE NEW SCANNING ELECTRON MICROSCOPES

Frequency selection rule for high definition and high frame rate Lissajous scanning.

PubMed

Hwang, Kyungmin; Seo, Yeong-Hyeon; Ahn, Jinhyo; Kim, Pilhan; Jeong, Ki-Hun

2017-10-26

Lissajous microscanners are very attractive in compact laser scanning applications such as endomicroscopy or pro-projection display owing to high mechanical stability and low operating voltages. The scanning frequency serves as a critical factor for determining the scanning imaging quality. Here we report the selection rule of scanning frequencies that can realize high definition and high frame-rate (HDHF) full-repeated Lissajous scanning imaging. The fill factor (FF) monotonically increases with the total lobe number of a Lissajous curve, i.e., the sum of scanning frequencies divided by the great common divisor (GCD) of bi-axial scanning frequencies. The frames per second (FPS), called the pattern repeated rate or the frame rate, linearly increases with GCD. HDHF Lissajous scanning is achieved at the bi-axial scanning frequencies, where the GCD has the maximum value among various sets of the scanning frequencies satisfying the total lobe number for a target FF. Based on this selection rule, the experimental results clearly demonstrate that conventional Lissajous scanners substantially increase both FF and FPS by slightly modulating the scanning frequencies at near the resonance within the resonance bandwidth of a Lissajous scanner. This selection rule provides a new guideline for HDHF Lissajous scanning in compact laser scanning systems.

Efficient use of retention time for the analysis of 302 drugs in equine plasma by liquid chromatography-MS/MS with scheduled multiple reaction monitoring and instant library searching for doping control.

PubMed

Liu, Ying; Uboh, Cornelius E; Soma, Lawrence R; Li, Xiaoqing; Guan, Fuyu; You, Youwen; Chen, Jin-Wen

2011-09-01

Multiple drug target analysis (MDTA) used in doping control is more efficient than single drug target analysis (SDTA). The number of drugs with the potential for abuse is so extensive that full coverage is not possible with SDTA. To address this problem, a liquid chromatography tandem mass spectrometric method was developed for simultaneous analysis of 302 drugs using a scheduled multiple reaction monitoring (s-MRM) algorithm. With a known retention time of an analyte, the s-MRM algorithm monitors each MRM transition only around its expected retention time. Analytes were recovered from plasma by liquid-liquid extraction. Information-dependent acquisition (IDA) functionality was used to combine s-MRM with enhanced product ion (EPI) scans within the same chromatographic analysis. An EPI spectrum library was also generated for rapid identification of analytes. Analysis time for the 302 drugs was 7 min. Scheduled MRM improved the quality of the chromatograms, signal response, reproducibility, and enhanced signal-to-noise ratio (S/N), resulting in more data points. Reduction in total cycle time from 2.4 s in conventional MRM (c-MRM) to 1 s in s-MRM allowed completion of the EPI scan at the same time. The speed for screening and identification of multiple drugs in equine plasma for doping control analysis was greatly improved by this method.

Figures of merit for laser beam quality

NASA Technical Reports Server (NTRS)

Milster, T. D.; Walker, E. P.

1993-01-01

It was shown how full-width at half maximum (FWHM), full-width at 1/e(sup 2) (FW1/e(sup 2)), Strehl ratio, and encircled energy figures of merit vary with different types of aberration and measurement methods. The array sampling method and the slit-scan method are examined in detail. Our irradiance in the exit pupil of the optical system is a simple gaussian. It was found that in general the slit-scan method and the array method do not yield the same result. The width measurements for the central lobe of the diffraction pattern are very insensitive to aberration.

Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

USGS Publications Warehouse

Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

2016-09-08

Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days preserved with HCl (1:1) to pH 2, and many are stable longer. Acrolein was retained in the method validation and initial method implementation and subsequently deleted because of instability and inconsistent performance. 2-Chloromethyl oxirane, methyl oxirane, and oxirane were tested using this method, but the compounds degraded quickly with the HCl (1:1) used for microbial preservation.The ambient purgeable method, USGS Method O-4436-16, operates with the mass spectrometer in the full scan mode. This method is a modification of USGS Method O-4127-96 (NWQL LS 2020). Several compounds were retained from Method O-4127-96 and will continue to be determined in Method O-4436-16. Eleven high priority compounds were added. MDLs for the high priority compounds range from 0.007 µg/L for 2,2-dichloro-1,1,1-trifluoroethane to 0.04 µg/L for 1,2,3,4-tetrahydronaphthalene and 1,3-butadiene. Historical MDLs for the compounds retained from Method O-4127-96 range from 0.009 µg/L for trans-1,2-dichloroethene to 0.1 µg/L for bromomethane. The calculated holding times for the compounds indicate the majority of the compounds are stable for a minimum of 14 days, or longer, at pH 2 with HCl (1:1) preservation. Four semivolatile compounds, 1,2-dimethylnaphthalene, 1,6-dimethylnaphthalene, 2,6-di-tert-butyl phenol, and 2-chloronapthalene, were tested and deleted from the method due to poor performance. Benzyl chloride was tested and deleted due to instability.

Utility of high-resolution accurate MS to eliminate interferences in the bioanalysis of ribavirin and its phosphate metabolites.

PubMed

Wei, Cong; Grace, James E; Zvyaga, Tatyana A; Drexler, Dieter M

2012-08-01

The polar nucleoside drug ribavirin (RBV) combined with IFN-α is a front-line treatment for chronic hepatitis C virus infection. RBV acts as a prodrug and exerts its broad antiviral activity primarily through its active phosphorylated metabolite ribavirin 5´-triphosphate (RTP), and also possibly through ribavirin 5´-monophosphate (RMP). To study RBV transport, diffusion, metabolic clearance and its impact on drug-metabolizing enzymes, a LC-MS method is needed to simultaneously quantify RBV and its phosphorylated metabolites (RTP, ribavirin 5´-diphosphate and RMP). In a recombinant human UGT1A1 assay, the assay buffer components uridine and its phosphorylated derivatives are isobaric with RBV and its phosphorylated metabolites, leading to significant interference when analyzed by LC-MS with the nominal mass resolution mode. Presented here is a LC-MS method employing LC coupled with full-scan high-resolution accurate MS analysis for the simultaneous quantitative determination of RBV, RMP, ribavirin 5´-diphosphate and RTP by differentiating RBV and its phosphorylated metabolites from uridine and its phosphorylated derivatives by accurate mass, thus avoiding interference. The developed LC-high-resolution accurate MS method allows for quantitation of RBV and its phosphorylated metabolites, eliminating the interferences from uridine and its phosphorylated derivatives in recombinant human UGT1A1 assays.

Highly sensitive screening method for nitroaromatic, nitramine and nitrate ester explosives by high performance liquid chromatography-atmospheric pressure ionization-mass spectrometry (HPLC-API-MS) in forensic applications.

PubMed

Xu, Xiaoma; van de Craats, Anick M; de Bruyn, Peter C A M

2004-11-01

A highly sensitive screening method based on high performance liquid chromatography atmospheric pressure ionization mass spectrometry (HPLC-API-MS) has been developed for the analysis of 21 nitroaromatic, nitramine and nitrate ester explosives, which include the explosives most commonly encountered in forensic science. Two atmospheric pressure ionization (API) methods, atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI), and various experimental conditions have been applied to allow for the detection of all 21 explosive compounds. The limit of detection (LOD) in the full-scan mode has been found to be 0.012-1.2 ng on column for the screening of most explosives investigated. For nitrobenzene, an LOD of 10 ng was found with the APCI method in the negative mode. Although the detection of nitrobenzene, 2-, 3-, and 4-nitrotoluene is hindered by the difficult ionization of these compounds, we have found that by forming an adduct with glycine, LOD values in the range of 3-16 ng on column can be achieved. Compared with previous screening methods with thermospray ionization, the API method has distinct advantages, including simplicity and stability of the method applied, an extended screening range and a low detection limit for the explosives studied.

Software for visualization, analysis, and manipulation of laser scan images

NASA Astrophysics Data System (ADS)

Burnsides, Dennis B.

1997-03-01

The recent introduction of laser surface scanning to scientific applications presents a challenge to computer scientists and engineers. Full utilization of this two- dimensional (2-D) and three-dimensional (3-D) data requires advances in techniques and methods for data processing and visualization. This paper explores the development of software to support the visualization, analysis and manipulation of laser scan images. Specific examples presented are from on-going efforts at the Air Force Computerized Anthropometric Research and Design (CARD) Laboratory.

