Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

PubMed

Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

2018-03-16

Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

High-throughput quantitative analysis by desorption electrospray ionization mass spectrometry.

PubMed

Manicke, Nicholas E; Kistler, Thomas; Ifa, Demian R; Cooks, R Graham; Ouyang, Zheng

2009-02-01

A newly developed high-throughput desorption electrospray ionization (DESI) source was characterized in terms of its performance in quantitative analysis. A 96-sample array, containing pharmaceuticals in various matrices, was analyzed in a single run with a total analysis time of 3 min. These solution-phase samples were examined from a hydrophobic PTFE ink printed on glass. The quantitative accuracy, precision, and limit of detection (LOD) were characterized. Chemical background-free samples of propranolol (PRN) with PRN-d(7) as internal standard (IS) and carbamazepine (CBZ) with CBZ-d(10) as IS were examined. So were two other sample sets consisting of PRN/PRN-d(7) at varying concentration in a biological milieu of 10% urine or porcine brain total lipid extract, total lipid concentration 250 ng/microL. The background-free samples, examined in a total analysis time of 1.5 s/sample, showed good quantitative accuracy and precision, with a relative error (RE) and relative standard deviation (RSD) generally less than 3% and 5%, respectively. The samples in urine and the lipid extract required a longer analysis time (2.5 s/sample) and showed RSD values of around 10% for the samples in urine and 4% for the lipid extract samples and RE values of less than 3% for both sets. The LOD for PRN and CBZ when analyzed without chemical background was 10 and 30 fmol, respectively. The LOD of PRN increased to 400 fmol analyzed in 10% urine, and 200 fmol when analyzed in the brain lipid extract.

Evaluating the efficiency of environmental monitoring programs

USGS Publications Warehouse

Levine, Carrie R.; Yanai, Ruth D.; Lampman, Gregory G.; Burns, Douglas A.; Driscoll, Charles T.; Lawrence, Gregory B.; Lynch, Jason; Schoch, Nina

2014-01-01

Statistical uncertainty analyses can be used to improve the efficiency of environmental monitoring, allowing sampling designs to maximize information gained relative to resources required for data collection and analysis. In this paper, we illustrate four methods of data analysis appropriate to four types of environmental monitoring designs. To analyze a long-term record from a single site, we applied a general linear model to weekly stream chemistry data at Biscuit Brook, NY, to simulate the effects of reducing sampling effort and to evaluate statistical confidence in the detection of change over time. To illustrate a detectable difference analysis, we analyzed a one-time survey of mercury concentrations in loon tissues in lakes in the Adirondack Park, NY, demonstrating the effects of sampling intensity on statistical power and the selection of a resampling interval. To illustrate a bootstrapping method, we analyzed the plot-level sampling intensity of forest inventory at the Hubbard Brook Experimental Forest, NH, to quantify the sampling regime needed to achieve a desired confidence interval. Finally, to analyze time-series data from multiple sites, we assessed the number of lakes and the number of samples per year needed to monitor change over time in Adirondack lake chemistry using a repeated-measures mixed-effects model. Evaluations of time series and synoptic long-term monitoring data can help determine whether sampling should be re-allocated in space or time to optimize the use of financial and human resources.

Transformation-cost time-series method for analyzing irregularly sampled data

NASA Astrophysics Data System (ADS)

Ozken, Ibrahim; Eroglu, Deniz; Stemler, Thomas; Marwan, Norbert; Bagci, G. Baris; Kurths, Jürgen

2015-06-01

Irregular sampling of data sets is one of the challenges often encountered in time-series analysis, since traditional methods cannot be applied and the frequently used interpolation approach can corrupt the data and bias the subsequence analysis. Here we present the TrAnsformation-Cost Time-Series (TACTS) method, which allows us to analyze irregularly sampled data sets without degenerating the quality of the data set. Instead of using interpolation we consider time-series segments and determine how close they are to each other by determining the cost needed to transform one segment into the following one. Using a limited set of operations—with associated costs—to transform the time series segments, we determine a new time series, that is our transformation-cost time series. This cost time series is regularly sampled and can be analyzed using standard methods. While our main interest is the analysis of paleoclimate data, we develop our method using numerical examples like the logistic map and the Rössler oscillator. The numerical data allows us to test the stability of our method against noise and for different irregular samplings. In addition we provide guidance on how to choose the associated costs based on the time series at hand. The usefulness of the TACTS method is demonstrated using speleothem data from the Secret Cave in Borneo that is a good proxy for paleoclimatic variability in the monsoon activity around the maritime continent.

Transformation-cost time-series method for analyzing irregularly sampled data.

PubMed

Ozken, Ibrahim; Eroglu, Deniz; Stemler, Thomas; Marwan, Norbert; Bagci, G Baris; Kurths, Jürgen

2015-06-01

Irregular sampling of data sets is one of the challenges often encountered in time-series analysis, since traditional methods cannot be applied and the frequently used interpolation approach can corrupt the data and bias the subsequence analysis. Here we present the TrAnsformation-Cost Time-Series (TACTS) method, which allows us to analyze irregularly sampled data sets without degenerating the quality of the data set. Instead of using interpolation we consider time-series segments and determine how close they are to each other by determining the cost needed to transform one segment into the following one. Using a limited set of operations-with associated costs-to transform the time series segments, we determine a new time series, that is our transformation-cost time series. This cost time series is regularly sampled and can be analyzed using standard methods. While our main interest is the analysis of paleoclimate data, we develop our method using numerical examples like the logistic map and the Rössler oscillator. The numerical data allows us to test the stability of our method against noise and for different irregular samplings. In addition we provide guidance on how to choose the associated costs based on the time series at hand. The usefulness of the TACTS method is demonstrated using speleothem data from the Secret Cave in Borneo that is a good proxy for paleoclimatic variability in the monsoon activity around the maritime continent.

A STRINGENT COMPARISON OF SAMPLING AND ANALYSIS METHODS FOR VOCS IN AMBIENT AIR

EPA Science Inventory

A carefully designed study was conducted during the summer of 1998 to simultaneously collect samples of ambient air by canisters and compare the analysis results to direct sorbent preconcentration results taken at the time of sample collection. A total of 32 1-h sample sets we...

Installation Restoration General Environmental Technology Development. Task 6. Materials Handling of Explosive Contaminated Soil and Sediment.

DTIC Science & Technology

1985-06-01

of chemical analysis and sensitivity testing on material samples . At this 4 time, these samples must be packaged and...preparation at a rate of three samples per hour. One analyst doing both sample preparation and the HPLC analysis can run 16 samples in an 8-hour day. II... study , sensitivity testing was reviewed to enable recommendations for complete analysis of contaminated soils. Materials handling techniques,

Rapidly differentiating grape seeds from different sources based on characteristic fingerprints using direct analysis in real time coupled with time-of-flight mass spectrometry combined with chemometrics.

PubMed

Song, Yuqiao; Liao, Jie; Dong, Junxing; Chen, Li

2015-09-01

The seeds of grapevine (Vitis vinifera) are a byproduct of wine production. To examine the potential value of grape seeds, grape seeds from seven sources were subjected to fingerprinting using direct analysis in real time coupled with time-of-flight mass spectrometry combined with chemometrics. Firstly, we listed all reported components (56 components) from grape seeds and calculated the precise m/z values of the deprotonated ions [M-H](-) . Secondly, the experimental conditions were systematically optimized based on the peak areas of total ion chromatograms of the samples. Thirdly, the seven grape seed samples were examined using the optimized method. Information about 20 grape seed components was utilized to represent characteristic fingerprints. Finally, hierarchical clustering analysis and principal component analysis were performed to analyze the data. Grape seeds from seven different sources were classified into two clusters; hierarchical clustering analysis and principal component analysis yielded similar results. The results of this study lay the foundation for appropriate utilization and exploitation of grape seed samples. Due to the absence of complicated sample preparation methods and chromatographic separation, the method developed in this study represents one of the simplest and least time-consuming methods for grape seed fingerprinting. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Spectrometer Sensitivity Investigations on the Spectrometric Oil Analysis Program.

DTIC Science & Technology

1983-04-22

31 H. ACID DISSOLUTION METHOD (ADM) ........... 90 31 I. ANALYSIS OF SAMPLES............................ 31 jJ. PARTICLE TRANSPORT EFFICIENCY OF...THE ROTATING *DISK.................................... 32 I .K. A/E35U-3 ACID DISSOLUTION METHOD.................. 32 L. BURN TIME... ACID DISSOLUTION METHOD ......... ,...,....... 95 3. EFFECT OF BURN TIME ............ 95 4. DIRECT SAMPLE INTRODUCTION .......................... 95

Electro-thermal vaporization direct analysis in real time-mass spectrometry for water contaminant analysis during space missions.

PubMed

Dwivedi, Prabha; Gazda, Daniel B; Keelor, Joel D; Limero, Thomas F; Wallace, William T; Macatangay, Ariel V; Fernández, Facundo M

2013-10-15

The development of a direct analysis in real time-mass spectrometry (DART-MS) method and first prototype vaporizer for the detection of low molecular weight (∼30-100 Da) contaminants representative of those detected in water samples from the International Space Station is reported. A temperature-programmable, electro-thermal vaporizer (ETV) was designed, constructed, and evaluated as a sampling interface for DART-MS. The ETV facilitates analysis of water samples with minimum user intervention while maximizing analytical sensitivity and sample throughput. The integrated DART-ETV-MS methodology was evaluated in both positive and negative ion modes to (1) determine experimental conditions suitable for coupling DART with ETV as a sample inlet and ionization platform for time-of-flight MS, (2) to identify analyte response ions, (3) to determine the detection limit and dynamic range for target analyte measurement, and (4) to determine the reproducibility of measurements made with the method when using manual sample introduction into the vaporizer. Nitrogen was used as the DART working gas, and the target analytes chosen for the study were ethyl acetate, acetone, acetaldehyde, ethanol, ethylene glycol, dimethylsilanediol, formaldehyde, isopropanol, methanol, methylethyl ketone, methylsulfone, propylene glycol, and trimethylsilanol.

Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

NASA Technical Reports Server (NTRS)

Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

2011-01-01

The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

Autocorrelation of location estimates and the analysis of radiotracking data

USGS Publications Warehouse

Otis, D.L.; White, Gary C.

1999-01-01

The wildlife literature has been contradictory about the importance of autocorrelation in radiotracking data used for home range estimation and hypothesis tests of habitat selection. By definition, the concept of a home range involves autocorrelated movements, but estimates or hypothesis tests based on sampling designs that predefine a time frame of interest, and that generate representative samples of an animal's movement during this time frame, should not be affected by length of the sampling interval and autocorrelation. Intensive sampling of the individual's home range and habitat use during the time frame of the study leads to improved estimates for the individual, but use of location estimates as the sample unit to compare across animals is pseudoreplication. We therefore recommend against use of habitat selection analysis techniques that use locations instead of individuals as the sample unit. We offer a general outline for sampling designs for radiotracking studies.

Measuring and mitigating inhibition during real-time, quantitative PCR analysis of viral nucleic acid extracts from large-volume environmental water samples

USDA-ARS?s Scientific Manuscript database

Naturally-occurring inhibitory compounds are a major concern during qPCR and RT-qPCR analysis of environmental samples, particularly large volume water samples. Here, a standardized method for measuring and mitigating sample inhibition in environmental water concentrates is described. Specifically, ...

Performance Evaluation of the Operational Air Quality Monitor for Water Testing Aboard the International Space Station

NASA Technical Reports Server (NTRS)

Wallace, William T.; Limero, Thomas F.; Gazda, Daniel B.; Minton, John M.; Macatangay, Ariel V.; Dwivedi, Prabha; Fernandez, Facundo M.

2014-01-01

Real-time environmental monitoring on ISS is necessary to provide data in a timely fashion and to help ensure astronaut health. Current real-time water TOC monitoring provides high-quality trending information, but compound-specific data is needed. The combination of ETV with the AQM showed that compounds of interest could be liberated from water and analyzed in the same manner as air sampling. Calibration of the AQM using water samples allowed for the quantitative analysis of ISS archival samples. Some calibration issues remain, but the excellent accuracy of DMSD indicates that ETV holds promise for as a sample introduction method for water analysis in spaceflight.

Consensus for second-order multi-agent systems with position sampled data

NASA Astrophysics Data System (ADS)

Wang, Rusheng; Gao, Lixin; Chen, Wenhai; Dai, Dameng

2016-10-01

In this paper, the consensus problem with position sampled data for second-order multi-agent systems is investigated. The interaction topology among the agents is depicted by a directed graph. The full-order and reduced-order observers with position sampled data are proposed, by which two kinds of sampled data-based consensus protocols are constructed. With the provided sampled protocols, the consensus convergence analysis of a continuous-time multi-agent system is equivalently transformed into that of a discrete-time system. Then, by using matrix theory and a sampled control analysis method, some sufficient and necessary consensus conditions based on the coupling parameters, spectrum of the Laplacian matrix and sampling period are obtained. While the sampling period tends to zero, our established necessary and sufficient conditions are degenerated to the continuous-time protocol case, which are consistent with the existing result for the continuous-time case. Finally, the effectiveness of our established results is illustrated by a simple simulation example. Project supported by the Natural Science Foundation of Zhejiang Province, China (Grant No. LY13F030005) and the National Natural Science Foundation of China (Grant No. 61501331).

Solid-phase nano-extraction and laser-excited time-resolved Shpol'skii spectroscopy for the analysis of polycyclic aromatic hydrocarbons in drinking water samples.

PubMed

Wang, Huiyong; Yu, Shenjiang; Campiglia, Andres D

2009-02-15

A unique method for screening polycyclic aromatic hydrocarbons in drinking water samples is reported. Water samples (500 microl) are mixed and centrifuged with 950 microl of a commercial solution of 20 nm gold nanoparticles for pollutants extraction. The precipitate is treated with 2 microl of 1-pentanethiol and 48 microl of n-octane, and the supernatant is then analyzed via laser-excited time-resolved Shpol'skii spectroscopy. Fifteen priority pollutants are directly determined at liquid helium temperature (4.2 K) with the aid of a cryogenic fiber-optic probe. Unambiguous pollutant determination is carried out via spectral and lifetime analysis. Limits of detection are at the parts-per-trillion level. Analytical recoveries are similar to those obtained via high-performance liquid chromatography. The simplicity of the experimental procedure, use of microliters of organic solvent, short analysis time, selectivity, and excellent analytical figures of merit demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

Gender Differentiation in the New York "Times": 1885 and 1985.

ERIC Educational Resources Information Center

Jolliffe, Lee

A study examined the descriptive language and sex-linked roles ascribed to women and men in articles of the New York "Times" from 1885 and 1985. Seven content analysis methods were applied to four random samples from the "Times"; one sample each for women and men from both years. Samples were drawn using randomly constructed…

Rapid DNA analysis for automated processing and interpretation of low DNA content samples.

PubMed

Turingan, Rosemary S; Vasantgadkar, Sameer; Palombo, Luke; Hogan, Catherine; Jiang, Hua; Tan, Eugene; Selden, Richard F

2016-01-01

Short tandem repeat (STR) analysis of casework samples with low DNA content include those resulting from the transfer of epithelial cells from the skin to an object (e.g., cells on a water bottle, or brim of a cap), blood spatter stains, and small bone and tissue fragments. Low DNA content (LDC) samples are important in a wide range of settings, including disaster response teams to assist in victim identification and family reunification, military operations to identify friend or foe, criminal forensics to identify suspects and exonerate the innocent, and medical examiner and coroner offices to identify missing persons. Processing LDC samples requires experienced laboratory personnel, isolated workstations, and sophisticated equipment, requires transport time, and involves complex procedures. We present a rapid DNA analysis system designed specifically to generate STR profiles from LDC samples in field-forward settings by non-technical operators. By performing STR in the field, close to the site of collection, rapid DNA analysis has the potential to increase throughput and to provide actionable information in real time. A Low DNA Content BioChipSet (LDC BCS) was developed and manufactured by injection molding. It was designed to function in the fully integrated Accelerated Nuclear DNA Equipment (ANDE) instrument previously designed for analysis of buccal swab and other high DNA content samples (Investigative Genet. 4(1):1-15, 2013). The LDC BCS performs efficient DNA purification followed by microfluidic ultrafiltration of the purified DNA, maximizing the quantity of DNA available for subsequent amplification and electrophoretic separation and detection of amplified fragments. The system demonstrates accuracy, precision, resolution, signal strength, and peak height ratios appropriate for casework analysis. The LDC rapid DNA analysis system is effective for the generation of STR profiles from a wide range of sample types. The technology broadens the range of sample types that can be processed and minimizes the time between sample collection, sample processing and analysis, and generation of actionable intelligence. The fully integrated Expert System is capable of interpreting a wide range or sample types and input DNA quantities, allowing samples to be processed and interpreted without a technical operator.

GET electronics samples data analysis

NASA Astrophysics Data System (ADS)

Giovinazzo, J.; Goigoux, T.; Anvar, S.; Baron, P.; Blank, B.; Delagnes, E.; Grinyer, G. F.; Pancin, J.; Pedroza, J. L.; Pibernat, J.; Pollacco, E.; Rebii, A.; Roger, T.; Sizun, P.

2016-12-01

The General Electronics for TPCs (GET) has been developed to equip a generation of time projection chamber detectors for nuclear physics, and may also be used for a wider range of detector types. The goal of this paper is to propose first analysis procedures to be applied on raw data samples from the GET system, in order to correct for systematic effects observed on test measurements. We also present a method to estimate the response function of the GET system channels. The response function is required in analysis where the input signal needs to be reconstructed, in terms of time distribution, from the registered output samples.

Soil Gas Sample Handling: Evaluation of Water Removal and Sample Ganging

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

Fritz, Brad G.; Abrecht, David G.; Hayes, James C.

2016-10-31

Soil gas sampling is currently conducted in support of Nuclear Test Ban treaty verification. Soil gas samples are collected and analyzed for isotopes of interest. Some issues that can impact sampling and analysis of these samples are excess moisture and sample processing time. Here we discuss three potential improvements to the current sampling protocol; a desiccant for water removal, use of molecular sieve to remove CO 2 from the sample during collection, and a ganging manifold to allow composite analysis of multiple samples.

Multimodal optical analysis discriminates freshly extracted human sample of gliomas, metastases and meningiomas from their appropriate controls

NASA Astrophysics Data System (ADS)

Zanello, Marc; Poulon, Fanny; Pallud, Johan; Varlet, Pascale; Hamzeh, H.; Abi Lahoud, Georges; Andreiuolo, Felipe; Ibrahim, Ali; Pages, Mélanie; Chretien, Fabrice; di Rocco, Federico; Dezamis, Edouard; Nataf, François; Turak, Baris; Devaux, Bertrand; Abi Haidar, Darine

2017-02-01

Delineating tumor margins as accurately as possible is of primordial importance in surgical oncology: extent of resection is associated with survival but respect of healthy surrounding tissue is necessary for preserved quality of life. The real-time analysis of the endogeneous fluorescence signal of brain tissues is a promising tool for defining margins of brain tumors. The present study aims to demonstrate the feasibility of multimodal optical analysis to discriminate fresh samples of gliomas, metastases and meningiomas from their appropriate controls. Tumor samples were studied on an optical fibered endoscope using spectral and fluorescence lifetime analysis and then on a multimodal set-up for acquiring spectral, one and two-photon fluorescence images, second harmonic generation signals and two-photon fluorescence lifetime datasets. The obtained data allowed us to differentiate healthy samples from tumor samples. These results confirmed the possible clinical relevance of this real-time multimodal optical analysis. This technique can be easily applied to neurosurgical procedures for a better delineation of surgical margins.

Laboratory Spectrometer for Wear Metal Analysis of Engine Lubricants.

DTIC Science & Technology

1986-04-01

analysis, the acid digestion technique for sample pretreatment is the best approach available to date because of its relatively large sample size (1000...microliters or more). However, this technique has two major shortcomings limiting its application: (1) it requires the use of hydrofluoric acid (a...accuracy. Sample preparation including filtration or acid digestion may increase analysis times by 20 minutes or more. b. Repeatability In the analysis

In situ laser annealing system for real-time surface kinetic analysis

NASA Astrophysics Data System (ADS)

Wang, Q.; Sun, Y.-M.; Zhao, W.; Campagna, J.; White, J. M.

2002-11-01

For real-time analysis during thermal annealing, a continuous wave CO2 infrared laser was coupled to a surface analysis system equipped for x-ray photoelectron spectroscopy (XPS) and ion scattering spectroscopy (ISS). The laser beam was directed into the vacuum chamber through a ZnSe window to the back side of the sample. With 10 W laser output, the sample temperature reached 563 K. The chamber remained below 10-8 Torr during annealing and allowed XPS and ISS data to be gathered as a function of time at selected temperatures. As a test example, real time Cu2O reduction at 563 K was investigated.

When continuous observations just won't do: developing accurate and efficient sampling strategies for the laying hen.

PubMed

Daigle, Courtney L; Siegford, Janice M

2014-03-01

Continuous observation is the most accurate way to determine animals' actual time budget and can provide a 'gold standard' representation of resource use, behavior frequency, and duration. Continuous observation is useful for capturing behaviors that are of short duration or occur infrequently. However, collecting continuous data is labor intensive and time consuming, making multiple individual or long-term data collection difficult. Six non-cage laying hens were video recorded for 15 h and behavioral data collected every 2 s were compared with data collected using scan sampling intervals of 5, 10, 15, 30, and 60 min and subsamples of 2 second observations performed for 10 min every 30 min, 15 min every 1 h, 30 min every 1.5 h, and 15 min every 2 h. Three statistical approaches were used to provide a comprehensive analysis to examine the quality of the data obtained via different sampling methods. General linear mixed models identified how the time budget from the sampling techniques differed from continuous observation. Correlation analysis identified how strongly results from the sampling techniques were associated with those from continuous observation. Regression analysis identified how well the results from the sampling techniques were associated with those from continuous observation, changes in magnitude, and whether a sampling technique had bias. Static behaviors were well represented with scan and time sampling techniques, while dynamic behaviors were best represented with time sampling techniques. Methods for identifying an appropriate sampling strategy based upon the type of behavior of interest are outlined and results for non-caged laying hens are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of drugs and drug-like compounds in different samples with direct analysis in real time mass spectrometry.

PubMed

Chernetsova, Elena S; Morlock, Gertrud E

2011-01-01

Direct analysis in real time (DART), a relatively new ionization source for mass spectrometry, ionizes small-molecule components from different kinds of samples without any sample preparation and chromatographic separation. The current paper reviews the published data available on the determination of drugs and drug-like compounds in different matrices with DART-MS, including identification and quantitation issues. Parameters that affect ionization efficiency and mass spectra composition are also discussed. Copyright © 2011 Wiley Periodicals, Inc.

Sample preparation techniques for the determination of trace residues and contaminants in foods.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2007-06-15

The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

[Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

PubMed

Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

2014-03-01

Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

Gas-phase detection of solid-state fission product complexes for post-detonation nuclear forensic analysis

DOE PAGES

Stratz, S. Adam; Jones, Steven A.; Oldham, Colton J.; ...

2016-06-27

This study presents the first known detection of fission products commonly found in post-detonation nuclear debris samples using solid sample introduction and a uniquely coupled gas chromatography inductively-coupled plasma time-of-flight mass spectrometer. Rare earth oxides were chemically altered to incorporate a ligand that enhances the volatility of the samples. These samples were injected (as solids) into the aforementioned instrument and detected for the first time. Repeatable results indicate the validity of the methodology, and this capability, when refined, will prove to be a valuable asset for rapid post-detonation nuclear forensic analysis.

Gas-phase detection of solid-state fission product complexes for post-detonation nuclear forensic analysis

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

Stratz, S. Adam; Jones, Steven A.; Oldham, Colton J.

This study presents the first known detection of fission products commonly found in post-detonation nuclear debris samples using solid sample introduction and a uniquely coupled gas chromatography inductively-coupled plasma time-of-flight mass spectrometer. Rare earth oxides were chemically altered to incorporate a ligand that enhances the volatility of the samples. These samples were injected (as solids) into the aforementioned instrument and detected for the first time. Repeatable results indicate the validity of the methodology, and this capability, when refined, will prove to be a valuable asset for rapid post-detonation nuclear forensic analysis.

Detectability of Granger causality for subsampled continuous-time neurophysiological processes.

PubMed

Barnett, Lionel; Seth, Anil K

2017-01-01

Granger causality is well established within the neurosciences for inference of directed functional connectivity from neurophysiological data. These data usually consist of time series which subsample a continuous-time biophysiological process. While it is well known that subsampling can lead to imputation of spurious causal connections where none exist, less is known about the effects of subsampling on the ability to reliably detect causal connections which do exist. We present a theoretical analysis of the effects of subsampling on Granger-causal inference. Neurophysiological processes typically feature signal propagation delays on multiple time scales; accordingly, we base our analysis on a distributed-lag, continuous-time stochastic model, and consider Granger causality in continuous time at finite prediction horizons. Via exact analytical solutions, we identify relationships among sampling frequency, underlying causal time scales and detectability of causalities. We reveal complex interactions between the time scale(s) of neural signal propagation and sampling frequency. We demonstrate that detectability decays exponentially as the sample time interval increases beyond causal delay times, identify detectability "black spots" and "sweet spots", and show that downsampling may potentially improve detectability. We also demonstrate that the invariance of Granger causality under causal, invertible filtering fails at finite prediction horizons, with particular implications for inference of Granger causality from fMRI data. Our analysis emphasises that sampling rates for causal analysis of neurophysiological time series should be informed by domain-specific time scales, and that state-space modelling should be preferred to purely autoregressive modelling. On the basis of a very general model that captures the structure of neurophysiological processes, we are able to help identify confounds, and offer practical insights, for successful detection of causal connectivity from neurophysiological recordings. Copyright © 2016 Elsevier B.V. All rights reserved.

It's Time to Develop a New "Draft Test Protocol" for a Mars Sample Return Mission (or Two....)

NASA Astrophysics Data System (ADS)

Rummel, J. D.

2018-04-01

A Mars Sample Return (MSR) will involve analysis of those samples in containment, including their safe receiving, handling, testing, and archiving. With an MSR planned for the end of the next decade, it is time to update the existing MSR protocol.

Potential Use of Passive Sampling for Environmental Monitoring of Petroleum E&P Operations

EPA Pesticide Factsheets

Traditional environmental monitoring relies on water or soil samples being taken at various time increments and sent to offsite laboratories for analysis. Reliance on grab samples generally captures limited “snapshots” of environmental contaminant concentrations, is time intensive, costly, and generates residual waste from excess sample and/or reagents used in the analysis procedures. As an alternative, we are evaluating swellable organosilica sorbents to create passive sampling systems for monitoring applications. Previous work has focused on absorption and detection of fuels, chlorinated solvents, endocrine disruptors, explosives, pesticides, fluorinated chemicals, and metals including Ba, Sr, Hg, Pb, Fe, Cu, and Zn. The advantages of swellable organosilica are that the material cancapture target compounds for an extended periods of time, does not absorb natural organic matter, and resists biofilm formation since the sorbent possesses an animated surface morphology.

Analysis of Ballast Water Sampling Port Designs Using Computational Fluid Dynamics

DTIC Science & Technology

2008-02-01

straight, vertical, upward-flowing pipe having a sample port diameter between 1.5 and 2.0 times the basic isokinetic diameter as defined in this report...water, flow modeling, sample port, sample pipe, particle trajectory, isokinetic sampling 18. Distribution Statement This document is available to...2.0 times the basic isokinetic diameter as defined in this report. Sample ports should use ball valves for isolation purposes and diaphragm or

Sampling design for groundwater solute transport: Tests of methods and analysis of Cape Cod tracer test data

USGS Publications Warehouse

Knopman, Debra S.; Voss, Clifford I.; Garabedian, Stephen P.

1991-01-01

Tests of a one-dimensional sampling design methodology on measurements of bromide concentration collected during the natural gradient tracer test conducted by the U.S. Geological Survey on Cape Cod, Massachusetts, demonstrate its efficacy for field studies of solute transport in groundwater and the utility of one-dimensional analysis. The methodology was applied to design of sparse two-dimensional networks of fully screened wells typical of those often used in engineering practice. In one-dimensional analysis, designs consist of the downstream distances to rows of wells oriented perpendicular to the groundwater flow direction and the timing of sampling to be carried out on each row. The power of a sampling design is measured by its effectiveness in simultaneously meeting objectives of model discrimination, parameter estimation, and cost minimization. One-dimensional models of solute transport, differing in processes affecting the solute and assumptions about the structure of the flow field, were considered for description of tracer cloud migration. When fitting each model using nonlinear regression, additive and multiplicative error forms were allowed for the residuals which consist of both random and model errors. The one-dimensional single-layer model of a nonreactive solute with multiplicative error was judged to be the best of those tested. Results show the efficacy of the methodology in designing sparse but powerful sampling networks. Designs that sample five rows of wells at five or fewer times in any given row performed as well for model discrimination as the full set of samples taken up to eight times in a given row from as many as 89 rows. Also, designs for parameter estimation judged to be good by the methodology were as effective in reducing the variance of parameter estimates as arbitrary designs with many more samples. Results further showed that estimates of velocity and longitudinal dispersivity in one-dimensional models based on data from only five rows of fully screened wells each sampled five or fewer times were practically equivalent to values determined from moments analysis of the complete three-dimensional set of 29,285 samples taken during 16 sampling times.

Imaging systems and algorithms to analyze biological samples in real-time using mobile phone microscopy.

PubMed

Shanmugam, Akshaya; Usmani, Mohammad; Mayberry, Addison; Perkins, David L; Holcomb, Daniel E

2018-01-01

Miniaturized imaging devices have pushed the boundaries of point-of-care imaging, but existing mobile-phone-based imaging systems do not exploit the full potential of smart phones. This work demonstrates the use of simple imaging configurations to deliver superior image quality and the ability to handle a wide range of biological samples. Results presented in this work are from analysis of fluorescent beads under fluorescence imaging, as well as helminth eggs and freshwater mussel larvae under white light imaging. To demonstrate versatility of the systems, real time analysis and post-processing results of the sample count and sample size are presented in both still images and videos of flowing samples.

Sampling of Stochastic Input Parameters for Rockfall Calculations and for Structural Response Calculations Under Vibratory Ground Motion

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

M. Gross

2004-09-01

The purpose of this scientific analysis is to define the sampled values of stochastic (random) input parameters for (1) rockfall calculations in the lithophysal and nonlithophysal zones under vibratory ground motions, and (2) structural response calculations for the drip shield and waste package under vibratory ground motions. This analysis supplies: (1) Sampled values of ground motion time history and synthetic fracture pattern for analysis of rockfall in emplacement drifts in nonlithophysal rock (Section 6.3 of ''Drift Degradation Analysis'', BSC 2004 [DIRS 166107]); (2) Sampled values of ground motion time history and rock mechanical properties category for analysis of rockfall inmore » emplacement drifts in lithophysal rock (Section 6.4 of ''Drift Degradation Analysis'', BSC 2004 [DIRS 166107]); (3) Sampled values of ground motion time history and metal to metal and metal to rock friction coefficient for analysis of waste package and drip shield damage to vibratory motion in ''Structural Calculations of Waste Package Exposed to Vibratory Ground Motion'' (BSC 2004 [DIRS 167083]) and in ''Structural Calculations of Drip Shield Exposed to Vibratory Ground Motion'' (BSC 2003 [DIRS 163425]). The sampled values are indices representing the number of ground motion time histories, number of fracture patterns and rock mass properties categories. These indices are translated into actual values within the respective analysis and model reports or calculations. This report identifies the uncertain parameters and documents the sampled values for these parameters. The sampled values are determined by GoldSim V6.04.007 [DIRS 151202] calculations using appropriate distribution types and parameter ranges. No software development or model development was required for these calculations. The calculation of the sampled values allows parameter uncertainty to be incorporated into the rockfall and structural response calculations that support development of the seismic scenario for the Total System Performance Assessment for the License Application (TSPA-LA). The results from this scientific analysis also address project requirements related to parameter uncertainty, as specified in the acceptance criteria in ''Yucca Mountain Review Plan, Final Report'' (NRC 2003 [DIRS 163274]). This document was prepared under the direction of ''Technical Work Plan for: Regulatory Integration Modeling of Drift Degradation, Waste Package and Drip Shield Vibratory Motion and Seismic Consequences'' (BSC 2004 [DIRS 170528]) which directed the work identified in work package ARTM05. This document was prepared under procedure AP-SIII.9Q, ''Scientific Analyses''. There are no specific known limitations to this analysis.« less

LIBS: a potential tool for industrial/agricultural waste water analysis

NASA Astrophysics Data System (ADS)

Karpate, Tanvi; K. M., Muhammed Shameem; Nayak, Rajesh; V. K., Unnikrishnan; Santhosh, C.

2016-04-01

Laser Induced Breakdown Spectroscopy (LIBS) is a multi-elemental analysis technique with various advantages and has the ability to detect any element in real time. This technique holds a potential for environmental monitoring and various such analysis has been done in soil, glass, paint, water, plastic etc confirms the robustness of this technique for such applications. Compared to the currently available water quality monitoring methods and techniques, LIBS has several advantages, viz. no need for sample preparation, fast and easy operation, and chemical free during the process. In LIBS, powerful pulsed laser generates plasma which is then analyzed to get quantitative and qualitative details of the elements present in the sample. Another main advantage of LIBS technique is that it can perform in standoff mode for real time analysis. Water samples from industries and agricultural strata tend to have a lot of pollutants making it harmful for consumption. The emphasis of this project is to determine such harmful pollutants present in trace amounts in industrial and agricultural wastewater. When high intensity laser is made incident on the sample, a plasma is generated which gives a multielemental emission spectra. LIBS analysis has shown outstanding success for solids samples. For liquid samples, the analysis is challenging as the liquid sample has the chances of splashing due to the high energy of laser and thus making it difficult to generate plasma. This project also deals with determining the most efficient method for testing of water sample for qualitative as well as quantitative analysis using LIBS.

Quantitation of Mycotoxins Using Direct Analysis in Real Time Mass Spectrometry (DART-MS).

PubMed

Busman, Mark

2018-05-01

Ambient ionization represents a new generation of MS ion sources and is used for the rapid ionization of small molecules under ambient conditions. The combination of ambient ionization and MS allows the analysis of multiple food samples with simple or no sample treatment or in conjunction with prevailing sample preparation methods. Two ambient ionization methods, desorptive electrospray ionization (DESI) and direct analysis in real time (DART) have been adapted for food safety application. Both ionization techniques provide unique advantages and capabilities. DART has been used for a variety of qualitative and quantitative applications. In particular, mycotoxin contamination of food and feed materials has been addressed by DART-MS. Applications to mycotoxin analysis by ambient ionization MS and particularly DART-MS are summarized.

Stochastic Stability of Sampled Data Systems with a Jump Linear Controller

NASA Technical Reports Server (NTRS)

Gonzalez, Oscar R.; Herencia-Zapana, Heber; Gray, W. Steven

2004-01-01

In this paper an equivalence between the stochastic stability of a sampled-data system and its associated discrete-time representation is established. The sampled-data system consists of a deterministic, linear, time-invariant, continuous-time plant and a stochastic, linear, time-invariant, discrete-time, jump linear controller. The jump linear controller models computer systems and communication networks that are subject to stochastic upsets or disruptions. This sampled-data model has been used in the analysis and design of fault-tolerant systems and computer-control systems with random communication delays without taking into account the inter-sample response. This paper shows that the known equivalence between the stability of a deterministic sampled-data system and the associated discrete-time representation holds even in a stochastic framework.

Online-LASIL: Laser Ablation of Solid Samples in Liquid with online-coupled ICP-OES detection for direct determination of the stoichiometry of complex metal oxide thin layers.

PubMed

Bonta, Maximilian; Frank, Johannes; Taibl, Stefanie; Fleig, Jürgen; Limbeck, Andreas

2018-02-13

Advanced materials such as complex metal oxides are used in a wide range of applications and have further promising perspectives in the form of thin films. The exact chemical composition essentially influences the electronic properties of these materials which makes correct assessment of their composition necessary. However, due to high chemical resistance and in the case of thin films low absolute analyte amounts, this procedure is in most cases not straightforward and extremely time-demanding. Commonly applied techniques either lack in ease of use (i.e., solution-based analysis with preceding sample dissolution), or adequately accurate quantification (i.e., solid sampling techniques). An analysis approach which combines the beneficial aspects of solution-based analysis as well as direct solid sampling is Laser Ablation of a Sample in Liquid (LASIL). In this work, it is shown that the analysis of major as well as minor sample constituents is possible using a novel online-LASIL setup, allowing sample analysis without manual sample handling after placing it in an ablation chamber. Strontium titanate (STO) thin layers with different compositions were analyzed in the course of this study. Precision of the newly developed online-LASIL method is comparable to conventional wet chemical approaches. With only about 15-20 min required for the analysis per sample, time demand is significantly reduced compared to often necessary fusion procedures lasting multiple hours. Copyright © 2017 Elsevier B.V. All rights reserved.

Sampling and sample processing in pesticide residue analysis.

PubMed

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Improving Efficiency with Work Sampling.

ERIC Educational Resources Information Center

Friedman, Mark; Hertz, Paul

1982-01-01

Work sampling is a managerial accounting technique which provides information about the efficiency of an operation. This analysis determines what tasks are being performed durinq a period of time to ascertain if time and effort are being allocated efficiently. (SK)

An Improved Manual Method for NOx Emission Measurement.

ERIC Educational Resources Information Center

Dee, L. A.; And Others

The current manual NO (x) sampling and analysis method was evaluated. Improved time-integrated sampling and rapid analysis methods were developed. In the new method, the sample gas is drawn through a heated bed of uniquely active, crystalline, Pb02 where NO (x) is quantitatively absorbed. Nitrate ion is later extracted with water and the…

Contamination Knowledge Strategy for the Mars 2020 Sample-Collecting Rover

NASA Technical Reports Server (NTRS)

Farley, K. A.; Williford, K.; Beaty, D W.; McSween, H. Y.; Czaja, A. D.; Goreva, Y. S.; Hausrath, E.; Herd, C. D. K.; Humayun, M.; McCubbin, F. M.;

Thermogravimetric analysis for the determination of water release rate from microcrystalline cellulose dry powder and wet bead systems.

PubMed

Mayville, Francis C; Wigent, Rodney J; Schwartz, Joseph B

2006-01-01

The purpose of this work was to determine the total amount of water contained in dry powder and wet bead samples of microcrystalline cellulose, MCC, (Avicel PH-101), taken from various stages of the extrusion/marumerization process used to make beads and to determine the kinetic rates of water release from each sample. These samples were allowed to equilibrate in controlled humidity chambers at 25 degrees C. The total amount of water in each sample, after equilibration, was determined by thermogravimetric analysis (TGA) as a function of temperature. The rates of water release from these samples were determined by using isothermal gravimetric analysis (ITGA) as a function of time. Analysis of the results for these studies suggest that water was released from these systems by several different kinetic mechanisms. The water release mechanisms for these systems include: zero order, second order, and diffusion controlled kinetics. It is believed that all three kinetic mechanisms will occur at the same time, however; only one mechanism will be prominent. The prominent mechanism was based on the amount of water present in the sample.

The Impact of Rendered Protein Meal Oxidation Level on Shelf-Life, Sensory Characteristics, and Acceptability in Extruded Pet Food

PubMed Central

Chanadang, Sirichat; Koppel, Kadri; Aldrich, Greg

2016-01-01

Simple Summary Sensory analysis was used to determine the changes due to the storage time on extruded pet food prepared from two different rendered protein meals: (i) beef meat and bone meal (BMBM); (ii) chicken byproduct meal (CPBM). Extrusion is a process where feed is pressed through a die in order to create shapes and increase digestibility. Descriptive sensory analysis using a human panel found an increase in undesirable sensory attributes (e.g., oxidized oil, rancid) in extruded pet food over storage time, especially the one prepared from chicken by product meal without antioxidants. The small increase in oxidized and rancid aromas of BMBM samples did not affect pet owners’ acceptability of the products. CPBM samples without antioxidants showed a notable increase in oxidized and rancid aroma over storage time and, thus, affected product acceptability negatively. This finding indicated that human sensory analysis can be used as a tool to track the changes of pet food characteristics due to storage, as well as estimate the shelf-life of the products. Abstract Pet foods are expected to have a shelf-life for 12 months or more. Sensory analysis can be used to determine changes in products and to estimate products’ shelf-life. The objectives of this study were to (1) investigate how increasing levels of oxidation in rendered protein meals used to produce extruded pet food affected the sensory properties and (2) determine the effect of shelf-life on pet owners’ acceptability of extruded pet food diet formulated without the use of preservative. Pet food diets contained beef meat bone meal (BMBM) and chicken byproduct meal (CBPM) in which the oxidation was retarded with ethoxyquin, mixed tocopherols, or none at all, and then extruded into dry pet foods. These samples represented low, medium, and high oxidation levels, respectively. Samples were stored for 0, 3, 6, 9, and 12 months at ambient temperature. Each time point, samples were evaluated by six highly trained descriptive panelists for sensory attributes related to oxidation. Samples without preservatives were chosen for the acceptability test, since the differences in sensory characteristics over storage time were more distinguishable in those samples. Pet owners evaluated samples for aroma, appearance and overall liking. Descriptive sensory analysis detected significant changes in oxidized-related sensory characteristics over storage time. However, the differences for CBPM samples were more pronounced and directional. The consumer study showed no differences in pet owners’ acceptability for BMBM samples. However, the noticeable increase in aroma characteristics (rancid aroma 0.33–4.21) in CBPM samples over storage time did have a negative effect on consumer’s liking (overall liking 5.52–4.95). PMID:27483326

Effect of ambient temperature storage on potable water coliform population estimations.

PubMed Central

Standridge, J H; Delfino, J J

1983-01-01

The effect of the length of time between sampling potable water and performing coliform analyses has been a long-standing controversial issue in environmental microbiology. The issue is of practical importance since reducing the sample-to-analysis time may substantially increase costs for water analysis programs. Randomly selected samples (from those routinely collected throughout the State of Wisconsin) were analyzed for total coliforms after being held at room temperature (20 +/- 2 degrees C) for 24 and 48 h. Differences in results for the two holding times were compared with differences predicted by probability calculations. The study showed that storage of the potable water for up to 48 h had little effect on the public health significance of most samples containing more than two coliforms per 100 ml. PMID:6651296

Broadband terahertz time-domain spectroscopy of drugs-of-abuse and the use of principal component analysis.

PubMed

Burnett, Andrew D; Fan, Wenhui; Upadhya, Prashanth C; Cunningham, John E; Hargreaves, Michael D; Munshi, Tasnim; Edwards, Howell G M; Linfield, Edmund H; Davies, A Giles

2009-08-01

Terahertz frequency time-domain spectroscopy has been used to analyse a wide range of samples containing cocaine hydrochloride, heroin and ecstasy--common drugs-of-abuse. We investigated real-world samples seized by law enforcement agencies, together with pure drugs-of-abuse, and pure drugs-of-abuse systematically adulterated in the laboratory to emulate real-world samples. In order to investigate the feasibility of automatic spectral recognition of such illicit materials by terahertz spectroscopy, principal component analysis was employed to cluster spectra of similar compounds.

Generalized sample entropy analysis for traffic signals based on similarity measure

NASA Astrophysics Data System (ADS)

Shang, Du; Xu, Mengjia; Shang, Pengjian

2017-05-01

Sample entropy is a prevailing method used to quantify the complexity of a time series. In this paper a modified method of generalized sample entropy and surrogate data analysis is proposed as a new measure to assess the complexity of a complex dynamical system such as traffic signals. The method based on similarity distance presents a different way of signals patterns match showing distinct behaviors of complexity. Simulations are conducted over synthetic data and traffic signals for providing the comparative study, which is provided to show the power of the new method. Compared with previous sample entropy and surrogate data analysis, the new method has two main advantages. The first one is that it overcomes the limitation about the relationship between the dimension parameter and the length of series. The second one is that the modified sample entropy functions can be used to quantitatively distinguish time series from different complex systems by the similar measure.

Study of the Effect of Temporal Sampling Frequency on DSCOVR Observations Using the GEOS-5 Nature Run Results. Part II; Cloud Coverage

NASA Technical Reports Server (NTRS)

Holdaway, Daniel; Yang, Yuekui

2016-01-01

This is the second part of a study on how temporal sampling frequency affects satellite retrievals in support of the Deep Space Climate Observatory (DSCOVR) mission. Continuing from Part 1, which looked at Earth's radiation budget, this paper presents the effect of sampling frequency on DSCOVR-derived cloud fraction. The output from NASA's Goddard Earth Observing System version 5 (GEOS-5) Nature Run is used as the "truth". The effect of temporal resolution on potential DSCOVR observations is assessed by subsampling the full Nature Run data. A set of metrics, including uncertainty and absolute error in the subsampled time series, correlation between the original and the subsamples, and Fourier analysis have been used for this study. Results show that, for a given sampling frequency, the uncertainties in the annual mean cloud fraction of the sunlit half of the Earth are larger over land than over ocean. Analysis of correlation coefficients between the subsamples and the original time series demonstrates that even though sampling at certain longer time intervals may not increase the uncertainty in the mean, the subsampled time series is further and further away from the "truth" as the sampling interval becomes larger and larger. Fourier analysis shows that the simulated DSCOVR cloud fraction has underlying periodical features at certain time intervals, such as 8, 12, and 24 h. If the data is subsampled at these frequencies, the uncertainties in the mean cloud fraction are higher. These results provide helpful insights for the DSCOVR temporal sampling strategy.

Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

PubMed

Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

2017-11-24

Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements. Copyright © 2017 Elsevier B.V. All rights reserved.

Miniaturized and direct spectrophotometric multi-sample analysis of trace metals in natural waters.

PubMed

Albendín, Gemma; López-López, José A; Pinto, Juan J

2016-03-15

Trends in the analysis of trace metals in natural waters are mainly based on the development of sample treatment methods to isolate and pre-concentrate the metal from the matrix in a simpler extract for further instrumental analysis. However, direct analysis is often possible using more accessible techniques such as spectrophotometry. In this case a proper ligand is required to form a complex that absorbs radiation in the ultraviolet-visible (UV-Vis) spectrum. In this sense, the hydrazone derivative, di-2-pyridylketone benzoylhydrazone (dPKBH), forms complexes with copper (Cu) and vanadium (V) that absorb light at 370 and 395 nm, respectively. Although spectrophotometric methods are considered as time- and reagent-consuming, this work focused on its miniaturization by reducing the volume of sample as well as time and cost of analysis. In both methods, a micro-amount of sample is placed into a microplate reader with a capacity for 96 samples, which can be analyzed in times ranging from 5 to 10 min. The proposed methods have been optimized using a Box-Behnken design of experiments. For Cu determination, concentration of phosphate buffer solution at pH 8.33, masking agents (ammonium fluoride and sodium citrate), and dPKBH were optimized. For V analysis, sample (pH 4.5) was obtained using acetic acid/sodium acetate buffer, and masking agents were ammonium fluoride and 1,2-cyclohexanediaminetetraacetic acid. Under optimal conditions, both methods were applied to the analysis of certified reference materials TMDA-62 (lake water), LGC-6016 (estuarine water), and LGC-6019 (river water). In all cases, results proved the accuracy of the method. Copyright © 2015 Elsevier Inc. All rights reserved.

SAMPLING AND ANALYSIS OF SEMIVOLATILE AEROSOLS

EPA Science Inventory

Denuder based samplers can effectively separate semivolatile gases from particles and 'freeze' the partitioning in time. Conversely, samples collected on filters partition mass according to the conditions of the influent airstream, which may change over time. As a result thes...

Exploring the temporal structure of heterochronous sequences using TempEst (formerly Path-O-Gen).

PubMed

Rambaut, Andrew; Lam, Tommy T; Max Carvalho, Luiz; Pybus, Oliver G

2016-01-01

Gene sequences sampled at different points in time can be used to infer molecular phylogenies on a natural timescale of months or years, provided that the sequences in question undergo measurable amounts of evolutionary change between sampling times. Data sets with this property are termed heterochronous and have become increasingly common in several fields of biology, most notably the molecular epidemiology of rapidly evolving viruses. Here we introduce the cross-platform software tool, TempEst (formerly known as Path-O-Gen), for the visualization and analysis of temporally sampled sequence data. Given a molecular phylogeny and the dates of sampling for each sequence, TempEst uses an interactive regression approach to explore the association between genetic divergence through time and sampling dates. TempEst can be used to (1) assess whether there is sufficient temporal signal in the data to proceed with phylogenetic molecular clock analysis, and (2) identify sequences whose genetic divergence and sampling date are incongruent. Examination of the latter can help identify data quality problems, including errors in data annotation, sample contamination, sequence recombination, or alignment error. We recommend that all users of the molecular clock models implemented in BEAST first check their data using TempEst prior to analysis.

Conducting On-orbit Gene Expression Analysis on ISS: WetLab-2

NASA Technical Reports Server (NTRS)

Parra, Macarena; Almeida, Eduardo; Boone, Travis; Jung, Jimmy; Lera, Matthew P.; Ricco, Antonio; Souza, Kenneth; Wu, Diana; Richey, C. Scott

2013-01-01

WetLab-2 will enable expanded genomic research on orbit by developing tools that support in situ sample collection, processing, and analysis on ISS. This capability will reduce the time-to-results for investigators and define new pathways for discovery on the ISS National Lab. The primary objective is to develop a research platform on ISS that will facilitate real-time quantitative gene expression analysis of biological samples collected on orbit. WetLab-2 will be capable of processing multiple sample types ranging from microbial cultures to animal tissues dissected on orbit. WetLab-2 will significantly expand the analytical capabilities onboard ISS and enhance science return from ISS.

Soft Ionization of Saturated Hydrocarbons, Alcohols and Nonpolar Compounds by Negative-Ion Direct Analysis in Real-Time Mass Spectrometry

NASA Astrophysics Data System (ADS)

Cody, Robert B.; Dane, A. John

2013-03-01

Large polarizable n-alkanes (approximately C18 and larger), alcohols, and other nonpolar compounds can be detected as negative ions when sample solutions are injected directly into the sampling orifice of the atmospheric pressure interface of the time-of-flight mass spectrometer with the direct analysis in real time (DART) ion source operating in negative-ion mode. The mass spectra are dominated by peaks corresponding to [M + O2]‾•. No fragmentation is observed, making this a very soft ionization technique for samples that are otherwise difficult to analyze by DART. Detection limits for cholesterol were determined to be in the low nanogram range.

Soft ionization of saturated hydrocarbons, alcohols and nonpolar compounds by negative-ion direct analysis in real-time mass spectrometry.

PubMed

Cody, Robert B; Dane, A John

2013-03-01

Large polarizable n-alkanes (approximately C18 and larger), alcohols, and other nonpolar compounds can be detected as negative ions when sample solutions are injected directly into the sampling orifice of the atmospheric pressure interface of the time-of-flight mass spectrometer with the direct analysis in real time (DART) ion source operating in negative-ion mode. The mass spectra are dominated by peaks corresponding to [M + O2]‾(•). No fragmentation is observed, making this a very soft ionization technique for samples that are otherwise difficult to analyze by DART. Detection limits for cholesterol were determined to be in the low nanogram range.

Automatic sample changer control software for automation of neutron activation analysis process in Malaysian Nuclear Agency

NASA Astrophysics Data System (ADS)

Yussup, N.; Ibrahim, M. M.; Rahman, N. A. A.; Mokhtar, M.; Salim, N. A. A.; Soh@Shaari, S. C.; Azman, A.; Lombigit, L.; Azman, A.; Omar, S. A.

2018-01-01

Most of the procedures in neutron activation analysis (NAA) process that has been established in Malaysian Nuclear Agency (Nuclear Malaysia) since 1980s were performed manually. These manual procedures carried out by the NAA laboratory personnel are time consuming and inefficient especially for sample counting and measurement process. The sample needs to be changed and the measurement software needs to be setup for every one hour counting time. Both of these procedures are performed manually for every sample. Hence, an automatic sample changer system (ASC) that consists of hardware and software is developed to automate sample counting process for up to 30 samples consecutively. This paper describes the ASC control software for NAA process which is designed and developed to control the ASC hardware and call GammaVision software for sample measurement. The software is developed by using National Instrument LabVIEW development package.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; use of a modified ultrasonic nebulizer for the analysis of low ionic-strength water by inductively coupled optical emission spectrometry

USGS Publications Warehouse

Harris, Carl M.; Litteral, Charles J.; Damrau, Donna L.

1997-01-01

The U.S. Geological Survey National Water Quality Laboratory has developed a method for the determination of dissolved calcium, iron, magnesium, manganese, silica, and sodium using a modified ultrasonic nebulizer sample-introduction system to an inductively coupled plasma-optical emission spectrometer. The nebulizer's spray chamber has been modified to avoid carryover and memory effects common in some conventional ultrasonic designs. The modified ultrasonic nebulizer is equipped with a high-speed rinse cycle to remove previously analyzed samples from the spray chamber without excessive flush times. This new rinse cycle decreases sample washout times by reducing carryover and memory effects from salt or analytes in previously analyzed samples by as much as 45 percent. Plasma instability has been reduced by repositioning the argon carrier gas inlet on the spray chamber and by directly pumping waste from the chamber, instead of from open drain traps, thereby maintaining constant pressure to the plasma. The ultrasonic nebulizer improves signal intensities, which are 8 to 16 times greater than for a conventional cross-flow pneumatic nebulizer, without being sensitive to clogging from salt buildup as in cross-flow nebulizers. Detection limits for the ultrasonic nebulizer are 4 to 18 times less than detection limits achievable using a cross-flow pneumatic nebulizer, with equivalent sample analysis time.

Imaging systems and algorithms to analyze biological samples in real-time using mobile phone microscopy

PubMed Central

Mayberry, Addison; Perkins, David L.; Holcomb, Daniel E.

2018-01-01

Miniaturized imaging devices have pushed the boundaries of point-of-care imaging, but existing mobile-phone-based imaging systems do not exploit the full potential of smart phones. This work demonstrates the use of simple imaging configurations to deliver superior image quality and the ability to handle a wide range of biological samples. Results presented in this work are from analysis of fluorescent beads under fluorescence imaging, as well as helminth eggs and freshwater mussel larvae under white light imaging. To demonstrate versatility of the systems, real time analysis and post-processing results of the sample count and sample size are presented in both still images and videos of flowing samples. PMID:29509786

Method of Analysis by the U.S. Geological Survey California District Sacramento Laboratory?Determination of Trihalomethane Formation Potential, Method Validation, and Quality-Control Practices

USGS Publications Warehouse

Crepeau, Kathryn L.; Fram, Miranda S.; Bush, Noel

2004-01-01

An analytical method for the determination of the trihalomethane formation potential of water samples has been developed. The trihalomethane formation potential is measured by dosing samples with chlorine under specified conditions of pH, temperature, incubation time, darkness, and residual-free chlorine, and then analyzing the resulting trihalomethanes by purge and trap/gas chromatography equipped with an electron capture detector. Detailed explanations of the method and quality-control practices are provided. Method validation experiments showed that the trihalomethane formation potential varies as a function of time between sample collection and analysis, residual-free chlorine concentration, method of sample dilution, and the concentration of bromide in the sample.

Sample size calculation for stepped wedge and other longitudinal cluster randomised trials.

PubMed

Hooper, Richard; Teerenstra, Steven; de Hoop, Esther; Eldridge, Sandra

2016-11-20

The sample size required for a cluster randomised trial is inflated compared with an individually randomised trial because outcomes of participants from the same cluster are correlated. Sample size calculations for longitudinal cluster randomised trials (including stepped wedge trials) need to take account of at least two levels of clustering: the clusters themselves and times within clusters. We derive formulae for sample size for repeated cross-section and closed cohort cluster randomised trials with normally distributed outcome measures, under a multilevel model allowing for variation between clusters and between times within clusters. Our formulae agree with those previously described for special cases such as crossover and analysis of covariance designs, although simulation suggests that the formulae could underestimate required sample size when the number of clusters is small. Whether using a formula or simulation, a sample size calculation requires estimates of nuisance parameters, which in our model include the intracluster correlation, cluster autocorrelation, and individual autocorrelation. A cluster autocorrelation less than 1 reflects a situation where individuals sampled from the same cluster at different times have less correlated outcomes than individuals sampled from the same cluster at the same time. Nuisance parameters could be estimated from time series obtained in similarly clustered settings with the same outcome measure, using analysis of variance to estimate variance components. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Data Streaming for Metabolomics: Accelerating Data Processing and Analysis from Days to Minutes

PubMed Central

2016-01-01

The speed and throughput of analytical platforms has been a driving force in recent years in the “omics” technologies and while great strides have been accomplished in both chromatography and mass spectrometry, data analysis times have not benefited at the same pace. Even though personal computers have become more powerful, data transfer times still represent a bottleneck in data processing because of the increasingly complex data files and studies with a greater number of samples. To meet the demand of analyzing hundreds to thousands of samples within a given experiment, we have developed a data streaming platform, XCMS Stream, which capitalizes on the acquisition time to compress and stream recently acquired data files to data processing servers, mimicking just-in-time production strategies from the manufacturing industry. The utility of this XCMS Online-based technology is demonstrated here in the analysis of T cell metabolism and other large-scale metabolomic studies. A large scale example on a 1000 sample data set demonstrated a 10 000-fold time savings, reducing data analysis time from days to minutes. Further, XCMS Stream has the capability to increase the efficiency of downstream biochemical dependent data acquisition (BDDA) analysis by initiating data conversion and data processing on subsets of data acquired, expanding its application beyond data transfer to smart preliminary data decision-making prior to full acquisition. PMID:27983788

Data streaming for metabolomics: Accelerating data processing and analysis from days to minutes

DOE PAGES

Montenegro-Burke, J. Rafael; Aisporna, Aries E.; Benton, H. Paul; ...

2016-12-16

The speed and throughput of analytical platforms has been a driving force in recent years in the “omics” technologies and while great strides have been accomplished in both chromatography and mass spectrometry, data analysis times have not benefited at the same pace. Even though personal computers have become more powerful, data transfer times still represent a bottleneck in data processing because of the increasingly complex data files and studies with a greater number of samples. To meet the demand of analyzing hundreds to thousands of samples within a given experiment, we have developed a data streaming platform, XCMS Stream, whichmore » capitalizes on the acquisition time to compress and stream recently acquired data files to data processing servers, mimicking just-in-time production strategies from the manufacturing industry. The utility of this XCMS Online-based technology is demonstrated here in the analysis of T cell metabolism and other large-scale metabolomic studies. A large scale example on a 1000 sample data set demonstrated a 10 000-fold time savings, reducing data analysis time from days to minutes. Here, XCMS Stream has the capability to increase the efficiency of downstream biochemical dependent data acquisition (BDDA) analysis by initiating data conversion and data processing on subsets of data acquired, expanding its application beyond data transfer to smart preliminary data decision-making prior to full acquisition.« less

Data Streaming for Metabolomics: Accelerating Data Processing and Analysis from Days to Minutes.

PubMed

Montenegro-Burke, J Rafael; Aisporna, Aries E; Benton, H Paul; Rinehart, Duane; Fang, Mingliang; Huan, Tao; Warth, Benedikt; Forsberg, Erica; Abe, Brian T; Ivanisevic, Julijana; Wolan, Dennis W; Teyton, Luc; Lairson, Luke; Siuzdak, Gary

2017-01-17

The speed and throughput of analytical platforms has been a driving force in recent years in the "omics" technologies and while great strides have been accomplished in both chromatography and mass spectrometry, data analysis times have not benefited at the same pace. Even though personal computers have become more powerful, data transfer times still represent a bottleneck in data processing because of the increasingly complex data files and studies with a greater number of samples. To meet the demand of analyzing hundreds to thousands of samples within a given experiment, we have developed a data streaming platform, XCMS Stream, which capitalizes on the acquisition time to compress and stream recently acquired data files to data processing servers, mimicking just-in-time production strategies from the manufacturing industry. The utility of this XCMS Online-based technology is demonstrated here in the analysis of T cell metabolism and other large-scale metabolomic studies. A large scale example on a 1000 sample data set demonstrated a 10 000-fold time savings, reducing data analysis time from days to minutes. Further, XCMS Stream has the capability to increase the efficiency of downstream biochemical dependent data acquisition (BDDA) analysis by initiating data conversion and data processing on subsets of data acquired, expanding its application beyond data transfer to smart preliminary data decision-making prior to full acquisition.

Time Delay Embedding Increases Estimation Precision of Models of Intraindividual Variability

ERIC Educational Resources Information Center

von Oertzen, Timo; Boker, Steven M.

2010-01-01

This paper investigates the precision of parameters estimated from local samples of time dependent functions. We find that "time delay embedding," i.e., structuring data prior to analysis by constructing a data matrix of overlapping samples, increases the precision of parameter estimates and in turn statistical power compared to standard…

Metabolic profiling of body fluids and multivariate data analysis.

PubMed

Trezzi, Jean-Pierre; Jäger, Christian; Galozzi, Sara; Barkovits, Katalin; Marcus, Katrin; Mollenhauer, Brit; Hiller, Karsten

2017-01-01

Metabolome analyses of body fluids are challenging due pre-analytical variations, such as pre-processing delay and temperature, and constant dynamical changes of biochemical processes within the samples. Therefore, proper sample handling starting from the time of collection up to the analysis is crucial to obtain high quality samples and reproducible results. A metabolomics analysis is divided into 4 main steps: 1) Sample collection, 2) Metabolite extraction, 3) Data acquisition and 4) Data analysis. Here, we describe a protocol for gas chromatography coupled to mass spectrometry (GC-MS) based metabolic analysis for biological matrices, especially body fluids. This protocol can be applied on blood serum/plasma, saliva and cerebrospinal fluid (CSF) samples of humans and other vertebrates. It covers sample collection, sample pre-processing, metabolite extraction, GC-MS measurement and guidelines for the subsequent data analysis. Advantages of this protocol include: •Robust and reproducible metabolomics results, taking into account pre-analytical variations that may occur during the sampling process•Small sample volume required•Rapid and cost-effective processing of biological samples•Logistic regression based determination of biomarker signatures for in-depth data analysis.

Rapid analysis of Δ-9-tetrahydrocannabinol in hair using direct analysis in real time ambient ionization orbitrap mass spectrometry.

PubMed

Duvivier, Wilco F; van Beek, Teris A; Pennings, Ed J M; Nielen, Michel W F

2014-04-15

Forensic hair analysis methods are laborious, time-consuming and provide only a rough retrospective estimate of the time of drug intake. Recently, hair imaging methods using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) were reported, but these methods require the application of MALDI matrix and are performed under vacuum. Direct analysis of entire locks of hair without any sample pretreatment and with improved spatial resolution would thus address a need. Hair samples were attached to stainless steel mesh screens and scanned in the X-direction using direct analysis in real time (DART) ambient ionization orbitrap MS. The DART gas temperature and the accuracy of the probed hair zone were optimized using Δ-9-tetrahydrocannabinol (THC) as a model compound. Since external contamination is a major issue in forensic hair analysis, sub-samples were measured before and after dichloromethane decontamination. The relative intensity of the THC signal in spiked blank hair versus that of quinine as the internal standard showed good reproducibility (26% RSD) and linearity of the method (R(2)  = 0.991). With the DART hair scan THC could be detected in hair samples from different chronic cannabis users. The presence of THC was confirmed by quantitative liquid chromatography/tandem mass spectrometry. Zones with different THC content could be clearly distinguished, indicating that the method might be used for retrospective timeline assessments. Detection of THC in decontaminated drug user hair showed that the DART hair scan not only probes THC on the surface of hair, but penetrates deeply enough to measure incorporated THC. A new approach in forensic hair analysis has been developed by probing complete locks of hair using DART-MS. Longitudinal scanning enables detection of incorporated compounds and can be used as pre-screening for THC without sample preparation. The method could also be adjusted for the analysis of other drugs of abuse. Copyright © 2014 John Wiley & Sons, Ltd.

Fast analysis of glycosides based on HKUST-1-coated monolith solid-phase microextraction and direct analysis in real-time mass spectrometry.

PubMed

Li, Xianjiang; Wang, Xin; Ma, Wen; Ai, Wanpeng; Bai, Yu; Ding, Li; Liu, Huwei

2017-04-01

Glycosides are a kind of highly important natural aromatic precursors in tobacco leaves. In this study, a novel HKUST-1-coated monolith dip-it sampler was designed for the fast and sensitive analysis of trace glycosides using direct analysis in real-time mass spectrometry. This device was prepared in two steps: in situ polymerization of monolith in a glass capillary of dip-it and layer-by-layer growth of HKUST-1 on the surface of monolith. Sufficient extraction was realized by immersing the tip to solution and in situ desorption was carried out by plasma direct analysis in real time. Compared with traditional solid-phase microextraction protocols, sample desorption was not needed anymore, and only extraction conditions were needed to be optimized in this method, including the gas temperature of direct analysis in real time, extraction time, and CH 3 COONH 4 additive concentration. This method enabled the simultaneous detection of six kinds of glycosides with the limits of detection of 0.02-0.05 μg/mL and the linear ranges covering two orders of magnitude with the limits of quantitation of 0.05-0.1 μg/mL. Moreover, the developed method was applied for the glycosides analysis of three tobacco samples, which only took about 2 s for every sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluating Composite Sampling Methods of Bacillus Spores at Low Concentrations

PubMed Central

Hess, Becky M.; Amidan, Brett G.; Anderson, Kevin K.; Hutchison, Janine R.

2016-01-01

Restoring all facility operations after the 2001 Amerithrax attacks took years to complete, highlighting the need to reduce remediation time. Some of the most time intensive tasks were environmental sampling and sample analyses. Composite sampling allows disparate samples to be combined, with only a single analysis needed, making it a promising method to reduce response times. We developed a statistical experimental design to test three different composite sampling methods: 1) single medium single pass composite (SM-SPC): a single cellulose sponge samples multiple coupons with a single pass across each coupon; 2) single medium multi-pass composite: a single cellulose sponge samples multiple coupons with multiple passes across each coupon (SM-MPC); and 3) multi-medium post-sample composite (MM-MPC): a single cellulose sponge samples a single surface, and then multiple sponges are combined during sample extraction. Five spore concentrations of Bacillus atrophaeus Nakamura spores were tested; concentrations ranged from 5 to 100 CFU/coupon (0.00775 to 0.155 CFU/cm2). Study variables included four clean surface materials (stainless steel, vinyl tile, ceramic tile, and painted dry wallboard) and three grime coated/dirty materials (stainless steel, vinyl tile, and ceramic tile). Analysis of variance for the clean study showed two significant factors: composite method (p< 0.0001) and coupon material (p = 0.0006). Recovery efficiency (RE) was higher overall using the MM-MPC method compared to the SM-SPC and SM-MPC methods. RE with the MM-MPC method for concentrations tested (10 to 100 CFU/coupon) was similar for ceramic tile, dry wall, and stainless steel for clean materials. RE was lowest for vinyl tile with both composite methods. Statistical tests for the dirty study showed RE was significantly higher for vinyl and stainless steel materials, but lower for ceramic tile. These results suggest post-sample compositing can be used to reduce sample analysis time when responding to a Bacillus anthracis contamination event of clean or dirty surfaces. PMID:27736999

Evaluating Composite Sampling Methods of Bacillus Spores at Low Concentrations.

PubMed

Hess, Becky M; Amidan, Brett G; Anderson, Kevin K; Hutchison, Janine R

2016-01-01

Restoring all facility operations after the 2001 Amerithrax attacks took years to complete, highlighting the need to reduce remediation time. Some of the most time intensive tasks were environmental sampling and sample analyses. Composite sampling allows disparate samples to be combined, with only a single analysis needed, making it a promising method to reduce response times. We developed a statistical experimental design to test three different composite sampling methods: 1) single medium single pass composite (SM-SPC): a single cellulose sponge samples multiple coupons with a single pass across each coupon; 2) single medium multi-pass composite: a single cellulose sponge samples multiple coupons with multiple passes across each coupon (SM-MPC); and 3) multi-medium post-sample composite (MM-MPC): a single cellulose sponge samples a single surface, and then multiple sponges are combined during sample extraction. Five spore concentrations of Bacillus atrophaeus Nakamura spores were tested; concentrations ranged from 5 to 100 CFU/coupon (0.00775 to 0.155 CFU/cm2). Study variables included four clean surface materials (stainless steel, vinyl tile, ceramic tile, and painted dry wallboard) and three grime coated/dirty materials (stainless steel, vinyl tile, and ceramic tile). Analysis of variance for the clean study showed two significant factors: composite method (p< 0.0001) and coupon material (p = 0.0006). Recovery efficiency (RE) was higher overall using the MM-MPC method compared to the SM-SPC and SM-MPC methods. RE with the MM-MPC method for concentrations tested (10 to 100 CFU/coupon) was similar for ceramic tile, dry wall, and stainless steel for clean materials. RE was lowest for vinyl tile with both composite methods. Statistical tests for the dirty study showed RE was significantly higher for vinyl and stainless steel materials, but lower for ceramic tile. These results suggest post-sample compositing can be used to reduce sample analysis time when responding to a Bacillus anthracis contamination event of clean or dirty surfaces.

Evaluating Composite Sampling Methods of Bacillus spores at Low Concentrations

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

Hess, Becky M.; Amidan, Brett G.; Anderson, Kevin K.

Restoring facility operations after the 2001 Amerithrax attacks took over three months to complete, highlighting the need to reduce remediation time. The most time intensive tasks were environmental sampling and sample analyses. Composite sampling allows disparate samples to be combined, with only a single analysis needed, making it a promising method to reduce response times. We developed a statistical experimental design to test three different composite sampling methods: 1) single medium single pass composite: a single cellulose sponge samples multiple coupons; 2) single medium multi-pass composite: a single cellulose sponge is used to sample multiple coupons; and 3) multi-medium post-samplemore » composite: a single cellulose sponge samples a single surface, and then multiple sponges are combined during sample extraction. Five spore concentrations of Bacillus atrophaeus Nakamura spores were tested; concentrations ranged from 5 to 100 CFU/coupon (0.00775 to 0.155CFU/cm2, respectively). Study variables included four clean surface materials (stainless steel, vinyl tile, ceramic tile, and painted wallboard) and three grime coated/dirty materials (stainless steel, vinyl tile, and ceramic tile). Analysis of variance for the clean study showed two significant factors: composite method (p-value < 0.0001) and coupon material (p-value = 0.0008). Recovery efficiency (RE) was higher overall using the post-sample composite (PSC) method compared to single medium composite from both clean and grime coated materials. RE with the PSC method for concentrations tested (10 to 100 CFU/coupon) was similar for ceramic tile, painted wall board, and stainless steel for clean materials. RE was lowest for vinyl tile with both composite methods. Statistical tests for the dirty study showed RE was significantly higher for vinyl and stainless steel materials, but significantly lower for ceramic tile. These results suggest post-sample compositing can be used to reduce sample analysis time when responding to a Bacillus anthracis contamination event of clean or dirty surfaces.« less

New approaches to wipe sampling methods for antineoplastic and other hazardous drugs in healthcare settings.

PubMed

Connor, Thomas H; Smith, Jerome P

2016-09-01

At the present time, the method of choice to determine surface contamination of the workplace with antineoplastic and other hazardous drugs is surface wipe sampling and subsequent sample analysis with a variety of analytical techniques. The purpose of this article is to review current methodology for determining the level of surface contamination with hazardous drugs in healthcare settings and to discuss recent advances in this area. In addition it will provide some guidance for conducting surface wipe sampling and sample analysis for these drugs in healthcare settings. Published studies on the use of wipe sampling to measure hazardous drugs on surfaces in healthcare settings drugs were reviewed. These studies include the use of well-documented chromatographic techniques for sample analysis in addition to newly evolving technology that provides rapid analysis of specific antineoplastic. Methodology for the analysis of surface wipe samples for hazardous drugs are reviewed, including the purposes, technical factors, sampling strategy, materials required, and limitations. The use of lateral flow immunoassay (LFIA) and fluorescence covalent microbead immunosorbent assay (FCMIA) for surface wipe sample evaluation is also discussed. Current recommendations are that all healthc a re settings where antineoplastic and other hazardous drugs are handled include surface wipe sampling as part of a comprehensive hazardous drug-safe handling program. Surface wipe sampling may be used as a method to characterize potential occupational dermal exposure risk and to evaluate the effectiveness of implemented controls and the overall safety program. New technology, although currently limited in scope, may make wipe sampling for hazardous drugs more routine, less costly, and provide a shorter response time than classical analytical techniques now in use.

Comparison of four-hour and twenty-four-hour refrigerated storage of nonpotable water for fecal coliform analysis.

PubMed Central

Standridge, J H; Lesar, D J

1977-01-01

The problem of extending the storage time of water samples for fecal coliform analysis was addressed. Included in this report is a literature review of the storage problem. Twenty-eight samples were analyzed in replicate to determine the effect of 24-h storage of water samples at 4 degrees C. A new statistical approach to data analysis, coupled with the concept of practical acceptability, is presented. According to our results, many samples can successfully be stored at 4 degrees C for 24 h. PMID:335972

Analysis of the aflatoxin AFB1 from corn by direct analysis in real time - mass spectrometry (DART-MS)

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to a high resolution mass spectrometer (MS) was used for screening of aflatoxins from a variety of surfaces and the rapid quantitative analysis of aflatoxins extracted from corn. Sample preparation procedure and instrument parameter settings wer...

Pharmaceutical identifier confirmation via DART-TOF.

PubMed

Easter, Jacob L; Steiner, Robert R

2014-07-01

Pharmaceutical analysis comprises a large amount of the casework in forensic controlled substances laboratories. In order to reduce the time of analysis for pharmaceuticals, a Direct Analysis in Real Time ion source coupled with an accurate mass time-of-flight (DART-TOF) mass spectrometer was used to confirm identity. DART-TOF spectral data for pharmaceutical samples were analyzed and evaluated by comparison to standard spectra. Identical mass pharmaceuticals were differentiated using collision induced dissociation fragmentation, present/absent ions, and abundance comparison box plots; principal component analysis (PCA) and linear discriminant analysis (LDA) were used for differentiation of identical mass mixed drug spectra. Mass assignment reproducibility and robustness tests were performed on the DART-TOF spectra. Impacts on the forensic science community include a decrease in analysis time over the traditional gas chromatograph/mass spectrometry (GC/MS) confirmations, better laboratory efficiency, and simpler sample preparation. Using physical identifiers and the DART-TOF to confirm pharmaceutical identity will eliminate the use of GC/MS and effectively reduce analysis time while still complying with accepted analysis protocols. This will prove helpful in laboratories with large backlogs and will simplify the confirmation process. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

PubMed

Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

2011-01-01

To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

Qualitative analysis of seized cocaine samples using desorption electrospray ionization- mass spectrometry (DESI-MS).

PubMed

Stojanovska, Natasha; Tahtouh, Mark; Kelly, Tamsin; Beavis, Alison; Fu, Shanlin

2015-05-01

Desorption electrospray ionization - mass spectrometry (DESI-MS) is a useful technique for the qualitative analysis of compounds found in seized drug material. In this study, DESI-MS was utilized in the screening analysis of illicit cocaine samples. The technique was also applied to the geographical origin determination of these samples. The limit of detection was determined to be 24.3 µg (or 3.47 µg/mm(2) ) and the analysis time was less than 1 minute per sample. The intra-day and inter-day precision for the detection of cocaine was 11 % and 42 %, respectively; therefore the quantitative data provided by DESI-MS was limited in its use for accurate determination of cocaine concentration in a sample. Using the quadrupole time-of-flight (QTOF) mass spectrometer, the presence of cocaine and impurities detected were confirmed by accurate tandem MS data. The qualitative chemical profiles obtained using DESI-MS were compared to two popular analysis techniques, GC-MS and LC-MS. The effects of a range of adulterants including caffeine, procaine, levamisole, lignocaine, paracetamol, and atropine on the detectability of cocaine were also investigated. It was found that the addition of these adulterants in a cocaine sample did not prevent the detection of the analyte itself (there was slight enhancement in some samples), which was useful in drug detection. The detection of truxillines in the seized samples by DESI-MS aided in the preliminary determination of geographical origin, i.e., Bolivian, Peruvian or Colombian leaf origin. The application of DESI-MS to the qualitative analysis and screening of seized cocaine samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples. Copyright © 2014 John Wiley & Sons, Ltd.

Real-time fMRI processing with physiological noise correction - Comparison with off-line analysis.

PubMed

Misaki, Masaya; Barzigar, Nafise; Zotev, Vadim; Phillips, Raquel; Cheng, Samuel; Bodurka, Jerzy

2015-12-30

While applications of real-time functional magnetic resonance imaging (rtfMRI) are growing rapidly, there are still limitations in real-time data processing compared to off-line analysis. We developed a proof-of-concept real-time fMRI processing (rtfMRIp) system utilizing a personal computer (PC) with a dedicated graphic processing unit (GPU) to demonstrate that it is now possible to perform intensive whole-brain fMRI data processing in real-time. The rtfMRIp performs slice-timing correction, motion correction, spatial smoothing, signal scaling, and general linear model (GLM) analysis with multiple noise regressors including physiological noise modeled with cardiac (RETROICOR) and respiration volume per time (RVT). The whole-brain data analysis with more than 100,000voxels and more than 250volumes is completed in less than 300ms, much faster than the time required to acquire the fMRI volume. Real-time processing implementation cannot be identical to off-line analysis when time-course information is used, such as in slice-timing correction, signal scaling, and GLM. We verified that reduced slice-timing correction for real-time analysis had comparable output with off-line analysis. The real-time GLM analysis, however, showed over-fitting when the number of sampled volumes was small. Our system implemented real-time RETROICOR and RVT physiological noise corrections for the first time and it is capable of processing these steps on all available data at a given time, without need for recursive algorithms. Comprehensive data processing in rtfMRI is possible with a PC, while the number of samples should be considered in real-time GLM. Copyright © 2015 Elsevier B.V. All rights reserved.

A novel method of multiple nucleic acid detection: Real-time RT-PCR coupled with probe-melting curve analysis.

PubMed

Han, Yang; Hou, Shao-Yang; Ji, Shang-Zhi; Cheng, Juan; Zhang, Meng-Yue; He, Li-Juan; Ye, Xiang-Zhong; Li, Yi-Min; Zhang, Yi-Xuan

2017-11-15

A novel method, real-time reverse transcription PCR (real-time RT-PCR) coupled with probe-melting curve analysis, has been established to detect two kinds of samples within one fluorescence channel. Besides a conventional TaqMan probe, this method employs another specially designed melting-probe with a 5' terminus modification which meets the same label with the same fluorescent group. By using an asymmetric PCR method, the melting-probe is able to detect an extra sample in the melting stage effectively while it almost has little influence on the amplification detection. Thus, this method allows the availability of united employment of both amplification stage and melting stage for detecting samples in one reaction. The further demonstration by simultaneous detection of human immunodeficiency virus (HIV) and hepatitis C virus (HCV) in one channel as a model system is presented in this essay. The sensitivity of detection by real-time RT-PCR coupled with probe-melting analysis was proved to be equal to that detected by conventional real-time RT-PCR. Because real-time RT-PCR coupled with probe-melting analysis can double the detection throughputs within one fluorescence channel, it is expected to be a good solution for the problem of low-throughput in current real-time PCR. Copyright © 2017 Elsevier Inc. All rights reserved.

Analysis of volatile organic compounds in compost samples: A potential tool to determine appropriate composting time.

PubMed

Zhu, Fengxiang; Pan, Zaifa; Hong, Chunlai; Wang, Weiping; Chen, Xiaoyang; Xue, Zhiyong; Yao, Yanlai

2016-12-01

Changes in volatile organic compound contents in compost samples during pig manure composting were studied using a headspace, solid-phase micro-extraction method (HS-SPME) followed by gas chromatography with mass spectrometric detection (GC/MS). Parameters affecting the SPME procedure were optimized as follows: the coating was carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) fiber, the temperature was 60°C and the time was 30min. Under these conditions, 87 compounds were identified from 17 composting samples. Most of the volatile components could only be detected before day 22. However, benzenes, alkanes and alkenes increased and eventually stabilized after day 22. Phenol and acid substances, which are important factors for compost quality, were almost undetectable on day 39 in natural compost (NC) samples and on day 13 in maggot-treated compost (MC) samples. Our results indicate that the approach can be effectively used to determine the composting times by analysis of volatile substances in compost samples. An appropriate composting time not only ensures the quality of compost and reduces the loss of composting material but also reduces the generation of hazardous substances. The appropriate composting times for MC and NC were approximately 22days and 40days, respectively, during the summer in Zhejiang. Copyright © 2016 Elsevier Ltd. All rights reserved.

Tank 30 and 37 Supernatant Sample Cross-Check and Evaporator Feed Qualification Analysis-2012

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

Oji, L. N.

2013-03-07

This report summarizes the analytical data reported by the F/H and Savannah River National Laboratories for the 2012 cross-check analysis for high level waste supernatant liquid samples from SRS Tanks 30 and 37. The intent of this Tank 30 and 37 sample analyses was to perform cross-checks against routine F/H Laboratory analyses (corrosion and evaporator feed qualification programs) using samples collected at the same time from both tanks as well as split samples from the tanks.

Preserved Proteins from Extinct Bison latifrons Identified by Tandem Mass Spectrometry; Hydroxylysine Glycosides are a Common Feature of Ancient Collagen*

PubMed Central

Hill, Ryan C.; Wither, Matthew J.; Nemkov, Travis; Barrett, Alexander; D'Alessandro, Angelo; Dzieciatkowska, Monika; Hansen, Kirk C.

2015-01-01

Bone samples from several vertebrates were collected from the Ziegler Reservoir fossil site, in Snowmass Village, Colorado, and processed for proteomics analysis. The specimens come from Pleistocene megafauna Bison latifrons, dating back ∼120,000 years. Proteomics analysis using a simplified sample preparation procedure and tandem mass spectrometry (MS/MS) was applied to obtain protein identifications. Several bioinformatics resources were used to obtain peptide identifications based on sequence homology to extant species with annotated genomes. With the exception of soil sample controls, all samples resulted in confident peptide identifications that mapped to type I collagen. In addition, we analyzed a specimen from the extinct B. latifrons that yielded peptide identifications mapping to over 33 bovine proteins. Our analysis resulted in extensive fibrillar collagen sequence coverage, including the identification of posttranslational modifications. Hydroxylysine glucosylgalactosylation, a modification thought to be involved in collagen fiber formation and bone mineralization, was identified for the first time in an ancient protein dataset. Meta-analysis of data from other studies indicates that this modification may be common in well-preserved prehistoric samples. Additional peptide sequences from extracellular matrix (ECM) and non-ECM proteins have also been identified for the first time in ancient tissue samples. These data provide a framework for analyzing ancient protein signatures in well-preserved fossil specimens, while also contributing novel insights into the molecular basis of organic matter preservation. As such, this analysis has unearthed common posttranslational modifications of collagen that may assist in its preservation over time. The data are available via ProteomeXchange with identifier PXD001827. PMID:25948757

Development of a pre-concentration system and auto-analyzer for dissolved methane, ethane, propane, and butane concentration measurements with a GC-FID

NASA Astrophysics Data System (ADS)

Chepigin, A.; Leonte, M.; Colombo, F.; Kessler, J. D.

2014-12-01

Dissolved methane, ethane, propane, and butane concentrations in natural waters are traditionally measured using a headspace equilibration technique and gas chromatograph with flame ionization detector (GC-FID). While a relatively simple technique, headspace equilibration suffers from slow equilibration times and loss of sensitivity due to concentration dilution with the pure gas headspace. Here we present a newly developed pre-concentration system and auto-analyzer for use with a GC-FID. This system decreases the time required for each analysis by eliminating the headspace equilibration time, increases the sensitivity and precision with a rapid pre-concentration step, and minimized operator time with an autoanalyzer. In this method, samples are collected from Niskin bottles in newly developed 1 L plastic sample bags rather than glass vials. Immediately following sample collection, the sample bags are placed in an incubator and individually connected to a multiport sampling valve. Water is pumped automatically from the desired sample bag through a small (6.5 mL) Liqui-Cel® membrane contactor where the dissolved gas is vacuum extracted and directly flushed into the GC sample loop. The gases of interest are preferentially extracted with the Liqui-Cel and thus a natural pre-concentration effect is obtained. Daily method calibration is achieved in the field with a five-point calibration curve that is created by analyzing gas standard-spiked water stored in 5 L gas-impermeable bags. Our system has been shown to substantially pre-concentrate the dissolved gases of interest and produce a highly linear response of peak areas to dissolved gas concentration. The system retains the high accuracy, precision, and wide range of measurable concentrations of the headspace equilibration method while simultaneously increasing the sensitivity due to the pre-concentration step. The time and labor involved in the headspace equilibration method is eliminated and replaced with the immediate and automatic analysis of a maximum of 13 sequential samples. The elapsed time between sample collection and analysis is reduced from approximately 12 hrs to < 10 min, enabling dynamic and highly resolved sampling plans.

Role of intensive milling in the processing of barium ferrite/magnetite/iron hybrid magnetic nano-composites via partial reduction of barium ferrite

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

Molaei, M.J., E-mail: mj.molaee@merc.ac.ir; Delft Chem Tech, Faculty of Applied Sciences, Delft University of Technology, Julianalaan 136, 2628 BL Delft; Ataie, A.