Attenuation and image noise level based online z-axis tube current modulation for CT scans independent with localizer radiograph: simulation study and results

NASA Astrophysics Data System (ADS)

Tian, Yi; Chen, Mahao; Kong, Jun

2009-02-01

With the online z-axis tube current modulation (OZTCM) technique proposed by this work, full automatic exposure control (AEC) for CT systems could be realized with online feedback not only for angular tube current modulation (TCM) but also for z-axis TCM either. Then the localizer radiograph was not required for TCM any more. OZTCM could be implemented with 2 schemes as attenuation based μ-OZTCM and image noise level based μ-OZTCM. Respectively the maximum attenuation of projection readings and standard deviation of reconstructed images can be used to modulate the tube current level in z-axis adaptively for each half (180 degree) or full (360 degree) rotation. Simulation results showed that OZTCM achieved better noise level than constant tube current scan case by using same total dose in mAs. The OZTCM can provide optimized base tube current level for angular TCM to realize an effective auto exposure control when localizer radiograph is not available or need to be skipped for simplified scan protocol in case of emergency procedure or children scan, etc.

Required experimental accuracy to select between supersymmetrical models

NASA Astrophysics Data System (ADS)

Grellscheid, David

2004-03-01

We will present a method to decide a priori whether various supersymmetrical scenarios can be distinguished based on sparticle mass data alone. For each model, a scan over all free SUSY breaking parameters reveals the extent of that model's physically allowed region of sparticle-mass-space. Based on the geometrical configuration of these regions in mass-space, it is possible to obtain an estimate of the required accuracy of future sparticle mass measurements to distinguish between the models. We will illustrate this algorithm with an example. This talk is based on work done in collaboration with B C Allanach (LAPTH, Annecy) and F Quevedo (DAMTP, Cambridge).

Around Marshall

NASA Image and Video Library

1995-07-08

Marshall researchers, in the Astrionics lab, study rotating unbalanced mass devices. These require less power, and are lighter than current devices used for scanning images, a slice at a time. They have a wide range of space-based applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Chen; Paudel, Naba R.; Yan, Yanfa

Atom probe tomography (APT) data acquired from a CAMECA LEAP 4000 XHR for the CdS/CdTe interface for a non-CdCl 2 treated CdTe solar cell as well as the mass spectrum of an APT data set including a GB in a CdCl 2-treated CdTe solar cell are presented. Scanning electron microscopy (SEM) data showing the evolution of sample preparation for APT and scanning transmission electron microscopy (STEM) electron beam induced current (EBIC) are also presented. As a result, these data show mass spectrometry peak decomposition of Cu and Te within an APT dataset, the CdS/CdTe interface of an untreated CdTe solarmore » cell, preparation of APT needles from the CdS/CdTe interface in superstrate grown CdTe solar cells, and the preparation of a cross-sectional STEM EBIC sample.« less

Unusual Presentation of Bladder Paraganglioma: Comparison of (131)I MIBG SPECT/CT and (68)Ga DOTANOC PET/CT.

PubMed

Jain, Tarun Kumar; Basher, Rajender Kumar; Gupta, Nitin; Shukla, Jaya; Singh, Shrawan Kumar; Mittal, Bhagwant Rai

2016-01-01

Extraadrenal chromaffin cell-related tumors or paragangliomas are rare, especially in the bladder, accounting for less than 1% of cases. We report a 16-year-old boy who presented with hematuria and paroxysmal headache and was found to have a prostatic growth infiltrating the urinary bladder on anatomical imaging. Iodine-131 ((131)I) metaiodobenzylguanidine (MIBG) whole-body scanning and subsequently gallium-68 ((68)Ga) DOTANOC positron emission tomography/computed tomography (PET/CT) were performed. The MIBG scan revealed a non-tracer-avid soft-tissue mass, while DOTANOC PET/CT revealed a tracer-avid primary soft-tissue mass involving the urinary bladder and prostate with metastasis to the iliac lymph nodes. He underwent surgical management; histopathology of the surgical specimen revealed a bladder paraganglioma, whereas the prostate was found to be free of tumor.

Gynaecomastia: an unusual presenting symptom of bladder cancer.