2015-03-15

In this research a mixture of barium ferrite and graphite was milled for different periods of time and then heat treated at different temperatures. The effects of milling time and heat treatment temperature on the phase composition, thermal behavior, morphology and magnetic properties of the samples have been investigated using X-ray diffraction, differential thermal analysis, high resolution transmission electron microscopy and vibrating sample magnetometer techniques, respectively. X-ray diffraction results revealed that BaFe{sub 12}O{sub 19}/Fe{sub 3}O{sub 4} nanocomposites form after a 20 h milling due to the partial reduction of BaFe{sub 12}O{sub 19}. High resolution transmission electron microscope images of amore » 40 h milled sample showed agglomerated structure consisting of nanoparticles with a mean particle size of 30 nm. Thermal analysis of the samples via differential thermal analysis indicated that for un-milled samples, heat treatment up to 900 °C did not result in α-Fe formation, while for a 20 h milled sample heat treatment at 700 °C resulted in reduction process progress to the formation of α-Fe. Wustite was disappeared in an X-ray diffraction pattern of a heat treated sample at 850 °C, by increasing the milling time from 20 to 40 h. By increasing the milling time, the structure of heat treated samples becomes magnetically softer due to an increase in saturation magnetization and a decrease in coercivity. Saturation magnetization and coercivity of a sample milled for 20 h and heat treated at 850 °C were 126.3 emu/g and 149.5 Oe which by increasing the milling time to 40 h, alter to 169.1 emu/g and 24.3 Oe, respectively. High coercivity values of milled and heat treated samples were attributed to the nano-scale formed iron particles. - Graphical abstract: Display Omitted - Highlights: • Barium ferrite and graphite were treated mechano-thermally. • Increasing milling time increases reduction progress after heat treatment. • Composites including iron nano-crystals forms by milling and heat treatment. • Shorter milling time results in higher H{sub C} of the milled and heat treated samples.« less

Optimization of analytical and pre-analytical conditions for MALDI-TOF-MS human urine protein profiles.

PubMed

Calvano, C D; Aresta, A; Iacovone, M; De Benedetto, G E; Zambonin, C G; Battaglia, M; Ditonno, P; Rutigliano, M; Bettocchi, C

2010-03-11

Protein analysis in biological fluids, such as urine, by means of mass spectrometry (MS) still suffers for insufficient standardization in protocols for sample collection, storage and preparation. In this work, the influence of these variables on healthy donors human urine protein profiling performed by matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was studied. A screening of various urine sample pre-treatment procedures and different sample deposition approaches on the MALDI target was performed. The influence of urine samples storage time and temperature on spectral profiles was evaluated by means of principal component analysis (PCA). The whole optimized procedure was eventually applied to the MALDI-TOF-MS analysis of human urine samples taken from prostate cancer patients. The best results in terms of detected ions number and abundance in the MS spectra were obtained by using home-made microcolumns packed with hydrophilic-lipophilic balance (HLB) resin as sample pre-treatment method; this procedure was also less expensive and suitable for high throughput analyses. Afterwards, the spin coating approach for sample deposition on the MALDI target plate was optimized, obtaining homogenous and reproducible spots. Then, PCA indicated that low storage temperatures of acidified and centrifuged samples, together with short handling time, allowed to obtain reproducible profiles without artifacts contribution due to experimental conditions. Finally, interesting differences were found by comparing the MALDI-TOF-MS protein profiles of pooled urine samples of healthy donors and prostate cancer patients. The results showed that analytical and pre-analytical variables are crucial for the success of urine analysis, to obtain meaningful and reproducible data, even if the intra-patient variability is very difficult to avoid. It has been proven how pooled urine samples can be an interesting way to make easier the comparison between healthy and pathological samples and to individuate possible differences in the protein expression between the two sets of samples. Copyright 2009 Elsevier B.V. All rights reserved.

Atmospheric Transformation of Volatile Organic Compounds

DTIC Science & Technology

2008-03-01

Study Analysis Reactant mixtures and standards from product identification experiments were sampled by exposing a 100% polydimethylsiloxane solid...later using the DNPH derivatization method described above and confirmed against a commercial standard. HPLC analysis of the DNPH cartridges also...reaction mixture for a combined total photolysis time ofapproximately 50 seconds. 2.3. Kinetic Study Analysis Samples from kinetic studies were

Modeling of human operator dynamics in simple manual control utilizing time series analysis. [tracking (position)

NASA Technical Reports Server (NTRS)

Agarwal, G. C.; Osafo-Charles, F.; Oneill, W. D.; Gottlieb, G. L.

1982-01-01

Time series analysis is applied to model human operator dynamics in pursuit and compensatory tracking modes. The normalized residual criterion is used as a one-step analytical tool to encompass the processes of identification, estimation, and diagnostic checking. A parameter constraining technique is introduced to develop more reliable models of human operator dynamics. The human operator is adequately modeled by a second order dynamic system both in pursuit and compensatory tracking modes. In comparing the data sampling rates, 100 msec between samples is adequate and is shown to provide better results than 200 msec sampling. The residual power spectrum and eigenvalue analysis show that the human operator is not a generator of periodic characteristics.

Monitoring lipase/esterase activity by stopped flow in a sequential injection analysis system using p-nitrophenyl butyrate.

PubMed

Pliego, Jorge; Mateos, Juan Carlos; Rodriguez, Jorge; Valero, Francisco; Baeza, Mireia; Femat, Ricardo; Camacho, Rosa; Sandoval, Georgina; Herrera-López, Enrique J

2015-01-27

Lipases and esterases are biocatalysts used at the laboratory and industrial level. To obtain the maximum yield in a bioprocess, it is important to measure key variables, such as enzymatic activity. The conventional method for monitoring hydrolytic activity is to take out a sample from the bioreactor to be analyzed off-line at the laboratory. The disadvantage of this approach is the long time required to recover the information from the process, hindering the possibility to develop control systems. New strategies to monitor lipase/esterase activity are necessary. In this context and in the first approach, we proposed a lab-made sequential injection analysis system to analyze off-line samples from shake flasks. Lipase/esterase activity was determined using p-nitrophenyl butyrate as the substrate. The sequential injection analysis allowed us to measure the hydrolytic activity from a sample without dilution in a linear range from 0.05-1.60 U/mL, with the capability to reach sample dilutions up to 1000 times, a sampling frequency of five samples/h, with a kinetic reaction of 5 min and a relative standard deviation of 8.75%. The results are promising to monitor lipase/esterase activity in real time, in which optimization and control strategies can be designed.

Monitoring Lipase/Esterase Activity by Stopped Flow in a Sequential Injection Analysis System Using p-Nitrophenyl Butyrate

PubMed Central

Pliego, Jorge; Mateos, Juan Carlos; Rodriguez, Jorge; Valero, Francisco; Baeza, Mireia; Femat, Ricardo; Camacho, Rosa; Sandoval, Georgina; Herrera-López, Enrique J.

2015-01-01

Lipases and esterases are biocatalysts used at the laboratory and industrial level. To obtain the maximum yield in a bioprocess, it is important to measure key variables, such as enzymatic activity. The conventional method for monitoring hydrolytic activity is to take out a sample from the bioreactor to be analyzed off-line at the laboratory. The disadvantage of this approach is the long time required to recover the information from the process, hindering the possibility to develop control systems. New strategies to monitor lipase/esterase activity are necessary. In this context and in the first approach, we proposed a lab-made sequential injection analysis system to analyze off-line samples from shake flasks. Lipase/esterase activity was determined using p-nitrophenyl butyrate as the substrate. The sequential injection analysis allowed us to measure the hydrolytic activity from a sample without dilution in a linear range from 0.05–1.60 U/mL, with the capability to reach sample dilutions up to 1000 times, a sampling frequency of five samples/h, with a kinetic reaction of 5 min and a relative standard deviation of 8.75%. The results are promising to monitor lipase/esterase activity in real time, in which optimization and control strategies can be designed. PMID:25633600

Application of porous metal enrichment probe sampling to single cell analysis using matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF-MS).

PubMed

Fu, Qiang; Tang, Jun; Cui, Meng; Xing, Junpeng; Liu, Zhiqiang; Liu, Shuying

2016-01-01

There is an increasing need for analyzing metabolism in a single cell, which is important to understand the nature of cellular heterogeneity, disease, growth and specialization, etc. However, single cell analysis is often challenging for the traces of samples. In the present study, porous metal enrichment probe sampling combined with matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF-MS) has been applied for in situ analysis of live onion epidemic cell. Porous probe, treated by corroding copper wire with HCl, was directly inserted into a single cell to get cell solution. A self-made linear actuator was enough to control the penetration of probe into the target cell accurately. Then samples on the tip of probe were eluted and detected by a commercial MALDI-TOF-MS directly. The formation of porous microstructure on the probe surface increased the adsorptive capacity of cell solution. The sensitivity of porous probe sampling was 6 times higher than uncorroded probes generally. This method provides a sensitive and convenient way for the sampling and detection of single cell solution. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Effect of short-term room temperature storage on the microbial community in infant fecal samples.

PubMed

Guo, Yong; Li, Sheng-Hui; Kuang, Ya-Shu; He, Jian-Rong; Lu, Jin-Hua; Luo, Bei-Jun; Jiang, Feng-Ju; Liu, Yao-Zhong; Papasian, Christopher J; Xia, Hui-Min; Deng, Hong-Wen; Qiu, Xiu

2016-05-26

Sample storage conditions are important for unbiased analysis of microbial communities in metagenomic studies. Specifically, for infant gut microbiota studies, stool specimens are often exposed to room temperature (RT) conditions prior to analysis. This could lead to variations in structural and quantitative assessment of bacterial communities. To estimate such effects of RT storage, we collected feces from 29 healthy infants (0-3 months) and partitioned each sample into 5 portions to be stored for different lengths of time at RT before freezing at -80 °C. Alpha diversity did not differ between samples with storage time from 0 to 2 hours. The UniFrac distances and microbial composition analysis showed significant differences by testing among individuals, but not by testing between different time points at RT. Changes in the relative abundance of some specific (less common, minor) taxa were still found during storage at room temperature. Our results support previous studies in children and adults, and provided useful information for accurate characterization of infant gut microbiomes. In particular, our study furnished a solid foundation and justification for using fecal samples exposed to RT for less than 2 hours for comparative analyses between various medical conditions.

Comparison of a real-time PCR method with a culture method for the detection of Salmonella enterica serotype enteritidis in naturally contaminated environmental samples from integrated poultry houses.

PubMed

Lungu, Bwalya; Waltman, W Douglas; Berghaus, Roy D; Hofacre, Charles L

2012-04-01

Conventional culture methods have traditionally been considered the "gold standard" for the isolation and identification of foodborne bacterial pathogens. However, culture methods are labor-intensive and time-consuming. A Salmonella enterica serotype Enteritidis-specific real-time PCR assay that recently received interim approval by the National Poultry Improvement Plan for the detection of Salmonella Enteritidis was evaluated against a culture method that had also received interim National Poultry Improvement Plan approval for the analysis of environmental samples from integrated poultry houses. The method was validated with 422 field samples collected by either the boot sock or drag swab method. The samples were cultured by selective enrichment in tetrathionate broth followed by transfer onto a modified semisolid Rappaport-Vassiliadis medium and then plating onto brilliant green with novobiocin and xylose lysine brilliant Tergitol 4 plates. One-milliliter aliquots of the selective enrichment broths from each sample were collected for DNA extraction by the commercial PrepSEQ nucleic acid extraction assay and analysis by the Salmonella Enteritidis-specific real-time PCR assay. The real-time PCR assay detected no significant differences between the boot sock and drag swab samples. In contrast, the culture method detected a significantly higher number of positive samples from boot socks. The diagnostic sensitivity of the real-time PCR assay for the field samples was significantly higher than that of the culture method. The kappa value obtained was 0.46, indicating moderate agreement between the real-time PCR assay and the culture method. In addition, the real-time PCR method had a turnaround time of 2 days compared with 4 to 8 days for the culture method. The higher sensitivity as well as the reduction in time and labor makes this real-time PCR assay an excellent alternative to conventional culture methods for diagnostic purposes, surveillance, and research studies to improve food safety.

Time dependence of the pH of rain

Treesearch

John A. Kadlecek; Volkar A. Mohnen

1976-01-01

Standard procedures for determining the pH of rain samples usually involve substantial delays from the time of rainfall to the time of analysis. This assumes that no change in pH occurs during the storage period. We have found that this is not always true. We have determined that individual rain water samples possess a time dependent pH which can be correlated with the...

Microcomputer Analysis of Children's Language Samples.

ERIC Educational Resources Information Center

Rosenkoetter, Sharon E.; Rice, Mabel L.

The workshop paper examines the use of microcomputer packages to analyze spontaneous language samples of children with communication disorders. Advantages of computerized analysis are seen to include time saving, more efficient data management, and increased objectivity. To help consumers determine which programs to buy, four aspects are…

40 CFR 98.34 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... on a specified time period (e.g., week, month, quarter, or half-year), fuel sampling and analysis is required only for those time periods in which the fuel or blend is combusted. The owner or operator may.... When the sampling frequency is based on a specified time period (e.g., week, month, quarter, or half...

40 CFR 98.34 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... on a specified time period (e.g., week, month, quarter, or half-year), fuel sampling and analysis is required only for those time periods in which the fuel or blend is combusted. The owner or operator may.... When the sampling frequency is based on a specified time period (e.g., week, month, quarter, or half...

40 CFR 98.34 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... on a specified time period (e.g., week, month, quarter, or half-year), fuel sampling and analysis is required only for those time periods in which the fuel or blend is combusted. The owner or operator may.... When the sampling frequency is based on a specified time period (e.g., week, month, quarter, or half...

Landsat image and sample design for water reservoirs (Rapel dam Central Chile).

PubMed

Lavanderos, L; Pozo, M E; Pattillo, C; Miranda, H

1990-01-01

Spatial heterogeneity of the Rapel reservoir surface waters is analyzed through Landsat images. The image digital counts are used with the aim or developing an aprioristic quantitative sample design.Natural horizontal stratification of the Rapel Reservoir (Central Chile) is produced mainly by suspended solids. The spatial heterogeneity conditions of the reservoir for the Spring 86-Summer 87 period were determined by qualitative analysis and image processing of the MSS Landsat, bands 1 and 3. The space-time variations of the different observed strata obtained with multitemporal image analysis.A random stratified sample design (r.s.s.d) was developed, based on the digital counts statistical analysis. Strata population size as well as the average, variance and sampling size of the digital counts were obtained by the r.s.s.d method.Stratification determined by analysis of satellite images were later correlated with ground data. Though the stratification of the reservoir is constant over time, the shape and size of the strata varys.

Chapter A5. Section 6.1.F. Wastewater, Pharmaceutical, and Antibiotic Compounds

USGS Publications Warehouse

Lewis, Michael Edward; Zaugg, Steven D.

2003-01-01

The USGS differentiates between samples collected for analysis of wastewater compounds and those collected for analysis of pharmaceutical and antibiotic compounds, based on the analytical schedule for the laboratory method. Currently, only the wastewater laboratory method for field-filtered samples (SH1433) is an approved, routine (production) method. (The unfiltered wastewater method LC 8033 also is available but requires a proposal for custom analysis.) At this time, analysis of samples for pharmaceutical and antibiotic compounds is confined to research studies and is available only on a custom basis.

QC-ART: A tool for real-time quality control assessment of mass spectrometry-based proteomics data.

PubMed

Stanfill, Bryan A; Nakayasu, Ernesto S; Bramer, Lisa M; Thompson, Allison M; Ansong, Charles K; Clauss, Therese; Gritsenko, Marina A; Monroe, Matthew E; Moore, Ronald J; Orton, Daniel J; Piehowski, Paul D; Schepmoes, Athena A; Smith, Richard D; Webb-Robertson, Bobbie-Jo; Metz, Thomas O

2018-04-17

Liquid chromatography-mass spectrometry (LC-MS)-based proteomics studies of large sample cohorts can easily require from months to years to complete. Acquiring consistent, high-quality data in such large-scale studies is challenging because of normal variations in instrumentation performance over time, as well as artifacts introduced by the samples themselves, such as those due to collection, storage and processing. Existing quality control methods for proteomics data primarily focus on post-hoc analysis to remove low-quality data that would degrade downstream statistics; they are not designed to evaluate the data in near real-time, which would allow for interventions as soon as deviations in data quality are detected.  In addition to flagging analyses that demonstrate outlier behavior, evaluating how the data structure changes over time can aide in understanding typical instrument performance or identify issues such as a degradation in data quality due to the need for instrument cleaning and/or re-calibration.  To address this gap for proteomics, we developed Quality Control Analysis in Real-Time (QC-ART), a tool for evaluating data as they are acquired in order to dynamically flag potential issues with instrument performance or sample quality.  QC-ART has similar accuracy as standard post-hoc analysis methods with the additional benefit of real-time analysis.  We demonstrate the utility and performance of QC-ART in identifying deviations in data quality due to both instrument and sample issues in near real-time for LC-MS-based plasma proteomics analyses of a sample subset of The Environmental Determinants of Diabetes in the Young cohort. We also present a case where QC-ART facilitated the identification of oxidative modifications, which are often underappreciated in proteomic experiments. Published under license by The American Society for Biochemistry and Molecular Biology, Inc.

The application of a novel optical SPM in biomedicine

NASA Astrophysics Data System (ADS)

Li, Yinli; Chen, Haibo; Wu, Shifa; Song, Linfeng; Zhang, Jian

2005-01-01

As an analysis tool, SPM has been broadly used in biomedicine in recent years, such as AFM and SNOM; they are effective instruments in detecting life nanostructures at atomic level. Atomic force and photon scanning tunneling microscope (AF/PSTM) is one of member of SPM, it can be used to obtain sample" optical and atomic fore images at once scanning, these images include the transmissivity image, reflection index image and topography image. This report mainly introduces the application of AF/PSTM in red blood membrane and the effect of different sample dealt with processes on the experiment result. The materials for preparing red cells membrane samples are anticoagulant blood, isotonic phosphatic buffer solution (PBS) and new two times distilled water. The images of AF/PSTM give real expression to the biology samples" fact despite of different sample dealt with processes, which prove that AF/PSTM suits to biology sample imaging. At the same time, the optical images and the topography image of AF/PSTM of the same sample are complementary with each other; this will make AF/PSTM a facile tool to analysis biologic samples" nanostructure. As another sample, this paper gives the application of AF/PSTM in immunoassay, the result shows that AF/PSTM is suit to analysis biologic sample, and it will become a new tool for biomedicine test.

Characterization of organic and conventional sweet basil leaves using chromatographic and flow-injection mass spectrometric (FIMS) fingerprints combined with principal component analysis

PubMed Central

Lu, Yingjian; Gao, Boyan; Chen, Pei; Charles, Denys; Yu, Liangli (Lucy)

2014-01-01

Sweet basil, Ocimum basilicum., is one of the most important and wildly used spices and has been shown to have antioxidant, antibacterial, and anti-diarrheal activities. In this study, high performance liquid chromatographic (HPLC) and flow-injection mass spectrometric (FIMS) fingerprinting techniques were used to differentiate organic and conventional sweet basil leaf samples. Principal component analysis (PCA) of the fingerprints indicated that both HPLC and FIMS fingerprints could effectively detect the chemical differences in the organic and conventional sweet basil leaf samples. This study suggested that the organic basil sample contained greater concentrations of almost all the major compounds than its conventional counterpart on a per same botanical weight basis. The FIMS method was able to rapidly differentiate the organic and conventional sweet basil leaf samples (1 min analysis time), whereas the HPLC fingerprints provided more information about the chemical composition of the basil samples with a longer analytical time. PMID:24518341

Characterisation of organic and conventional sweet basil leaves using chromatographic and flow-injection mass spectrometric (FIMS) fingerprints combined with principal component analysis.

PubMed

Lu, Yingjian; Gao, Boyan; Chen, Pei; Charles, Denys; Yu, Liangli Lucy

2014-07-01

Sweet basil, Ocimum basilicum, is one of the most important and wildly used spices and has been shown to have antioxidant, antibacterial, and anti-diarrheal activities. In this study, high performance liquid chromatographic (HPLC) and flow-injection mass spectrometric (FIMS) fingerprinting techniques were used to differentiate organic and conventional sweet basil leaf samples. Principal component analysis (PCA) of the fingerprints indicated that both HPLC and FIMS fingerprints could effectively detect the chemical differences in the organic and conventional sweet basil leaf samples. This study suggested that the organic basil sample contained greater concentrations of almost all the major compounds than its conventional counterpart on a per same botanical weight basis. The FIMS method was able to rapidly differentiate the organic and conventional sweet basil leaf samples (1min analysis time), whereas the HPLC fingerprints provided more information about the chemical composition of the basil samples with a longer analytical time. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid-viability PCR method for detection of live, virulent Bacillus anthracis in environmental samples.

PubMed

Létant, Sonia E; Murphy, Gloria A; Alfaro, Teneile M; Avila, Julie R; Kane, Staci R; Raber, Ellen; Bunt, Thomas M; Shah, Sanjiv R

2011-09-01

In the event of a biothreat agent release, hundreds of samples would need to be rapidly processed to characterize the extent of contamination and determine the efficacy of remediation activities. Current biological agent identification and viability determination methods are both labor- and time-intensive such that turnaround time for confirmed results is typically several days. In order to alleviate this issue, automated, high-throughput sample processing methods were developed in which real-time PCR analysis is conducted on samples before and after incubation. The method, referred to as rapid-viability (RV)-PCR, uses the change in cycle threshold after incubation to detect the presence of live organisms. In this article, we report a novel RV-PCR method for detection of live, virulent Bacillus anthracis, in which the incubation time was reduced from 14 h to 9 h, bringing the total turnaround time for results below 15 h. The method incorporates a magnetic bead-based DNA extraction and purification step prior to PCR analysis, as well as specific real-time PCR assays for the B. anthracis chromosome and pXO1 and pXO2 plasmids. A single laboratory verification of the optimized method applied to the detection of virulent B. anthracis in environmental samples was conducted and showed a detection level of 10 to 99 CFU/sample with both manual and automated RV-PCR methods in the presence of various challenges. Experiments exploring the relationship between the incubation time and the limit of detection suggest that the method could be further shortened by an additional 2 to 3 h for relatively clean samples.

Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis.

PubMed

Quaresma, Maria Cristina Baptista; de Carvalho, Maria de Fátima Batista; Meirelles, Francis Assis; Santiago, Vânia Maria Junqueira; Santelli, Ricardo Erthal

2007-02-01

A sample preparation procedure for the quantitative determination of free and total cyanides in industrial effluents has been developed that involves hydrocyanic acid vapor generation via focused microwave radiation. Hydrocyanic acid vapor was generated from free cyanides using only 5 min of irradiation time (90 W power) and a purge time of 5 min. The HCN generated was absorbed into an accepting NaOH solution using very simple glassware apparatus that was appropriate for the microwave oven cavity. After that, the cyanide concentration was determined within 90 s using a well-known spectrophotometric flow injection analysis system. Total cyanide analysis required 15 min irradiation time (90 W power), as well as chemical conditions such as the presence of EDTA-acetate buffer solution or ascorbic acid, depending on the effluent to be analyzed (petroleum refinery or electroplating effluents, respectively). The detection limit was 0.018 mg CN l(-1) (quantification limit of 0.05 mg CN l(-1)), and the measured RSD was better than 8% for ten independent analyses of effluent samples (1.4 mg l(-1) cyanide). The accuracy of the procedure was assessed via analyte spiking (with free and complex cyanides) and by performing an independent sample analysis based on the standard methodology recommended by the APHA for comparison. The sample preparation procedure takes only 10 min for free and 20 min for total cyanide, making this procedure much faster than traditional methodologies (conventional heating and distillation), which are time-consuming (they require at least 1 h). Samples from oil (sour and stripping tower bottom waters) and electroplating effluents were analyzed successfully.

Polar plot representation of time-resolved fluorescence.

PubMed

Eichorst, John Paul; Wen Teng, Kai; Clegg, Robert M

2014-01-01

Measuring changes in a molecule's fluorescence emission is a common technique to study complex biological systems such as cells and tissues. Although the steady-state fluorescence intensity is frequently used, measuring the average amount of time that a molecule spends in the excited state (the fluorescence lifetime) reveals more detailed information about its local environment. The lifetime is measured in the time domain by detecting directly the decay of fluorescence following excitation by short pulse of light. The lifetime can also be measured in the frequency domain by recording the phase and amplitude of oscillation in the emitted fluorescence of the sample in response to repetitively modulated excitation light. In either the time or frequency domain, the analysis of data to extract lifetimes can be computationally intensive. For example, a variety of iterative fitting algorithms already exist to determine lifetimes from samples that contain multiple fluorescing species. However, recently a method of analysis referred to as the polar plot (or phasor plot) is a graphical tool that projects the time-dependent features of the sample's fluorescence in either the time or frequency domain into the Cartesian plane to characterize the sample's lifetime. The coordinate transformations of the polar plot require only the raw data, and hence, there are no uncertainties from extensive corrections or time-consuming fitting in this analysis. In this chapter, the history and mathematical background of the polar plot will be presented along with examples that highlight how it can be used in both cuvette-based and imaging applications.

Interaction effects between the 5-hydroxy tryptamine transporter-linked polymorphic region (5-HTTLPR) genotype and family conflict on adolescent alcohol use and misuse.

PubMed

Kim, Jueun; Park, Aesoon; Glatt, Stephen J; Eckert, Tanya L; Vanable, Peter A; Scott-Sheldon, Lori A J; Carey, Kate B; Ewart, Craig K; Carey, Michael P

2015-02-01

To investigate whether the effects of family conflict on adolescent drinking differed as a function of 5-hydroxy tryptamine transporter-linked polymorphic region (5-HTTLPR) genotype cross-sectionally and prospectively in two independent samples of adolescents. Path analysis and multi-group analysis of two prospective datasets were conducted. United States and United Kingdom. Sample 1 was 175 adolescents in the United States (mean age = 15 at times 1 and 2 with a 6-month interval); Sample 2 was 4916 adolescents in the United Kingdon (mean age = 12 at time 1 and 15 at time 2). In both samples, demographics, tri-allelic 5-HTTLPR genotype and perceived family conflict were assessed at time 1. Alcohol use (frequency of drinking) and alcohol misuse (frequency of intoxication, frequency of drinking three or more drinks, maximum number of drinks) were assessed at times 1 and 2. A significant gene-environment interaction on alcohol misuse at time 1 was found in both sample 1 (β = 0.57, P = 0.001) and sample 2 (β = 0.19, P = 0.01), indicating that the 5-HTTLPR low-activity allele carriers exposed to higher levels of family conflict were more likely to engage in alcohol misuse than non-carriers. A significant gene-environment interaction effect on change in alcohol misuse over time was found only in sample 1 (β = 0.48, P = 0.04) but not in sample 2. Compared with non-carriers, adolescents carrying the 5-HTTLPR low-activity allele are more susceptible to the effects of family conflict on alcohol misuse. © 2014 Society for the Study of Addiction.

High-resolution time-of-flight mass spectrometry fingerprinting of metabolites from cecum and distal colon contents of rats fed resistant starch

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

Anderson, Timothy J.; Jones, Roger W.; Ai, Yongfeng

Time-of-flight mass spectrometry along with statistical analysis was utilized to study metabolic profiles among rats fed resistant starch (RS) diets. Fischer 344 rats were fed four starch diets consisting of 55 % (w/w, dbs) starch. A control starch diet consisting of corn starch was compared against three RS diets. The RS diets were high-amylose corn starch (HA7), HA7 chemically modified with octenyl succinic anhydride, and stearic-acid-complexed HA7 starch. A subgroup received antibiotic treatment to determine if perturbations in the gut microbiome were long lasting. A second subgroup was treated with azoxymethane (AOM), a carcinogen. At the end of the 8-weekmore » study, cecal and distal colon content samples were collected from the sacrificed rats. Metabolites were extracted from cecal and distal colon samples into acetonitrile. The extracts were then analyzed on an accurate-mass time-of-flight mass spectrometer to obtain their metabolic profile. The data were analyzed using partial least-squares discriminant analysis (PLS-DA). The PLS-DA analysis utilized a training set and verification set to classify samples within diet and treatment groups. PLS-DA could reliably differentiate the diet treatments for both cecal and distal colon samples. The PLS-DA analyses of the antibiotic and no antibiotic-treated subgroups were well classified for cecal samples and modestly separated for distal colon samples. PLS-DA analysis had limited success separating distal colon samples for rats given AOM from those not treated; the cecal samples from AOM had very poor classification. Mass spectrometry profiling coupled with PLS-DA can readily classify metabolite differences among rats given RS diets.« less

An Improved, Automated Whole-Air Sampler and VOC Analysis System: Results from SONGNEX 2015

NASA Astrophysics Data System (ADS)

Lerner, B. M.; Gilman, J.; Tokarek, T. W.; Peischl, J.; Koss, A.; Yuan, B.; Warneke, C.; Isaacman-VanWertz, G. A.; Sueper, D.; De Gouw, J. A.; Aikin, K. C.

2015-12-01

Accurate measurement of volatile organic compounds (VOCs) in the troposphere is critical for the understanding of emissions and physical and chemical processes that can impact both air quality and climate. Airborne VOC measurements have proven challenging due to the requirements of short sample collection times (=10 s) to maximize spatial resolution and sampling frequency and high sensitivity (pptv) to chemically diverse hydrocarbons, halocarbons, oxygen- and nitrogen-containing VOCs. NOAA ESRL CSD has built an improved whole air sampler (iWAS) which collects compressed ambient air samples in electropolished stainless steel canisters, based on the NCAR HAIS Advanced Whole Air Sampler [Atlas and Blake]. Post-flight chemical analysis is performed with a custom-built gas chromatograph-mass spectrometer system that pre-concentrates analyte cryostatically via a Stirling cooler, an electromechanical chiller which precludes the need for liquid nitrogen to reach trapping temperatures. For the 2015 Shale Oil and Natural Gas Nexus Study (SONGNEX), CSD conducted iWAS measurements on 19 flights aboard the NOAA WP-3D aircraft between March 19th and April 27th. Nine oil and natural gas production regions were surveyed during SONGNEX and more than 1500 air samples were collected and analyzed. For the first time, we employed real-time mapping of sample collection combined with live data from fast time-response measurements (e.g. ethane) for more uniform surveying and improved target plume sampling. Automated sample handling allowed for more than 90% of iWAS canisters to be analyzed within 96 hours of collection - for the second half of the campaign improved efficiencies reduced the median sample age at analysis to 36 hours. A new chromatography peak-fitting software package was developed to minimize data reduction time by an order of magnitude without a loss of precision or accuracy. Here we report mixing ratios for aliphatic and aromatic hydrocarbons (C2-C8) along with select oxygenated species (alcohols and ketones) and cycloalkanes. We present an intercomparison of the GC-MS analysis system and iWAS samples from SONGNEX with a new H3O+ CIMS-TOF and a spectroscopic ethane measurement that also flew aboard the NOAA WP-3D aircraft during SONGNEX. We also consider the effect of sample age on observed mixing ratio.

Time- and cost-saving apparatus for analytical sample filtration

Treesearch

William R. Kenealy; Joseph C. Destree

2005-01-01

Simple and cost-effective protocols were developed for removing particulates from samples prior to analysis by high performance liquid chromatography and gas chromatography. A filter and vial holder were developed for use with a 96-well filtration plate. The device saves preparation time and costs.

Graft polymerization of guar gum with acryl amide irradiated by microwaves for colonic drug delivery.

PubMed

Shahid, Muhammad; Bukhari, Shazia Anwer; Gul, Yousra; Munir, Hira; Anjum, Fozia; Zuber, Mohammad; Jamil, Tahir; Zia, Khalid Mahmood

2013-11-01

This article is aimed to discuss the modification of guar gum through microwave irradiation by varying the time of irradiation. The characterization of the modified products was carried out using FTIR spectroscopic analysis. The FT-IR spectrum of the pure guar gum (GG) sample showed a broad peak at 3298 cm(-1) while the modified GG sample displayed a peak at 1541 cm(-1) which was absent in the crude sample. The X-ray diffraction (XRD) analysis confirmed the increase in crystallinity due to grafting of the sample with polyacrylamide (GG-g-PAM). Scanning electron microscope (SEM) images revealed that granular form of guar gum was changed into fibrillar structure after grafting. Thermo-gravimetric analysis of the modified samples was also carried out and discussed. The role of guar gum as a matrix for controlled release of drug triamcinolone was evaluated. The GG-acrylamide grafted samples presented a correlation between drug release and time of microwave exposure. The results revealed that such modified product has potential applications in colonic drug delivery system. Copyright © 2013 Elsevier B.V. All rights reserved.

Reliability of the Parabola Approximation Method in Heart Rate Variability Analysis Using Low-Sampling-Rate Photoplethysmography.

PubMed

Baek, Hyun Jae; Shin, JaeWook; Jin, Gunwoo; Cho, Jaegeol

2017-10-24

Photoplethysmographic signals are useful for heart rate variability analysis in practical ambulatory applications. While reducing the sampling rate of signals is an important consideration for modern wearable devices that enable 24/7 continuous monitoring, there have not been many studies that have investigated how to compensate the low timing resolution of low-sampling-rate signals for accurate heart rate variability analysis. In this study, we utilized the parabola approximation method and measured it against the conventional cubic spline interpolation method for the time, frequency, and nonlinear domain variables of heart rate variability. For each parameter, the intra-class correlation, standard error of measurement, Bland-Altman 95% limits of agreement and root mean squared relative error were presented. Also, elapsed time taken to compute each interpolation algorithm was investigated. The results indicated that parabola approximation is a simple, fast, and accurate algorithm-based method for compensating the low timing resolution of pulse beat intervals. In addition, the method showed comparable performance with the conventional cubic spline interpolation method. Even though the absolute value of the heart rate variability variables calculated using a signal sampled at 20 Hz were not exactly matched with those calculated using a reference signal sampled at 250 Hz, the parabola approximation method remains a good interpolation method for assessing trends in HRV measurements for low-power wearable applications.

Progressive Sampling Technique for Efficient and Robust Uncertainty and Sensitivity Analysis of Environmental Systems Models: Stability and Convergence

NASA Astrophysics Data System (ADS)

Sheikholeslami, R.; Hosseini, N.; Razavi, S.

2016-12-01

Modern earth and environmental models are usually characterized by a large parameter space and high computational cost. These two features prevent effective implementation of sampling-based analysis such as sensitivity and uncertainty analysis, which require running these computationally expensive models several times to adequately explore the parameter/problem space. Therefore, developing efficient sampling techniques that scale with the size of the problem, computational budget, and users' needs is essential. In this presentation, we propose an efficient sequential sampling strategy, called Progressive Latin Hypercube Sampling (PLHS), which provides an increasingly improved coverage of the parameter space, while satisfying pre-defined requirements. The original Latin hypercube sampling (LHS) approach generates the entire sample set in one stage; on the contrary, PLHS generates a series of smaller sub-sets (also called `slices') while: (1) each sub-set is Latin hypercube and achieves maximum stratification in any one dimensional projection; (2) the progressive addition of sub-sets remains Latin hypercube; and thus (3) the entire sample set is Latin hypercube. Therefore, it has the capability to preserve the intended sampling properties throughout the sampling procedure. PLHS is deemed advantageous over the existing methods, particularly because it nearly avoids over- or under-sampling. Through different case studies, we show that PHLS has multiple advantages over the one-stage sampling approaches, including improved convergence and stability of the analysis results with fewer model runs. In addition, PLHS can help to minimize the total simulation time by only running the simulations necessary to achieve the desired level of quality (e.g., accuracy, and convergence rate).

HIGH VOLUME INJECTION FOR GCMS ANALYSIS OF PARTICULATE ORGANIC SPECIES IN AMBIENT AIR

EPA Science Inventory

Detection of organic species in ambient particulate matter typically requires large air sample volumes, frequently achieved by grouping samples into monthly composites. Decreasing the volume of air sample required would allow shorter collection times and more convenient sample c...

Qualitative analysis of tackifier resins in pressure sensitive adhesives using direct analysis in real time time-of-flight mass spectrometry.

PubMed

Mess, Aylin; Vietzke, Jens-Peter; Rapp, Claudius; Francke, Wittko

2011-10-01

Tackifier resins play an important role as additives in pressure sensitive adhesives (PSAs) to modulate their desired properties. With dependence on their origin and processing, tackifier resins can be multicomponent mixtures. Once they have been incorporated in a polymer matrix, conventional chemical analysis of tackifiers usually tends to be challenging because a suitable sample pretreatment and/or separation is necessary and all characteristic components have to be detected for an unequivocal identification of the resin additive. Nevertheless, a reliable analysis of tackifiers is essential for product quality and safety reasons. A promising approach for the examination of tackifier resins in PSAs is the novel direct analysis in real time mass spectrometry (DART-MS) technique, which enables screening analysis without time-consuming sample preparation. In the present work, four key classes of tackifier resins were studied (rosin, terpene phenolic, polyterpene, and hydrocarbon resins). Their corresponding complex mass spectra were interpreted and used as reference spectra for subsequent analyses. These data were used to analyze tackifier additives in synthetic rubber and acrylic adhesive matrixes. To prove the efficiency of the developed method, complete PSA products containing two or three different tackifiers were analyzed. The tackifier resins were successfully identified, while measurement time and interpretation took less than 10 mins per sample. Determination of resin additives in PSAs can be performed down to 0.1% (w/w, limit of detection) using the three most abundant signals for each tackifier. In summary, DART-MS is a rapid and efficient screening method for the analysis of various tackifiers in PSAs.

Computer graphics for quality control in the INAA of geological samples

USGS Publications Warehouse

Grossman, J.N.; Baedecker, P.A.

1987-01-01

A data reduction system for the routine instrumental activation analysis of samples is described, with particular emphasis on interactive graphics capabilities for evaluating analytical quality. Graphics procedures have been developed to interactively control the analysis of selected photopeaks during spectral analysis, and to evaluate detector performance during a given counting cycle. Graphics algorithms are also used to compare the data on reference samples with accepted values, to prepare quality control charts to evaluate long term precision and to search for systematic variations in data on reference samples as a function of time. ?? 1987 Akade??miai Kiado??.

TimesVector: a vectorized clustering approach to the analysis of time series transcriptome data from multiple phenotypes.

PubMed

Jung, Inuk; Jo, Kyuri; Kang, Hyejin; Ahn, Hongryul; Yu, Youngjae; Kim, Sun

2017-12-01

Identifying biologically meaningful gene expression patterns from time series gene expression data is important to understand the underlying biological mechanisms. To identify significantly perturbed gene sets between different phenotypes, analysis of time series transcriptome data requires consideration of time and sample dimensions. Thus, the analysis of such time series data seeks to search gene sets that exhibit similar or different expression patterns between two or more sample conditions, constituting the three-dimensional data, i.e. gene-time-condition. Computational complexity for analyzing such data is very high, compared to the already difficult NP-hard two dimensional biclustering algorithms. Because of this challenge, traditional time series clustering algorithms are designed to capture co-expressed genes with similar expression pattern in two sample conditions. We present a triclustering algorithm, TimesVector, specifically designed for clustering three-dimensional time series data to capture distinctively similar or different gene expression patterns between two or more sample conditions. TimesVector identifies clusters with distinctive expression patterns in three steps: (i) dimension reduction and clustering of time-condition concatenated vectors, (ii) post-processing clusters for detecting similar and distinct expression patterns and (iii) rescuing genes from unclassified clusters. Using four sets of time series gene expression data, generated by both microarray and high throughput sequencing platforms, we demonstrated that TimesVector successfully detected biologically meaningful clusters of high quality. TimesVector improved the clustering quality compared to existing triclustering tools and only TimesVector detected clusters with differential expression patterns across conditions successfully. The TimesVector software is available at http://biohealth.snu.ac.kr/software/TimesVector/. sunkim.bioinfo@snu.ac.kr. Supplementary data are available at Bioinformatics online. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

Probabilistic Round Trip Contamination Analysis of a Mars Sample Acquisition and Handling Process Using Markovian Decompositions

NASA Technical Reports Server (NTRS)

Hudson, Nicolas; Lin, Ying; Barengoltz, Jack

2010-01-01

A method for evaluating the probability of a Viable Earth Microorganism (VEM) contaminating a sample during the sample acquisition and handling (SAH) process of a potential future Mars Sample Return mission is developed. A scenario where multiple core samples would be acquired using a rotary percussive coring tool, deployed from an arm on a MER class rover is analyzed. The analysis is conducted in a structured way by decomposing sample acquisition and handling process into a series of discrete time steps, and breaking the physical system into a set of relevant components. At each discrete time step, two key functions are defined: The probability of a VEM being released from each component, and the transport matrix, which represents the probability of VEM transport from one component to another. By defining the expected the number of VEMs on each component at the start of the sampling process, these decompositions allow the expected number of VEMs on each component at each sampling step to be represented as a Markov chain. This formalism provides a rigorous mathematical framework in which to analyze the probability of a VEM entering the sample chain, as well as making the analysis tractable by breaking the process down into small analyzable steps.

EPA Method 3031 (SW-846): Acid Digestion of Oils for Metals Analysis by Atomic Absorption or ICP Spectrometry

EPA Pesticide Factsheets

Procedures are described for analysis of water samples and may be adapted for assessment of solid, particulate and liquid samples. The method uses real-time PCR assay for detecting Toxoplasma gondii DNA using gene-specific primers and probe.

Recent results of synchrotron radiation induced total reflection X-ray fluorescence analysis at HASYLAB, beamline L

NASA Astrophysics Data System (ADS)

Streli, C.; Pepponi, G.; Wobrauschek, P.; Jokubonis, C.; Falkenberg, G.; Záray, G.; Broekaert, J.; Fittschen, U.; Peschel, B.

2006-11-01

At the Hamburger Synchrotronstrahlungslabor (HASYLAB), Beamline L, a vacuum chamber for synchrotron radiation-induced total reflection X-ray fluorescence analysis, is now available which can easily be installed using the adjustment components for microanalysis present at this beamline. The detector is now in the final version of a Vortex silicon drift detector with 50-mm 2 active area from Radiant Detector Technologies. With the Ni/C multilayer monochromator set to 17 keV extrapolated detection limits of 8 fg were obtained using the 50-mm 2 silicon drift detector with 1000 s live time on a sample containing 100 pg of Ni. Various applications are presented, especially of samples which are available in very small amounts: As synchrotron radiation-induced total reflection X-ray fluorescence analysis is much more sensitive than tube-excited total reflection X-ray fluorescence analysis, the sampling time of aerosol samples can be diminished, resulting in a more precise time resolution of atmospheric events. Aerosols, directly sampled on Si reflectors in an impactor were investigated. A further application was the determination of contamination elements in a slurry of high-purity Al 2O 3. No digestion is required; the sample is pipetted and dried before analysis. A comparison with laboratory total reflection X-ray fluorescence analysis showed the higher sensitivity of synchrotron radiation-induced total reflection X-ray fluorescence analysis, more contamination elements could be detected. Using the Si-111 crystal monochromator also available at beamline L, XANES measurements to determine the chemical state were performed. This is only possible with lower sensitivity as the flux transmitted by the crystal monochromator is about a factor of 100 lower than that transmitted by the multilayer monochromator. Preliminary results of X-ray absorption near-edge structure measurements for As in xylem sap from cucumber plants fed with As(III) and As(V) are reported. Detection limits of 170 ng/l of As in xylem sap were achieved.

Development of automation software for neutron activation analysis process in Malaysian nuclear agency

NASA Astrophysics Data System (ADS)

Yussup, N.; Rahman, N. A. A.; Ibrahim, M. M.; Mokhtar, M.; Salim, N. A. A.; Soh@Shaari, S. C.; Azman, A.

2017-01-01

Neutron Activation Analysis (NAA) process has been established in Malaysian Nuclear Agency (Nuclear Malaysia) since 1980s. Most of the procedures established especially from sample registration to sample analysis are performed manually. These manual procedures carried out by the NAA laboratory personnel are time consuming and inefficient. Hence, a software to support the system automation is developed to provide an effective method to replace redundant manual data entries and produce faster sample analysis and calculation process. This paper describes the design and development of automation software for NAA process which consists of three sub-programs. The sub-programs are sample registration, hardware control and data acquisition; and sample analysis. The data flow and connection between the sub-programs will be explained. The software is developed by using National Instrument LabView development package.

Rushed, unhappy, and drained: an experience sampling study of relations between time pressure, perceived control, mood, and emotional exhaustion in a group of accountants.

PubMed

Teuchmann, K; Totterdell, P; Parker, S K

1999-01-01

Experience sampling methodology was used to examine how work demands translate into acute changes in affective response and thence into chronic response. Seven accountants reported their reactions 3 times a day for 4 weeks on pocket computers. Aggregated analysis showed that mood and emotional exhaustion fluctuated in parallel with time pressure over time. Disaggregated time-series analysis confirmed the direct impact of high-demand periods on the perception of control, time pressure, and mood and the indirect impact on emotional exhaustion. A curvilinear relationship between time pressure and emotional exhaustion was shown. The relationships between work demands and emotional exhaustion changed between high-demand periods and normal working periods. The results suggest that enhancing perceived control may alleviate the negative effects of time pressure.

Wavelength Selection Method Based on Differential Evolution for Precise Quantitative Analysis Using Terahertz Time-Domain Spectroscopy.

PubMed

Li, Zhi; Chen, Weidong; Lian, Feiyu; Ge, Hongyi; Guan, Aihong

2017-12-01

Quantitative analysis of component mixtures is an important application of terahertz time-domain spectroscopy (THz-TDS) and has attracted broad interest in recent research. Although the accuracy of quantitative analysis using THz-TDS is affected by a host of factors, wavelength selection from the sample's THz absorption spectrum is the most crucial component. The raw spectrum consists of signals from the sample and scattering and other random disturbances that can critically influence the quantitative accuracy. For precise quantitative analysis using THz-TDS, the signal from the sample needs to be retained while the scattering and other noise sources are eliminated. In this paper, a novel wavelength selection method based on differential evolution (DE) is investigated. By performing quantitative experiments on a series of binary amino acid mixtures using THz-TDS, we demonstrate the efficacy of the DE-based wavelength selection method, which yields an error rate below 5%.

Interval sampling methods and measurement error: a computer simulation.

PubMed

Wirth, Oliver; Slaven, James; Taylor, Matthew A

2014-01-01

A simulation study was conducted to provide a more thorough account of measurement error associated with interval sampling methods. A computer program simulated the application of momentary time sampling, partial-interval recording, and whole-interval recording methods on target events randomly distributed across an observation period. The simulation yielded measures of error for multiple combinations of observation period, interval duration, event duration, and cumulative event duration. The simulations were conducted up to 100 times to yield measures of error variability. Although the present simulation confirmed some previously reported characteristics of interval sampling methods, it also revealed many new findings that pertain to each method's inherent strengths and weaknesses. The analysis and resulting error tables can help guide the selection of the most appropriate sampling method for observation-based behavioral assessments. © Society for the Experimental Analysis of Behavior.

[Rapid screening the alkaloids of poppy shell in hot pot condiment, beef noodle soup and seasoning by direct analysis in real time-tandem mass spectrometry].

PubMed

Zhang, Baile; Gao, Lihong; Xie, Yingshuang; Zhou, Wei; Chen, Xiaofeng; Lei, Chunni; Zhang, Huan

2017-07-08

A direct analysis in real time tandem mass spectrometry (DART-MS/MS) method was established for quickly screening five illegally added alkaloids of poppy shell from the hot pot condiment, beef noodle soup and seasoning. The samples were extracted and purified by acetonitrile, and then injected under the conditions of ionization temperature of 300℃, grid electrode voltage of 150 V and sampling rate of 0.8 mm/s using DART in the positive ion mode. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. The method is simple and rapid, and can meet the requirement of rapid screening and analysis of large quantities of samples.

Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

Mutual information estimation for irregularly sampled time series

NASA Astrophysics Data System (ADS)

Rehfeld, K.; Marwan, N.; Heitzig, J.; Kurths, J.

2012-04-01

For the automated, objective and joint analysis of time series, similarity measures are crucial. Used in the analysis of climate records, they allow for a complimentary, unbiased view onto sparse datasets. The irregular sampling of many of these time series, however, makes it necessary to either perform signal reconstruction (e.g. interpolation) or to develop and use adapted measures. Standard linear interpolation comes with an inevitable loss of information and bias effects. We have recently developed a Gaussian kernel-based correlation algorithm with which the interpolation error can be substantially lowered, but this would not work should the functional relationship in a bivariate setting be non-linear. We therefore propose an algorithm to estimate lagged auto and cross mutual information from irregularly sampled time series. We have extended the standard and adaptive binning histogram estimators and use Gaussian distributed weights in the estimation of the (joint) probabilities. To test our method we have simulated linear and nonlinear auto-regressive processes with Gamma-distributed inter-sampling intervals. We have then performed a sensitivity analysis for the estimation of actual coupling length, the lag of coupling and the decorrelation time in the synthetic time series and contrast our results to the performance of a signal reconstruction scheme. Finally we applied our estimator to speleothem records. We compare the estimated memory (or decorrelation time) to that from a least-squares estimator based on fitting an auto-regressive process of order 1. The calculated (cross) mutual information results are compared for the different estimators (standard or adaptive binning) and contrasted with results from signal reconstruction. We find that the kernel-based estimator has a significantly lower root mean square error and less systematic sampling bias than the interpolation-based method. It is possible that these encouraging results could be further improved by using non-histogram mutual information estimators, like k-Nearest Neighbor or Kernel-Density estimators, but for short (<1000 points) and irregularly sampled datasets the proposed algorithm is already a great improvement.

Critical evaluation of sample pretreatment techniques.

PubMed

Hyötyläinen, Tuulia

2009-06-01

Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure. Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis, and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis. The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.

[Research on Time-frequency Characteristics of Magneto-acoustic Signal of Different Thickness Medium Based on Wave Summing Method].

PubMed

Zhang, Shunqi; Yin, Tao; Ma, Ren; Liu, Zhipeng

2015-08-01

Functional imaging method of biological electrical characteristics based on magneto-acoustic effect gives valuable information of tissue in early tumor diagnosis, therein time and frequency characteristics analysis of magneto-acoustic signal is important in image reconstruction. This paper proposes wave summing method based on Green function solution for acoustic source of magneto-acoustic effect. Simulations and analysis under quasi 1D transmission condition are carried out to time and frequency characteristics of magneto-acoustic signal of models with different thickness. Simulation results of magneto-acoustic signal were verified through experiments. Results of the simulation with different thickness showed that time-frequency characteristics of magneto-acoustic signal reflected thickness of sample. Thin sample, which is less than one wavelength of pulse, and thick sample, which is larger than one wavelength, showed different summed waveform and frequency characteristics, due to difference of summing thickness. Experimental results verified theoretical analysis and simulation results. This research has laid a foundation for acoustic source and conductivity reconstruction to the medium with different thickness in magneto-acoustic imaging.

A system architecture for online data interpretation and reduction in fluorescence microscopy

NASA Astrophysics Data System (ADS)

Röder, Thorsten; Geisbauer, Matthias; Chen, Yang; Knoll, Alois; Uhl, Rainer

2010-01-01

In this paper we present a high-throughput sample screening system that enables real-time data analysis and reduction for live cell analysis using fluorescence microscopy. We propose a novel system architecture capable of analyzing a large amount of samples during the experiment and thus greatly minimizing the post-analysis phase that is the common practice today. By utilizing data reduction algorithms, relevant information of the target cells is extracted from the online collected data stream, and then used to adjust the experiment parameters in real-time, allowing the system to dynamically react on changing sample properties and to control the microscope setup accordingly. The proposed system consists of an integrated DSP-FPGA hybrid solution to ensure the required real-time constraints, to execute efficiently the underlying computer vision algorithms and to close the perception-action loop. We demonstrate our approach by addressing the selective imaging of cells with a particular combination of markers. With this novel closed-loop system the amount of superfluous collected data is minimized, while at the same time the information entropy increases.

Multidimensional scaling analysis of financial time series based on modified cross-sample entropy methods

NASA Astrophysics Data System (ADS)

He, Jiayi; Shang, Pengjian; Xiong, Hui

2018-06-01

Stocks, as the concrete manifestation of financial time series with plenty of potential information, are often used in the study of financial time series. In this paper, we utilize the stock data to recognize their patterns through out the dissimilarity matrix based on modified cross-sample entropy, then three-dimensional perceptual maps of the results are provided through multidimensional scaling method. Two modified multidimensional scaling methods are proposed in this paper, that is, multidimensional scaling based on Kronecker-delta cross-sample entropy (MDS-KCSE) and multidimensional scaling based on permutation cross-sample entropy (MDS-PCSE). These two methods use Kronecker-delta based cross-sample entropy and permutation based cross-sample entropy to replace the distance or dissimilarity measurement in classical multidimensional scaling (MDS). Multidimensional scaling based on Chebyshev distance (MDSC) is employed to provide a reference for comparisons. Our analysis reveals a clear clustering both in synthetic data and 18 indices from diverse stock markets. It implies that time series generated by the same model are easier to have similar irregularity than others, and the difference in the stock index, which is caused by the country or region and the different financial policies, can reflect the irregularity in the data. In the synthetic data experiments, not only the time series generated by different models can be distinguished, the one generated under different parameters of the same model can also be detected. In the financial data experiment, the stock indices are clearly divided into five groups. Through analysis, we find that they correspond to five regions, respectively, that is, Europe, North America, South America, Asian-Pacific (with the exception of mainland China), mainland China and Russia. The results also demonstrate that MDS-KCSE and MDS-PCSE provide more effective divisions in experiments than MDSC.

Development of portable defocusing micro-scale spatially offset Raman spectroscopy.

PubMed

Realini, Marco; Botteon, Alessandra; Conti, Claudia; Colombo, Chiara; Matousek, Pavel

2016-05-10

We present, for the first time, portable defocusing micro-Spatially Offset Raman Spectroscopy (micro-SORS). Micro-SORS is a concept permitting the analysis of thin, highly turbid stratified layers beyond the reach of conventional Raman microscopy. The technique is applicable to the analysis of painted layers in cultural heritage (panels, canvases and mural paintings, painted statues and decorated objects in general) as well as in many other areas including polymer, biological and biomedical applications, catalytic and forensics sciences where highly turbid stratified layers are present and where invasive analysis is undesirable or impossible. So far the technique has been demonstrated only on benchtop Raman microscopes precluding the non-invasive analysis of larger samples and samples in situ. The new set-up is characterised conceptually on a range of artificially assembled two-layer systems demonstrating its benefits and performance across several application areas. These included stratified polymer sample, pharmaceutical tablet and layered paint samples. The same samples were also analysed by a high performance (non-portable) benchtop Raman microscope to provide benchmarking against our earlier research. The realisation of the vision of delivering portability to micro-SORS has a transformative potential spanning across multiple disciplines as it fully unlocks, for the first time, the non-invasive and non-destructive aspects of micro-SORS enabling it to be applied also to large and non-portable samples in situ without recourse to removing samples, or their fragments, for laboratory analysis on benchtop Raman microscopes.

Model-Based Design of Long-Distance Tracer Transport Experiments in Plants.

PubMed

Bühler, Jonas; von Lieres, Eric; Huber, Gregor J

2018-01-01

Studies of long-distance transport of tracer isotopes in plants offer a high potential for functional phenotyping, but so far measurement time is a bottleneck because continuous time series of at least 1 h are required to obtain reliable estimates of transport properties. Hence, usual throughput values are between 0.5 and 1 samples h -1 . Here, we propose to increase sample throughput by introducing temporal gaps in the data acquisition of each plant sample and measuring multiple plants one after each other in a rotating scheme. In contrast to common time series analysis methods, mechanistic tracer transport models allow the analysis of interrupted time series. The uncertainties of the model parameter estimates are used as a measure of how much information was lost compared to complete time series. A case study was set up to systematically investigate different experimental schedules for different throughput scenarios ranging from 1 to 12 samples h -1 . Selected designs with only a small amount of data points were found to be sufficient for an adequate parameter estimation, implying that the presented approach enables a substantial increase of sample throughput. The presented general framework for automated generation and evaluation of experimental schedules allows the determination of a maximal sample throughput and the respective optimal measurement schedule depending on the required statistical reliability of data acquired by future experiments.

Ocean wavenumber estimation from wave-resolving time series imagery

USGS Publications Warehouse

Plant, N.G.; Holland, K.T.; Haller, M.C.

2008-01-01

We review several approaches that have been used to estimate ocean surface gravity wavenumbers from wave-resolving remotely sensed image sequences. Two fundamentally different approaches that utilize these data exist. A power spectral density approach identifies wavenumbers where image intensity variance is maximized. Alternatively, a cross-spectral correlation approach identifies wavenumbers where intensity coherence is maximized. We develop a solution to the latter approach based on a tomographic analysis that utilizes a nonlinear inverse method. The solution is tolerant to noise and other forms of sampling deficiency and can be applied to arbitrary sampling patterns, as well as to full-frame imagery. The solution includes error predictions that can be used for data retrieval quality control and for evaluating sample designs. A quantitative analysis of the intrinsic resolution of the method indicates that the cross-spectral correlation fitting improves resolution by a factor of about ten times as compared to the power spectral density fitting approach. The resolution analysis also provides a rule of thumb for nearshore bathymetry retrievals-short-scale cross-shore patterns may be resolved if they are about ten times longer than the average water depth over the pattern. This guidance can be applied to sample design to constrain both the sensor array (image resolution) and the analysis array (tomographic resolution). ?? 2008 IEEE.

Ultrafast Screening and Quantitation of Pesticides in Food and Environmental Matrices by Solid-Phase Microextraction-Transmission Mode (SPME-TM) and Direct Analysis in Real Time (DART).

PubMed

Gómez-Ríos, Germán Augusto; Gionfriddo, Emanuela; Poole, Justen; Pawliszyn, Janusz

2017-07-05

The direct interface of microextraction technologies to mass spectrometry (MS) has unquestionably revolutionized the speed and efficacy at which complex matrices are analyzed. Solid Phase Micro Extraction-Transmission Mode (SPME-TM) is a technology conceived as an effective synergy between sample preparation and ambient ionization. Succinctly, the device consists of a mesh coated with polymeric particles that extracts analytes of interest present in a given sample matrix. This coated mesh acts as a transmission-mode substrate for Direct Analysis in Real Time (DART), allowing for rapid and efficient thermal desorption/ionization of analytes previously concentrated on the coating, and dramatically lowering the limits of detection attained by sole DART analysis. In this study, we present SPME-TM as a novel tool for the ultrafast enrichment of pesticides present in food and environmental matrices and their quantitative determination by MS via DART ionization. Limits of quantitation in the subnanogram per milliliter range can be attained, while total analysis time does not exceed 2 min per sample. In addition to target information obtained via tandem MS, retrospective studies of the same sample via high-resolution mass spectrometry (HRMS) were accomplished by thermally desorbing a different segment of the microextraction device.

Rapid analysis of caffeine in various coffee samples employing direct analysis in real-time ionization-high-resolution mass spectrometry.

PubMed

Danhelova, Hana; Hradecky, Jaromir; Prinosilova, Sarka; Cajka, Tomas; Riddellova, Katerina; Vaclavik, Lukas; Hajslova, Jana

2012-07-01

The development and use of a fast method employing a direct analysis in real time (DART) ion source coupled to high-resolution time-of-flight mass spectrometry (TOFMS) for the quantitative analysis of caffeine in various coffee samples has been demonstrated in this study. A simple sample extraction procedure employing hot water was followed by direct, high-throughput (<1 min per run) examination of the extracts spread on a glass rod under optimized conditions of ambient mass spectrometry, without any prior chromatographic separation. For quantification of caffeine using DART-TOFMS, an external calibration was used. Isotopically labeled caffeine was used to compensate for the variations of the ion intensities of caffeine signal. Recoveries of the DART-TOFMS method were 97% for instant coffee at the spiking levels of 20 and 60 mg/g, respectively, while for roasted ground coffee, the obtained values were 106% and 107% at the spiking levels of 10 and 30 mg/g, respectively. The repeatability of the whole analytical procedure (expressed as relative standard deviation, RSD, %) was <5% for all tested spiking levels and matrices. Since the linearity range of the method was relatively narrow (two orders of magnitude), an optimization of sample dilution prior the DART-TOFMS measurement to avoid saturation of the detector was needed.

Direct analysis of hCGβcf glycosylation in normal and aberrant pregnancy by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

PubMed

Iles, Ray K; Cole, Laurence A; Butler, Stephen A

2014-06-05

The analysis of human chorionic gonadotropin (hCG) in clinical chemistry laboratories by specific immunoassay is well established. However, changes in glycosylation are not as easily assayed and yet alterations in hCG glycosylation is associated with abnormal pregnancy. hCGβ-core fragment (hCGβcf) was isolated from the urine of women, pregnant with normal, molar and hyperemesis gravidarum pregnancies. Each sample was subjected to matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS) analysis following dithiothreitol (DTT) reduction and fingerprint spectra of peptide hCGβ 6-40 were analyzed. Samples were variably glycosylated, where most structures were small, core and largely mono-antennary. Larger single bi-antennary and mixtures of larger mono-antennary and bi-antennary moieties were also observed in some samples. Larger glycoforms were more abundant in the abnormal pregnancies and tri-antennary carbohydrate moieties were only observed in the samples from molar and hyperemesis gravidarum pregnancies. Given that such spectral profiling differences may be characteristic, development of small sample preparation for mass spectral analysis of hCG may lead to a simpler and faster approach to glycostructural analysis and potentially a novel clinical diagnostic test.

Laser-Induced Breakdown Spectroscopy Based Protein Assay for Cereal Samples.

PubMed

Sezer, Banu; Bilge, Gonca; Boyaci, Ismail Hakki

2016-12-14

Protein content is an important quality parameter in terms of price, nutritional value, and labeling of various cereal samples. However, conventional analysis methods, namely, Kjeldahl and Dumas, have major drawbacks such as long analysis time, titration mistakes, and carrier gas dependence with high purity. For this reason, there is an urgent need for rapid, reliable, and environmentally friendly technologies for protein analysis. The present study aims to develop a new method for protein analysis in wheat flour and whole meal by using laser-induced breakdown spectroscopy (LIBS), which is a multielemental, fast, and simple spectroscopic method. Unlike the Kjeldahl and Dumas methods, it has potential to analyze a high number of samples in considerably short time. In the study, nitrogen peaks in LIBS spectra of wheat flour and whole meal samples with different protein contents were correlated with results of the standard Dumas method with the aid of chemometric methods. A calibration graph showed good linearity with the protein content between 7.9 and 20.9% and a 0.992 coefficient of determination (R 2 ). The limit of detection was calculated as 0.26%. The results indicated that LIBS is a promising and reliable method with its high sensitivity for routine protein analysis in wheat flour and whole meal samples.

Microfluidic-Based Robotic Sampling System for Radioactive Solutions

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

Jack D. Law; Julia L. Tripp; Tara E. Smith

A novel microfluidic based robotic sampling system has been developed for sampling and analysis of liquid solutions in nuclear processes. This system couples the use of a microfluidic sample chip with a robotic system designed to allow remote, automated sampling of process solutions in-cell and facilitates direct coupling of the microfluidic sample chip with analytical instrumentation. This system provides the capability for near real time analysis, reduces analytical waste, and minimizes the potential for personnel exposure associated with traditional sampling methods. A prototype sampling system was designed, built and tested. System testing demonstrated operability of the microfluidic based sample systemmore » and identified system modifications to optimize performance.« less

Reconstructing genealogies of serial samples under the assumption of a molecular clock using serial-sample UPGMA.

PubMed

Drummond, A; Rodrigo, A G

2000-12-01

Reconstruction of evolutionary relationships from noncontemporaneous molecular samples provides a new challenge for phylogenetic reconstruction methods. With recent biotechnological advances there has been an increase in molecular sequencing throughput, and the potential to obtain serial samples of sequences from populations, including rapidly evolving pathogens, is fast being realized. A new method called the serial-sample unweighted pair grouping method with arithmetic means (sUPGMA) is presented that reconstructs a genealogy or phylogeny of sequences sampled serially in time using a matrix of pairwise distances. The resulting tree depicts the terminal lineages of each sample ending at a different level consistent with the sample's temporal order. Since sUPGMA is a variant of UPGMA, it will perform best when sequences have evolved at a constant rate (i.e., according to a molecular clock). On simulated data, this new method performs better than standard cluster analysis under a variety of longitudinal sampling strategies. Serial-sample UPGMA is particularly useful for analysis of longitudinal samples of viruses and bacteria, as well as ancient DNA samples, with the minimal requirement that samples of sequences be ordered in time.

Differentiating organically and conventionally grown oregano using ultraperformance liquid chromatography mass spectrometry (UPLC-MS), headspace gas chromatography with flame ionization detection (headspace-GC-FID), and flow injection mass spectrum (FIMS) fingerprints combined with multivariate data analysis.

PubMed

Gao, Boyan; Qin, Fang; Ding, Tingting; Chen, Yineng; Lu, Weiying; Yu, Liangli Lucy

2014-08-13

Ultraperformance liquid chromatography mass spectrometry (UPLC-MS), flow injection mass spectrometry (FIMS), and headspace gas chromatography (headspace-GC) combined with multivariate data analysis techniques were examined and compared in differentiating organically grown oregano from that grown conventionally. It is the first time that headspace-GC fingerprinting technology is reported in differentiating organically and conventionally grown spice samples. The results also indicated that UPLC-MS, FIMS, and headspace-GC-FID fingerprints with OPLS-DA were able to effectively distinguish oreganos under different growing conditions, whereas with PCA, only FIMS fingerprint could differentiate the organically and conventionally grown oregano samples. UPLC fingerprinting provided detailed information about the chemical composition of oregano with a longer analysis time, whereas FIMS finished a sample analysis within 1 min. On the other hand, headspace GC-FID fingerprinting required no sample pretreatment, suggesting its potential as a high-throughput method in distinguishing organically and conventionally grown oregano samples. In addition, chemical components in oregano were identified by their molecular weight using QTOF-MS and headspace-GC-MS.

Simulation of time-dispersion spectral device with sample spectra accumulation

NASA Astrophysics Data System (ADS)

Zhdanov, Arseny; Khansuvarov, Ruslan; Korol, Georgy

2014-09-01

This research is conducted in order to design a spectral device for light sources power spectrum analysis. The spectral device should process radiation from sources, direct contact with radiation of which is either impossible or undesirable. Such sources include jet blast of an aircraft, optical radiation in metallurgy and textile industry. In proposed spectral device optical radiation is guided out of unfavorable environment via a piece of optical fiber with high dispersion. It is necessary for analysis to make samples of analyzed radiation as short pulses. Dispersion properties of such optical fiber cause spectral decomposition of input optical pulses. The faster time of group delay vary the stronger the spectral decomposition effect. This effect allows using optical fiber with high dispersion as a major element of proposed spectral device. Duration of sample must be much shorter than group delay time difference of a dispersive system. In the given frequency range this characteristic has to be linear. The frequency range is 400 … 500 THz for typical optical fiber. Using photonic-crystal fiber (PCF) gives much wider spectral range for analysis. In this paper we propose simulation of single pulse transmission through dispersive system with linear dispersion characteristic and quadratic-detected output responses accumulation. During simulation we propose studying influence of optical fiber dispersion characteristic angle on spectral measurement results. We also consider pulse duration and group delay time difference impact on output pulse shape and duration. Results show the most suitable dispersion characteristic that allow choosing the structure of PCF - major element of time-dispersion spectral analysis method and required number of samples for reliable assessment of measured spectrum.

Principal component analysis of TOF-SIMS spectra, images and depth profiles: an industrial perspective

NASA Astrophysics Data System (ADS)

Pacholski, Michaeleen L.

2004-06-01

Principal component analysis (PCA) has been successfully applied to time-of-flight secondary ion mass spectrometry (TOF-SIMS) spectra, images and depth profiles. Although SIMS spectral data sets can be small (in comparison to datasets typically discussed in literature from other analytical techniques such as gas or liquid chromatography), each spectrum has thousands of ions resulting in what can be a difficult comparison of samples. Analysis of industrially-derived samples means the identity of most surface species are unknown a priori and samples must be analyzed rapidly to satisfy customer demands. PCA enables rapid assessment of spectral differences (or lack there of) between samples and identification of chemically different areas on sample surfaces for images. Depth profile analysis helps define interfaces and identify low-level components in the system.

CADDIS Volume 4. Data Analysis: Getting Started

EPA Pesticide Factsheets

Assembling data for an ecological causal analysis, matching biological and environmental samples in time and space, organizing data along conceptual causal pathways, data quality and quantity requirements, Data Analysis references.

Cross-Sectional Analysis of Time-Dependent Data: Mean-Induced Association in Age-Heterogeneous Samples and an Alternative Method Based on Sequential Narrow Age-Cohort Samples

ERIC Educational Resources Information Center

Hofer, Scott M.; Flaherty, Brian P.; Hoffman, Lesa

2006-01-01

The effect of time-related mean differences on estimates of association in cross-sectional studies has not been widely recognized in developmental and aging research. Cross-sectional studies of samples varying in age have found moderate to high levels of shared age-related variance among diverse age-related measures. These findings may be…

Correlation based networks of equity returns sampled at different time horizons

NASA Astrophysics Data System (ADS)

Tumminello, M.; di Matteo, T.; Aste, T.; Mantegna, R. N.

2007-01-01

We investigate the planar maximally filtered graphs of the portfolio of the 300 most capitalized stocks traded at the New York Stock Exchange during the time period 2001 2003. Topological properties such as the average length of shortest paths, the betweenness and the degree are computed on different planar maximally filtered graphs generated by sampling the returns at different time horizons ranging from 5 min up to one trading day. This analysis confirms that the selected stocks compose a hierarchical system progressively structuring as the sampling time horizon increases. Finally, a cluster formation, associated to economic sectors, is quantitatively investigated.

Rapid-Viability PCR Method for Detection of Live, Virulent Bacillus anthracis in Environmental Samples ▿

PubMed Central

Létant, Sonia E.; Murphy, Gloria A.; Alfaro, Teneile M.; Avila, Julie R.; Kane, Staci R.; Raber, Ellen; Bunt, Thomas M.; Shah, Sanjiv R.

2011-01-01

In the event of a biothreat agent release, hundreds of samples would need to be rapidly processed to characterize the extent of contamination and determine the efficacy of remediation activities. Current biological agent identification and viability determination methods are both labor- and time-intensive such that turnaround time for confirmed results is typically several days. In order to alleviate this issue, automated, high-throughput sample processing methods were developed in which real-time PCR analysis is conducted on samples before and after incubation. The method, referred to as rapid-viability (RV)-PCR, uses the change in cycle threshold after incubation to detect the presence of live organisms. In this article, we report a novel RV-PCR method for detection of live, virulent Bacillus anthracis, in which the incubation time was reduced from 14 h to 9 h, bringing the total turnaround time for results below 15 h. The method incorporates a magnetic bead-based DNA extraction and purification step prior to PCR analysis, as well as specific real-time PCR assays for the B. anthracis chromosome and pXO1 and pXO2 plasmids. A single laboratory verification of the optimized method applied to the detection of virulent B. anthracis in environmental samples was conducted and showed a detection level of 10 to 99 CFU/sample with both manual and automated RV-PCR methods in the presence of various challenges. Experiments exploring the relationship between the incubation time and the limit of detection suggest that the method could be further shortened by an additional 2 to 3 h for relatively clean samples. PMID:21764960

QuickNGS elevates Next-Generation Sequencing data analysis to a new level of automation.

PubMed

Wagle, Prerana; Nikolić, Miloš; Frommolt, Peter

2015-07-01

Next-Generation Sequencing (NGS) has emerged as a widely used tool in molecular biology. While time and cost for the sequencing itself are decreasing, the analysis of the massive amounts of data remains challenging. Since multiple algorithmic approaches for the basic data analysis have been developed, there is now an increasing need to efficiently use these tools to obtain results in reasonable time. We have developed QuickNGS, a new workflow system for laboratories with the need to analyze data from multiple NGS projects at a time. QuickNGS takes advantage of parallel computing resources, a comprehensive back-end database, and a careful selection of previously published algorithmic approaches to build fully automated data analysis workflows. We demonstrate the efficiency of our new software by a comprehensive analysis of 10 RNA-Seq samples which we can finish in only a few minutes of hands-on time. The approach we have taken is suitable to process even much larger numbers of samples and multiple projects at a time. Our approach considerably reduces the barriers that still limit the usability of the powerful NGS technology and finally decreases the time to be spent before proceeding to further downstream analysis and interpretation of the data.

Preanalytical influence of pneumatic tube delivery system on results of routine biochemistry and haematology analysis.

PubMed

Petit, Morgane; Mine, Louis; Pascreau, Tiffany; Brouzes, Chantal; Majoux, Sandrine; Borgel, Delphine; Beaudeux, Jean-Louis; Lasne, Dominique; Hennequin, Carole

2017-12-01

Pneumatic tube delivery system (PTS) enables to reduce considerably turnaround times. The aim of the study was to assess the influence of the PTS on the quality of routine biochemical and hematological tests in our laboratory. Blood samples from 6 hospitalized patients and 8 healthy volunteers were analyzed. Blood samples were delivered to the laboratory by a PTS and by a human courier. We performed the following analysis: ionized calcium, sodium, potassium, lactate deshydrogenase (LDH), aspartate aminotransferase (ASAT), arterial blood gas, complete blood count and coagulation test as prothrombin time, activated partial thromboplastin time, factors V and VIII. Results were compared between the both method of transport according to the recommendation of the Société française de biologie clinique and the French committee for accreditation (SH-GTA01, norme NF ISO 5275-6). The hemolysis index of plasma was similar between the groups and no morphological differences were found on blood cells. For three samples, when delivered by PTS, LDH levels (two samples) and neutrophil polynuclear count (one sample) were above the recommended guidelines compared to those delivered by courier. Conversely, LDH levels and FVIII were below in two samples delivered by PTS. LDH levels, PNN count or factor VIII can be affected by PTS without the clinical interpretation being modified. We concluded that the PTS can be used to transport blood samples for routine biochemical and hematological analysis in our hospital.

Ultra‐high performance supercritical fluid chromatography of lignin‐derived phenols from alkaline cupric oxide oxidation

PubMed Central

Sun, Mingzhe; Lidén, Gunnar; Sandahl, Margareta

2016-01-01

Traditional chromatographic methods for the analysis of lignin‐derived phenolic compounds in environmental samples are generally time consuming. In this work, an ultra‐high performance supercritical fluid chromatography method with a diode array detector for the analysis of major lignin‐derived phenolic compounds produced by alkaline cupric oxide oxidation was developed. In an analysis of a collection of 11 representative monomeric lignin phenolic compounds, all compounds were clearly separated within 6 min with excellent peak shapes, with a limit of detection of 0.5–2.5 μM, a limit of quantification of 2.5–5.0 μM, and a dynamic range of 5.0–2.0 mM (R 2 > 0.997). The new ultra‐high performance supercritical fluid chromatography method was also applied for the qualitative and quantitative analysis of lignin‐derived phenolic compounds obtained upon alkaline cupric oxide oxidation of a commercial humic acid. Ten out of the previous eleven model compounds could be quantified in the oxidized humic acid sample. The high separation power and short analysis time obtained demonstrate for the first time that supercritical fluid chromatography is a fast and reliable technique for the analysis of lignin‐derived phenols in complex environmental samples. PMID:27452148

Impact of urine preservation methods and duration of storage on measured levels of environmental contaminants.

PubMed

Hoppin, Jane A; Ulmer, Ross; Calafat, Antonia M; Barr, Dana B; Baker, Susan V; Meltzer, Helle M; Rønningen, Kjersti S

2006-01-01

Collection of urine samples in human studies involves choices regarding shipping, sample preservation, and storage that may ultimately influence future analysis. As more studies collect and archive urine samples to evaluate environmental exposures in the future, we were interested in assessing the impact of urine preservative, storage temperature, and time since collection on nonpersistent contaminants in urine samples. In spiked urine samples stored in three types of urine vacutainers (no preservative, boric acid, and chlorhexidine), we measured five groups of contaminants to assess the levels of these analytes at five time points (0, 24, 48, and 72 h, and 1 week) and at two temperatures (room temperature and 4 degrees C). The target chemicals were bisphenol A (BPA), metabolites of organophosphate (OP), carbamate, and pyrethroid insecticides, chlorinated phenols, and phthalate monoesters, and were measured using five different mass spectrometry-based methods. Three samples were analyzed at each time point, with the exception of BPA. Repeated measures analysis of variance was used to evaluate effects of storage time, temperature, and preservative. Stability was summarized with percent change in mean concentration from time 0. In general, most analytes were stable under all conditions with changes in mean concentration over time, temperature, and preservative being generally less than 20%, with the exception of the OP metabolites in the presence of boric acid. The effect of storage temperature was less important than time since collection. The precision of the laboratory measurements was high allowing us to observe small differences, which may not be important when categorizing individuals into broader exposure groups.

Qualitative analysis of Pb liquid sample using laser-induced breakdown spectroscopy (LIBS)

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

Suyanto, Hery; Rupiasih, Ni Nyoman; Winardi, T. B.

2013-09-03

Qualitative analysis of liquid sample containing 1,000 ppm of Pb was performed by using LIBS technique. In order to avoid splashing off of the liquid sample during laser irradiation, a sample pretreatment was done, namely the liquid sample was absorbed by using commercial available stomach medicine. Two kinds of absorbent materials were chosen in this experiment, first containing 125 mg activated carbon and second 600 mg activated attapulgite. These absorbent materials were used since carbon sample gives better absorption of infrared laser irradiation used in this experiment. In order to characterize the absorption process, three treatments were conducted in thismore » experiment; first, without heating the sample but varying the absorption time before laser irradiation; second by varying the heating temperature after certain time of absorption process and third by varying the temperature only. The maximum emission intensity of Pb I 405.7 nm was found in the second treatment of heating the sample till 85°C after 30 minutes absorption of the liquid sample in both absorbent materials.« less

Automated Microflow NMR: Routine Analysis of Five-Microliter Samples

PubMed Central

Jansma, Ariane; Chuan, Tiffany; Geierstanger, Bernhard H.; Albrecht, Robert W.; Olson, Dean L.; Peck, Timothy L.

2006-01-01

A microflow CapNMR probe double-tuned for 1H and 13C was installed on a 400-MHz NMR spectrometer and interfaced to an automated liquid handler. Individual samples dissolved in DMSO-d6 are submitted for NMR analysis in vials containing as little as 10 μL of sample. Sets of samples are submitted in a low-volume 384-well plate. Of the 10 μL of sample per well, as with vials, 5 μL is injected into the microflow NMR probe for analysis. For quality control of chemical libraries, 1D NMR spectra are acquired under full automation from 384-well plates on as many as 130 compounds within 24 h using 128 scans per spectrum and a sample-to-sample cycle time of ∼11 min. Because of the low volume requirements and high mass sensitivity of the microflow NMR system, 30 nmol of a typical small molecule is sufficient to obtain high-quality, well-resolved, 1D proton or 2D COSY NMR spectra in ∼6 or 20 min of data acquisition time per experiment, respectively. Implementation of pulse programs with automated solvent peak identification and suppression allow for reliable data collection, even for samples submitted in fully protonated DMSO. The automated microflow NMR system is controlled and monitored using web-based software. PMID:16194121

Offline solid phase microextraction sampling system

DOEpatents

Harvey, Chris A.

2008-12-16

An offline solid phase microextraction (SPME) sampling apparatus for enabling SPME samples to be taken a number of times from a previously collected fluid sample (e.g. sample atmosphere) stored in a fused silica lined bottle which keeps volatile organics in the fluid sample stable for weeks at a time. The offline SPME sampling apparatus has a hollow body surrounding a sampling chamber, with multiple ports through which a portion of a previously collected fluid sample may be (a) released into the sampling chamber, (b) SPME sampled to collect analytes for subsequent GC analysis, and (c) flushed/purged using a fluidically connected vacuum source and purging fluid source to prepare the sampling chamber for additional SPME samplings of the same original fluid sample, such as may have been collected in situ from a headspace.

Piecewise multivariate modelling of sequential metabolic profiling data.

PubMed

Rantalainen, Mattias; Cloarec, Olivier; Ebbels, Timothy M D; Lundstedt, Torbjörn; Nicholson, Jeremy K; Holmes, Elaine; Trygg, Johan

2008-02-19

Modelling the time-related behaviour of biological systems is essential for understanding their dynamic responses to perturbations. In metabolic profiling studies, the sampling rate and number of sampling points are often restricted due to experimental and biological constraints. A supervised multivariate modelling approach with the objective to model the time-related variation in the data for short and sparsely sampled time-series is described. A set of piecewise Orthogonal Projections to Latent Structures (OPLS) models are estimated, describing changes between successive time points. The individual OPLS models are linear, but the piecewise combination of several models accommodates modelling and prediction of changes which are non-linear with respect to the time course. We demonstrate the method on both simulated and metabolic profiling data, illustrating how time related changes are successfully modelled and predicted. The proposed method is effective for modelling and prediction of short and multivariate time series data. A key advantage of the method is model transparency, allowing easy interpretation of time-related variation in the data. The method provides a competitive complement to commonly applied multivariate methods such as OPLS and Principal Component Analysis (PCA) for modelling and analysis of short time-series data.

Optimisation and validation of a rapid and efficient microemulsion liquid chromatographic (MELC) method for the determination of paracetamol (acetaminophen) content in a suppository formulation.

PubMed

McEvoy, Eamon; Donegan, Sheila; Power, Joe; Altria, Kevin

2007-05-09

A rapid and efficient oil-in-water microemulsion liquid chromatographic method has been optimised and validated for the analysis of paracetamol in a suppository formulation. Excellent linearity, accuracy, precision and assay results were obtained. Lengthy sample pre-treatment/extraction procedures were eliminated due to the solubilising power of the microemulsion and rapid analysis times were achieved. The method was optimised to achieve rapid analysis time and relatively high peak efficiencies. A standard microemulsion composition of 33 g SDS, 66 g butan-1-ol, 8 g n-octane in 1l of 0.05% TFA modified with acetonitrile has been shown to be suitable for the rapid analysis of paracetamol in highly hydrophobic preparations under isocratic conditions. Validated assay results and overall analysis time of the optimised method was compared to British Pharmacopoeia reference methods. Sample preparation and analysis times for the MELC analysis of paracetamol in a suppository were extremely rapid compared to the reference method and similar assay results were achieved. A gradient MELC method using the same microemulsion has been optimised for the resolution of paracetamol and five of its related substances in approximately 7 min.

Novel Laser-Based Technique is Ideal for Real-Time Environmental Analysis

ERIC Educational Resources Information Center

Journal of Chemical Education, 2005

2005-01-01

Ocean Optics offers laser-induced breakdown spectrometer systems (LIBS) that can be used to identify light to heavy metals in a variety of sample types and geometries in environmental analysis applications. LIBS are versatile, real-time, high-resolution analyzers for qualitative analysis, in less than one second, of every element in solids,…

Determination of the aflatoxin AFB1 from corn by direct analysis in real time-mass spectrometry (DART-MS)

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to a high resolution mass spectrometer (MS) was used for screening of aflatoxins from a variety of surfaces and the rapid quantitative analysis of a common form of aflatoxin, AFB1, extracted from corn. Sample preparation procedure and instrument...

Determination of T-2 and HT-2 toxins from maize by direct analysis in real time mass spectrometry

USDA-ARS?s Scientific Manuscript database

Direct analysis in real time (DART) ionization coupled to mass spectrometry (MS) was used for the rapid quantitative analysis of T-2 toxin, and the related HT-2 toxin, extracted from corn. Sample preparation procedures and instrument parameters were optimized to obtain sensitive and accurate determi...

Stochastic Stability of Nonlinear Sampled Data Systems with a Jump Linear Controller

NASA Technical Reports Server (NTRS)

Gonzalez, Oscar R.; Herencia-Zapana, Heber; Gray, W. Steven

2004-01-01

This paper analyzes the stability of a sampled- data system consisting of a deterministic, nonlinear, time- invariant, continuous-time plant and a stochastic, discrete- time, jump linear controller. The jump linear controller mod- els, for example, computer systems and communication net- works that are subject to stochastic upsets or disruptions. This sampled-data model has been used in the analysis and design of fault-tolerant systems and computer-control systems with random communication delays without taking into account the inter-sample response. To analyze stability, appropriate topologies are introduced for the signal spaces of the sampled- data system. With these topologies, the ideal sampling and zero-order-hold operators are shown to be measurable maps. This paper shows that the known equivalence between the stability of a deterministic, linear sampled-data system and its associated discrete-time representation as well as between a nonlinear sampled-data system and a linearized representation holds even in a stochastic framework.

Current Protocols in Pharmacology

PubMed Central

2016-01-01

Determination of drug or drug metabolite concentrations in biological samples, particularly in serum or plasma, is fundamental to describing the relationships between administered dose, route of administration, and time after dose to the drug concentrations achieved and to the observed effects of the drug. A well-characterized, accurate analytical method is needed, but it must also be established that the analyte concentration in the sample at the time of analysis is the same as the concentration at sample acquisition. Drugs and metabolites may be susceptible to degradation in samples due to metabolism or to physical and chemical processes, resulting in a lower measured concentration than was in the original sample. Careful examination of analyte stability during processing and storage and adjustment of procedures and conditions to maximize that stability are a critical part of method validation for the analysis, and can ensure the accuracy of the measured concentrations. PMID:27960029

Application of Raman spectroscopy for on-line monitoring of low dose blend uniformity.