PubMed

Ahmed, Mashrafi; Kanji, Aleem; Begum, Tahmina

2015-06-25

A 74-year-old man presented to the outpatient clinic with painful gynaecomastia. A detailed physical examination to sort out possible causes of the gynaecomastia, including intracranial tumour, liver cirrhosis, hyperthyroidism, and adrenal and testicular tumour, was negative. No offending agent was found in his medication list. A CT scan of the head and ultrasound of the scrotum did not show any mass lesion. His serum β-human chorionic gonadotropin (β-hCG) and oestradiol levels were elevated. A CT scan of the abdomen and pelvis revealed bladder wall thickening with soft tissue mass. A cystoscopic biopsy confirmed transitional cell carcinoma with muscle invasion. The patient was started on chemotherapy but responded poorly. This case report describes the β-hCG and oestradiol-secreting transitional cell carcinoma of the bladder presenting as gynaecomastia in an older man. 2015 BMJ Publishing Group Ltd.

Scanning mass spectrometry with integrated constant distance positioning

NASA Astrophysics Data System (ADS)

Li, Nan; Eckhard, Kathrin; Aßmann, Jens; Hagen, Volker; Otto, Horst; Chen, Xingxing; Schuhmann, Wolfgang; Muhler, Martin

2006-08-01

Scanning mass spectrometry is of growing importance for the characterization of catalytically active surfaces. The instrument presented here is capable of measuring catalytic activity spatially resolved by means of two concentric capillaries. The outer one is used for cofeeding reactants such as ethene and hydrogen to the sample surface, whereas the inner one is pumping off the product mixture as inlet to a quadrupole mass spectrometer. Three-dimensional measurements under stagnant-point flow conditions become possible based on a home-built capillary positioning unit. Step-motor driven positioning stages exhibiting a minimum step width of 2.5μm̸half step are used for the x, y positioning, and the step motor in z direction has a resolution of 1μm̸half step. The system is additionally equipped with a feedback loop for following the topography of the sample throughout scanning. Hence, the obtained catalytic data are unimpaired by signal changes caused by the morphology of the investigated structure. For distance control the argon ion current is used originating from externally fed argon diffusing into the confined space between the accurately positioned capillaries and the sample surface. A well-defined microchannel flow field with 400μm wide channels and 200μm wide mounds was chosen to evaluate the developed method. The catalytic activity of a Pt catalyst deposited on glassy carbon was successfully visualized in constant probe to sample distance. Simultaneously, the topography of the sample was recorded derived from the z positioning of the capillaries.

Profiling and classification of French propolis by combined multivariate data analysis of planar chromatograms and scanning direct analysis in real time mass spectra.

PubMed

Chasset, Thibaut; Häbe, Tim T; Ristivojevic, Petar; Morlock, Gertrud E

2016-09-23

Quality control of propolis is challenging, as it is a complex natural mixture of compounds, and thus, very difficult to analyze and standardize. Shown on the example of 30 French propolis samples, a strategy for an improved quality control was demonstrated in which high-performance thin-layer chromatography (HPTLC) fingerprints were evaluated in combination with selected mass signals obtained by desorption-based scanning mass spectrometry (MS). The French propolis sample extracts were separated by a newly developed reversed phase (RP)-HPTLC method. The fingerprints obtained by two different detection modes, i.e. after (1) derivatization and fluorescence detection (FLD) at UV 366nm and (2) scanning direct analysis in real time (DART)-MS, were analyzed by multivariate data analysis. Thus, RP-HPTLC-FLD and RP-HPTLC-DART-MS fingerprints were explored and the best classification was obtained using both methods in combination with pattern recognition techniques, such as principal component analysis. All investigated French propolis samples were divided in two types and characteristic patterns were observed. Phenolic compounds such as caffeic acid, p-coumaric acid, chrysin, pinobanksin, pinobanksin-3-acetate, galangin, kaempferol, tectochrysin and pinocembrin were identified as characteristic marker compounds of French propolis samples. This study expanded the research on the European poplar type of propolis and confirmed the presence of two botanically different types of propolis, known as the blue and orange types. Copyright © 2016 Elsevier B.V. All rights reserved.

Automated aortic calcification detection in low-dose chest CT images

NASA Astrophysics Data System (ADS)

Xie, Yiting; Htwe, Yu Maw; Padgett, Jennifer; Henschke, Claudia; Yankelevitz, David; Reeves, Anthony P.