PubMed

Hausman, Debra S; Cambron, R Thomas; Sakr, Adel

2005-07-14

On-line Raman spectroscopy was used to evaluate the effect of blending time on low dose, 1%, blend uniformity of azimilide dihydrochloride. An 8 qt blender was used for the experiments and instrumented with a Raman probe through the I-bar port. The blender was slowed to 6.75 rpm to better illustrate the blending process (normal speed is 25 rpm). Uniformity was reached after 20 min of blending at 6.75 rpm (135 revolutions or 5.4 min at 25 rpm). On-line Raman analysis of blend uniformity provided more benefits than traditional thief sampling and off-line analysis. On-line Raman spectroscopy enabled generating data rich blend profiles, due to the ability to collect a large number of samples during the blending process (sampling every 20s). In addition, the Raman blend profile was rapidly generated, compared to the lengthy time to complete a blend profile with thief sampling and off-line analysis. The on-line Raman blend uniformity results were also significantly correlated (p-value < 0.05) to the HPLC uniformity results of thief samples.

Quantitative Methods for Analysing Joint Questionnaire Data: Exploring the Role of Joint in Force Design

DTIC Science & Technology

2015-08-01

the nine questions. The Statistical Package for the Social Sciences ( SPSS ) [11] was used to conduct statistical analysis on the sample. Two types...constructs. SPSS was again used to conduct statistical analysis on the sample. This time factor analysis was conducted. Factor analysis attempts to...Business Research Methods and Statistics using SPSS . P432. 11 IBM SPSS Statistics . (2012) 12 Burns, R.B., Burns, R.A. (2008) ‘Business Research

Hierarchical model analysis of the Atlantic Flyway Breeding Waterfowl Survey

USGS Publications Warehouse

Sauer, John R.; Zimmerman, Guthrie S.; Klimstra, Jon D.; Link, William A.

2014-01-01

We used log-linear hierarchical models to analyze data from the Atlantic Flyway Breeding Waterfowl Survey. The survey has been conducted by state biologists each year since 1989 in the northeastern United States from Virginia north to New Hampshire and Vermont. Although yearly population estimates from the survey are used by the United States Fish and Wildlife Service for estimating regional waterfowl population status for mallards (Anas platyrhynchos), black ducks (Anas rubripes), wood ducks (Aix sponsa), and Canada geese (Branta canadensis), they are not routinely adjusted to control for time of day effects and other survey design issues. The hierarchical model analysis permits estimation of year effects and population change while accommodating the repeated sampling of plots and controlling for time of day effects in counting. We compared population estimates from the current stratified random sample analysis to population estimates from hierarchical models with alternative model structures that describe year to year changes as random year effects, a trend with random year effects, or year effects modeled as 1-year differences. Patterns of population change from the hierarchical model results generally were similar to the patterns described by stratified random sample estimates, but significant visibility differences occurred between twilight to midday counts in all species. Controlling for the effects of time of day resulted in larger population estimates for all species in the hierarchical model analysis relative to the stratified random sample analysis. The hierarchical models also provided a convenient means of estimating population trend as derived statistics from the analysis. We detected significant declines in mallard and American black ducks and significant increases in wood ducks and Canada geese, a trend that had not been significant for 3 of these 4 species in the prior analysis. We recommend using hierarchical models for analysis of the Atlantic Flyway Breeding Waterfowl Survey.

Metabolic profiling of rat hair and screening biomarkers using ultra performance liquid chromatography with electrospray ionization time-of-flight mass spectrometry.

PubMed

Inagaki, Shinsuke; Noda, Takumi; Min, Jun Zhe; Toyo'oka, Toshimasa

2007-12-28

An exhaustive analysis of metabolites in hair samples has been performed for the first time using ultra performance liquid chromatography with electrospray ionization time-of-flight mass spectrometry (UPLC-ESI-TOF-MS). The hair samples were collected from spontaneously hypertensive model rats (SHR/Izm), stroke-prone SHR (SHRSP/Izm) and Wistar Kyoto (WKY/Izm) rats, and were analyzed by UPLC-ESI-TOF-MS; a multivariate statistical analysis method, such as the principal component analysis (PCA), was then used for screening the biomarkers. From the samples derived from the group of SHRSP/Izm at weeks 10, 18, 26 and 34, we successfully detected a potential biomarker of stroke, which existed at much higher concentrations as compared with that in the other groups. However, a significant difference could not be found at weeks less than 7 before the rats were subjected to stroke and hypertension. In addition, the present method was applicable to screening not only the disease markers, but also the markers related to aging. The method utilizing hair samples is expected to be quite useful for screening biomarkers of many other diseases, and not limited to stroke and hypertension.

Evaluation of volatile aldehydes as discriminating parameters in quality vinegars with protected European geographical indication.

PubMed

Durán-Guerrero, Enrique; Chinnici, Fabio; Natali, Nadia; Riponi, Claudio

2015-09-01

Thirty-six high-quality vinegars with geographical indication belonging to Sherry and Modena areas (vinegars of Jerez, balsamic vinegars of Modena and traditional balsamic vinegars of Modena) with all possible aging periods were analyzed to determine the content of volatile aldehydes. A solid-phase extraction method with in-cartridge derivatization using O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine followed by gas chromatography-mass spectrometry was employed. Twenty-two volatile aldehydes were identified and determined in the samples. Analysis of variance provided significant differences among the samples as a function of the type of vinegar, aging time and raw material. Principal component analysis and linear discriminant analysis demonstrated the possibility of discriminating the samples in terms of aging time and raw material. Linear aldehydes and compounds such as furfural, methional, nonenal, hexenal, 2-methylbutanal and i-butyraldehyde were the most significant variables able to discriminate the samples. Aldehyde content of premium quality vinegars is a function of both ageing time and raw material. Their evaluation could be a useful tool with a view to ascertaining vinegar origin and genuineness. © 2014 Society of Chemical Industry.

Coagulation dynamics of a blood sample by multiple scattering analysis

NASA Astrophysics Data System (ADS)

Faivre, Magalie; Peltié, Philippe; Planat-Chrétien, Anne; Cosnier, Marie-Line; Cubizolles, Myriam; Nougier, Christophe; Négrier, Claude; Pouteau, Patrick

2011-05-01

We report a new technique to measure coagulation dynamics on whole-blood samples. The method relies on the analysis of the speckle figure resulting from a whole-blood sample mixed with coagulation reagent and introduced in a thin chamber illuminated with a coherent light. A dynamic study of the speckle reveals a typical behavior due to coagulation. We compare our measured coagulation times to a reference method obtained in a medical laboratory.

Rapid detection of Opisthorchis viverrini and Strongyloides stercoralis in human fecal samples using a duplex real-time PCR and melting curve analysis.

PubMed

Janwan, Penchom; Intapan, Pewpan M; Thanchomnang, Tongjit; Lulitanond, Viraphong; Anamnart, Witthaya; Maleewong, Wanchai

2011-12-01

Human opisthorchiasis caused by the liver fluke Opisthorchis viverrini is an endemic disease in Southeast Asian countries including the Lao People's Democratic Republic, Cambodia, Vietnam, and Thailand. Infection with the soil-transmitted roundworm Strongyloides stercoralis is an important problem worldwide. In some areas, both parasitic infections are reported as co-infections. A duplex real-time fluorescence resonance energy transfer (FRET) PCR merged with melting curve analysis was developed for the rapid detection of O. viverrini and S. stercoralis in human fecal samples. Duplex real-time FRET PCR is based on fluorescence melting curve analysis of a hybrid of amplicons generated from two genera of DNA elements: the 162 bp pOV-A6 DNA sequence specific to O. viverrini and the 244 bp 18S rRNA sequence specific to S. stercoralis, and two pairs of specific fluorophore-labeled probes. Both O. viverrini and S. stercoralis can be differentially detected in infected human fecal samples by this process through their different fluorescence channels and melting temperatures. Detection limit of the method was as little as two O. viverrini eggs and four S. stercoralis larvae in 100 mg of fecal sample. The assay could distinguish the DNA of both parasites from the DNA of negative fecal samples and fecal samples with other parasite materials, as well as from the DNA of human leukocytes and other control parasites. The technique showed 100% sensitivity and specificity. The introduced duplex real-time FRET PCR can reduce labor time and reagent costs and is not prone to carry over contamination. The method is important for simultaneous detection especially in areas where both parasites overlap incidence and is useful as the screening tool in the returning travelers and immigrants to industrialized countries where number of samples in the diagnostic units will become increasing.

Multivariate survivorship analysis using two cross-sectional samples.

PubMed

Hill, M E

1999-11-01

As an alternative to survival analysis with longitudinal data, I introduce a method that can be applied when one observes the same cohort in two cross-sectional samples collected at different points in time. The method allows for the estimation of log-probability survivorship models that estimate the influence of multiple time-invariant factors on survival over a time interval separating two samples. This approach can be used whenever the survival process can be adequately conceptualized as an irreversible single-decrement process (e.g., mortality, the transition to first marriage among a cohort of never-married individuals). Using data from the Integrated Public Use Microdata Series (Ruggles and Sobek 1997), I illustrate the multivariate method through an investigation of the effects of race, parity, and educational attainment on the survival of older women in the United States.

Rapid quantification and sex determination of forensic evidence materials.

PubMed

Andréasson, Hanna; Allen, Marie

2003-11-01

DNA quantification of forensic evidence is very valuable for an optimal use of the available biological material. Moreover, sex determination is of great importance as additional information in criminal investigations as well as in identification of missing persons, no suspect cases, and ancient DNA studies. While routine forensic DNA analysis based on short tandem repeat markers includes a marker for sex determination, analysis of samples containing scarce amounts of DNA is often based on mitochondrial DNA, and sex determination is not performed. In order to allow quantification and simultaneous sex determination on minute amounts of DNA, an assay based on real-time PCR analysis of a marker within the human amelogenin gene has been developed. The sex determination is based on melting curve analysis, while an externally standardized kinetic analysis allows quantification of the nuclear DNA copy number in the sample. This real-time DNA quantification assay has proven to be highly sensitive, enabling quantification of single DNA copies. Although certain limitations were apparent, the system is a rapid, cost-effective, and flexible assay for analysis of forensic casework samples.

Estimation of transit times in a Karst Aquifer system using environmental tracers: Application on the Jeita Aquifer system-Lebanon.

NASA Astrophysics Data System (ADS)

Doummar, Joanna; Hamdan, Ahmad

2016-04-01

Estimating transit times is essential for the assessment of aquifer vulnerability to contaminants. Groundwater in karst aquifer is assumed to be relatively young due to fast preferential pathways; slow flow components are present in water stored in the fissured matrix. Furthermore, transit times are site specific as they depend on recharge rates, temperatures, elevation, and flow media; saturated and unsaturated zones. These differences create significant variation in the groundwater age in karst systems as the water sampled will be a mix of different water that has been transported through different flow pathways (fissured matrix and conduits). Several methods can be applied to estimate water transit time of an aquifer such as artificial tracers, which provide an estimate for fast flow velocities. In this study, groundwater residence times in the Jeita spring aquifer (Lebanon) were estimated using several environmental tracers such as Chlorofluorocarbons (CFCs), Sulfur Hexafluoride (SF6), Helium-Tritium (3H, 3H- 3He). Additional stable isotope and major ion analysis was performed to characterize water types. Groundwater samples were collected from six different wells in the Jeita catchment area (Jurassic Kesrouane aquifer) as well as from the spring and cave itself. The results are reproducible for the Tritium-Helium method, unlike for the CFC/SF6 methods that yielded poor results due to sampling problems. Tritium concentrations in all groundwater samples show nearly the same concentration (~2.73 TU) except for one sample with relatively lower tritium concentration (~2.26 TU). Ages ranging from 0.07 ± 0.07 years to 23.59 ± 0.00 years were obtained. The youngest age is attributed to the spring/ cave while the oldest ages were obtained in wells tapping the fissured matrix. Neon in these samples showed considerable variations and high delta Ne in some samples indicating high excess air. Four (4) samples showed extreme excess air (Delta-Ne is greater than 70 %) and the remaining 3 samples have Delta-Ne in the expected range between (10-35%). Moreover Tritium-Helium analysis has showed some radiogenic Helium (4He) in one sample along with lower tritium concentrations signifying a mixture of new groundwater with old groundwater (older than 50 yrs). Furthermore, this study is complemented with published analysis of a series of 26 artificial tracer experiments performed in the Jeita karst system (Doummar, 2012). Transit times calculated from tracer experiments ranged between 3 and 300 hours (12 days). The shortest ones were recorded in the Jeita subsurface conduit. While injections in sinkholes yielded moderate transit times, fissured matrix and unsaturated zone resulted in relatively long ones. In Lebanon this type of spatial groundwater age dating using environmental tracers was not applied to date, to the exception of grab sample analysis. A second round of sampling for Tritium-Helium, CFCs and SF6 analysis will be undertaken under different flow periods in February 2016 to validate the obtained results. References Geyer, T. 2008: Process-based characterization of flow and transport in karst aquifers at catchment scale. Dissertation, Georg-August-Universität Göttingen, 103 S. Geyer, T., and Doummar, J. 2013. Protection of the Jeita Spring: Bestimmung der mittleren Verweilzeit des Grundwassers im Einzugsgebiet der Jeita Quelle-Libanon. Special report. Protection of the Jeita Spring. Applied Geosciences. Georg August University, Göttingen.

Direct Analysis in Real Time-Mass Spectrometry for the Rapid Detection of Metabolites of Aconite Alkaloids in Intestinal Bacteria

NASA Astrophysics Data System (ADS)

Li, Xue; Hou, Guangyue; Xing, Junpeng; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

2014-12-01

In the present work, direct analysis of real time ionization combined with multi-stage tandem mass spectrometry (DART-MSn) was used to investigate the metabolic profile of aconite alkaloids in rat intestinal bacteria. A total of 36 metabolites from three aconite alkaloids were identified by using DART-MSn, and the feasibility of quantitative analysis of these analytes was examined. Key parameters of the DART ion source, such as helium gas temperature and pressure, the source-to-MS distance, and the speed of the autosampler, were optimized to achieve high sensitivity, enhance reproducibility, and reduce the occurrence of fragmentation. The instrument analysis time for one sample can be less than 10 s for this method. Compared with ESI-MS and UPLC-MS, the DART-MS is more efficient for directly detecting metabolic samples, and has the advantage of being a simple, high-speed, high-throughput method.

Direct analysis in real time-mass spectrometry for the rapid detection of metabolites of aconite alkaloids in intestinal bacteria.

PubMed

Li, Xue; Hou, Guangyue; Xing, Junpeng; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

2014-12-01

In the present work, direct analysis of real time ionization combined with multi-stage tandem mass spectrometry (DART-MS(n)) was used to investigate the metabolic profile of aconite alkaloids in rat intestinal bacteria. A total of 36 metabolites from three aconite alkaloids were identified by using DART-MS(n), and the feasibility of quantitative analysis of these analytes was examined. Key parameters of the DART ion source, such as helium gas temperature and pressure, the source-to-MS distance, and the speed of the autosampler, were optimized to achieve high sensitivity, enhance reproducibility, and reduce the occurrence of fragmentation. The instrument analysis time for one sample can be less than 10 s for this method. Compared with ESI-MS and UPLC-MS, the DART-MS is more efficient for directly detecting metabolic samples, and has the advantage of being a simple, high-speed, high-throughput method.

[The Role of Segmental Analysis of Clonazepam in Hair in Drug Facilitated Cases].

PubMed

Chen, H; Xiang, P; Shen, M

2017-06-01

To infer the frequency of dosage and medication history investigate of the victims in drug facilitated cases by the segmental analysis of clonazepam in hair. Freezing milling under liquid nitrogen environment combined with ultrasonic bath was used as sample pretreatment in this study, and liquid chromatography-tandem mass spectrometry was used for the segmental analysis of the hair samples collected from 6 victims in different cases. The concentrations of clonazepam and 7-aminoclonazepam were detected in each hair section. Clonazepam and its metabolite 7-aminoclonazepam were detected in parts of hair sections from the 6 victims. The occurrence time of drug peak concentration was consistent with the intake timing provided by victims. Segmental analysis of hair can provide the information of frequency of dosage and intake timing, which shows an unique evidential value in drug facilitated crimes. Copyright© by the Editorial Department of Journal of Forensic Medicine

Use of on-site high performance liquid chromatography to evaluate the magnitude and extent of organic contaminants in aquifers

USGS Publications Warehouse

Goerlitz, D.F.; Franks, B.J.

1989-01-01

Appraisal of ground water contaminated by organic substances raises problems of difficult sample collection and timely chemical analysis. High-performance liquid chromatography was evaluated for on-site determination of specific organic contaminants in ground water samples and was used at three study sites. Organic solutes were determined directly in water samples, with little or no preparation, and usually in less than an hour after collection. This information improved sampling efficiency and was useful in screening for subsequent laboratory analysis. On two occasions, on-site analysis revealed that samples were undergoing rapid change, with major solutes being upgraded and alteration products being formed. In addition to sample stability, this technique proved valuable for monitoring other sampling factors such as compositional changes with respect to pumping, filtration, and cross contamination. -Authors

Solvent Hold Tank Sample Results for MCU-16-1247-1248-1249: August 2016 Monthly Sample

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

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-1247-1248-1249), pulled on 08/22/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1247-1248-1249 indicated the Isopar™L concentration is above its nominal level (101%). The extractant (MaxCalix) and the modifier (CS-7SB) are 7% and 9 % below their nominal concentrations. The suppressor (TiDG) is 63% below its nominal concentration. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier and MaxCalix to restore then to nominal levels. Based on the current monthly sample, the levelsmore » of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. At the time of writing this report, A solvent trim batch containing TiDG, modifier and MaxCalix, was added to the SHT (October 2016) and expect the concentration of these components to be at their nominal values.« less

Integrated chemical/biochemical sample collection, pre-concentration, and analysis on a digital microfluidic lab-on-a-chip platform

NASA Astrophysics Data System (ADS)

Fair, Richard B.; Khlystov, A.; Srinivasan, Vijay; Pamula, Vamsee K.; Weaver, Kathryn N.

2004-12-01

An ideal on-site chemical/biochemical analysis system must be inexpensive, sensitive, fully automated and integrated, reliable, and compatible with a broad range of samples. The advent of digital microfluidic lab-on-a-chip (LoC) technology offers such a detection system due to the advantages in portability, reduction of the volumes of the sample and reagents, faster analysis times, increased automation, low power consumption, compatibility with mass manufacturing, and high throughput. We describe progress towards integrating sample collection onto a digital microfluidic LoC that is a component of a cascade impactor device. The sample collection is performed by impacting airborne particles directly onto the surface of the chip. After the collection phase, the surface of the chip is washed with a micro-droplet of solvent. The droplet will be digitally directed across the impaction surface, dissolving sample constituents. Because of the very small droplet volume used for extraction of the sample from a wide colection area, the resulting solution is realatively concentrated and the analytes can be detected after a very short sampling time (1 min) due to such pre-concentration. After the washing phase, the droplet is mixed with specific reagents that produce colored reaction products. The concentration of the analyte is quantitatively determined by measuring absorption at target wavelengths using a simple light emitting diode and photodiode setup. Specific applications include automatic measurements of major inorganic ions in aerosols, such as sulfate, nitrate and ammonium, with a time resolution of 1 min and a detection limit of 30 nm/m3. We have already demonstrated the detection and quantification of nitroaromatic explosives without integrating the sample collection. Other applications being developed include airborne bioagent detection.

Development of automated high throughput single molecular microfluidic detection platform for signal transduction analysis

NASA Astrophysics Data System (ADS)

Huang, Po-Jung; Baghbani Kordmahale, Sina; Chou, Chao-Kai; Yamaguchi, Hirohito; Hung, Mien-Chie; Kameoka, Jun

2016-03-01

Signal transductions including multiple protein post-translational modifications (PTM), protein-protein interactions (PPI), and protein-nucleic acid interaction (PNI) play critical roles for cell proliferation and differentiation that are directly related to the cancer biology. Traditional methods, like mass spectrometry, immunoprecipitation, fluorescence resonance energy transfer, and fluorescence correlation spectroscopy require a large amount of sample and long processing time. "microchannel for multiple-parameter analysis of proteins in single-complex (mMAPS)"we proposed can reduce the process time and sample volume because this system is composed by microfluidic channels, fluorescence microscopy, and computerized data analysis. In this paper, we will present an automated mMAPS including integrated microfluidic device, automated stage and electrical relay for high-throughput clinical screening. Based on this result, we estimated that this automated detection system will be able to screen approximately 150 patient samples in a 24-hour period, providing a practical application to analyze tissue samples in a clinical setting.

Detection of airborne genetically modified maize pollen by real-time PCR.

PubMed

Folloni, Silvia; Kagkli, Dafni-Maria; Rajcevic, Bojan; Guimarães, Nilson C C; Van Droogenbroeck, Bart; Valicente, Fernando H; Van den Eede, Guy; Van den Bulcke, Marc

2012-09-01

The cultivation of genetically modified (GM) crops has raised numerous concerns in the European Union and other parts of the world about their environmental and economic impact. Especially outcrossing of genetically modified organisms (GMO) was from the beginning a critical issue as airborne pollen has been considered an important way of GMO dispersal. Here, we investigate the use of airborne pollen sampling combined with microscopic analysis and molecular PCR analysis as an approach to monitor GM maize cultivations in a specific area. Field trial experiments in the European Union and South America demonstrated the applicability of the approach under different climate conditions, in rural and semi-urban environment, even at very low levels of airborne pollen. The study documents in detail the sampling of GM pollen, sample DNA extraction and real-time PCR analysis. Our results suggest that this 'GM pollen monitoring by bioaerosol sampling and PCR screening' approach might represent an useful aid in the surveillance of GM-free areas, centres of origin and natural reserves. © 2012 Blackwell Publishing Ltd.

Evaporator Feed Qualification Analysis Of Tank 38H And 43H Samples: January 2010 Through April 2013

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

Martino, C. J.; Coleman, C. J.

2013-08-21

This report provides the results of analyses that focused on the chemical species that pertain to the sodium aluminosilicate formation potential for archived Tank 38H and 43H subsurface samples from January 2010 through April 2013. Analyses included warm acid strike preparation followed by analysis of silicon, aluminum, and sodium and water dilution preparation followed by analysis for anions. The Tank 43H and 38H supernatant liquid silicon measurements for the January 2010 through April 2013 time period exhibit a slight increasing trend. Over this time period, the silicon concentration in the Tank 43H and Tank 38H samples averaged 179 mg/L andmore » 235 mg/L, respectively. Comparison of Tank 43H sample results from 2005 through April 2013 to the previously developed process control models indicates that the current formation of sodium aluminosilicate in the 2H system is due to the seeded direct precipitation of cancrinite and sodalite.« less

An optimization based sampling approach for multiple metrics uncertainty analysis using generalized likelihood uncertainty estimation

NASA Astrophysics Data System (ADS)

Zhou, Rurui; Li, Yu; Lu, Di; Liu, Haixing; Zhou, Huicheng

2016-09-01

This paper investigates the use of an epsilon-dominance non-dominated sorted genetic algorithm II (ɛ-NSGAII) as a sampling approach with an aim to improving sampling efficiency for multiple metrics uncertainty analysis using Generalized Likelihood Uncertainty Estimation (GLUE). The effectiveness of ɛ-NSGAII based sampling is demonstrated compared with Latin hypercube sampling (LHS) through analyzing sampling efficiency, multiple metrics performance, parameter uncertainty and flood forecasting uncertainty with a case study of flood forecasting uncertainty evaluation based on Xinanjiang model (XAJ) for Qing River reservoir, China. Results obtained demonstrate the following advantages of the ɛ-NSGAII based sampling approach in comparison to LHS: (1) The former performs more effective and efficient than LHS, for example the simulation time required to generate 1000 behavioral parameter sets is shorter by 9 times; (2) The Pareto tradeoffs between metrics are demonstrated clearly with the solutions from ɛ-NSGAII based sampling, also their Pareto optimal values are better than those of LHS, which means better forecasting accuracy of ɛ-NSGAII parameter sets; (3) The parameter posterior distributions from ɛ-NSGAII based sampling are concentrated in the appropriate ranges rather than uniform, which accords with their physical significance, also parameter uncertainties are reduced significantly; (4) The forecasted floods are close to the observations as evaluated by three measures: the normalized total flow outside the uncertainty intervals (FOUI), average relative band-width (RB) and average deviation amplitude (D). The flood forecasting uncertainty is also reduced a lot with ɛ-NSGAII based sampling. This study provides a new sampling approach to improve multiple metrics uncertainty analysis under the framework of GLUE, and could be used to reveal the underlying mechanisms of parameter sets under multiple conflicting metrics in the uncertainty analysis process.

A general theory on frequency and time-frequency analysis of irregularly sampled time series based on projection methods - Part 2: Extension to time-frequency analysis

NASA Astrophysics Data System (ADS)

Lenoir, Guillaume; Crucifix, Michel

2018-03-01

Geophysical time series are sometimes sampled irregularly along the time axis. The situation is particularly frequent in palaeoclimatology. Yet, there is so far no general framework for handling the continuous wavelet transform when the time sampling is irregular. Here we provide such a framework. To this end, we define the scalogram as the continuous-wavelet-transform equivalent of the extended Lomb-Scargle periodogram defined in Part 1 of this study (Lenoir and Crucifix, 2018). The signal being analysed is modelled as the sum of a locally periodic component in the time-frequency plane, a polynomial trend, and a background noise. The mother wavelet adopted here is the Morlet wavelet classically used in geophysical applications. The background noise model is a stationary Gaussian continuous autoregressive-moving-average (CARMA) process, which is more general than the traditional Gaussian white and red noise processes. The scalogram is smoothed by averaging over neighbouring times in order to reduce its variance. The Shannon-Nyquist exclusion zone is however defined as the area corrupted by local aliasing issues. The local amplitude in the time-frequency plane is then estimated with least-squares methods. We also derive an approximate formula linking the squared amplitude and the scalogram. Based on this property, we define a new analysis tool: the weighted smoothed scalogram, which we recommend for most analyses. The estimated signal amplitude also gives access to band and ridge filtering. Finally, we design a test of significance for the weighted smoothed scalogram against the stationary Gaussian CARMA background noise, and provide algorithms for computing confidence levels, either analytically or with Monte Carlo Markov chain methods. All the analysis tools presented in this article are available to the reader in the Python package WAVEPAL.

Implementation guide for turbidity threshold sampling: principles, procedures, and analysis

Treesearch

Jack Lewis; Rand Eads

2009-01-01

Turbidity Threshold Sampling uses real-time turbidity and river stage information to automatically collect water quality samples for estimating suspended sediment loads. The system uses a programmable data logger in conjunction with a stage measurement device, a turbidity sensor, and a pumping sampler. Specialized software enables the user to control the sampling...

Algae viability over time in a ballast water sample

NASA Astrophysics Data System (ADS)

Gollasch, Stephan; David, Matej

2018-03-01

The biology of vessels' ballast water needs to be analysed for several reasons, one of these being performance tests of ballast water management systems. This analysis includes a viability assessment of phytoplankton. To overcome logistical problems to get algae sample processing gear on board of a vessel to document algae viability, samples may be transported to land-based laboratories. Concerns were raised how the storage conditions of the sample may impact algae viability over time and what the most appropriate storage conditions were. Here we answer these questions with a long-term algae viability study with daily sample analysis using Pulse-Amplitude Modulated (PAM) fluorometry. The sample was analysed over 79 days. We tested different storage conditions: fridge and room temperature with and without light. It seems that during the first two weeks of the experiment the viability remains almost unchanged with a slight downwards trend. In the continuing period, before the sample was split, a slightly stronger downwards viability trend was observed, which occurred at a similar rate towards the end of the experiment. After the sample was split, the strongest viability reduction was measured for the sample stored without light at room temperature. We concluded that the storage conditions, especially regarding temperature and light exposure, have a stronger impact on algae viability compared to the storage duration and that inappropriate storage conditions reduce algal viability. A sample storage time of up to two weeks in a dark and cool environment has little influence on the organism viability. This indicates that a two week time duration between sample taking on board a vessel and the viability measurement in a land-based laboratory may not be very critical.

WetLab-2: Tools for Conducting On-Orbit Quantitative Real-Time Gene Expression Analysis on ISS

NASA Technical Reports Server (NTRS)

Parra, Macarena; Almeida, Eduardo; Boone, Travis; Jung, Jimmy; Schonfeld, Julie

2014-01-01

The objective of NASA Ames Research Centers WetLab-2 Project is to place on the ISS a research platform capable of conducting gene expression analysis via quantitative real-time PCR (qRT-PCR) of biological specimens sampled or cultured on orbit. The project has selected a Commercial-Off-The-Shelf (COTS) qRT-PCR system, the Cepheid SmartCycler and will fly it in its COTS configuration. The SmartCycler has a number of advantages including modular design (16 independent PCR modules), low power consumption, rapid ramp times and the ability to detect up to four separate fluorescent channels at one time enabling multiplex assays that can be used for normalization and to study multiple genes of interest in each module. The team is currently working with Cepheid to enable the downlink of data from the ISS to the ground and provide uplink capabilities for programming, commanding, monitoring, and instrument maintenance. The project has adapted commercial technology to design a module that can lyse cells and extract RNA of sufficient quality and quantity for use in qRT-PCR reactions while using a housekeeping gene to normalize RNA concentration and integrity. The WetLab-2 system is capable of processing multiple sample types ranging from microbial cultures to animal tissues dissected on-orbit. The ability to conduct qRT-PCR on-orbit eliminates the confounding effects on gene expression of reentry stresses and shock acting on live cells and organisms or the concern of RNA degradation of fixed samples. The system can be used to validate terrestrial analyses of samples returned from ISS by providing on-orbit gene expression benchmarking prior to sample return. The ability to get on orbit data will provide investigators with the opportunity to adjust experiment parameters for subsequent trials based on the real-time data analysis without need for sample return and re-flight. Researchers will also be able to sample multigenerational changes in organisms. Finally, the system can be used for analysis of air, surface, water, and clinical samples to monitor environmental contaminants and crew health. The verification flight of the instrument is scheduled to launch on SpaceX-7 in June 2015.

A recurrence-weighted prediction algorithm for musical analysis

NASA Astrophysics Data System (ADS)

Colucci, Renato; Leguizamon Cucunuba, Juan Sebastián; Lloyd, Simon

2018-03-01

Forecasting the future behaviour of a system using past data is an important topic. In this article we apply nonlinear time series analysis in the context of music, and present new algorithms for extending a sample of music, while maintaining characteristics similar to the original piece. By using ideas from ergodic theory, we adapt the classical prediction method of Lorenz analogues so as to take into account recurrence times, and demonstrate with examples, how the new algorithm can produce predictions with a high degree of similarity to the original sample.

SAVLOC, computer program for automatic control and analysis of X-ray fluorescence experiments

NASA Technical Reports Server (NTRS)

Leonard, R. F.

1977-01-01

A program for a PDP-15 computer is presented which provides for control and analysis of trace element determinations by using X-ray fluorescence. The program simultaneously handles data accumulation for one sample and analysis of data from previous samples. Data accumulation consists of sample changing, timing, and data storage. Analysis requires the locating of peaks in X-ray spectra, determination of intensities of peaks, identification of origins of peaks, and determination of a real density of the element responsible for each peak. The program may be run in either a manual (supervised) mode or an automatic (unsupervised) mode.

On the incidence of Mg II absorbers along the blazar sightlines

NASA Astrophysics Data System (ADS)

Mishra, S.; Chand, H.; Krishna, Gopal-; Joshi, R.; Shchekinov, Y. A.; Fatkhullin, T. A.

2018-02-01

It is widely believed that the cool gas clouds traced by Mg II absorption, within a velocity offset of 5000 km s-1 relative to the background quasar are mostly associated with the quasar itself, whereas the absorbers seen at larger velocity offsets towards us are intervening absorber systems and hence their existence is completely independent of the background quasar. Recent evidence by Bergeron et al. (hereinafter BBM) has seriously questioned this paradigm, by showing that the number density of intervening Mg II absorbers towards the 45 blazars in their sample is nearly two times the expectation based on the Mg II absorption systems seen towards normal quasars (QSOs). Given its serious implications, it becomes important to revisit this finding, by enlarging the blazar sample and subjecting it to an independent analysis. Here, we first report the outcome of our re-analysis of the available spectroscopic data for the BBM sample itself. Our analysis of the BBM sample reproduces their claimed factor of 2 excess of dN/dz along blazar sightlines, vis-à-vis normal QSOs. We have also assembled an approxmately three times larger sample of blazars, albeit with moderately sensitive optical spectra. Using this sample together with the BBM sample, our analysis shows that the dN/dz of the Mg II absorbers statistically matches that known for normal QSO sightlines. Further, the analysis indicates that associated absorbers might be contributing significantly to the estimated dN/dz up to offset speeds Δv ∼ 0.2c relative to the blazar.

Time Spent on Social Network Sites and Psychological Well-Being: A Meta-Analysis.

PubMed

Huang, Chiungjung

2017-06-01

This meta-analysis examines the relationship between time spent on social networking sites and psychological well-being factors, namely self-esteem, life satisfaction, loneliness, and depression. Sixty-one studies consisting of 67 independent samples involving 19,652 participants were identified. The mean correlation between time spent on social networking sites and psychological well-being was low at r = -0.07. The correlations between time spent on social networking sites and positive indicators (self-esteem and life satisfaction) were close to 0, whereas those between time spent on social networking sites and negative indicators (depression and loneliness) were weak. The effects of publication outlet, site on which users spent time, scale of time spent, and participant age and gender were not significant. As most included studies used student samples, future research should be conducted to examine this relationship for adults.

System for sensing droplet formation time delay in a flow cytometer

DOEpatents

Van den Engh, Ger; Esposito, Richard J.

1997-01-01

A droplet flow cytometer system which includes a system to optimize the droplet formation time delay based on conditions actually experienced includes an automatic droplet sampler which rapidly moves a plurality of containers stepwise through the droplet stream while simultaneously adjusting the droplet time delay. Through the system sampling of an actual substance to be processed can be used to minimize the effect of the substances variations or the determination of which time delay is optimal. Analysis such as cell counting and the like may be conducted manually or automatically and input to a time delay adjustment which may then act with analysis equipment to revise the time delay estimate actually applied during processing. The automatic sampler can be controlled through a microprocessor and appropriate programming to bracket an initial droplet formation time delay estimate. When maximization counts through volume, weight, or other types of analysis exists in the containers, the increment may then be reduced for a more accurate ultimate setting. This may be accomplished while actually processing the sample without interruption.

A new method for simultaneous detection and discrimination of Bovine herpesvirus types 1 (BoHV-1) and 5 (BoHV-5) using real time PCR with high resolution melting (HRM) analysis.

PubMed

Marin, M S; Quintana, S; Leunda, M R; Recavarren, M; Pagnuco, I; Späth, E; Pérez, S; Odeón, A

2016-01-01

Bovine herpesvirus types 1 (BoHV-1) and 5 (BoHV-5) are antigenically and genetically similar. The aim of this study was to develop a simple and reliable one-step real time PCR assay with high resolution melting (HRM) analysis for the simultaneous detection and differentiation of BoHV-1 and BoHV-5. Optimization of assay conditions was performed with DNA from reference strains. Then, DNA from field isolates, clinical samples and tissue samples of experimentally infected animals were studied by real time PCR-HRM. An efficient amplification of real time PCR products was obtained, and a clear melting curve and appropriate melting peaks for both viruses were achieved in the HRM curve analysis for BoHV type identification. BoHV was identified in all of the isolates and clinical samples, and BoHV types were properly differentiated. Furthermore, viral DNA was detected in 12/18 and 7/18 samples from BoHV-1- and BoHV-5-infected calves, respectively. Real time PCR-HRM achieved a higher sensitivity compared with virus isolation or conventional PCR. In this study, HRM was used as a novel procedure. This method provides rapid, sensitive, specific and simultaneous detection of bovine alpha-herpesviruses DNA. Thus, this technique is an excellent tool for diagnosis, research and epidemiological studies of these viruses in cattle. Copyright © 2015 Elsevier B.V. All rights reserved.

A rapid method for estimation of Pu-isotopes in urine samples using high volume centrifuge.

PubMed

Kumar, Ranjeet; Rao, D D; Dubla, Rupali; Yadav, J R

2017-07-01

The conventional radio-analytical technique used for estimation of Pu-isotopes in urine samples involves anion exchange/TEVA column separation followed by alpha spectrometry. This sequence of analysis consumes nearly 3-4 days for completion. Many a times excreta analysis results are required urgently, particularly under repeat and incidental/emergency situations. Therefore, there is need to reduce the analysis time for the estimation of Pu-isotopes in bioassay samples. This paper gives the details of standardization of a rapid method for estimation of Pu-isotopes in urine samples using multi-purpose centrifuge, TEVA resin followed by alpha spectrometry. The rapid method involves oxidation of urine samples, co-precipitation of plutonium along with calcium phosphate followed by sample preparation using high volume centrifuge and separation of Pu using TEVA resin. Pu-fraction was electrodeposited and activity estimated using 236 Pu tracer recovery by alpha spectrometry. Ten routine urine samples of radiation workers were analyzed and consistent radiochemical tracer recovery was obtained in the range 47-88% with a mean and standard deviation of 64.4% and 11.3% respectively. With this newly standardized technique, the whole analytical procedure is completed within 9h (one working day hour). Copyright © 2017 Elsevier Ltd. All rights reserved.

Comparative analysis of detection methods for congenital cytomegalovirus infection in a Guinea pig model.

PubMed

Park, Albert H; Mann, David; Error, Marc E; Miller, Matthew; Firpo, Matthew A; Wang, Yong; Alder, Stephen C; Schleiss, Mark R

2013-01-01

To assess the validity of the guinea pig as a model for congenital cytomegalovirus (CMV) infection by comparing the effectiveness of detecting the virus by real-time polymerase chain reaction (PCR) in blood, urine, and saliva. Case-control study. Academic research. Eleven pregnant Hartley guinea pigs. Blood, urine, and saliva samples were collected from guinea pig pups delivered from pregnant dams inoculated with guinea pig CMV. These samples were then evaluated for the presence of guinea pig CMV by real-time PCR assuming 100% transmission. Thirty-one pups delivered from 9 inoculated pregnant dams and 8 uninfected control pups underwent testing for guinea pig CMV and for auditory brainstem response hearing loss. Repeated-measures analysis of variance demonstrated no statistically significantly lower weight for the infected pups compared with the noninfected control pups. Six infected pups demonstrated auditory brainstem response hearing loss. The sensitivity and specificity of the real-time PCR assay on saliva samples were 74.2% and 100.0%, respectively. The sensitivity of the real-time PCR on blood and urine samples was significantly lower than that on saliva samples. Real-time PCR assays of blood, urine, and saliva revealed that saliva samples show high sensitivity and specificity for detecting congenital CMV infection in guinea pigs. This finding is consistent with recent screening studies in human newborns. The guinea pig may be a good animal model in which to compare different diagnostic assays for congenital CMV infection.

7 CFR 160.202 - Fees generally for laboratory analysis and testing.

Code of Federal Regulations, 2012 CFR

2012-01-01

... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

7 CFR 160.202 - Fees generally for laboratory analysis and testing.

Code of Federal Regulations, 2011 CFR

2011-01-01

... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

7 CFR 160.202 - Fees generally for laboratory analysis and testing.

Code of Federal Regulations, 2013 CFR

2013-01-01

... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

7 CFR 160.202 - Fees generally for laboratory analysis and testing.

Code of Federal Regulations, 2010 CFR

2010-01-01

... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

7 CFR 160.202 - Fees generally for laboratory analysis and testing.

Code of Federal Regulations, 2014 CFR

2014-01-01

... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

Molecular detection of Toxoplasma gondii in water samples from Scotland and a comparison between the 529bp real-time PCR and ITS1 nested PCR.

PubMed

Wells, Beth; Shaw, Hannah; Innocent, Giles; Guido, Stefano; Hotchkiss, Emily; Parigi, Maria; Opsteegh, Marieke; Green, James; Gillespie, Simon; Innes, Elisabeth A; Katzer, Frank

2015-12-15

Waterborne transmission of Toxoplasma gondii is a potential public health risk and there are currently no agreed optimised methods for the recovery, processing and detection of T. gondii oocysts in water samples. In this study modified methods of T. gondii oocyst recovery and DNA extraction were applied to 1427 samples collected from 147 public water supplies throughout Scotland. T. gondii DNA was detected, using real time PCR (qPCR) targeting the 529bp repeat element, in 8.79% of interpretable samples (124 out of 1411 samples). The samples which were positive for T. gondii DNA originated from a third of the sampled water sources. The samples which were positive by qPCR and some of the negative samples were reanalysed using ITS1 nested PCR (nPCR) and results compared. The 529bp qPCR was the more sensitive technique and a full analysis of assay performance, by Bayesian analysis using a Markov Chain Monte Carlo method, was completed which demonstrated the efficacy of this method for the detection of T. gondii in water samples. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

"Soft"or "hard" ionisation? Investigation of metastable gas temperature effect on direct analysis in real-time analysis of Voriconazole.

PubMed

Lapthorn, Cris; Pullen, Frank

2009-01-01

The performance of the direct analysis in real-time (DART) technique was evaluated across a range of metastable gas temperatures for a pharmaceutical compound, Voriconazole, in order to investigate the effect of metastable gas temperature on molecular ion intensity and fragmentation. The DART source has been used to analyse a range of analytes and from a range of matrices including drugs in solid tablet form and preparations, active ingredients in ointment, naturally occurring plant alkaloids, flavours and fragrances, from thin layer chromatography (TLC) plates, melting point tubes and biological matrices including hair, urine and blood. The advantages of this technique include rapid analysis time (as little as 5 s), a reduction in sample preparation requirements, elimination of mobile phase requirement and analysis of samples not typically amenable to atmospheric pressure ionisation (API) techniques. This technology has therefore been proposed as an everyday tool for identification of components in crude organic reaction mixtures.

Sampling factors influencing accuracy of sperm kinematic analysis.