2014-03-01

The extent of aortic calcification has been shown to be a risk indicator for vascular events including cardiac events. We have developed a fully automated computer algorithm to segment and measure aortic calcification in low-dose noncontrast, non-ECG gated, chest CT scans. The algorithm first segments the aorta using a pre-computed Anatomy Label Map (ALM). Then based on the segmented aorta, aortic calcification is detected and measured in terms of the Agatston score, mass score, and volume score. The automated scores are compared with reference scores obtained from manual markings. For aorta segmentation, the aorta is modeled as a series of discrete overlapping cylinders and the aortic centerline is determined using a cylinder-tracking algorithm. Then the aortic surface location is detected using the centerline and a triangular mesh model. The segmented aorta is used as a mask for the detection of aortic calcification. For calcification detection, the image is first filtered, then an elevated threshold of 160 Hounsfield units (HU) is used within the aorta mask region to reduce the effect of noise in low-dose scans, and finally non-aortic calcification voxels (bony structures, calcification in other organs) are eliminated. The remaining candidates are considered as true aortic calcification. The computer algorithm was evaluated on 45 low-dose non-contrast CT scans. Using linear regression, the automated Agatston score is 98.42% correlated with the reference Agatston score. The automated mass and volume score is respectively 98.46% and 98.28% correlated with the reference mass and volume score.

Full-thickness knee articular cartilage defects in national football league combine athletes undergoing magnetic resonance imaging: prevalence, location, and association with previous surgery.

PubMed

Nepple, Jeffrey J; Wright, Rick W; Matava, Matthew J; Brophy, Robert H

2012-06-01

To better define the prevalence and location of full-thickness articular cartilage lesions in elite football players undergoing knee magnetic resonance imaging (MRI) at the National Football League (NFL) Invitational Combine and assess the association of these lesions with previous knee surgery. We performed a retrospective review of all participants in the NFL Combine undergoing a knee MRI scan from 2005 to 2009. Each MRI scan was reviewed for evidence of articular cartilage disease. History of previous knee surgery including anterior cruciate ligament reconstruction, meniscal procedures, and articular cartilage surgery was recorded for each athlete. Knees with a history of previous articular cartilage restoration surgery were excluded from the analysis. A total of 704 knee MRI scans were included in the analysis. Full-thickness articular cartilage lesions were associated with a history of any previous knee surgery (P < .001) and, specifically, previous meniscectomy (P < .001) but not with anterior cruciate ligament reconstruction (P = .7). Full-thickness lesions were present in 27% of knees with a previous meniscectomy compared with 12% of knees without any previous meniscal surgery. Full-thickness lesions in the lateral compartment were associated with previous lateral meniscectomy (P < .001); a similar relation was seen for medial meniscus tears in the medial compartment (P = .01). Full-thickness articular cartilage lesions of the knee were present in 17.3% of elite American football players at the NFL Combine undergoing MRI. The lateral compartment appears to be at greater risk for full-thickness cartilage loss. Previous knee surgery, particularly meniscectomy, is associated with these lesions. Level IV, therapeutic case series. Copyright © 2012 Arthroscopy Association of North America. Published by Elsevier Inc. All rights reserved.

Supersonic molecular beam-hyperthermal surface ionisation coupled with time-of-flight mass spectrometry applied to trace level detection of polynuclear aromatic hydrocarbons in drinking water for reduced sample preparation and analysis time.

PubMed

Davis, S C; Makarov, A A; Hughes, J D

1999-01-01

Analysis of sub-ppb levels of polynuclear aromatic hydrocarbons (PAHs) in drinking water by high performance liquid chromatography (HPLC) fluorescence detection typically requires large water samples and lengthy extraction procedures. The detection itself, although selective, does not give compound identity confirmation. Benchtop gas chromatography/mass spectrometry (GC/MS) systems operating in the more sensitive selected ion monitoring (SIM) acquisition mode discard spectral information and, when operating in scanning mode, are less sensitive and scan too slowly. The selectivity of hyperthermal surface ionisation (HSI), the high column flow rate capacity of the supersonic molecular beam (SMB) GC/MS interface, and the high acquisition rate of time-of-flight (TOF) mass analysis, are combined here to facilitate a rapid, specific and sensitive technique for the analysis of trace levels of PAHs in water. This work reports the advantages gained by using the GC/HSI-TOF system over the HPLC fluorescence method, and discusses in some detail the nature of the instrumentation used.

Case report: retroperitoneal fibrosis simulating local relapse of sarcomatoid renal cell carcinoma.

PubMed

Esquena, Salvador; Abascal, José Maria; Trilla, Enrique; De Torres, Inés; Morote, Juan

2006-01-01

Generally, retroperitoneal fibrosis is an idiopathic process that envelopes and displaces ureters, causing hydronefrosis and renal failure. CT scan is the best choice for diagnosis. Other aetiologies described are malignancies, drugs, aorta aneurisms and immunological or rheumatological diseases. A 53-year-old male with hypertension and diabetes was operated on radical nephrectomy for renal mass. Pathological examination showed sarcomatoid renal cell carcinoma, Fürhman 3 grade, pT2 N0. Within 6 months of surgery, control CT scan demonstrated a left retroperitoneal mass, without separation with pancreas queue and spleen hilium, suggesting local relapse. Resection of the mass with splenectomy and partial pancreatectomy en bloc was performed. Microscopic evaluation revealed a dense collagenic tissue with a prominent inflammatory infiltrate, and the immunohistochemical study was negative for cytokeratin AE1-AE3. There was no evidence of malignancy in the histological examination. All these findings aided to diagnose a retroperitoneal fibrosis. Sometimes retroperitoneal fibrosis can simulate or is associated to malignancies. Presentation of a retroperitoneal fibrosis simulating local relapse of sarcomatoid renal cell carcinoma has not been previously reported in the English literature.

Phenolic profiling of the skin, pulp and seeds of Albariño grapes using hybrid quadrupole time-of-flight and triple-quadrupole mass spectrometry.

PubMed

Di Lecce, Giuseppe; Arranz, Sara; Jáuregui, Olga; Tresserra-Rimbau, Anna; Quifer-Rada, Paola; Lamuela-Raventós, Rosa M

2014-02-15

This paper describes for the first time a complete characterisation of the phenolic compounds in different anatomical parts of the Albariño grape. The application of high-performance liquid chromatography coupled with two complementary techniques, hybrid quadrupole time-of-flight and triple-quadrupole mass spectrometry, allowed the phenolic composition of the Albariño grape to be unambiguously identified and quantified. A more complete phenolic profile was obtained by product ion and precursor ion scans, while a neutral loss scan at 152 u enabled a fast screening of procyanidin dimers, trimers and their galloylated derivatives. The compounds were confirmed by accurate mass measurements in QqToF-MS and QqToF-MS/MS modes at high resolution, and good fits were obtained for all investigated ions, with errors ranging from 0.2 to 4.5 mDa. To the best of our knowledge, two flavanol monomer hexosides were detected in the grape berry for the first time. Copyright © 2013 Elsevier Ltd. All rights reserved.

Giant solitary fibrous tumor of the diaphragm: a case report and review of literature

PubMed Central

Ge, Wei; Yu, De-Cai; Jiang, Chun-Ping; Ding, Yi-Tao

2014-01-01

A young gentleman presented with difficulty in breathing. Computed tomography (CT) scan showed a huge mass located between the heart and stomach, which might have rooted in the diaphragm. Magnetic resonance imaging (MRI) with enhanced three dimensional construction showed a lobulated, heterogeneous soft tissue mass with short T1 weighted imaging signal and flake long T2-weighted imaging (T2WI). Tumor-enhanced scanning demonstrated heterogeneous contrast enhancement. The preliminary diagnosis was intra-abdominal huge mass and considering sarcoma. Resection was conducted where the base of the tumor was located in the diaphragm oppressing the left liver lobe and heart. The base of the tumor, together with partial surrounding of the diaphragm, pericardium base, and the left lateral hepatic segment, was resected. The defect in the diaphragm and pericardium was repaired by patching, and thoracic close drainage and abdominal drainage were placed following the surgical operation. The pathological report showed giant solitary fibrous tumor (SFT). This case report may provide a reference resource for the diagnosis and treatment of SFT located in the diaphragm. PMID:25674285

A new method for differentiating adducts of common drinking water DBPs from higher molecular weight DBPs in electrospray ionization-mass spectrometry analysis.