PubMed

Owen, D H; Katz, D F

1993-01-01

Sampling conditions that influence the accuracy of experimental measurement of sperm head kinematics were studied by computer simulation methods. Several archetypal sperm trajectories were studied. First, mathematical models of typical flagellar beats were input to hydrodynamic equations of sperm motion. The instantaneous swimming velocities of such sperm were computed over sequences of flagellar beat cycles, from which the resulting trajectories were determined. In a second, idealized approach, direct mathematical models of trajectories were utilized, based upon similarities to the previous hydrodynamic constructs. In general, it was found that analyses of sampling factors produced similar results for the hydrodynamic and idealized trajectories. A number of experimental sampling factors were studied, including the number of sperm head positions measured per flagellar beat, and the time interval over which these measurements are taken. It was found that when one flagellar beat is sampled, values of amplitude of lateral head displacement (ALH) and linearity (LIN) approached their actual values when five or more sample points per beat were taken. Mean angular displacement (MAD) values, however, remained sensitive to sampling rate even when large sampling rates were used. Values of MAD were also much more sensitive to the initial starting point of the sampling procedure than were ALH or LIN. On the basis of these analyses of measurement accuracy for individual sperm, simulations were then performed of cumulative effects when studying entire populations of motile cells. It was found that substantial (double digit) errors occurred in the mean values of curvilinear velocity (VCL), LIN, and MAD under the conditions of 30 video frames per second and 0.5 seconds of analysis time. Increasing the analysis interval to 1 second did not appreciably improve the results. However, increasing the analysis rate to 60 frames per second significantly reduced the errors. These findings thus suggest that computer-aided sperm analysis (CASA) application at 60 frames per second will significantly improve the accuracy of kinematic analysis in most applications to human and other mammalian sperm.

Mass Spectrometry and Fourier Transform Infrared Spectroscopy for Analysis of Biological Materials

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

Anderson, Timothy J.

Time-of-flight mass spectrometry along with statistical analysis was utilized to study metabolic profiles among rats fed resistant starch (RS) diets. Fischer 344 rats were fed four starch diets consisting of 55% (w/w, dbs) starch. A control starch diet consisting of corn starch was compared against three RS diets. The RS diets were high-amylose corn starch (HA7), HA7 chemically modified with octenyl succinic anhydride, and stearic-acid-complexed HA7 starch. A subgroup received antibiotic treatment to determine if perturbations in the gut microbiome were long lasting. A second subgroup was treated with azoxymethane (AOM), a carcinogen. At the end of the eight weekmore » study, cecal and distal-colon contents samples were collected from the sacrificed rats. Metabolites were extracted from cecal and distal colon samples into acetonitrile. The extracts were then analyzed on an accurate-mass time-of-flight mass spectrometer to obtain their metabolic profile. The data were analyzed using partial least-squares discriminant analysis (PLS-DA). The PLS-DA analysis utilized a training set and verification set to classify samples within diet and treatment groups. PLS-DA could reliably differentiate the diet treatments for both cecal and distal colon samples. The PLS-DA analyses of the antibiotic and no antibiotic treated subgroups were well classified for cecal samples and modestly separated for distal-colon samples. PLS-DA analysis had limited success separating distal colon samples for rats given AOM from those not treated; the cecal samples from AOM had very poor classification. Mass spectrometry profiling coupled with PLS-DA can readily classify metabolite differences among rats given RS diets.« less

Analysis of single ion channel data incorporating time-interval omission and sampling

PubMed Central

The, Yu-Kai; Timmer, Jens

2005-01-01

Hidden Markov models are widely used to describe single channel currents from patch-clamp experiments. The inevitable anti-aliasing filter limits the time resolution of the measurements and therefore the standard hidden Markov model is not adequate anymore. The notion of time-interval omission has been introduced where brief events are not detected. The developed, exact solutions to this problem do not take into account that the measured intervals are limited by the sampling time. In this case the dead-time that specifies the minimal detectable interval length is not defined unambiguously. We show that a wrong choice of the dead-time leads to considerably biased estimates and present the appropriate equations to describe sampled data. PMID:16849220

Effect of varying postmortem deboning time and sampling position on visible and near infrared spectra of broiler breast filets

USDA-ARS?s Scientific Manuscript database

Visible-Near Infrared spectroscopy (Vis-NIR) was used to characterize broiler breast filets with varied deboning times and identify how the side and position of the sampling affects the chemometric analysis and prediction capabilities. This study served to identify what differences, if any, exist wh...

A timed solenoid injector for flow analysis.

PubMed

Rothwell, S D; Woolf, A A

1985-05-01

Samples can be reproducibly injected into flow-streams by timed switching of a sample stream with a miniature solenoid valve and timer circuit. The device is simpler to assemble and use than the standard rotary valve and a direct comparison under the same operating conditions shows that the solenoid valve is an adequate replacement for the rotary valve.

System for high throughput water extraction from soil material for stable isotope analysis of water

USDA-ARS?s Scientific Manuscript database

A major limitation in the use of stable isotope of water in ecological studies is the time that is required to extract water from soil and plant samples. Using vacuum distillation the extraction time can be less than one hour per sample. Therefore, assembling a distillation system that can process m...

A Comparison of Momentary Time Sampling and Partial-Interval Recording for Assessment of Effects of Social Skills Training

ERIC Educational Resources Information Center

Radley, Keith C.; O'Handley, Roderick D.; Labrot, Zachary C.

2015-01-01

Assessment in social skills training often utilizes procedures such as partial-interval recording (PIR) and momentary time sampling (MTS) to estimate changes in duration in social engagements due to intervention. Although previous research suggests PIR to be more inaccurate than MTS in estimating levels of behavior, treatment analysis decisions…

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

NASA Astrophysics Data System (ADS)

Rahman, Nur Aira Abd; Yussup, Nolida; Salim, Nazaratul Ashifa Bt. Abdullah; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh@Shaari, Syirrazie Bin Che; Azman, Azraf B.; Ismail, Nadiah Binti

2015-04-01

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on `Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)'. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

Inverse Analysis of Irradiated NuclearMaterial Gamma Spectra via Nonlinear Optimization

NASA Astrophysics Data System (ADS)

Dean, Garrett James

Nuclear forensics is the collection of technical methods used to identify the provenance of nuclear material interdicted outside of regulatory control. Techniques employed in nuclear forensics include optical microscopy, gas chromatography, mass spectrometry, and alpha, beta, and gamma spectrometry. This dissertation focuses on the application of inverse analysis to gamma spectroscopy to estimate the history of pulse irradiated nuclear material. Previous work in this area has (1) utilized destructive analysis techniques to supplement the nondestructive gamma measurements, and (2) been applied to samples composed of spent nuclear fuel with long irradiation and cooling times. Previous analyses have employed local nonlinear solvers, simple empirical models of gamma spectral features, and simple detector models of gamma spectral features. The algorithm described in this dissertation uses a forward model of the irradiation and measurement process within a global nonlinear optimizer to estimate the unknown irradiation history of pulse irradiated nuclear material. The forward model includes a detector response function for photopeaks only. The algorithm uses a novel hybrid global and local search algorithm to quickly estimate the irradiation parameters, including neutron fluence, cooling time and original composition. Sequential, time correlated series of measurements are used to reduce the uncertainty in the estimated irradiation parameters. This algorithm allows for in situ measurements of interdicted irradiated material. The increase in analysis speed comes with a decrease in information that can be determined, but the sample fluence, cooling time, and composition can be determined within minutes of a measurement. Furthermore, pulse irradiated nuclear material has a characteristic feature that irradiation time and flux cannot be independently estimated. The algorithm has been tested against pulse irradiated samples of pure special nuclear material with cooling times of four minutes to seven hours. The algorithm described is capable of determining the cooling time and fluence the sample was exposed to within 10% as well as roughly estimating the relative concentrations of nuclides present in the original composition.

Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

PubMed

Heisterkamp, M; Adams, F C

2001-07-01

The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

Comparative analysis between saliva and buccal swabs as source of DNA: lesson from HLA-B*57:01 testing.

PubMed

Cascella, Raffaella; Stocchi, Laura; Strafella, Claudia; Mezzaroma, Ivano; Mannazzu, Marco; Vullo, Vincenzo; Montella, Francesco; Parruti, Giustino; Borgiani, Paola; Sangiuolo, Federica; Novelli, Giuseppe; Pirazzoli, Antonella; Zampatti, Stefania; Giardina, Emiliano

2015-01-01

Our work aimed to designate the optimal DNA source for pharmacogenetic assays, such as the screening for HLA-B*57:01 allele. A saliva and four buccal swab samples were taken from 104 patients. All the samples were stored at different time and temperature conditions and then genotyped for the HLA-B*57:01 allele by SSP-PCR and classical/capillary electrophoresis. The genotyping analysis reported different performance rates depending on the storage conditions of the samples. Given our results, the buccal swab demonstrated to be more resistant and stable in time with respect to the saliva. Our investigation designates the buccal swab as the optimal DNA source for pharmacogenetic assays in terms of resistance, low infectivity, low-invasiveness and easy sampling, and safe transport in centralized medical centers providing specialized pharmacogenetic tests.

Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (Strasbourg, France) during agricultural application.

PubMed

Liaud, Céline; Brucher, Michel; Schummer, Claude; Coscollà, Clara; Wolff, Hélène; Schwartz, Jean-Jacques; Yusà, Vicent; Millet, Maurice

2016-10-02

Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used in maize crops (acetochlor, benoxacor, dicamba, s-metolachlor, pendimethalin, and bromoxynil), in cereal crops (benoxacor, chlorothalonil, fenpropimorph, and propiconazole), in vineyards (tebuconazole), and as herbicides for orchards, meadows of green spaces (2,4-MCPA, trichlopyr). This is in accordance with the diversity of crops found in the Alsace region and trends observed are in accordance with the period of application of these pesticides. Variations observed permit also to demonstrate that the long time sampling duration used in this study is efficient to visualize temporal variations of airborne pesticides concentrations. Then, long time high-volume sampling could be a simple method permitting atmospheric survey of atmospheric contamination without any long analysis time and consequently low cost.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

NASA Astrophysics Data System (ADS)

Bischoff, James L.; Wooden, Joe; Murphy, Fred; Williams, Ross W.

2005-04-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ˜60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few μm deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

USGS Publications Warehouse

Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

2005-01-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

Effective Analysis of Reaction Time Data

ERIC Educational Resources Information Center

Whelan, Robert

2008-01-01

Most analyses of reaction time (RT) data are conducted by using the statistical techniques with which psychologists are most familiar, such as analysis of variance on the sample mean. Unfortunately, these methods are usually inappropriate for RT data, because they have little power to detect genuine differences in RT between conditions. In…

Detection of Illicit Drugs on Surfaces Using Direct Analysis in Real Time (DART)/Time-of-Flight Mass Spectrometry

EPA Science Inventory

Methamphetamine (meth) residues from meth syntheses or habitual meth smoking pose human health hazards. State health departments require remediation of meth labs before properties are sold. NIOSH methods for meth analysis require wipe sampling, extraction, cleanup, solvent excha...

EVALUATION OF RAPID DNA EXTRACTION PROCEDURES FOR THE QUANTITATIVE DETECTION OF FUNGAL CELLS USING REAL TIME PCR ANALYSIS

EPA Science Inventory

The ease and rapidity of quantitative DNA sequence detection by real-time PCR instruments promises to make their use increasingly common for the microbial analysis many different types of environmental samples. To fully exploit the capabilities of these instruments, correspondin...

A Field Investigation of Bacillus anthracis Contamination of U.S. Department of Agriculture and Other Washington, D.C., Buildings during the Anthrax Attack of October 2001

PubMed Central

Higgins, James A.; Cooper, Mary; Schroeder-Tucker, Linda; Black, Scott; Miller, David; Karns, Jeffrey S.; Manthey, Erlynn; Breeze, Roger; Perdue, Michael L.

2003-01-01

In response to a bioterrorism attack in the Washington, D.C., area in October 2001, a mobile laboratory (ML) was set up in the city to conduct rapid molecular tests on environmental samples for the presence of Bacillus anthracis spores and to route samples for further culture analysis. The ML contained class I laminar-flow hoods, a portable autoclave, two portable real-time PCR devices (Ruggedized Advanced Pathogen Identification Device [RAPID]), and miscellaneous supplies and equipment to process samples. Envelopes and swab and air samples collected from 30 locations in the metropolitan area once every three days were subjected to visual examination and DNA extraction, followed by real-time PCR using freeze-dried, fluorescent-probe-based reagents. Surface swabs and air samples were also cultured for B. anthracis at the National Veterinary Service Laboratory (NVSL) in Ames, Iowa. From 24 October 2001 to 15 September 2002, 2,092 pieces of mail were examined, 405 real-time PCR assays were performed (comprising 4,639 samples), and at the NVSL 6,275 samples were subjected to over 18,000 platings. None of the PCR assays on DNA extracted from swab and air samples were positive, but viable spores were cultured from surface swabs taken from six locations in the metropolitan area in October, November, and December 2001 and February, March, and May 2002. DNA extracted from these suspected B. anthracis colonies was positive by real-time and conventional PCRs for the lethal factor, pXO1, and for capA and vrr genes; sequence analysis of the latter amplicons indicated >99% homology with the Ames, vollum, B6273-93, C93022281, and W-21 strains of B. anthracis, suggesting they arose from cross-contamination during the attack through the mail. The RAPID-based PCR analysis provided fast confirmation of suspect colonies from an overnight incubation on agar plates. PMID:12514046

Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

PubMed

Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

2018-01-01

Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

Algorithm-based arterial blood sampling recognition increasing safety in point-of-care diagnostics.

PubMed

Peter, Jörg; Klingert, Wilfried; Klingert, Kathrin; Thiel, Karolin; Wulff, Daniel; Königsrainer, Alfred; Rosenstiel, Wolfgang; Schenk, Martin

2017-08-04

To detect blood withdrawal for patients with arterial blood pressure monitoring to increase patient safety and provide better sample dating. Blood pressure information obtained from a patient monitor was fed as a real-time data stream to an experimental medical framework. This framework was connected to an analytical application which observes changes in systolic, diastolic and mean pressure to determine anomalies in the continuous data stream. Detection was based on an increased mean blood pressure caused by the closing of the withdrawal three-way tap and an absence of systolic and diastolic measurements during this manipulation. For evaluation of the proposed algorithm, measured data from animal studies in healthy pigs were used. Using this novel approach for processing real-time measurement data of arterial pressure monitoring, the exact time of blood withdrawal could be successfully detected retrospectively and in real-time. The algorithm was able to detect 422 of 434 (97%) blood withdrawals for blood gas analysis in the retrospective analysis of 7 study trials. Additionally, 64 sampling events for other procedures like laboratory and activated clotting time analyses were detected. The proposed algorithm achieved a sensitivity of 0.97, a precision of 0.96 and an F1 score of 0.97. Arterial blood pressure monitoring data can be used to perform an accurate identification of individual blood samplings in order to reduce sample mix-ups and thereby increase patient safety.

The relevance of time series in molecular ecology and conservation biology.

PubMed

Habel, Jan C; Husemann, Martin; Finger, Aline; Danley, Patrick D; Zachos, Frank E

2014-05-01

The genetic structure of a species is shaped by the interaction of contemporary and historical factors. Analyses of individuals from the same population sampled at different points in time can help to disentangle the effects of current and historical forces and facilitate the understanding of the forces driving the differentiation of populations. The use of such time series allows for the exploration of changes at the population and intraspecific levels over time. Material from museum collections plays a key role in understanding and evaluating observed population structures, especially if large numbers of individuals have been sampled from the same locations at multiple time points. In these cases, changes in population structure can be assessed empirically. The development of new molecular markers relying on short DNA fragments (such as microsatellites or single nucleotide polymorphisms) allows for the analysis of long-preserved and partially degraded samples. Recently developed techniques to construct genome libraries with a reduced complexity and next generation sequencing and their associated analysis pipelines have the potential to facilitate marker development and genotyping in non-model species. In this review, we discuss the problems with sampling and available marker systems for historical specimens and demonstrate that temporal comparative studies are crucial for the estimation of important population genetic parameters and to measure empirically the effects of recent habitat alteration. While many of these analyses can be performed with samples taken at a single point in time, the measurements are more robust if multiple points in time are studied. Furthermore, examining the effects of habitat alteration, population declines, and population bottlenecks is only possible if samples before and after the respective events are included. © 2013 The Authors. Biological Reviews © 2013 Cambridge Philosophical Society.

Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

NASA Astrophysics Data System (ADS)

Stosnach, Hagen; Mages, Margarete

2009-04-01

In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

Concept for facilitating analyst-mediated interpretation of qualitative chromatographic-mass spectral data: an alternative to manual examination of extracted ion chromatograms.

PubMed

Borges, Chad R

2007-07-01

A chemometrics-based data analysis concept has been developed as a substitute for manual inspection of extracted ion chromatograms (XICs), which facilitates rapid, analyst-mediated interpretation of GC- and LC/MS(n) data sets from samples undergoing qualitative batchwise screening for prespecified sets of analytes. Automatic preparation of data into two-dimensional row space-derived scatter plots (row space plots) eliminates the need to manually interpret hundreds to thousands of XICs per batch of samples while keeping all interpretation of raw data directly in the hands of the analyst-saving great quantities of human time without loss of integrity in the data analysis process. For a given analyte, two analyte-specific variables are automatically collected by a computer algorithm and placed into a data matrix (i.e., placed into row space): the first variable is the ion abundance corresponding to scan number x and analyte-specific m/z value y, and the second variable is the ion abundance corresponding to scan number x and analyte-specific m/z value z (a second ion). These two variables serve as the two axes of the aforementioned row space plots. In order to collect appropriate scan number (retention time) information, it is necessary to analyze, as part of every batch, a sample containing a mixture of all analytes to be tested. When pure standard materials of tested analytes are unavailable, but representative ion m/z values are known and retention time can be approximated, data are evaluated based on two-dimensional scores plots from principal component analysis of small time range(s) of mass spectral data. The time-saving efficiency of this concept is directly proportional to the percentage of negative samples and to the total number of samples processed simultaneously.

Adjustment of pesticide concentrations for temporal changes in analytical recovery, 1992–2010

USGS Publications Warehouse

Martin, Jeffrey D.; Eberle, Michael

2011-01-01

Recovery is the proportion of a target analyte that is quantified by an analytical method and is a primary indicator of the analytical bias of a measurement. Recovery is measured by analysis of quality-control (QC) water samples that have known amounts of target analytes added ("spiked" QC samples). For pesticides, recovery is the measured amount of pesticide in the spiked QC sample expressed as a percentage of the amount spiked, ideally 100 percent. Temporal changes in recovery have the potential to adversely affect time-trend analysis of pesticide concentrations by introducing trends in apparent environmental concentrations that are caused by trends in performance of the analytical method rather than by trends in pesticide use or other environmental conditions. This report presents data and models related to the recovery of 44 pesticides and 8 pesticide degradates (hereafter referred to as "pesticides") that were selected for a national analysis of time trends in pesticide concentrations in streams. Water samples were analyzed for these pesticides from 1992 through 2010 by gas chromatography/mass spectrometry. Recovery was measured by analysis of pesticide-spiked QC water samples. Models of recovery, based on robust, locally weighted scatterplot smooths (lowess smooths) of matrix spikes, were developed separately for groundwater and stream-water samples. The models of recovery can be used to adjust concentrations of pesticides measured in groundwater or stream-water samples to 100 percent recovery to compensate for temporal changes in the performance (bias) of the analytical method.

Rapid and specific detection of Salmonella in water samples using real-time PCR and High Resolution Melt (HRM) curve analysis.

PubMed

van Blerk, G N; Leibach, L; Mabunda, A; Chapman, A; Louw, D

2011-01-01

A real-time PCR assay combined with a pre-enrichment step for the specific and rapid detection of Salmonella in water samples is described. Following amplification of the invA gene target, High Resolution Melt (HRM) curve analysis was used to discriminate between products formed and to positively identify invA amplification. The real-time PCR assay was evaluated for specificity and sensitivity. The assay displayed 100% specificity for Salmonella and combined with a 16-18 h non-selective pre-enrichment step, the assay proved to be highly sensitive with a detection limit of 1.0 CFU/ml for surface water samples. The detection assay also demonstrated a high intra-run and inter-run repeatability with very little variation in invA amplicon melting temperature. When applied to water samples received routinely by the laboratory, the assay showed the presence of Salmonella in particularly surface water and treated effluent samples. Using the HRM based assay, the time required for Salmonella detection was drastically shortened to less than 24 h compared to several days when using standard culturing methods. This assay provides a useful tool for routine water quality monitoring as well as for quick screening during disease outbreaks.

High resolution DNA melting analysis: an application for prenatal control of alpha-thalassemia.

PubMed

Sirichotiyakul, Supatra; Wanapirak, Chanane; Saetung, Rattika; Sanguansermsri, Torpong

2010-04-01

To report the use of real-time gap-PCR using SYTO9 with high-resolution melting analysis (HRMA) in prenatal diagnosis of alpha-thalassemia 1. Real-time gap-PCR using SYTO9 with HRMA was performed in 33 DNA samples from chorionic villi sampling (8 normal, 16 heterozygous, and 9 homozygous) to determine the alpha-thalassemia 1 gene [normal and Southeast Asia (-SEA) allele]. The dissociation curve analysis in normal and - SEA allele gave a peak of T(m) at 91.80 +/- 0.14 degrees C and 88.67 +/- 0.08 degrees C, respectively. Normal genotype and homozygous alpha-thalassemia 1 showed a single peak of T(m) that corresponded to their alleles. The heterozygotes gave both peaks with higher normal peak and smaller - SEA peak. Thirty one samples showed consistent results with the conventional gap-PCR. Two samples with ambiguous results were confirmed to be maternal DNA contamination on real-time quantitative PCR and microsatellite assay. HRMA from both samples showed similar pattern to that of heterozygotes. However, they showed much smaller normal peak compared with the - SEA peak, which is in contrast to those of heterozygotes and can readily be distinguished. HRMA with SYTO9 is feasible for prenatal diagnosis of alpha-thalassemia. It had potential advantage of prompt detection maternal DNA contamination. Copyright (c) 2010 John Wiley & Sons, Ltd.

Use of laser ablation-inductively coupled plasma-time of flight-mass spectrometry to identify the elemental composition of vanilla and determine the geographic origin by discriminant function analysis.

PubMed

Hondrogiannis, Ellen M; Ehrlinger, Erin; Poplaski, Alyssa; Lisle, Meredith

2013-11-27

A total of 11 elements found in 25 vanilla samples from Uganda, Madagascar, Indonesia, and Papua New Guinea were measured by laser ablation-inductively coupled plasma-time-of-flight-mass spectrometry (LA-ICP-TOF-MS) for the purpose of collecting data that could be used to discriminate among the origins. Pellets were prepared of the samples, and elemental concentrations were obtained on the basis of external calibration curves created using five National Institute of Standards and Technology (NIST) standards and one Chinese standard with (13)C internal standardization. These curves were validated using NIST 1573a (tomato leaves) as a check standard. Discriminant analysis was used to successfully classify the vanilla samples by their origin. Our method illustrates the feasibility of using LA-ICP-TOF-MS with an external calibration curve for high-throughput screening of spice screening analysis.

Comparison of field-enhanced and pressure-assisted field-enhanced sample injection techniques for the analysis of water-soluble vitamins using CZE.

PubMed

Liu, Qingqing; Liu, Yaling; Guan, Yu; Jia, Li

2009-04-01

A new online concentration method, namely pressure-assisted field-enhanced sample injection (PA-FESI), was developed and compared with FESI for the analysis of water-soluble vitamins by CZE with UV detection. In PA-FESI, negative voltage and positive pressure were simultaneously applied to initialize PA-FESI. PA-FESI uses the hydrodynamic flow generated by the positive pressure to counterbalance the reverse EOF in the capillary column during electrokinetic sample injection, which allowed a longer injection time than usual FESI mode without compromising the separation efficiency. Using the PA-FESI method, the LODs of the vitamins were at ng/mL level based on the S/N of 3 and the RSDs of migration time and peak area for each vitamin (1 microg/mL) were less than 5.1%. The developed method was applied to the analysis of water-soluble vitamins in corns.

Ultra-high performance supercritical fluid chromatography of lignin-derived phenols from alkaline cupric oxide oxidation.

PubMed

Sun, Mingzhe; Lidén, Gunnar; Sandahl, Margareta; Turner, Charlotta

2016-08-01

Traditional chromatographic methods for the analysis of lignin-derived phenolic compounds in environmental samples are generally time consuming. In this work, an ultra-high performance supercritical fluid chromatography method with a diode array detector for the analysis of major lignin-derived phenolic compounds produced by alkaline cupric oxide oxidation was developed. In an analysis of a collection of 11 representative monomeric lignin phenolic compounds, all compounds were clearly separated within 6 min with excellent peak shapes, with a limit of detection of 0.5-2.5 μM, a limit of quantification of 2.5-5.0 μM, and a dynamic range of 5.0-2.0 mM (R(2) > 0.997). The new ultra-high performance supercritical fluid chromatography method was also applied for the qualitative and quantitative analysis of lignin-derived phenolic compounds obtained upon alkaline cupric oxide oxidation of a commercial humic acid. Ten out of the previous eleven model compounds could be quantified in the oxidized humic acid sample. The high separation power and short analysis time obtained demonstrate for the first time that supercritical fluid chromatography is a fast and reliable technique for the analysis of lignin-derived phenols in complex environmental samples. © 2016 The Authors, Journal of Separation Science Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Topochemical Analysis of Cell Wall Components by TOF-SIMS.

PubMed

Aoki, Dan; Fukushima, Kazuhiko

2017-01-01

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a recently developing analytical tool and a type of imaging mass spectrometry. TOF-SIMS provides mass spectral information with a lateral resolution on the order of submicrons, with widespread applicability. Sometimes, it is described as a surface analysis method without the requirement for sample pretreatment; however, several points need to be taken into account for the complete utilization of the capabilities of TOF-SIMS. In this chapter, we introduce methods for TOF-SIMS sample treatments, as well as basic knowledge of wood samples TOF-SIMS spectral and image data analysis.

A Mixed Methods Investigation of Mixed Methods Sampling Designs in Social and Health Science Research

ERIC Educational Resources Information Center

Collins, Kathleen M. T.; Onwuegbuzie, Anthony J.; Jiao, Qun G.

2007-01-01

A sequential design utilizing identical samples was used to classify mixed methods studies via a two-dimensional model, wherein sampling designs were grouped according to the time orientation of each study's components and the relationship of the qualitative and quantitative samples. A quantitative analysis of 121 studies representing nine fields…

Lithography hotspot discovery at 70nm DRAM 300mm fab: process window qualification using design base binning

NASA Astrophysics Data System (ADS)

Chen, Daniel; Chen, Damian; Yen, Ray; Cheng, Mingjen; Lan, Andy; Ghaskadvi, Rajesh

2008-11-01

Identifying hotspots--structures that limit the lithography process window--become increasingly important as the industry relies heavily on RET to print sub-wavelength designs. KLA-Tencor's patented Process Window Qualification (PWQ) methodology has been used for this purpose in various fabs. PWQ methodology has three key advantages (a) PWQ Layout--to obtain the best sensitivity (b) Design Based Binning--for pattern repeater analysis (c) Intelligent sampling--for the best DOI sampling rate. This paper evaluates two different analysis strategies for SEM review sampling successfully deployed at Inotera Memories, Inc. We propose a new approach combining the location repeater and pattern repeaters. Based on a recent case study the new sampling flow reduces the data analysis and sampling time from 6 hours to 1.5 hour maintaining maximum DOI sample rate.

Optimization conditions of samples saponification for tocopherol analysis.

PubMed

Souza, Aloisio Henrique Pereira; Gohara, Aline Kirie; Rodrigues, Ângela Claudia; Ströher, Gisely Luzia; Silva, Danielle Cristina; Visentainer, Jesuí Vergílio; Souza, Nilson Evelázio; Matsushita, Makoto

2014-09-01

A full factorial design 2(2) (two factors at two levels) with duplicates was performed to investigate the influence of the factors agitation time (2 and 4 h) and the percentage of KOH (60% and 80% w/v) in the saponification of samples for the determination of α, β and γ+δ-tocopherols. The study used samples of peanuts (cultivar armadillo), produced and marketed in Maringá, PR. The factors % KOH and agitation time were significant, and an increase in their values contributed negatively to the responses. The interaction effect was not significant for the response δ-tocopherol, and the contribution of this effect to the other responses was positive, but less than 10%. The ANOVA and response surfaces analysis showed that the most efficient saponification procedure was obtained using a 60% (w/v) solution of KOH and with an agitation time of 2 h. Copyright © 2014 Elsevier Ltd. All rights reserved.

Detection of central nervous system leukemia in children with acute lymphoblastic leukemia by real-time polymerase chain reaction.

PubMed

Pine, Sharon R; Yin, Changhong; Matloub, Yousif H; Sabaawy, Hatem E; Sandoval, Claudio; Levendoglu-Tugal, Oya; Ozkaynak, M Fevzi; Jayabose, Somasundaram

2005-02-01

Accurate detection of central nervous system (CNS) involvement in children with newly diagnosed acute lymphoblastic leukemia (ALL) could have profound prognostic and therapeutic implications. We examined various cerebrospinal fluid (CSF) preservation methods to yield adequate DNA stability for polymerase chain reaction (PCR) analysis and developed a quantitative real-time PCR assay to detect occult CNS leukemia. Sixty CSF specimens were maintained in several storage conditions for varying amounts of time, and we found that preserving CSF in 1:1 serum-free RPMI tissue culture medium offers the best stability of DNA for PCR analysis. Sixty CSF samples (30 at diagnosis and 30 at the end of induction therapy) from 30 children with ALL were tested for CNS leukemic involvement by real-time PCR using patient-specific antigen receptor gene rearrangement primers. Six of thirty patient diagnosis samples were PCR-positive at levels ranging from 0.5 to 66% leukemic blasts in the CSF. Four of these patients had no clinical or cytomorphological evidence of CNS leukemia involvement at that time. All 30 CSF samples drawn at the end of induction therapy were PCR-negative. The data indicate that real-time PCR analysis of CSF is an excellent tool to assess occult CNS leukemia involvement in patients with ALL and can possibly be used to refine CNS status classification.

Detection of Central Nervous System Leukemia in Children with Acute Lymphoblastic Leukemia by Real-Time Polymerase Chain Reaction

PubMed Central

Pine, Sharon R.; Yin, Changhong; Matloub, Yousif H.; Sabaawy, Hatem E.; Sandoval, Claudio; Levendoglu-Tugal, Oya; Ozkaynak, M. Fevzi; Jayabose, Somasundaram

2005-01-01

Accurate detection of central nervous system (CNS) involvement in children with newly diagnosed acute lymphoblastic leukemia (ALL) could have profound prognostic and therapeutic implications. We examined various cerebrospinal fluid (CSF) preservation methods to yield adequate DNA stability for polymerase chain reaction (PCR) analysis and developed a quantitative real-time PCR assay to detect occult CNS leukemia. Sixty CSF specimens were maintained in several storage conditions for varying amounts of time, and we found that preserving CSF in 1:1 serum-free RPMI tissue culture medium offers the best stability of DNA for PCR analysis. Sixty CSF samples (30 at diagnosis and 30 at the end of induction therapy) from 30 children with ALL were tested for CNS leukemic involvement by real-time PCR using patient-specific antigen receptor gene rearrangement primers. Six of thirty patient diagnosis samples were PCR-positive at levels ranging from 0.5 to 66% leukemic blasts in the CSF. Four of these patients had no clinical or cytomorphological evidence of CNS leukemia involvement at that time. All 30 CSF samples drawn at the end of induction therapy were PCR-negative. The data indicate that real-time PCR analysis of CSF is an excellent tool to assess occult CNS leukemia involvement in patients with ALL and can possibly be used to refine CNS status classification. PMID:15681484

The Determination of Metals in Welding Fume by X-RaySpectrometry

NASA Astrophysics Data System (ADS)

Kuznetsova, O. V.; Begunova, L. A.; Romanenko, S. V.; Solodsky, S. A.

2018-01-01

Analysis of the current hygienic situation in the welding production showed that the intensification of welding processes involves the deterioration of air quality, which negatively affects the welders health. Respiratory effects seen in full-time welders have included bronchitis, airway irritation, lung function changes, and a possible increase in the incidence of lung cancer. The metal concentration in the air of the working area have been determined using the photometric method of analysis, which involves the stage of decomposition of the sample material before analysis. However, losses of the analyzed elements are possible when the sample is decomposed. The X-ray fluorescence method of analysis has the advantage of being nondestructive. The investigations shown the data of photometric determination of metals in welding aerosols is 1.5÷2 times lower than the results of X-ray fluorescence analysis.

Solid-phase microextraction coupled to liquid chromatography for the analysis of phenolic compounds in water.

PubMed

González-Toledo, E; Prat, M D; Alpendurada, M F

2001-07-20

Solid-phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC) has been applied to the analysis of priority pollutant phenolic compounds in water samples. Two types of polar fibers [50 microm Carbowax-templated resin (CW-TPR) and 60 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB)] were evaluated. The effects of equilibration time and ionic strength of samples on the adsorption step were studied. The parameters affecting the desorption process, such as desorption mode, solvent composition and desorption time, were optimized. The developed method was used to determine the phenols in spiked river water samples collected in the Douro River, Portugal. Detection limits of 1-10 microg l(-1) were achieved under the optimized conditions.

Direct analysis in real time--high resolution mass spectrometry as a valuable tool for the pharmaceutical drug development.

PubMed

Srbek, Jan; Klejdus, Bořivoj; Douša, Michal; Břicháč, Jiří; Stasiak, Pawel; Reitmajer, Josef; Nováková, Lucie

2014-12-01

In this study, direct analysis in real time-mass spectrometry (DART-MS) was assessed for the analysis of various pharmaceutical formulations with intention to summarize possible applications for the routine pharmaceutical development. As DART is an ambient ionization technique, it allows direct analysis of pharmaceutical samples in solid or liquid form without complex sample preparation, which is often the most time-consuming part of the analytical method. This makes the technique suitable for many application fields, including pharmaceutical drug development. DART mass spectra of more than twenty selected tablets and other common pharmaceutical formulations, i.e. injection solutions, ointments and suppositories developed in the pharmaceutical industry during several recent years are presented. Moreover, as thin-layer chromatography (TLC) is still very popular for the monitoring of the reactions in the synthetic chemistry, several substances were analyzed directly from the TLC plates to demonstrate the simplicity of the technique. Pure substance solutions were spotted onto a TLC plate and then analyzed with DART without separation. This was the first DART-MS study of pharmaceutical dosage forms using DART-Orbitrap combination. The duration of sample analysis by the DART-MS technique lasted several seconds, allowing enough time to collect sufficient number of data points for compound identification. The experimental setup provided excellent mass accuracy and high resolution of the mass spectra which allowed unambiguous identification of the compounds of interest. Finally, DART mass spectrometry was also used for the monitoring of the selected impurity distribution in the atorvastatin tablets. These measurements demonstrated DART to be robust ionization technique, which provided easy-to-interpret mass spectra for the broad range of compounds. DART has high-throughput potential for various types of pharmaceutical analyses and therefore eliminates the time for sample cleanup and chromatographic separation. Copyright © 2014 Elsevier B.V. All rights reserved.

Optimal measurement counting time and statistics in gamma spectrometry analysis: The time balance

NASA Astrophysics Data System (ADS)

Joel, Guembou Shouop Cebastien; Penabei, Samafou; Maurice, Ndontchueng Moyo; Gregoire, Chene; Jilbert, Nguelem Mekontso Eric; Didier, Takoukam Serge; Werner, Volker; David, Strivay

2017-01-01

The optimal measurement counting time for gamma-ray spectrometry analysis using HPGe detectors was determined in our laboratory by comparing twelve hours measurement counting time at day and twelve hours measurement counting time at night. The day spectrum does not fully cover the night spectrum for the same sample. It is observed that the perturbation come to the sun-light. After several investigations became clearer: to remove all effects of radiation from outside (earth, the sun, and universe) our system, it is necessary to measure the background for 24, 48 or 72 hours. In the same way, the samples have to be measured for 24, 48 or 72 hours to be safe to be purified the measurement (equality of day and night measurement). It is also possible to not use the background of the winter in summer. Depend on to the energy of radionuclide we seek, it is clear that the most important steps of a gamma spectrometry measurement are the preparation of the sample and the calibration of the detector.

The detection of NBOMe designer drugs on blotter paper by high resolution time-of-flight mass spectrometry (TOFMS) with and without chromatography.

PubMed

Botch-Jones, Sabra; Foss, Jamie; Barajas, David; Kero, Frank; Young, Craig; Weisenseel, Jason

2016-10-01

New psychoactive substances (NPS) have been associated with fatalities and severe injuries in a number of cases in the United States and have led investigators to rethink traditional drug monitoring protocols. Of particular interest are the variable phenethylamine chemical structures known as 'NBOMes', which pose an emerging threat to public health with incidence steadily growing over the past decade. In this study, direct sample analysis (DSA)-time of flight mass spectrometry was employed to leverage rapid and sensitive ambient ionization mass spectrometry without chromatographic separation as verified with an authentic case sample. Samples for method development were prepared at Boston University School of Medicine's Biomedical Forensic Sciences program (Boston, MA) and analyzed at the State of Maine Health and Environmental Testing Laboratory's Forensic Chemistry Section (Augusta, ME). Preliminary method development work was performed at the University of Central Florida (Orlando, FL). DSA without any extraction step in addition to the evaluation of methanol, dichloromethane and hexane extractions were conducted. Methanol was found to not be a suitable extraction solvent for DSA analysis of these compounds. For the screening of NBOMe designer drug variables on blotter paper, DSA-TOFMS was successful at reducing analysis time to ∼15s per sample, for qualitative identification for the selected analytes of interest. The analysis of an authentic forensic case sample by DSA-TOFMS using the method development parameters demonstrates its utility in forensic laboratories. 25C-NBOMe was identified with an exact mass accuracy of 0.60ppm. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Optimization of a direct analysis in real time/time-of-flight mass spectrometry method for rapid serum metabolomic fingerprinting.

PubMed

Zhou, Manshui; McDonald, John F; Fernández, Facundo M

2010-01-01

Metabolomic fingerprinting of bodily fluids can reveal the underlying causes of metabolic disorders associated with many diseases, and has thus been recognized as a potential tool for disease diagnosis and prognosis following therapy. Here we report a rapid approach in which direct analysis in real time (DART) coupled with time-of-flight (TOF) mass spectrometry (MS) and hybrid quadrupole TOF (Q-TOF) MS is used as a means for metabolomic fingerprinting of human serum. In this approach, serum samples are first treated to precipitate proteins, and the volatility of the remaining metabolites increased by derivatization, followed by DART MS analysis. Maximum DART MS performance was obtained by optimizing instrumental parameters such as ionizing gas temperature and flow rate for the analysis of identical aliquots of a healthy human serum samples. These variables were observed to have a significant effect on the overall mass range of the metabolites detected as well as the signal-to-noise ratios in DART mass spectra. Each DART run requires only 1.2 min, during which more than 1500 different spectral features are observed in a time-dependent fashion. A repeatability of 4.1% to 4.5% was obtained for the total ion signal using a manual sampling arm. With the appealing features of high-throughput, lack of memory effects, and simplicity, DART MS has shown potential to become an invaluable tool for metabolomic fingerprinting. 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

Modified Right Heart Contrast Echocardiography Versus Traditional Method in Diagnosis of Right-to-Left Shunt: A Comparative Study.

PubMed

Wang, Yi; Zeng, Jie; Yin, Lixue; Zhang, Mei; Hou, Dailun

2016-01-01

The purpose of this study was to evaluate the reliability, effectiveness, and safety of modified right heart contrast transthoracic echocardiography (cTTE) in comparison with the traditional method. We performed a modified right heart cTTE using saline mixed with a small sample of patient's own blood. Samples were agitated with varying intensity. This study protocol involved microscopic analysis and patient evaluation. 1. Microscopic analysis: After two contrast samples had been agitated 10 or 20 times, they underwent a comparison of bubble size, bubble number, and red blood cell morphology. 2. Patient analysis: 40 patients with suspected RLS (right- to-left shunt) were enrolled. All patients underwent right heart contrast echocardiography. Oxygen saturation, transit time and duration, presence of RLS, change in indirect bilirubin and urobilinogen concentrations were compared afterward. Modified method generated more bubbles (P<0.05), but the differences in bubble size were not significant (P>0.05). Twenty-four patients were diagnosed with RLS (60%) using the modified method compared to 16 patients (40%) with the traditional method. The transit time of ASb20 group was the shortest (P<0.05). However, the duration time in this group was much longer (P<0.05). Also, in semi-quantitative analysis mean rank of RLS was higher after injecting the modified contrast agent agitated 20 times (P<0.05). Modified right heart contrast echocardiography is a reliable, effective and safe method of detecting cardiovascular RLS.

An automated method of on-line extraction coupled with flow injection and capillary electrophoresis for phytochemical analysis.

PubMed

Chen, Hongli; Ding, Xiuping; Wang, Min; Chen, Xingguo

2010-11-01

In this study, an automated system for phytochemical analysis was successfully fabricated for the first time in our laboratory. The system included on-line decocting, filtering, cooling, sample introducing, separation, and detection, which greatly simplified the sample preparation and shortened the analysis time. Samples from the decoction extract were drawn every 5 min through an on-line filter and a condenser pipe to the sample loop from which 20-μL samples were injected into the running buffer and transported into a split-flow interface coupling the flow injection and capillary electrophoresis systems. The separation of glycyrrhetinic acid (GTA) and glycyrrhizic acid (GA) took less than 5 min by using a 10 mM borate buffer (adjusted pH to 8.8) and +10 kV voltage. Calibration curves showed good linearity with correlation coefficients (R) more than 0.9991. The intra-day repeatabilities (n = 5, expressed as relative standard deviation) of the proposed system, obtained using GTA and GA standards, were 1.1% and 0.8% for migration time and 0.7% and 0.9% for peak area, respectively. The mean recoveries of GTA and GA in the off-line extract of Glycyrrhiza uralensis Fisch root were better than 99.0%. The limits of detection (signal-to-noise ratio = 3) of the proposed method were 6.2 μg/mL and 6.9 μg/mL for GTA and GA, respectively. The dynamic changes of GTA and GA on the decoction time were obtained during the on-line decoction process of Glycyrrhiza uralensis Fisch root.

Micromagnetic Cancer Cell Immobilization and Release for Real-Time Single Cell Analysis

NASA Astrophysics Data System (ADS)

Jaiswal, Devina; Rad, Armin Tahmasbi; Nieh, Mu-Ping; Claffey, Kevin P.; Hoshino, Kazunori

2017-04-01

Understanding the interaction of live cells with macromolecules is crucial for designing efficient therapies. Considering the functional heterogeneity found in cancer cells, real-time single cell analysis is necessary to characterize responses. In this study, we have designed and fabricated a microfluidic channel with patterned micromagnets which can temporarily immobilize the cells during analysis and release them after measurements. The microchannel is composed of plain coverslip top and bottom panels to facilitate easy microscopic observation and undisturbed application of analytes to the cells. Cells labeled with functionalized magnetic beads were immobilized in the device with an efficiency of 90.8±3.6%. Since the micromagnets are made of soft magnetic material (Ni), they released cells when external magnetic field was turned off from the channel. This allows the reuse of the channel for a new sample. As a model drug analysis, the immobilized breast cancer cells (MCF7) were exposed to fluorescent lipid nanoparticles and association and dissociation were measured through fluorescence analysis. Two concentrations of nanoparticles, 0.06 μg/ml and 0.08 μg/ml were tested and time lapse images were recorded and analyzed. The microfluidic device was able to provide a microenvironment for sample analysis, making it an efficient platform for real-time analysis.

FastID: Extremely Fast Forensic DNA Comparisons

DTIC Science & Technology

2017-05-19

FastID: Extremely Fast Forensic DNA Comparisons Darrell O. Ricke, PhD Bioengineering Systems & Technologies Massachusetts Institute of...Technology Lincoln Laboratory Lexington, MA USA Darrell.Ricke@ll.mit.edu Abstract—Rapid analysis of DNA forensic samples can have a critical impact on...time sensitive investigations. Analysis of forensic DNA samples by massively parallel sequencing is creating the next gold standard for DNA

Sampling Utterances and Grammatical Analysis Revised (SUGAR): New Normative Values for Language Sample Analysis Measures

ERIC Educational Resources Information Center

Pavelko, Stacey L.; Owens, Robert E., Jr.

2017-01-01

Purpose: The purpose of this study was to document whether mean length of utterance (MLU[subscript S]), total number of words (TNW), clauses per sentence (CPS), and/or words per sentence (WPS) demonstrated age-related changes in children with typical language and to document the average time to collect, transcribe, and analyze conversational…

Membrane inlet mass spectrometry of volatile organohalogen compounds in drinking water.

PubMed

Bocchini, P; Pozzi, R; Andalò, C; Galletti, G C

1999-01-01

The analysis of organic pollutants in drinking water is a topic of wide interest, reflecting on public health and life quality. Many different methodologies have been developed and are currently employed in this context, but they often require a time-consuming sample pre-treatment. This step affects the recovery of the highly volatile compounds. Trace analysis of volatile organic pollutants in water can be performed 'on-line' by membrane inlet mass spectrometry (MIMS). In MIMS, the sample is separated from the vacuum of the mass spectrometer by a thin polymeric hollow-fibre membrane. Gases and organic volatile compounds diffuse and concentrate from the sample into the hollow-fibre membrane, and from there into the mass spectrometer. The main advantages of the technique are that no pre-treatment of samples before analysis is needed and that it has fast response times and on-line monitoring capabilities. This paper reports the set-up of the analytical conditions for the analysis of volatile organohalogen compounds (chloroform, bromoform, bromodichloromethane, chlorodibromomethane, tetrachloroethylene, trichloroethylene, 1,1,1-trichloroethane, and carbon tetrachloride). Linearity of response, repeatability, detection limits, and spectra quality are evaluated. Copyright 1999 John Wiley & Sons, Ltd.

Wavelet-Based Interpolation and Representation of Non-Uniformly Sampled Spacecraft Mission Data

NASA Technical Reports Server (NTRS)

Bose, Tamal

2000-01-01

A well-documented problem in the analysis of data collected by spacecraft instruments is the need for an accurate, efficient representation of the data set. The data may suffer from several problems, including additive noise, data dropouts, an irregularly-spaced sampling grid, and time-delayed sampling. These data irregularities render most traditional signal processing techniques unusable, and thus the data must be interpolated onto an even grid before scientific analysis techniques can be applied. In addition, the extremely large volume of data collected by scientific instrumentation presents many challenging problems in the area of compression, visualization, and analysis. Therefore, a representation of the data is needed which provides a structure which is conducive to these applications. Wavelet representations of data have already been shown to possess excellent characteristics for compression, data analysis, and imaging. The main goal of this project is to develop a new adaptive filtering algorithm for image restoration and compression. The algorithm should have low computational complexity and a fast convergence rate. This will make the algorithm suitable for real-time applications. The algorithm should be able to remove additive noise and reconstruct lost data samples from images.

Evaluation of micro-organism-detaching efficacy from meat samples by spindle or stomacher treatment and quality analysis of suspensions.

PubMed

Kim, S-J; Kim, D-K; Kang, D-H

2016-04-01

We investigated and compared the efficacy of a new apparatus for detaching micro-organisms from meat samples. The efficacy of Spindle and stomacher in detaching micro-organisms from meat samples was evaluated. Also, evaluation of appropriateness of suspensions generated by both methods for carrying out molecular biological analysis was implemented. A nearly identical correlation and high R(2) were obtained between Spindle and stomacher in Aerobic Plate Count (APC), and no significant differences were observed in detachment of three major foodborne pathogens. The suspension generated by the Spindle showed lower turbidity and total protein concentration. Also, significantly different threshold cycles were observed in Real-time PCR analysis using suspensions generated by both methods. The Spindle shows nearly identical efficacy with stomacher treatment in detaching micro-organisms from meat samples. Furthermore, the high quality of suspensions generated by the Spindle, in terms of turbidity and total protein assay, allows for a lower threshold cycle than stomached suspension in Real-time PCR. The Spindle could be an alternative method for detaching micro-organisms, yielding a higher quality of suspensions which may be better suited for further molecular microbiological analysis. © 2016 The Society for Applied Microbiology.

Flow injection gas chromatography with sulfur chemiluminescence detection for the analysis of total sulfur in complex hydrocarbon matrixes.

PubMed

Hua, Yujuan; Hawryluk, Myron; Gras, Ronda; Shearer, Randall; Luong, Jim

2018-01-01

A fast and reliable analytical technique for the determination of total sulfur levels in complex hydrocarbon matrices is introduced. The method employed flow injection technique using a gas chromatograph as a sample introduction device and a gas phase dual-plasma sulfur chemiluminescence detector for sulfur quantification. Using the technique described, total sulfur measurement in challenging hydrocarbon matrices can be achieved in less than 10 s with sample-to-sample time <2 min. The high degree of selectivity and sensitivity toward sulfur compounds of the detector offers the ability to measure low sulfur levels with a detection limit in the range of 20 ppb w/w S. The equimolar response characteristic of the detector allows the quantitation of unknown sulfur compounds and simplifies the calibration process. Response is linear over a concentration range of five orders of magnitude, with a high degree of repeatability. The detector's lack of response to hydrocarbons enables direct analysis without the need for time-consuming sample preparation and chromatographic separation processes. This flow injection-based sulfur chemiluminescence detection technique is ideal for fast analysis or trace sulfur analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

NEW COLUMN SEPARATION METHOD FOR EMERGENCY URINE SAMPLES

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

Maxwell, S; Brian Culligan, B

2007-08-28

The Savannah River Site Environmental Bioassay Lab participated in the 2007 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2007. A new rapid column separation method was applied directly to the NRIP 2007 emergency urine samples, with only minimal sample preparation to reduce preparation time. Calcium phosphate precipitation, previously used to pre-concentrate actinides and Sr-90 in NRIP 2006 urine and water samples, was not used for the NRIP 2007 urine samples. Instead, the raw urine was acidified and passed directly through the stacked resin columns (TEVA+TRU+SR Resins) to separate the actinides andmore » strontium from the NRIP urine samples more quickly. This improvement reduced sample preparation time for the NRIP 2007 emergency urine analyses significantly. This approach works well for small volume urine samples expected during an emergency response event. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and strontium-90 analyses for NRIP 2007 urine samples.« less

Standoff spectroscopic interrogation of samples irradiated by high energy lasers

NASA Astrophysics Data System (ADS)

Daigle, Jean-François; Pudo, Dominik; Théberge, Francis

2017-10-01

We report on a novel method that shows the potential to provide real-time, standoff forensic analysis of samples being irradiated by a high energy laser (HEL). The interaction of the HEL beam with matter produces specific optical signatures that can be detected from the location of the HEL system. A spectroscopic analysis of these signals can then provide useful information to the operator including the impact the laser has on the sample as well as providing data about the its structure and composition.

Identification of varying time scales in sediment transport using the Hilbert-Huang Transform method

NASA Astrophysics Data System (ADS)

Kuai, Ken Z.; Tsai, Christina W.

2012-02-01

SummarySediment transport processes vary at a variety of time scales - from seconds, hours, days to months and years. Multiple time scales exist in the system of flow, sediment transport and bed elevation change processes. As such, identification and selection of appropriate time scales for flow and sediment processes can assist in formulating a system of flow and sediment governing equations representative of the dynamic interaction of flow and particles at the desired details. Recognizing the importance of different varying time scales in the fluvial processes of sediment transport, we introduce the Hilbert-Huang Transform method (HHT) to the field of sediment transport for the time scale analysis. The HHT uses the Empirical Mode Decomposition (EMD) method to decompose a time series into a collection of the Intrinsic Mode Functions (IMFs), and uses the Hilbert Spectral Analysis (HSA) to obtain instantaneous frequency data. The EMD extracts the variability of data with different time scales, and improves the analysis of data series. The HSA can display the succession of time varying time scales, which cannot be captured by the often-used Fast Fourier Transform (FFT) method. This study is one of the earlier attempts to introduce the state-of-the-art technique for the multiple time sales analysis of sediment transport processes. Three practical applications of the HHT method for data analysis of both suspended sediment and bedload transport time series are presented. The analysis results show the strong impact of flood waves on the variations of flow and sediment time scales at a large sampling time scale, as well as the impact of flow turbulence on those time scales at a smaller sampling time scale. Our analysis reveals that the existence of multiple time scales in sediment transport processes may be attributed to the fractal nature in sediment transport. It can be demonstrated by the HHT analysis that the bedload motion time scale is better represented by the ratio of the water depth to the settling velocity, h/ w. In the final part, HHT results are compared with an available time scale formula in literature.

Lifetime fluorescence spectroscopy for in situ investigation of osteogenic differentiation

NASA Astrophysics Data System (ADS)

Marcu, Laura; Elbarbary, Amir; Zuk, Patricia; De Ugarte, Daniel A.; Benhaim, Prosper; Kurt, Hamza; Hedrick, Marc H.; Ashjian, Peter

2003-07-01

Time-Resolved Laser-Induced Fluorescence Spectroscopy (TR-LIFS) represents a potential tool for the in-situ characterization of bioengineered tissues. In this study, we evaluate the application of TR-LIFS to non-intrusive monitoring of matrix composition during osteogenetic differentiation. Human adipose-derived stem cells, harvested from 3 patients, were induced in osteogenic media for 3, 5, and 7 weeks. Samples were subsequently collected and probed for time-resolved fluorescence emission with a pulsed nitrogen laser. Fluorescence parameters, derived from both spectral- and time-domain, were used for sample characterization. The samples were further analyzed using Western blot analysis and computer-based densitometry. A significant change in the fluorescence parameters was detected for samples beyond 3 weeks of osteogenic differentiation. The spectroscopic observations: 1) show increase of collagen I when contrasted against the time-resolved fluorescence spectra of commercially available collagens; and 2) are in agreement with Western blot analysis that demonstrated significant increase in collagen I content between 3- vs. 5-weeks and 3- vs. 7-weeks and no changes for collagens III, IV, and V. Our results suggest that TR-LIFS can be used as a non-invasive means for the detection of specific collagens in maturing connective tissues.

Measuring discharge with ADCPs: Inferences from synthetic velocity profiles

USGS Publications Warehouse

Rehmann, C.R.; Mueller, D.S.; Oberg, K.A.

2009-01-01

Synthetic velocity profiles are used to determine guidelines for sampling discharge with acoustic Doppler current profilers (ADCPs). The analysis allows the effects of instrument characteristics, sampling parameters, and properties of the flow to be studied systematically. For mid-section measurements, the averaging time required for a single profile measurement always exceeded the 40 s usually recommended for velocity measurements, and it increased with increasing sample interval and increasing time scale of the large eddies. Similarly, simulations of transect measurements show that discharge error decreases as the number of large eddies sampled increases. The simulations allow sampling criteria that account for the physics of the flow to be developed. ?? 2009 ASCE.

Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

PubMed

Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

2014-04-01

Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

The SDF1-CXCR4 Axis Functions through p38-MAPK Signaling to Drive Breast Cancer Progression and Metastasis

DTIC Science & Technology

2008-09-01

with breast cancer cells (MCF7 cell line) could induce proliferation and lead to hormone independent tumors in vivo. Upon analysis of these tumors by...S.5 MCS induce gene expression of ER mediated genes. Endpoint tumors from above studies were harvested for use in Real-time PCR analysis . As...subjected to real-time PCR analysis for quantification. A. Real time PCR results from matrigel + estrogen tumor samples. MCF7 + E2 control tumors are

Use of a Smartphone as a Colorimetric Analyzer in Paper-based Devices for Sensitive and Selective Determination of Mercury in Water Samples.

PubMed

Jarujamrus, Purim; Meelapsom, Rattapol; Pencharee, Somkid; Obma, Apinya; Amatatongchai, Maliwan; Ditcharoen, Nadh; Chairam, Sanoe; Tamuang, Suparb

2018-01-01

A smartphone application, called CAnal, was developed as a colorimetric analyzer in paper-based devices for sensitive and selective determination of mercury(II) in water samples. Measurement on the double layer of a microfluidic paper-based analytical device (μPAD) fabricated by alkyl ketene dimer (AKD)-inkjet printing technique with special design doped with unmodified silver nanoparticles (AgNPs) onto the detection zones was performed by monitoring the gray intensity in the blue channel of AgNPs, which disintegrated when exposed to mercury(II) on μPAD. Under the optimized conditions, the developed approach showed high sensitivity, low limit of detection (0.003 mg L -1 , 3SD blank/slope of the calibration curve), small sample volume uptake (two times of 2 μL), and short analysis time. The linearity range of this technique ranged from 0.01 to 10 mg L -1 (r 2 = 0.993). Furthermore, practical analysis of various water samples was also demonstrated to have acceptable performance that was in agreement with the data from cold vapor atomic absorption spectrophotometry (CV-AAS), a conventional method. The proposed technique allows for a rapid, simple (instant report of the final mercury(II) concentration in water samples via smartphone display), sensitive, selective, and on-site analysis with high sample throughput (48 samples h -1 , n = 3) of trace mercury(II) in water samples, which is suitable for end users who are unskilled in analyzing mercury(II) in water samples.

Investigation of the influence of sampling schemes on quantitative dynamic fluorescence imaging

PubMed Central

Dai, Yunpeng; Chen, Xueli; Yin, Jipeng; Wang, Guodong; Wang, Bo; Zhan, Yonghua; Nie, Yongzhan; Wu, Kaichun; Liang, Jimin

2018-01-01

Dynamic optical data from a series of sampling intervals can be used for quantitative analysis to obtain meaningful kinetic parameters of probe in vivo. The sampling schemes may affect the quantification results of dynamic fluorescence imaging. Here, we investigate the influence of different sampling schemes on the quantification of binding potential (BP) with theoretically simulated and experimentally measured data. Three groups of sampling schemes are investigated including the sampling starting point, sampling sparsity, and sampling uniformity. In the investigation of the influence of the sampling starting point, we further summarize two cases by considering the missing timing sequence between the probe injection and sampling starting time. Results show that the mean value of BP exhibits an obvious growth trend with an increase in the delay of the sampling starting point, and has a strong correlation with the sampling sparsity. The growth trend is much more obvious if throwing the missing timing sequence. The standard deviation of BP is inversely related to the sampling sparsity, and independent of the sampling uniformity and the delay of sampling starting time. Moreover, the mean value of BP obtained by uniform sampling is significantly higher than that by using the non-uniform sampling. Our results collectively suggest that a suitable sampling scheme can help compartmental modeling of dynamic fluorescence imaging provide more accurate results and simpler operations. PMID:29675325

The Impact of Rendered Protein Meal Oxidation Level on Shelf-Life, Sensory Characteristics, and Acceptability in Extruded Pet Food.

PubMed

Chanadang, Sirichat; Koppel, Kadri; Aldrich, Greg

2016-07-28

Pet foods are expected to have a shelf-life for 12 months or more. Sensory analysis can be used to determine changes in products and to estimate products' shelf-life. The objectives of this study were to (1) investigate how increasing levels of oxidation in rendered protein meals used to produce extruded pet food affected the sensory properties and (2) determine the effect of shelf-life on pet owners' acceptability of extruded pet food diet formulated without the use of preservative. Pet food diets contained beef meat bone meal (BMBM) and chicken byproduct meal (CBPM) in which the oxidation was retarded with ethoxyquin, mixed tocopherols, or none at all, and then extruded into dry pet foods. These samples represented low, medium, and high oxidation levels, respectively. Samples were stored for 0, 3, 6, 9, and 12 months at ambient temperature. Each time point, samples were evaluated by six highly trained descriptive panelists for sensory attributes related to oxidation. Samples without preservatives were chosen for the acceptability test, since the differences in sensory characteristics over storage time were more distinguishable in those samples. Pet owners evaluated samples for aroma, appearance and overall liking. Descriptive sensory analysis detected significant changes in oxidized-related sensory characteristics over storage time. However, the differences for CBPM samples were more pronounced and directional. The consumer study showed no differences in pet owners' acceptability for BMBM samples. However, the noticeable increase in aroma characteristics (rancid aroma 0.33-4.21) in CBPM samples over storage time did have a negative effect on consumer's liking (overall liking 5.52-4.95).

Analysis of arson fire debris by low temperature dynamic headspace adsorption porous layer open tubular columns.

PubMed

Nichols, Jessica E; Harries, Megan E; Lovestead, Tara M; Bruno, Thomas J

2014-03-21

In this paper we present results of the application of PLOT-cryoadsorption (PLOT-cryo) to the analysis of ignitable liquids in fire debris. We tested ignitable liquids, broadly divided into fuels and solvents (although the majority of the results presented here were obtained with gasoline and diesel fuel) on three substrates: Douglas fir, oak plywood and Nylon carpet. We determined that PLOT-cryo allows the analyst to distinguish all of the ignitable liquids tested by use of a very rapid sampling protocol, and performs better (more recovered components, higher efficiency, lower elution solvent volumes) than a conventional purge and trap method. We also tested the effect of latency (the time period between applying the ignitable liquid and ignition), and we tested a variety of sampling times and a variety of PLOT capillary lengths. Reliable results can be obtained with sampling time periods as short as 3min, and on PLOT capillaries as short as 20cm. The variability of separate samples was also assessed, a study made possible by the high throughput nature of the PLOT-cryo method. We also determined that the method performs better than the conventional carbon strip method that is commonly used in fire debris analysis. Published by Elsevier B.V.

Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration.

PubMed

Olofsson, Madelen A; Bylund, Dan

2015-10-01

A liquid chromatography with electrospray ionization mass spectrometry method was developed to quantitatively and qualitatively analyze 13 hydroxamate siderophores (ferrichrome, ferrirubin, ferrirhodin, ferrichrysin, ferricrocin, ferrioxamine B, D1 , E and G, neocoprogen I and II, coprogen and triacetylfusarinine C). Samples were preconcentrated on-line by a switch-valve setup prior to analyte separation on a Kinetex C18 column. Gradient elution was performed using a mixture of an ammonium formate buffer and acetonitrile. Total analysis time including column conditioning was 20.5 min. Analytes were fragmented by applying collision-induced dissociation, enabling structural identification by tandem mass spectrometry. Limit of detection values for the selected ion monitoring method ranged from 71 pM to 1.5 nM with corresponding values of two to nine times higher for the multiple reaction monitoring method. The liquid chromatography with mass spectrometry method resulted in a robust and sensitive quantification of hydroxamate siderophores as indicated by retention time stability, linearity, sensitivity, precision and recovery. The analytical error of the methods, assessed through random-order, duplicate analysis of soil samples extracted with a mixture of 10 mM phosphate buffer and methanol, appears negligible in relation to between-sample variations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct Detection of Pharmaceuticals and Personal Care Products from Aqueous Samples with Thermally-Assisted Desorption Electrospray Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Campbell, Ian S.; Ton, Alain T.; Mulligan, Christopher C.

2011-07-01

An ambient mass spectrometric method based on desorption electrospray ionization (DESI) has been developed to allow rapid, direct analysis of contaminated water samples, and the technique was evaluated through analysis of a wide array of pharmaceutical and personal care product (PPCP) contaminants. Incorporating direct infusion of aqueous sample and thermal assistance into the source design has allowed low ppt detection limits for the target analytes in drinking water matrices. With this methodology, mass spectral information can be collected in less than 1 min, consuming ~100 μL of total sample. Quantitative ability was also demonstrated without the use of an internal standard, yielding decent linearity and reproducibility. Initial results suggest that this source configuration is resistant to carryover effects and robust towards multi-component samples. The rapid, continuous analysis afforded by this method offers advantages in terms of sample analysis time and throughput over traditional hyphenated mass spectrometric techniques.

Dielectrophoresis-Based Sample Handling in General-Purpose Programmable Diagnostic Instruments

PubMed Central

Gascoyne, Peter R. C.; Vykoukal, Jody V.

2009-01-01

As the molecular origins of disease are better understood, the need for affordable, rapid, and automated technologies that enable microscale molecular diagnostics has become apparent. Widespread use of microsystems that perform sample preparation and molecular analysis could ensure that the benefits of new biomedical discoveries are realized by a maximum number of people, even those in environments lacking any infrastructure. While progress has been made in developing miniaturized diagnostic systems, samples are generally processed off-device using labor-intensive and time-consuming traditional sample preparation methods. We present the concept of an integrated programmable general-purpose sample analysis processor (GSAP) architecture where raw samples are routed to separation and analysis functional blocks contained within a single device. Several dielectrophoresis-based methods that could serve as the foundation for building GSAP functional blocks are reviewed including methods for cell and particle sorting, cell focusing, cell ac impedance analysis, cell lysis, and the manipulation of molecules and reagent droplets. PMID:19684877

Direct detection of pharmaceuticals and personal care products from aqueous samples with thermally-assisted desorption electrospray ionization mass spectrometry.

PubMed

Campbell, Ian S; Ton, Alain T; Mulligan, Christopher C

2011-07-01

An ambient mass spectrometric method based on desorption electrospray ionization (DESI) has been developed to allow rapid, direct analysis of contaminated water samples, and the technique was evaluated through analysis of a wide array of pharmaceutical and personal care product (PPCP) contaminants. Incorporating direct infusion of aqueous sample and thermal assistance into the source design has allowed low ppt detection limits for the target analytes in drinking water matrices. With this methodology, mass spectral information can be collected in less than 1 min, consuming ~100 μL of total sample. Quantitative ability was also demonstrated without the use of an internal standard, yielding decent linearity and reproducibility. Initial results suggest that this source configuration is resistant to carryover effects and robust towards multi-component samples. The rapid, continuous analysis afforded by this method offers advantages in terms of sample analysis time and throughput over traditional hyphenated mass spectrometric techniques.

The use of frozen plasma samples in thromboelastometry.

PubMed

Schoergenhofer, Christian; Buchtele, Nina; Schwameis, Michael; Bartko, Johann; Jilma, Bernd; Jilma-Stohlawetz, Petra

2017-11-01

Thromboelastometry is increasingly used in the clinical and scientific setting. The use of frozen plasma samples may be useful in overcoming certain limitations such as local and timely availability. Whole blood (WB) samples of 20 healthy volunteers were obtained, and plasma was generated. NATEM (n = 20), EXTEM (n = 20) and INTEM (n = 8) analyses were performed in WB, fresh plasma and frozen and thawed plasma. Dabigatran (500, 1000 ng/ml), rivaroxaban (100, 200 ng/ml) or alteplase (333 ng/ml) were added ex vivo to WB, and thromboelastometry was performed in WB and in frozen and thawed plasma samples. Clot formation time, mean clot firmness and the area under the curve were significantly altered in plasma compared to WB. In INTEM and EXTEM analysis, clotting time (CT) was comparable between WB (100%) and fresh (INTEM 114% and EXTEM 93%, ratio of the means) and frozen plasma samples (85 and 99%), whereas in NATEM analysis, the CT increased in fresh (193%) and frozen plasma samples (130%). Dabigatran dose-dependently increased the CT approximately 5- and 9-fold in WB and even more pronounced 10- and 26-fold in plasma. Accordingly, rivaroxaban dose-dependently increased the CT 2- and 2.7-fold in WB, and 3.5- and 4-fold in plasma samples. Hyperfibrinolysis was achieved by addition of alteplase in all WB samples and was reproducible in plasma samples. In conclusion, thromboelastometry, especially INTEM and EXTEM analyses, is possible using frozen and stored plasma samples with comparable results to the corresponding whole blood samples.

Protein Analysis Using Real-Time PCR Instrumentation: Incorporation in an Integrated, Inquiry-Based Project

ERIC Educational Resources Information Center

Southard, Jonathan N.

2014-01-01

Instrumentation for real-time PCR is used primarily for amplification and quantitation of nucleic acids. The capability to measure fluorescence while controlling temperature in multiple samples can also be applied to the analysis of proteins. Conformational stability and changes in stability due to ligand binding are easily assessed. Protein…

Solving chromatographic challenges in comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry using multivariate curve resolution-alternating least squares.

PubMed

Parastar, Hadi; Radović, Jagoš R; Bayona, Josep M; Tauler, Roma

2013-07-01

Multivariate curve resolution-alternating least squares (MCR-ALS) analysis is proposed to solve chromatographic challenges during two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) analysis of complex samples, such as crude oil extract. In view of the fact that the MCR-ALS method is based on the fulfillment of the bilinear model assumption, three-way and four-way GC × GC-TOFMS data are preferably arranged in a column-wise superaugmented data matrix in which mass-to-charge ratios (m/z) are in its columns and the elution times in the second and first chromatographic columns are in its rows. Since m/z values are common for all measured spectra in all second-column modulations, unavoidable chromatographic challenges such as retention time shifts within and between GC × GC-TOFMS experiments are properly handled. In addition, baseline/background contributions can be modeled by adding extra components to the MCR-ALS model. Another outstanding aspect of MCR-ALS analysis is its extreme flexibility to consider all samples (standards, unknowns, and replicates) in a single superaugmented data matrix, allowing joint analysis. In this way, resolution, identification, and quantification results can be simultaneously obtained in a very fast and reliable way. The potential of MCR-ALS analysis is demonstrated in GC × GC-TOFMS analysis of a North Sea crude oil extract sample with relative errors in estimated concentrations of target compounds below 6.0 % and relative standard deviations lower than 7.0 %. The results obtained, along with reasonable values for the lack of fit of the MCR-ALS model and high values of the reversed match factor in mass spectra similarity searches, confirm the reliability of the proposed strategy for GC × GC-TOFMS data analysis.

Optimized Design and Analysis of Sparse-Sampling fMRI Experiments

PubMed Central

Perrachione, Tyler K.; Ghosh, Satrajit S.

2013-01-01

Sparse-sampling is an important methodological advance in functional magnetic resonance imaging (fMRI), in which silent delays are introduced between MR volume acquisitions, allowing for the presentation of auditory stimuli without contamination by acoustic scanner noise and for overt vocal responses without motion-induced artifacts in the functional time series. As such, the sparse-sampling technique has become a mainstay of principled fMRI research into the cognitive and systems neuroscience of speech, language, hearing, and music. Despite being in use for over a decade, there has been little systematic investigation of the acquisition parameters, experimental design considerations, and statistical analysis approaches that bear on the results and interpretation of sparse-sampling fMRI experiments. In this report, we examined how design and analysis choices related to the duration of repetition time (TR) delay (an acquisition parameter), stimulation rate (an experimental design parameter), and model basis function (an analysis parameter) act independently and interactively to affect the neural activation profiles observed in fMRI. First, we conducted a series of computational simulations to explore the parameter space of sparse design and analysis with respect to these variables; second, we validated the results of these simulations in a series of sparse-sampling fMRI experiments. Overall, these experiments suggest the employment of three methodological approaches that can, in many situations, substantially improve the detection of neurophysiological response in sparse fMRI: (1) Sparse analyses should utilize a physiologically informed model that incorporates hemodynamic response convolution to reduce model error. (2) The design of sparse fMRI experiments should maintain a high rate of stimulus presentation to maximize effect size. (3) TR delays of short to intermediate length can be used between acquisitions of sparse-sampled functional image volumes to increase the number of samples and improve statistical power. PMID:23616742

Optimized design and analysis of sparse-sampling FMRI experiments.

PubMed

Perrachione, Tyler K; Ghosh, Satrajit S

2013-01-01

Sparse-sampling is an important methodological advance in functional magnetic resonance imaging (fMRI), in which silent delays are introduced between MR volume acquisitions, allowing for the presentation of auditory stimuli without contamination by acoustic scanner noise and for overt vocal responses without motion-induced artifacts in the functional time series. As such, the sparse-sampling technique has become a mainstay of principled fMRI research into the cognitive and systems neuroscience of speech, language, hearing, and music. Despite being in use for over a decade, there has been little systematic investigation of the acquisition parameters, experimental design considerations, and statistical analysis approaches that bear on the results and interpretation of sparse-sampling fMRI experiments. In this report, we examined how design and analysis choices related to the duration of repetition time (TR) delay (an acquisition parameter), stimulation rate (an experimental design parameter), and model basis function (an analysis parameter) act independently and interactively to affect the neural activation profiles observed in fMRI. First, we conducted a series of computational simulations to explore the parameter space of sparse design and analysis with respect to these variables; second, we validated the results of these simulations in a series of sparse-sampling fMRI experiments. Overall, these experiments suggest the employment of three methodological approaches that can, in many situations, substantially improve the detection of neurophysiological response in sparse fMRI: (1) Sparse analyses should utilize a physiologically informed model that incorporates hemodynamic response convolution to reduce model error. (2) The design of sparse fMRI experiments should maintain a high rate of stimulus presentation to maximize effect size. (3) TR delays of short to intermediate length can be used between acquisitions of sparse-sampled functional image volumes to increase the number of samples and improve statistical power.

Refining Collective Coordinates and Improving Free Energy Representation in Variational Enhanced Sampling.

PubMed

Yang, Yi Isaac; Parrinello, Michele

2018-06-12

Collective variables are used often in many enhanced sampling methods, and their choice is a crucial factor in determining sampling efficiency. However, at times, searching for good collective variables can be challenging. In a recent paper, we combined time-lagged independent component analysis with well-tempered metadynamics in order to obtain improved collective variables from metadynamics runs that use lower quality collective variables [ McCarty, J.; Parrinello, M. J. Chem. Phys. 2017 , 147 , 204109 ]. In this work, we extend these ideas to variationally enhanced sampling. This leads to an efficient scheme that is able to make use of the many advantages of the variational scheme. We apply the method to alanine-3 in water. From an alanine-3 variationally enhanced sampling trajectory in which all the six dihedral angles are biased, we extract much better collective variables able to describe in exquisite detail the protein complex free energy surface in a low dimensional representation. The success of this investigation is helped by a more accurate way of calculating the correlation functions needed in the time-lagged independent component analysis and from the introduction of a new basis set to describe the dihedral angles arrangement.

Analysis of formaldehyde and acrolein in the aqueous samples using a novel needle trap device containing nanoporous silica aerogel sorbent.

PubMed

Barkhordari, Abdullah; Azari, Mansour R; Zendehdel, Rezvan; Heidari, Mahmoud

2017-04-01

In this research, a needle trap device (NTD) packed with nanoporous silica aerogel as a sorbent was used as a new technique for sampling and analysis of formaldehyde and acrolein compounds in aqueous and urine samples. The obtained results were compared with those of the commercial sorbent Carboxen1000. Active sampling was used and a 21-G needle was applied for extraction of gas in the sample headspace. The optimization of experimental parameters like salt addition, temperature and desorption time was done and the performance of the NTD for the extraction of the compounds was evaluated. The optimum temperature and time of desorption were 280 °C and 2 min, respectively. The ranges of limit of detection, limit of quantification and relative standard deviation (RSD) were 0.01-0.03 μg L -1 , 0.03-0.1 μg L -1 and 2.8-7.3%, respectively. It was found that the NTD containing nanoporous silica aerogel had a better performance. Thus, this technique can be applied as an effective and reliable method for sampling and analysis of aldehyde compounds from different biological matrices like urine, exhalation and so on.

A Guideline to Univariate Statistical Analysis for LC/MS-Based Untargeted Metabolomics-Derived Data

PubMed Central

Vinaixa, Maria; Samino, Sara; Saez, Isabel; Duran, Jordi; Guinovart, Joan J.; Yanes, Oscar

2012-01-01

Several metabolomic software programs provide methods for peak picking, retention time alignment and quantification of metabolite features in LC/MS-based metabolomics. Statistical analysis, however, is needed in order to discover those features significantly altered between samples. By comparing the retention time and MS/MS data of a model compound to that from the altered feature of interest in the research sample, metabolites can be then unequivocally identified. This paper reports on a comprehensive overview of a workflow for statistical analysis to rank relevant metabolite features that will be selected for further MS/MS experiments. We focus on univariate data analysis applied in parallel on all detected features. Characteristics and challenges of this analysis are discussed and illustrated using four different real LC/MS untargeted metabolomic datasets. We demonstrate the influence of considering or violating mathematical assumptions on which univariate statistical test rely, using high-dimensional LC/MS datasets. Issues in data analysis such as determination of sample size, analytical variation, assumption of normality and homocedasticity, or correction for multiple testing are discussed and illustrated in the context of our four untargeted LC/MS working examples. PMID:24957762

A Guideline to Univariate Statistical Analysis for LC/MS-Based Untargeted Metabolomics-Derived Data.

PubMed

Vinaixa, Maria; Samino, Sara; Saez, Isabel; Duran, Jordi; Guinovart, Joan J; Yanes, Oscar

2012-10-18

Several metabolomic software programs provide methods for peak picking, retention time alignment and quantification of metabolite features in LC/MS-based metabolomics. Statistical analysis, however, is needed in order to discover those features significantly altered between samples. By comparing the retention time and MS/MS data of a model compound to that from the altered feature of interest in the research sample, metabolites can be then unequivocally identified. This paper reports on a comprehensive overview of a workflow for statistical analysis to rank relevant metabolite features that will be selected for further MS/MS experiments. We focus on univariate data analysis applied in parallel on all detected features. Characteristics and challenges of this analysis are discussed and illustrated using four different real LC/MS untargeted metabolomic datasets. We demonstrate the influence of considering or violating mathematical assumptions on which univariate statistical test rely, using high-dimensional LC/MS datasets. Issues in data analysis such as determination of sample size, analytical variation, assumption of normality and homocedasticity, or correction for multiple testing are discussed and illustrated in the context of our four untargeted LC/MS working examples.

A Review of Biological Agent Sampling Methods and ...

EPA Pesticide Factsheets

Report This study was conducted to evaluate current sampling and analytical capabilities, from a time and resource perspective, for a large-scale biological contamination incident. The analysis will be useful for strategically directing future research investment.

Precise turnaround time measurement of laboratory processes using radiofrequency identification technology.

PubMed

Mayer, Horst; Brümmer, Jens; Brinkmann, Thomas

2011-01-01

To implement Lean Six Sigma in our central laboratory we conducted a project to measure single pre-analytical steps influencing turnaround time (TAT) of emergency department (ED) serum samples. The traditional approach of extracting data from the Laboratory Information System (LIS) for a retrospective calculation of a mean TAT is not suitable. Therefore, we used radiofrequency identification (RFID) chips for real time tracking of individual samples at any pre-analytical step. 1,200 serum tubes were labelled with RFID chips and were provided to the emergency department. 3 RFID receivers were installed in the laboratory: at the outlet of the pneumatic tube system, at the centrifuge, and in the analyser area. In addition, time stamps of sample entry at the automated sample distributor and communication of results from the analyser were collected from LIS. 1,023 labelled serum tubes arrived at our laboratory. 899 RFID tags were used for TAT calculation. The following transfer times were determined (median 95th percentile in min:sec): pneumatic tube system --> centrifuge (01:25/04:48), centrifuge --> sample distributor (14:06/5:33), sample distributor --> analysis system zone (02:39/15:07), analysis system zone --> result communication (12:42/22:21). Total TAT was calculated at 33:19/57:40 min:sec. Manual processes around centrifugation were identified as a major part of TAT with 44%/60% (median/95th percentile). RFID is a robust, easy to use, and error-free technology and not susceptible to interferences in the laboratory environment. With this study design we were able to measure significant variations in a single manual sample transfer process. We showed that TAT is mainly influenced by manual steps around the centrifugation process and we concluded that centrifugation should be integrated in solutions for total laboratory automation.

Wireless, battery-operated data acquisition system for mobile spectrometry applications and (potentially) for the Internet of things

NASA Astrophysics Data System (ADS)

Fitzgerald, Ryan; Karanassios, Vassili

2017-05-01

There are many applications requiring chemical analysis in the field and analytical results in (near) real-time. For example, when accidental spills occur. In others, collecting samples in the field followed by analysis in a lab increases costs and introduces time-delays. In such cases, "bring part of the lab to the sample" would be ideal. Toward this ideal (and to further reduce size and weight), we developed a relatively inexpensive, battery-operated, wireless data acquisition hardware system around an Arduino nano micro-controller and a 16-bit ADC (Analog-to- Digital Converter) with a max sampling rate of 860 samples/s. The hardware communicates the acquired data using low-power Bluetooth. Software for data acquisition and data display was written in Python. Potential ways of making the hardware-software approach described here a part of the Internet-of-Things (IoT) are presented.

Assessment of laboratory test utilization for HIV/AIDS care in urban ART clinics of Lilongwe, Malawi.

PubMed

Palchaudhuri, Sonali; Tweya, Hannock; Hosseinipour, Mina

2014-06-01

The 2011 Malawi HIV guidelines promote CD4 monitoring for pre-ART assessment and considering HIVRNA monitoring for ART response assessment, while some clinics used CD4 for both. We assessed clinical ordering practices as compared to guidelines, and determined whether the samples were successfully and promptly processed. We conducted a retrospective review of all patients seen in from August 2010 through July 2011,, in two urban HIV-care clinics that utilized 6-monthly CD4 monitoring regardless of ART status. We calculated the percentage of patients on whom clinicians ordered CD4 or HIVRNA analysis. For all samples sent, we determined rates of successful lab-processing, and mean time to returned results. Of 20581 patients seen, 8029 (39%) had at least one blood draw for CD4 count. Among pre-ART patients, 2668/2844 (93.8%) had CD4 counts performed for eligibility. Of all CD4 samples sent, 8082/9207 (89%) samples were successfully processed. Of those, mean time to processing was 1.6 days (s.d 1.5) but mean time to results being available to clinician was 9.3 days (s.d. 3.7). Regarding HIVRNA, 172 patients of 17737 on ART had a blood draw and only 118/213 (55%) samples were successfully processed. Mean processing time was 39.5 days (s.d. 21.7); mean time to results being available to clinician was 43.1 days (s.d. 25.1). During the one-year evaluated, there were multiple lapses in processing HIVRNA samples for up to 2 months. Clinicians underutilize CD4 and HIVRNA as monitoring tools in HIV care. Laboratory processing failures and turnaround times are unacceptably high for viral load analysis. Alternative strategies need to be considered in order to meet laboratory monitoring needs.

Accelerated Optical Projection Tomography Applied to In Vivo Imaging of Zebrafish

PubMed Central

Correia, Teresa; Yin, Jun; Ramel, Marie-Christine; Andrews, Natalie; Katan, Matilda; Bugeon, Laurence; Dallman, Margaret J.; McGinty, James; Frankel, Paul; French, Paul M. W.; Arridge, Simon

2015-01-01

Optical projection tomography (OPT) provides a non-invasive 3-D imaging modality that can be applied to longitudinal studies of live disease models, including in zebrafish. Current limitations include the requirement of a minimum number of angular projections for reconstruction of reasonable OPT images using filtered back projection (FBP), which is typically several hundred, leading to acquisition times of several minutes. It is highly desirable to decrease the number of required angular projections to decrease both the total acquisition time and the light dose to the sample. This is particularly important to enable longitudinal studies, which involve measurements of the same fish at different time points. In this work, we demonstrate that the use of an iterative algorithm to reconstruct sparsely sampled OPT data sets can provide useful 3-D images with 50 or fewer projections, thereby significantly decreasing the minimum acquisition time and light dose while maintaining image quality. A transgenic zebrafish embryo with fluorescent labelling of the vasculature was imaged to acquire densely sampled (800 projections) and under-sampled data sets of transmitted and fluorescence projection images. The under-sampled OPT data sets were reconstructed using an iterative total variation-based image reconstruction algorithm and compared against FBP reconstructions of the densely sampled data sets. To illustrate the potential for quantitative analysis following rapid OPT data acquisition, a Hessian-based method was applied to automatically segment the reconstructed images to select the vasculature network. Results showed that 3-D images of the zebrafish embryo and its vasculature of sufficient visual quality for quantitative analysis can be reconstructed using the iterative algorithm from only 32 projections—achieving up to 28 times improvement in imaging speed and leading to total acquisition times of a few seconds. PMID:26308086

Inter-pulse high-resolution gamma-ray spectra using a 14 MeV pulsed neutron generator

USGS Publications Warehouse

Evans, L.G.; Trombka, J.I.; Jensen, D.H.; Stephenson, W.A.; Hoover, R.A.; Mikesell, J.L.; Tanner, A.B.; Senftle, F.E.

1984-01-01

A neutron generator pulsed at 100 s-1 was suspended in an artificial borehole containing a 7.7 metric ton mixture of sand, aragonite, magnetite, sulfur, and salt. Two Ge(HP) gamma-ray detectors were used: one in a borehole sonde, and one at the outside wall of the sample tank opposite the neutron generator target. Gamma-ray spectra were collected by the outside detector during each of 10 discrete time windows during the 10 ms period following the onset of gamma-ray build-up after each neutron burst. The sample was measured first when dry and then when saturated with water. In the dry sample, gamma rays due to inelastic neutron scattering, neutron capture, and decay were counted during the first (150 ??s) time window. Subsequently only capture and decay gamma rays were observed. In the wet sample, only neutron capture and decay gamma rays were observed. Neutron capture gamma rays dominated the spectrum during the period from 150 to 400 ??s after the neutron burst in both samples, but decreased with time much more rapidly in the wet sample. A signal-to-noise-ratio (S/N) analysis indicates that optimum conditions for neutron capture analysis occurred in the 350-800 ??s window. A poor S/N in the first 100-150 ??s is due to a large background continuum during the first time interval. Time gating can be used to enhance gamma-ray spectra, depending on the nuclides in the target material and the reactions needed to produce them, and should improve the sensitivity of in situ well logging. ?? 1984.

Characterization and forensic analysis of soil samples using laser-induced breakdown spectroscopy (LIBS).