PubMed

Zhai, Hongyan; Zhang, Xiangru

2009-05-01

With the presence of bromide in source waters, numerous brominated disinfection byproducts (DBPs) are formed during chlorination. Many of them are polar/highly polar DBPs and thus hard to be detected by gas chromatography mass spectrometry. Electrospray ionization triple quadrupole mass spectrometry (ESI-MS/MS) is reported to be an effective method in finding polar brominated DBPs by setting precursor ion scans of m/z 79 and 81. But as a soft ionization technique, ESI could form adducts of common DBPs, which may complicate ESI-MS/MS spectra and hinder the efforts in finding new brominated DBPs. In this paper, a new method was developed for differentiating adducts of common DBPs from higher molecular weight DBPs. This method was based on the ESI-MS/MS precursor ion scans of the fragments that correspond to the molecular ions of common DBPs. Adducts of common DBPs were selectively detected in the ESI-MS/MS spectra of a simulated drinking water sample. Moreover, the structures of several new brominated DBPs in the sample were tentatively proposed.

Suppression of motion-induced streak artifacts along chords in fan-beam BPF-reconstructions of motion-contaminated projection data

NASA Astrophysics Data System (ADS)

King, Martin; Xia, Dan; Yu, Lifeng; Pan, Xiaochuan; Giger, Maryellen

2006-03-01

Usage of the backprojection filtration (BPF) algorithm for reconstructing images from motion-contaminated fan-beam data may result in motion-induced streak artifacts, which appear in the direction of the chords on which images are reconstructed. These streak artifacts, which are most pronounced along chords tangent to the edges of the moving object, may be suppressed by use of the weighted BPF (WBPF) algorithm, which can exploit the inherent redundancies in fan-beam data. More specifically, reconstructions using full-scan and short-scan data can allow for substantial suppression of these streaks, whereas those using reduced-scan data can allow for partial suppression. Since multiple different reconstructions of the same chord can be obtained by varying the amount of redundant data used, we have laid the groundwork for a possible method to characterize the amount of motion encoded within the data used for reconstructing an image on a particular chord. Furthermore, since motion artifacts in WBPF reconstructions using full-scan and short-scan data appear similar to those in corresponding fan-beam filtered backprojection (FFBP) reconstructions for the cases performed in this study, the BPF and WBPF algorithms potentially may be used to arrive at a more fundamental characterization of how motion artifacts appear in FFBP reconstructions.

Scan-Based Implementation of JPEG 2000 Extensions

NASA Technical Reports Server (NTRS)

Rountree, Janet C.; Webb, Brian N.; Flohr, Thomas J.; Marcellin, Michael W.

2001-01-01

JPEG 2000 Part 2 (Extensions) contains a number of technologies that are of potential interest in remote sensing applications. These include arbitrary wavelet transforms, techniques to limit boundary artifacts in tiles, multiple component transforms, and trellis-coded quantization (TCQ). We are investigating the addition of these features to the low-memory (scan-based) implementation of JPEG 2000 Part 1. A scan-based implementation of TCQ has been realized and tested, with a very small performance loss as compared with the full image (frame-based) version. A proposed amendment to JPEG 2000 Part 2 will effect the syntax changes required to make scan-based TCQ compatible with the standard.

High-Speed Automatic Microscopy for Real Time Tracks Reconstruction in Nuclear Emulsion

NASA Astrophysics Data System (ADS)

D'Ambrosio, N.

2006-06-01

The Oscillation Project with Emulsion-tRacking Apparatus (OPERA) experiment will use a massive nuclear emulsion detector to search for /spl nu//sub /spl mu///spl rarr//spl nu//sub /spl tau// oscillation by identifying /spl tau/ leptons through the direct detection of their decay topology. The feasibility of experiments using a large mass emulsion detector is linked to the impressive progress under way in the development of automatic emulsion analysis. A new generation of scanning systems requires the development of fast automatic microscopes for emulsion scanning and image analysis to reconstruct tracks of elementary particles. The paper presents the European Scanning System (ESS) developed in the framework of OPERA collaboration.

Melting point of high-purity germanium stable isotopes

NASA Astrophysics Data System (ADS)

Gavva, V. A.; Bulanov, A. D.; Kut'in, A. M.; Plekhovich, A. D.; Churbanov, M. F.

2018-05-01

The melting point (Tm) of germanium stable isotopes 72Ge, 73Ge, 74Ge, 76Ge was determined by differential scanning calorimetry. With the increase in atomic mass of isotope the decrease in Tm is observed. The decrease was equal to 0.15 °C per the unit of atomic mass which qualitatively agrees with the value calculated by Lindemann formula accounting for the effect of "isotopic compression" of elementary cell.

Virtual forensic anthropology: Novel applications of anthropometry and technology in a child death case.

PubMed

Davy-Jow, Stephanie Lynn; Lees, Duncan M B; Russell, Sean

2013-01-10

Full-body 3D virtual reconstructions were generated using 3D technology and anthropometry following the death of a young girl, allegedly from severe malnutrition as a result of abuse and neglect. Close range laser scanning, in conjunction with full colour digital texture photography, was used to document the child's condition shortly after death in order to demonstrate the number and pattern of injuries and to be able to demonstrate her condition forensically. Full-body digital reconstructions were undertaken to illustrate the extent of the malnutrition by comparing the processed post mortem scans with reconstructed images at normal weight for height and age. This is the first known instance of such an investigative tool. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Continuous-scanning laser Doppler vibrometry: Extensions to arbitrary areas, multi-frequency and 3D capture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weekes, B.; Ewins, D.; Acciavatti, F.

2014-05-27

To date, differing implementations of continuous scan laser Doppler vibrometry have been demonstrated by various academic institutions, but since the scan paths were defined using step or sine functions from function generators, the paths were typically limited to 1D line scans or 2D areas such as raster paths or Lissajous trajectories. The excitation was previously often limited to a single frequency due to the specific signal processing performed to convert the scan data into an ODS. In this paper, a configuration of continuous-scan laser Doppler vibrometry is demonstrated which permits scanning of arbitrary areas, with the benefit of allowing multi-frequency/broadbandmore » excitation. Various means of generating scan paths to inspect arbitrary areas are discussed and demonstrated. Further, full 3D vibration capture is demonstrated by the addition of a range-finding facility to the described configuration, and iteratively relocating a single scanning laser head. Here, the range-finding facility was provided by a Microsoft Kinect, an inexpensive piece of consumer electronics.« less

Membrane Vibration Studies Using a Scanning Laser Vibrometer

NASA Technical Reports Server (NTRS)

Gaspar, James L.; Solter, Micah J.; Pappa, Richard S.

2001-01-01

This paper summarizes on-going experimental work at NASA Langley Research Center to measure the dynamics of a 1.016 m (40 in.) square polyimide film Kapton membrane. A fixed fully automated impact hammer and Polytec PSV-300-H scanning laser vibrometer were used for non-contact modal testing of the membrane with zero-mass-loading. The paper discusses the results obtained by testing the membrane at various tension levels and at various excitation locations. Results obtained by direct shaker excitation to the membrane are also discussed.

A laser induced local transfer for patterning of RGB-OLED-displays

NASA Astrophysics Data System (ADS)

Kroeger, Michael; Hueske, Marc; Dobbertin, Thomas; Meyer, Jens; Krautwald, Henning; Riedl, Thomas; Johannes, Hans-Hermann; Kowalsky, Wolfgang

2005-07-01

RGB-OLED-displays can be realized by at least three different approaches: Color from white, color from blue or patterning of red, green and blue OLEDs, which is favorable for reasons of higher efficiency and lower costs. Common patterning techniques like photolithography cannot be applied due to the degradation of the OLEDs after the exposure to solvents. Shadow masking which is currently widely applied is not applicable for bigger substrate sizes of future mass production tools. Therefore a novel approach for patterning of organic semiconductors will be demonstrated. The laser induced local transfer (LILT) of organic small molecule materials allows for mass production of high resolution RGB-OLED-displays. An infrared absorbing target is coated with the desired emitting material, which is placed in a short distance in front of an OLED substrate. A scanner deflects and focuses an infrared laser beam onto the target. By adjusting scanning speed and laser power accurately the target locally heats up to a temperature where the organic material sublimes and will be deposited on the opposite OLED substrate. By repeating this for red, green and blue emitting materials a RGB-OLED-display can be realized. For process evaluation and development a LILT-module has been built, incorporating two custom vacuum chambers, several lift and transfer stages, a high-speed high-precision scanner and an infrared continuous-wave laser (cw). This module is designed to be part of a future inline deposition system for full-color OLED displays. In the first experiments it could be observed, that the pattern resolution is strongly dependent on the scanning speed, exhibiting minimum feature sizes of 40μm. It can be deducted that this is due to the laser's beam profile (TEM00), which allows for the smallest focus possible, but may not allow for rugged process conditions suitable for production. Rectangular steep-edged beam profiles may overcome this problem.