PubMed

Jantzi, Sarah C; Almirall, José R

2011-07-01

A method for the quantitative elemental analysis of surface soil samples using laser-induced breakdown spectroscopy (LIBS) was developed and applied to the analysis of bulk soil samples for discrimination between specimens. The use of a 266 nm laser for LIBS analysis is reported for the first time in forensic soil analysis. Optimization of the LIBS method is discussed, and the results compared favorably to a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method previously developed. Precision for both methods was <10% for most elements. LIBS limits of detection were <33 ppm and bias <40% for most elements. In a proof of principle study, the LIBS method successfully discriminated samples from two different sites in Dade County, FL. Analysis of variance, Tukey's post hoc test and Student's t test resulted in 100% discrimination with no type I or type II errors. Principal components analysis (PCA) resulted in clear groupings of the two sites. A correct classification rate of 99.4% was obtained with linear discriminant analysis using leave-one-out validation. Similar results were obtained when the same samples were analyzed by LA-ICP-MS, showing that LIBS can provide similar information to LA-ICP-MS. In a forensic sampling/spatial heterogeneity study, the variation between sites, between sub-plots, between samples and within samples was examined on three similar Dade sites. The closer the sampling locations, the closer the grouping on a PCA plot and the higher the misclassification rate. These results underscore the importance of careful sampling for geographic site characterization.

DART-MS: A New Analytical Technique for Forensic Paint Analysis.

PubMed

Marić, Mark; Marano, James; Cody, Robert B; Bridge, Candice

2018-06-05

Automotive paint evidence is one of the most significant forms of evidence obtained in automotive-related incidents. Therefore, the analysis of automotive paint evidence is imperative in forensic casework. Most analytical schemes for automotive paint characterization involve optical microscopy, followed by infrared spectroscopy and pyrolysis-gas chromatography mass spectrometry ( py-GCMS) if required. The main drawback with py-GCMS, aside from its destructive nature, is that this technique is relatively time intensive in comparison to other techniques. Direct analysis in real-time-time-of-flight mass spectrometry (DART-TOFMS) may provide an alternative to py-GCMS, as the rapidity of analysis and minimal sample preparation affords a significant advantage. In this study, automotive clear coats from four vehicles were characterized by DART-TOFMS and a standard py-GCMS protocol. Principal component analysis was utilized to interpret the resultant data and suggested the two techniques provided analogous sample discrimination. Moreover, in some instances DART-TOFMS was able to identify components not observed by py-GCMS and vice versa, which indicates that the two techniques may provide complementary information. Additionally, a thermal desorption/pyrolysis DART-TOFMS methodology was also evaluated to characterize the intact paint chips from the vehicles to ascertain if the linear temperature gradient provided additional discriminatory information. All the paint samples were able to be discriminated based on the distinctive thermal desorption plots afforded from this technique, which may also be utilized for sample discrimination. On the basis of the results, DART-TOFMS may provide an additional tool to the forensic paint examiner.

Noise and drift analysis of non-equally spaced timing data

NASA Technical Reports Server (NTRS)

Vernotte, F.; Zalamansky, G.; Lantz, E.

1994-01-01

Generally, it is possible to obtain equally spaced timing data from oscillators. The measurement of the drifts and noises affecting oscillators is then performed by using a variance (Allan variance, modified Allan variance, or time variance) or a system of several variances (multivariance method). However, in some cases, several samples, or even several sets of samples, are missing. In the case of millisecond pulsar timing data, for instance, observations are quite irregularly spaced in time. Nevertheless, since some observations are very close together (one minute) and since the timing data sequence is very long (more than ten years), information on both short-term and long-term stability is available. Unfortunately, a direct variance analysis is not possible without interpolating missing data. Different interpolation algorithms (linear interpolation, cubic spline) are used to calculate variances in order to verify that they neither lose information nor add erroneous information. A comparison of the results of the different algorithms is given. Finally, the multivariance method was adapted to the measurement sequence of the millisecond pulsar timing data: the responses of each variance of the system are calculated for each type of noise and drift, with the same missing samples as in the pulsar timing sequence. An estimation of precision, dynamics, and separability of this method is given.

Integration of paper spray ionization high-field asymmetric waveform ion mobility spectrometry for forensic applications.

PubMed

Tsai, Chia-Wei; Tipple, Christopher A; Yost, Richard A

2018-04-15

Paper spray ionization (PSI) is an attractive ambient ionization source for mass spectrometry (MS) since it allows the combination of surface sampling and ionization. The minimal sample preparation inherent in this approach greatly reduces the time needed for analysis. However, the ions generated from interfering compounds in the sample and the paper substrate may interfere with the analyte ions. Therefore, the integration of PSI with high-field asymmetric ion mobility spectrometry (FAIMS) is of significant interest since it should reduce the background ions entering the mass analyzer without complicating the analysis or increasing analysis time. Here we demonstrate the integration of PSI with FAIMS/MS and its potential for analysis of samples of forensic interest. In this work, the parameters that can influence the integration, including sampling and ionization by paper spray, the FAIMS separation of analytes from each other and background interferences, and the length of time that a usable signal can be observed for explosives on paper, were evaluated with the integrated system. In the negative ion analysis of 2,4,6-trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), and 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), amounts as low as 1 ng on paper were readily observed. The successful positive ion separation of a set of illicit drugs including heroin, methamphetamine, and cocaine was also achieved. In addition, the positive ion analysis of the chemical warfare agent simulants dimethyl methylphosphonate (DMMP) and diisopropyl methylphosphonate (DIMP) was evaluated. The integration of PSI-FAIMS/MS was demonstrated for the analyses of explosives in negative ion mode and for illicit drugs and CW simulants in positive mode. Paper background ions that could interfere with these analyses were separated by FAIMS. The compensation voltage of an ion obtained by FAIMS provided an additional identification parameter to be combined with the mass spectrum for each analyte. Copyright © 2018 John Wiley & Sons, Ltd.

Technological, rheological and sensory characterizations of a yogurt containing an exopolysaccharide extract from Lactobacillus fermentum Lf2, a new food additive.

PubMed

Ale, Elisa C; Perezlindo, Marcos J; Pavón, Yanina; Peralta, Guillermo H; Costa, Silvia; Sabbag, Nora; Bergamini, Carina; Reinheimer, Jorge A; Binetti, Ana G

2016-12-01

Lactobacillus fermentum Lf2, an autochthonous strain isolated as a non starter culture in Cremoso cheese, produces high EPS levels (~1g/L) in optimized conditions (SDM broth, pH6.0, 30°C, 72h). Technological (texture profile and rheological analysis) and sensory properties of non-fat yogurts with 300 and 600mg EPS/L were studied at 3 and 25days after manufacture. Yogurts with different EPS concentrations showed higher hardness values than the control group at both periods of time, being the only significant difference that remained stable during time. The consistency index was also higher for the treated samples at both times evaluated, being significantly different for samples with 300mg/L of EPS extract, while the flow behavior index was lower for EPS-added yogurts. The thixotropic index was lower (P<0.05) for samples with the highest EPS extract concentration at the end of the storage time. Regarding the sensory analysis, those yogurts with 600mg/L of EPS extract presented the highest values of consistency at 3days of storage. No considerable differences for defects (milk powder, acid, bitter and cooked milk flavors) were perceived between treated and control samples at both times evaluated. Syneresis was also studied and samples with 600mg/L of EPS extract presented the lowest syneresis values at 25days of storage, which considerably decreased with the time of storage. In conclusion, the EPS from L. fermentum Lf2, used as an additive, provided yogurt with creamy consistency and increased hardness, without the presence of unwanted defects and improving the water holding capacity of the product. All the analysis done showed the potential of this extract to be used as a technofunctional natural ingredient, and it should be considered its positive impact on health, according to previous studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of two thin-film microextractions for the analysis of estrogens in aqueous tea extract and environmental water samples by high performance liquid chromatography-ultraviolet detection.

PubMed

Cai, Pei-Shan; Li, Dan; Chen, Jing; Xiong, Chao-Mei; Ruan, Jin-Lan

2015-04-15

Two thin-film microextractions (TFME), octadecylsilane (ODS)-polyacrylonitrile (PAN)-TFME and polar enhanced phase (PEP)-PAN-TFME have been proposed for the analysis of bisphenol-A, diethylstilbestrol and 17β-estradiol in aqueous tea extract and environmental water samples followed by high performance liquid chromatography-ultraviolet detection. Both thin-films were prepared by spraying. The influencing factors including pH, extraction time, desorption solvent, desorption volume, desorption time, ion strength and reusability were investigated. Under the optimal conditions, the two TFME methods are similar in terms of the analytical performance evaluated by standard addition method. The limits of detection for three estrogens in environmental water and aqueous tea extract matrix ranged from 1.3 to 1.6 and 2.8 to 7.1 ng mL(-1) by the two TFME methods, respectively. Both approaches were applied for the analysis of analytes in real aqueous tea extract and environmental water samples, presenting satisfactory recoveries ranged from 87.3% to 109.4% for the spiked samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Selective extraction of halogenated compounds from data measured by comprehensive multidimensional gas chromatography/high resolution time-of-flight mass spectrometry for non-target analysis of environmental and biological samples.

PubMed

Hashimoto, Shunji; Zushi, Yasuyuki; Fushimi, Akihiro; Takazawa, Yoshikatsu; Tanabe, Kiyoshi; Shibata, Yasuyuki

2013-03-22

We developed a method that selectively extracts a subset from comprehensive 2D gas chromatography (GC×GC) and high-resolution time-of-flight mass spectrometry (HRTOFMS) data to detect and identify trace levels of organohalogens. The data were obtained by measuring several environmental and biological samples, namely fly ash, soil, sediment, the atmosphere, and human urine. For global analysis, some samples were measured without purification. By using our novel software, the mass spectra of organochlorines or organobromines were then extracted into a data subset under high mass accuracy conditions that were approximately equivalent to a mass resolution of 6000 for some samples. Mass defect filtering as pre-screening for the data extraction was very effective in removing the mass spectra of hydrocarbons. Those results showed that data obtained with HRTOFMS are valuable for global analysis of organohalogens, and probably of other compounds if specific data extraction methods can be devised. Copyright © 2013 Elsevier B.V. All rights reserved.

Influence of flavor solvent on flavor release and perception in sugar-free chewing gum.

PubMed

Potineni, Rajesh V; Peterson, Devin G

2008-05-14

The influence of flavor solvent [triacetin (TA), propylene glycol (PG), medium chained triglycerides (MCT), or no flavor solvent (NFS)] on the flavor release profile, the textural properties, and the sensory perception of a sugar-free chewing gum was investigated. Time course analysis of the exhaled breath and saliva during chewing gum mastication indicated that flavor solvent addition or type did not influence the aroma release profile; however, the sorbitol release rate was statistically lower for the TA formulated sample in comparison to those with PG, MCT, or NFS. Sensory time-intensity analysis also indicated that the TA formulated sample was statistically lower in perceived sweetness intensity, in comparison with the other chewing gum samples, and also had lower cinnamon-like aroma intensity, presumably due to an interaction between sweetness intensity on aroma perception. Measurement of the chewing gum macroscopic texture by compression analysis during consumption was not correlated to the unique flavor release properties of the TA-chewing gum. However, a relationship between gum base plasticity and retention of sugar alcohol during mastication was proposed to explain the different flavor properties of the TA sample.

Analysis of the 2H-evaporator scale samples (HTF-17-56, -57)

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

Hay, M.; Coleman, C.; Diprete, D.

Savannah River National Laboratory analyzed scale samples from both the wall and cone sections of the 242-16H Evaporator prior to chemical cleaning. The samples were analyzed for uranium and plutonium isotopes required for a Nuclear Criticality Safety Assessment of the scale removal process. The analysis of the scale samples found the material to contain crystalline nitrated cancrinite and clarkeite. Samples from both the wall and cone contain depleted uranium. Uranium concentrations of 16.8 wt% 4.76 wt% were measured in the wall and cone samples, respectively. The ratio of plutonium isotopes in both samples is ~85% Pu-239 and ~15% Pu-238 bymore » mass and shows approximately the same 3.5 times higher concentration in the wall sample versus the cone sample as observed in the uranium concentrations. The mercury concentrations measured in the scale samples were higher than previously reported values. The wall sample contains 19.4 wt% mercury and the cone scale sample 11.4 wt% mercury. The results from the current scales samples show reasonable agreement with previous 242-16H Evaporator scale sample analysis; however, the uranium concentration in the current wall sample is substantially higher than previous measurements.« less

Solvent Hold Tank Sample Results for MCU-16-596-597-598: April 2016 Monthly Sample

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

Fondeur, F. F.; Jones, D. H.

2016-07-12

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-596-597-598), pulled on 04/30/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-596-597-598 indicated the Isopar™L concentration is above its nominal level (102%). The modifier (CS-7SB) is 14% below its nominal concentration, while the TiDG and MaxCalix concentrations are at and above their nominal concentrations, respectively. This analysis confirms the solvent may require the addition of modifier. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expectedmore » to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

Analysis of peptides using an integrated microchip HPLC-MS/MS system.

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

Kirby, Brian J.; Chirica, Gabriela S.; Reichmuth, David S.

Hyphendated LC-MS techniques are quickly becoming the standard tool for protemic analyses. For large homogeneous samples, bulk processing methods and capillary injection and separation techniques are suitable. However, for analysis of small or heterogeneous samples, techniques that can manipulate picoliter samples without dilution are required or samples will be lost or corrupted; further, static nanospray-type flowrates are required to maximize SNR. Microchip-level integration of sample injection with separation and mass spectrometry allow small-volume analytes to be processed on chip and immediately injected without dilution for analysis. An on-chip HPLC was fabricated using in situ polymerization of both fixed and mobilemore » polymer monoliths. Integration of the chip with a nanospray MS emitter enables identification of peptides by the use of tandem MS. The chip is capable of analyzing of very small sample volumes (< 200 pl) in short times (< 3 min).« less

Characterization of potassium bromide crystals grown in the aqueous solution of picric acid

NASA Astrophysics Data System (ADS)

Maheswari, J. Uma; Krishnan, C.; Kalyanaraman, S.; Selvarajan, P.

2016-12-01

Potassium bromide crystals were grown in the aqueous solution of picric acid by slow evaporation technique at room temperature. X-ray Diffraction (XRD) analysis ensures that the grown sample is in Fm3m space group and FCC structure. Energy Dispersive X-ray Spectroscopy (EDX) reveals the presence of elements in the title compound. UV-Vis-NIR spectrum reveals that the grown sample is a promising nonlinear optical (NLO) material. FTIR analysis confirms the functional groups present in the sample. The thermogravimetric (TG) and differential thermogravimetric (DTA) analyses ensure that the sample material is thermally stable up to 160 °C. The second harmonic efficiency of the sample is 1.3 times greater than that of standard KDP. The mechanical strength of the grown sample is estimated by Vickers microhardness tester. The electrical properties were investigated by impedance analysis and the results of various studies of the grown crystals are discussed.

Quality assurance in the pre-analytical phase of human urine samples by (1)H NMR spectroscopy.

PubMed

Budde, Kathrin; Gök, Ömer-Necmi; Pietzner, Maik; Meisinger, Christine; Leitzmann, Michael; Nauck, Matthias; Köttgen, Anna; Friedrich, Nele

2016-01-01

Metabolomic approaches investigate changes in metabolite profiles, which may reflect changes in metabolic pathways and provide information correlated with a specific biological process or pathophysiology. High-resolution (1)H NMR spectroscopy is used to identify metabolites in biofluids and tissue samples qualitatively and quantitatively. This pre-analytical study evaluated the effects of storage time and temperature on (1)H NMR spectra from human urine in two settings. Firstly, to evaluate short time effects probably due to acute delay in sample handling and secondly, the effect of prolonged storage up to one month to find markers of sample miss-handling. A number of statistical procedures were used to assess the differences between samples stored under different conditions, including Projection to Latent Structure Discriminant Analysis (PLS-DA), non-parametric testing as well as mixed effect linear regression analysis. The results indicate that human urine samples can be stored at 10 °C for 24 h or at -80 °C for 1 month, as no relevant changes in (1)H NMR fingerprints were observed during these time periods and temperature conditions. However, some metabolites most likely of microbial origin showed alterations during prolonged storage but without facilitating classification. In conclusion, the presented protocol for urine sample handling and semi-automatic metabolite quantification is suitable for large-scale epidemiological studies. Copyright © 2015 Elsevier Inc. All rights reserved.

Combined PIXE and X-ray SEM studies on time-resolved deposits of welding shop aerosols

NASA Astrophysics Data System (ADS)

Barfoot, K. M.; Mitchell, I. V.; Verheyen, F.; Babeliowsky, T.

1981-03-01

Time-resolved deposits of welding shop air particulates have been obtained using a streak sampling system. PIXE analysis of these deposits, using 2 MeV protons, typically revealed the presence of a large number of elements, with many in the range Z = 11-30. Strong variations, up to three orders of magnitude, in the concentrations of several elements such as Al, Si and Fe as well as Zn, Na, K and Ca were found. The 2 h sampling resolution normally used was found to be insufficient to follow the short pollution episodes that regularly occur in a welding shop environment and so sampling with a 20 min resolution was used. The variation of elemental concentrations for different sampling times together with information on the physical nature of these air particulates, determined with a scanning electron microscope (SEM) and Si(Li) X-ray detector attachment, are presented. This type of information together with that obtained from the PIXE analysis is of importance in industrial hygiene studies. The need to make corrections for partial filter clogging, based on air-flow rate monitoring, is discussed.

Frequency-Modulated Continuous Flow Analysis Electrospray Ionization Mass Spectrometry (FM-CFA-ESI-MS) for Sample Multiplexing.

PubMed

Filla, Robert T; Schrell, Adrian M; Coulton, John B; Edwards, James L; Roper, Michael G

2018-02-20

A method for multiplexed sample analysis by mass spectrometry without the need for chemical tagging is presented. In this new method, each sample is pulsed at unique frequencies, mixed, and delivered to the mass spectrometer while maintaining a constant total flow rate. Reconstructed ion currents are then a time-dependent signal consisting of the sum of the ion currents from the various samples. Spectral deconvolution of each reconstructed ion current reveals the identity of each sample, encoded by its unique frequency, and its concentration encoded by the peak height in the frequency domain. This technique is different from other approaches that have been described, which have used modulation techniques to increase the signal-to-noise ratio of a single sample. As proof of concept of this new method, two samples containing up to 9 analytes were multiplexed. The linear dynamic range of the calibration curve was increased with extended acquisition times of the experiment and longer oscillation periods of the samples. Because of the combination of the samples, salt had little effect on the ability of this method to achieve relative quantitation. Continued development of this method is expected to allow for increased numbers of samples that can be multiplexed.

16S Based Microbiome Analysis from Healthy Subjects’ Skin Swabs Stored for Different Storage Periods Reveal Phylum to Genus Level Changes

PubMed Central

Klymiuk, Ingeborg; Bambach, Isabella; Patra, Vijaykumar; Trajanoski, Slave; Wolf, Peter

2016-01-01

Microbiome research and improvements in high throughput sequencing technologies revolutionize our current scientific viewpoint. The human associated microbiome is a prominent focus of clinical research. Large cohort studies are often required to investigate the human microbiome composition and its changes in a multitude of human diseases. Reproducible analyses of large cohort samples require standardized protocols in study design, sampling, storage, processing, and data analysis. In particular, the effect of sample storage on actual results is critical for reproducibility. So far, the effect of storage conditions on the results of microbial analysis has been examined for only a few human biological materials (e.g., stool samples). There is a lack of data and information on appropriate storage conditions on other human derived samples, such as skin. Here, we analyzed skin swab samples collected from three different body locations (forearm, V of the chest and back) of eight healthy volunteers. The skin swabs were soaked in sterile buffer and total DNA was isolated after freezing at -80°C for 24 h, 90 or 365 days. Hypervariable regions V1-2 were amplified from total DNA and libraries were sequenced on an Illumina MiSeq desktop sequencer in paired end mode. Data were analyzed using Qiime 1.9.1. Summarizing all body locations per time point, we found no significant differences in alpha diversity and multivariate community analysis among the three time points. Considering body locations separately significant differences in the richness of forearm samples were found between d0 vs. d90 and d90 vs. d365. Significant differences in the relative abundance of major skin genera (Propionibacterium, Streptococcus, Bacteroides, Corynebacterium, and Staphylococcus) were detected in our samples in Bacteroides only among all time points in forearm samples and between d0 vs. d90 and d90 vs. d365 in V of the chest and back samples. Accordingly, significant differences were detected in the ratios of the main phyla Actinobacteria, Firmicutes, and Bacteroidetes: Actinobacteria vs. Bacteroidetes at d0 vs. d90 (p-value = 0.0234), at d0 vs. d365 (p-value = 0.0234) and d90 vs. d365 (p-value = 0.0234) in forearm samples and at d90 vs. d365 in V of the chest (p-value = 0.0234) and back samples (p-value = 0.0234). The ratios of Firmicutes vs. Bacteroidetes showed no significant changes in any of the body locations as well as the ratios of Actinobacteria vs. Firmicutes at any time point. Studies with larger sample sizes are required to verify our results and determine long term storage effects with regard to specific biological questions. PMID:28066342

Analysis of Marine Aerosol Polysaccharides by Pyrolysis Time-of-Flight Mass Spectrometry

NASA Astrophysics Data System (ADS)

Lawler, M. J.; Grieman, M. M.; Sengur, I.; Saltzman, E. S.

2017-12-01

The relationship between surface ocean biological productivity and marine cloud formation and properties has been explored for decades, but the impacts of marine biogenic emissions on cloudiness and climate remain highly uncertain. This is in part due to the challenge of directly linking biogenic materials in the surface ocean with cloud-forming aerosol. It has been shown that polysaccharide gel-forming materials, also known as transparent exopolymers, may be mechanically ejected from the sea surface during air bubble bursting (Leck and Bigg, 2005). Existing analysis methods for such aerosols require considerable sample mass and sample preparation. As part of the multi-year seasonal North Atlantic Aerosols and Marine Ecosystems Study (NAAMES), ambient submicron marine aerosol was collected in November 2015 and May 2016 from the R/V Atlantis at using a Particle into Liquid Sampler (PILS). These samples of roughly 15 minute time resolution were frozen and returned to UC Irvine for analysis. A new technique has been developed to attempt to quantify polysaccharide material in these ambient samples. A small subsample (1- 5 µL) is taken from the PILS vial samples and allowed to dry on a Pt ribbon filament in the chemical ionization source region of a time-of-flight mass spectrometer. The sample then undergoes a two-step heating process, in which volatilizable molecules are first desorbed and then non-volatilizable large molecules such as polysaccharides are pyrolyzed. These desorbed molecules and decomposition products are ionized using either O2- or H3O+ reagent ion and are directly sampled into the mass spectrometer. The resulting spectra can then be compared to standards of known polysaccharide materials for quantification and potentially structural and/or compositional information.

Computer image analysis of etched tracks from ionizing radiation

NASA Technical Reports Server (NTRS)

Blanford, George E.

1994-01-01

I proposed to continue a cooperative research project with Dr. David S. McKay concerning image analysis of tracks. Last summer we showed that we could measure track densities using the Oxford Instruments eXL computer and software that is attached to an ISI scanning electron microscope (SEM) located in building 31 at JSC. To reduce the dependence on JSC equipment, we proposed to transfer the SEM images to UHCL for analysis. Last summer we developed techniques to use digitized scanning electron micrographs and computer image analysis programs to measure track densities in lunar soil grains. Tracks were formed by highly ionizing solar energetic particles and cosmic rays during near surface exposure on the Moon. The track densities are related to the exposure conditions (depth and time). Distributions of the number of grains as a function of their track densities can reveal the modality of soil maturation. As part of a consortium effort to better understand the maturation of lunar soil and its relation to its infrared reflectance properties, we worked on lunar samples 67701,205 and 61221,134. These samples were etched for a shorter time (6 hours) than last summer's sample and this difference has presented problems for establishing the correct analysis conditions. We used computer counting and measurement of area to obtain preliminary track densities and a track density distribution that we could interpret for sample 67701,205. This sample is a submature soil consisting of approximately 85 percent mature soil mixed with approximately 15 percent immature, but not pristine, soil.

PTR-ToF-MS Coupled with an Automated Sampling System and Tailored Data Analysis for Food Studies: Bioprocess Monitoring, Screening and Nose-space Analysis.

PubMed

Capozzi, Vittorio; Yener, Sine; Khomenko, Iuliia; Farneti, Brian; Cappellin, Luca; Gasperi, Flavia; Scampicchio, Matteo; Biasioli, Franco

2017-05-11

Proton Transfer Reaction (PTR), combined with a Time-of-Flight (ToF) Mass Spectrometer (MS) is an analytical approach based on chemical ionization that belongs to the Direct-Injection Mass Spectrometric (DIMS) technologies. These techniques allow the rapid determination of volatile organic compounds (VOCs), assuring high sensitivity and accuracy. In general, PTR-MS requires neither sample preparation nor sample destruction, allowing real time and non-invasive analysis of samples. PTR-MS are exploited in many fields, from environmental and atmospheric chemistry to medical and biological sciences. More recently, we developed a methodology based on coupling PTR-ToF-MS with an automated sampler and tailored data analysis tools, to increase the degree of automation and, consequently, to enhance the potential of the technique. This approach allowed us to monitor bioprocesses (e.g. enzymatic oxidation, alcoholic fermentation), to screen large sample sets (e.g. different origins, entire germoplasms) and to analyze several experimental modes (e.g. different concentrations of a given ingredient, different intensities of a specific technological parameter) in terms of VOC content. Here, we report the experimental protocols exemplifying different possible applications of our methodology: i.e. the detection of VOCs released during lactic acid fermentation of yogurt (on-line bioprocess monitoring), the monitoring of VOCs associated with different apple cultivars (large-scale screening), and the in vivo study of retronasal VOC release during coffee drinking (nosespace analysis).

Fast Fourier Transform Spectral Analysis Program

NASA Technical Reports Server (NTRS)

Daniel, J. A., Jr.; Graves, M. L.; Hovey, N. M.

1969-01-01

Fast Fourier Transform Spectral Analysis Program is used in frequency spectrum analysis of postflight, space vehicle telemetered trajectory data. This computer program with a digital algorithm can calculate power spectrum rms amplitudes and cross spectrum of sampled parameters at even time increments.

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

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

Rahman, Nur Aira Abd, E-mail: nur-aira@nuclearmalaysia.gov.my; Yussup, Nolida; Ibrahim, Maslina Bt. Mohd

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on ‘Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)’. The objective ofmore » the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.« less

Automated high-throughput flow-through real-time diagnostic system

DOEpatents

Regan, John Frederick

2012-10-30

An automated real-time flow-through system capable of processing multiple samples in an asynchronous, simultaneous, and parallel fashion for nucleic acid extraction and purification, followed by assay assembly, genetic amplification, multiplex detection, analysis, and decontamination. The system is able to hold and access an unlimited number of fluorescent reagents that may be used to screen samples for the presence of specific sequences. The apparatus works by associating extracted and purified sample with a series of reagent plugs that have been formed in a flow channel and delivered to a flow-through real-time amplification detector that has a multiplicity of optical windows, to which the sample-reagent plugs are placed in an operative position. The diagnostic apparatus includes sample multi-position valves, a master sample multi-position valve, a master reagent multi-position valve, reagent multi-position valves, and an optical amplification/detection system.

A new analysis system for whole air sampling: description and results from 2013 SENEX

NASA Astrophysics Data System (ADS)

Lerner, B. M.; Gilman, J.; Dumas, M.; Hughes, D.; Jaksich, A.; Hatch, C. D.; Graus, M.; Warneke, C.; Apel, E. C.; Hornbrook, R. S.; Holloway, J. S.; De Gouw, J. A.

2014-12-01

Accurate measurement of volatile organic compounds (VOCs) in the troposphere is critical for the understanding of emissions and physical and chemical processes that can impact both air quality and climate. Airborne VOC measurements have proven especially challenging due to the requirement of both high sensitivity (pptv) and short sample collection times (≤15 s) to maximize spatial resolution and sampling frequency for targeted plume analysis. The use of stainless steel canisters to collect whole air samples (WAS) for post-flight analysis has been pioneered by the groups of D. Blake and E. Atlas [Blake et al., 1992; Atlas et al., 1993]. For the 2013 Southeast Nexus Study (SENEX), the NOAA ESRL CSD laboratory undertook WAS measurements for the first time. This required the construction of three new, highly-automated, and field-portable instruments designed to sample, analyze, and clean the canisters for re-use. Analysis was performed with a new custom-built gas chromatograph-mass spectrometer system. The instrument pre-concentrates analyte cryostatically into two parallel traps by means of a Stirling engine, a novel technique which obviates the need for liquid nitrogen to reach trapping temperatures of -175C. Here we present an evaluation of the retrieval of target VOC species from WAS canisters. We discuss the effects of humidity and sample age on the analyte, particularly upon C8+ alkane and aromatic species and biogenic species. Finally, we present results from several research flights during SENEX that targeted emissions from oil/natural gas production.

[Modal failure analysis and effects in the detection of errors in the transport of samples to the clinical laboratory].

PubMed

Parés-Pollán, L; Gonzalez-Quintana, A; Docampo-Cordeiro, J; Vargas-Gallego, C; García-Álvarez, G; Ramos-Rodríguez, V; Diaz Rubio-García, M P

2014-01-01

Owing to the decrease in values of biochemical glucose parameter in some samples from external extraction centres, and the risk this implies to patient safety; it was decided to apply an adaptation of the «Health Services Failure Mode and Effects Analysis» (HFMEA) to manage risk during the pre-analytical phase of sample transportation from external centres to clinical laboratories. A retrospective study of glucose parameter was conducted during two consecutive months. The analysis was performed in its different phases: to define the HFMEA topic, assemble the team, graphically describe the process, conduct a hazard analysis, design the intervention and indicators, and identify a person to be responsible for ensuring completion of each action. The results of glucose parameter in one of the transport routes, were significantly lower (P=.006). The errors and potential causes of this problem were analysed, and criteria of criticality and detectability were applied (score≥8) in the decision tree. It was decided to: develop a document management system; reorganise extractions and transport routes in some centres; quality control of the sample container ice-packs, and the time and temperature during transportation. This work proposes quality indicators for controlling time and temperature of transported samples in the pre-analytical phase. Periodic review of certain laboratory parameters can help to detect problems in transporting samples. The HFMEA technique is useful for the clinical laboratory. Copyright © 2013 SECA. Published by Elsevier Espana. All rights reserved.

A novel PMT test system based on waveform sampling

NASA Astrophysics Data System (ADS)

Yin, S.; Ma, L.; Ning, Z.; Qian, S.; Wang, Y.; Jiang, X.; Wang, Z.; Yu, B.; Gao, F.; Zhu, Y.; Wang, Z.

2018-01-01

Comparing with the traditional test system based on a QDC and TDC and scaler, a test system based on waveform sampling is constructed for signal sampling of the 8"R5912 and the 20"R12860 Hamamatsu PMT in different energy states from single to multiple photoelectrons. In order to achieve high throughput and to reduce the dead time in data processing, the data acquisition software based on LabVIEW is developed and runs with a parallel mechanism. The analysis algorithm is realized in LabVIEW and the spectra of charge, amplitude, signal width and rising time are analyzed offline. The results from Charge-to-Digital Converter, Time-to-Digital Converter and waveform sampling are discussed in detailed comparison.

Sensor-triggered sampling to determine instantaneous airborne vapor exposure concentrations.

PubMed

Smith, Philip A; Simmons, Michael K; Toone, Phillip

2018-06-01

It is difficult to measure transient airborne exposure peaks by means of integrated sampling for organic chemical vapors, even with very short-duration sampling. Selection of an appropriate time to measure an exposure peak through integrated sampling is problematic, and short-duration time-weighted average (TWA) values obtained with integrated sampling are not likely to accurately determine actual peak concentrations attained when concentrations fluctuate rapidly. Laboratory analysis for integrated exposure samples is preferred from a certainty standpoint over results derived in the field from a sensor, as a sensor user typically must overcome specificity issues and a number of potential interfering factors to obtain similarly reliable data. However, sensors are currently needed to measure intra-exposure period concentration variations (i.e., exposure peaks). In this article, the digitized signal from a photoionization detector (PID) sensor triggered collection of whole-air samples when toluene or trichloroethylene vapors attained pre-determined levels in a laboratory atmosphere generation system. Analysis by gas chromatography-mass spectrometry of whole-air samples (with both 37 and 80% relative humidity) collected using the triggering mechanism with rapidly increasing vapor concentrations showed good agreement with the triggering set point values. Whole-air samples (80% relative humidity) in canisters demonstrated acceptable 17-day storage recoveries, and acceptable precision and bias were obtained. The ability to determine exceedance of a ceiling or peak exposure standard by laboratory analysis of an instantaneously collected sample, and to simultaneously provide a calibration point to verify the correct operation of a sensor was demonstrated. This latter detail may increase the confidence in reliability of sensor data obtained across an entire exposure period.

Detecting spatial patterns of rivermouth processes using a geostatistical framework for near-real-time analysis

USGS Publications Warehouse

Xu, Wenzhao; Collingsworth, Paris D.; Bailey, Barbara; Carlson Mazur, Martha L.; Schaeffer, Jeff; Minsker, Barbara

2017-01-01

This paper proposes a geospatial analysis framework and software to interpret water-quality sampling data from towed undulating vehicles in near-real time. The framework includes data quality assurance and quality control processes, automated kriging interpolation along undulating paths, and local hotspot and cluster analyses. These methods are implemented in an interactive Web application developed using the Shiny package in the R programming environment to support near-real time analysis along with 2- and 3-D visualizations. The approach is demonstrated using historical sampling data from an undulating vehicle deployed at three rivermouth sites in Lake Michigan during 2011. The normalized root-mean-square error (NRMSE) of the interpolation averages approximately 10% in 3-fold cross validation. The results show that the framework can be used to track river plume dynamics and provide insights on mixing, which could be related to wind and seiche events.

Development of an online SPE-UHPLC-MS/MS method for the multiresidue analysis of the 17 compounds from the EU "Watch list".

PubMed

Gusmaroli, Lucia; Insa, Sara; Petrovic, Mira

2018-04-24

During the last decades, the quality of aquatic ecosystems has been threatened by increasing levels of pollutions, caused by the discharge of man-made chemicals, both via accidental release of pollutants as well as a consequence of the constant outflow of inadequately treated wastewater effluents. For this reason, the European Union is updating its legislations with the aim of limiting the release of emerging contaminants. The Commission Implementing Decision (EU) 2015/495 published in March 2015 drafts a "Watch list" of compounds to be monitored Europe-wide. In this study, a methodology based on online solid-phase extraction (SPE) ultra-high-performance liquid chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-MS/MS) was developed for the simultaneous determination of the 17 compounds listed therein. The proposed method offers advantages over already available methods, such as versatility (all 17 compounds can be analyzed simultaneously), shorter time required for analysis, robustness, and sensitivity. The employment of online sample preparation minimized sample manipulation and reduced dramatically the sample volume needed and time required, dramatically the sample volume needed and time required, thus making the analysis fast and reliable. The method was successfully validated in surface water and influent and effluent wastewater. Limits of detection ranged from sub- to low-nanogram per liter levels, in compliance with the EU limits, with the only exception of EE2. Graphical abstract Schematic of the workflow for the analysis of the Watch list compounds.

Dating ivory by determination of 14C, 90Sr and 228/232Th.

PubMed

Schmied, Stefanie A K; Brunnermeier, Matthias J; Schupfner, Robert; Wolfbeis, Otto S

2012-09-10

A method is described to determine the time of death of elephants. This is accomplished by analysis of the radionuclides 14C, 90Sr and 228/232Th in known samples of ivory, and in samples of unknown age. The reliability of this method is considerably increased by multi nuclide analysis. Copyright © 2012 Elsevier Ireland 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.

Rapid detection of terbufos in stomach contents using desorption electrospray ionization mass spectrometry.

PubMed

Wilson, Christina R; Mulligan, Christopher C; Strueh, Kurt D; Stevenson, Gregory W; Hooser, Stephen B

2014-05-01

Desorption electrospray ionization mass spectrometry (DESI-MS) is an emerging analytical technique that permits the rapid and direct analysis of biological or environmental samples under ambient conditions. Highlighting the versatility of this technique, DESI-MS has been used for the rapid detection of illicit drugs, chemical warfare agents, agricultural chemicals, and pharmaceuticals from a variety of sample matrices. In diagnostic veterinary toxicology, analyzing samples using traditional analytical instrumentation typically includes extensive sample extraction procedures, which can be time consuming and labor intensive. Therefore, efforts to expedite sample analyses are a constant goal for diagnostic toxicology laboratories. In the current report, DESI-MS was used to directly analyze stomach contents from a dog exposed to the organophosphate insecticide terbufos. The total DESI-MS analysis time required to confirm the presence of terbufos and diagnose organophosphate poisoning in this case was approximately 5 min. This highlights the potential of this analytical technique in the field of veterinary toxicology for the rapid diagnosis and detection of toxicants in biological samples. © 2014 The Author(s).

Detection of Babesia canis vogeli and Hepatozoon canis in canine blood by a single-tube real-time fluorescence resonance energy transfer polymerase chain reaction assay and melting curve analysis.

PubMed

Kongklieng, Amornmas; Intapan, Pewpan M; Boonmars, Thidarut; Thanchomnang, Tongjit; Janwan, Penchom; Sanpool, Oranuch; Lulitanond, Viraphong; Taweethavonsawat, Piyanan; Chungpivat, Sudchit; Maleewong, Wanchai

2015-03-01

A real-time fluorescence resonance energy transfer polymerase chain reaction (qFRET PCR) coupled with melting curve analysis was developed for detection of Babesia canis vogeli and Hepatozoon canis infections in canine blood samples in a single tube assay. The target of the assay was a region within the 18S ribosomal RNA gene amplified in either species by a single pair of primers. Following amplification from the DNA of infected dog blood, a fluorescence melting curve analysis was done. The 2 species, B. canis vogeli and H. canis, could be detected and differentiated in infected dog blood samples (n = 37) with high sensitivity (100%). The detection limit for B. canis vogeli was 15 copies of a positive control plasmid, and for H. canis, it was 150 copies of a positive control plasmid. The assay could simultaneously distinguish the DNA of both parasites from the DNA of controls. Blood samples from 5 noninfected dogs were negative, indicating high specificity. Several samples can be run at the same time. The assay can reduce misdiagnosis and the time associated with microscopic examination, and is not prone to the carryover contamination associated with the agarose gel electrophoresis step of conventional PCR. In addition, this qFRET PCR method would be useful to accurately determine the range of endemic areas or to discover those areas where the 2 parasites co-circulate. © 2015 The Author(s).

Modified cross sample entropy and surrogate data analysis method for financial time series

NASA Astrophysics Data System (ADS)

Yin, Yi; Shang, Pengjian

2015-09-01

For researching multiscale behaviors from the angle of entropy, we propose a modified cross sample entropy (MCSE) and combine surrogate data analysis with it in order to compute entropy differences between original dynamics and surrogate series (MCSDiff). MCSDiff is applied to simulated signals to show accuracy and then employed to US and Chinese stock markets. We illustrate the presence of multiscale behavior in the MCSDiff results and reveal that there are synchrony containing in the original financial time series and they have some intrinsic relations, which are destroyed by surrogate data analysis. Furthermore, the multifractal behaviors of cross-correlations between these financial time series are investigated by multifractal detrended cross-correlation analysis (MF-DCCA) method, since multifractal analysis is a multiscale analysis. We explore the multifractal properties of cross-correlation between these US and Chinese markets and show the distinctiveness of NQCI and HSI among the markets in their own region. It can be concluded that the weaker cross-correlation between US markets gives the evidence for the better inner mechanism in the US stock markets than that of Chinese stock markets. To study the multiscale features and properties of financial time series can provide valuable information for understanding the inner mechanism of financial markets.

Accelerometer Data Analysis and Presentation Techniques

NASA Technical Reports Server (NTRS)

Rogers, Melissa J. B.; Hrovat, Kenneth; McPherson, Kevin; Moskowitz, Milton E.; Reckart, Timothy

1997-01-01

The NASA Lewis Research Center's Principal Investigator Microgravity Services project analyzes Orbital Acceleration Research Experiment and Space Acceleration Measurement System data for principal investigators of microgravity experiments. Principal investigators need a thorough understanding of data analysis techniques so that they can request appropriate analyses to best interpret accelerometer data. Accelerometer data sampling and filtering is introduced along with the related topics of resolution and aliasing. Specific information about the Orbital Acceleration Research Experiment and Space Acceleration Measurement System data sampling and filtering is given. Time domain data analysis techniques are discussed and example environment interpretations are made using plots of acceleration versus time, interval average acceleration versus time, interval root-mean-square acceleration versus time, trimmean acceleration versus time, quasi-steady three dimensional histograms, and prediction of quasi-steady levels at different locations. An introduction to Fourier transform theory and windowing is provided along with specific analysis techniques and data interpretations. The frequency domain analyses discussed are power spectral density versus frequency, cumulative root-mean-square acceleration versus frequency, root-mean-square acceleration versus frequency, one-third octave band root-mean-square acceleration versus frequency, and power spectral density versus frequency versus time (spectrogram). Instructions for accessing NASA Lewis Research Center accelerometer data and related information using the internet are provided.

Description of a Portable Wireless Device for High-Frequency Body Temperature Acquisition and Analysis

PubMed Central

Cuesta-Frau, David; Varela, Manuel; Aboy, Mateo; Miró-Martínez, Pau

2009-01-01

We describe a device for dual channel body temperature monitoring. The device can operate as a real time monitor or as a data logger, and has Bluetooth capabilities to enable for wireless data download to the computer used for data analysis. The proposed device is capable of sampling temperature at a rate of 1 sample per minute with a resolution of 0.01 °C . The internal memory allows for stand-alone data logging of up to 10 days. The device has a battery life of 50 hours in continuous real-time mode. In addition to describing the proposed device in detail, we report the results of a statistical analysis conducted to assess its accuracy and reproducibility. PMID:22408473

Description of a portable wireless device for high-frequency body temperature acquisition and analysis.

PubMed

Cuesta-Frau, David; Varela, Manuel; Aboy, Mateo; Miró-Martínez, Pau

2009-01-01

We describe a device for dual channel body temperature monitoring. The device can operate as a real time monitor or as a data logger, and has Bluetooth capabilities to enable for wireless data download to the computer used for data analysis. The proposed device is capable of sampling temperature at a rate of 1 sample per minute with a resolution of 0.01 °C . The internal memory allows for stand-alone data logging of up to 10 days. The device has a battery life of 50 hours in continuous real-time mode. In addition to describing the proposed device in detail, we report the results of a statistical analysis conducted to assess its accuracy and reproducibility.

Improving laboratory results turnaround time by reducing pre analytical phase.

PubMed

Khalifa, Mohamed; Khalid, Parwaiz

2014-01-01

Laboratory turnaround time is considered one of the most important indicators of work efficiency in hospitals, physicians always need timely results to take effective clinical decisions especially in the emergency department where these results can guide physicians whether to admit patients to the hospital, discharge them home or do further investigations. A retrospective data analysis study was performed to identify the effects of ER and Lab staff training on new routines for sample collection and transportation on the pre-analytical phase of turnaround time. Renal profile tests requested by the ER and performed in 2013 has been selected as a sample, and data about 7,519 tests were retrieved and analyzed to compare turnaround time intervals before and after implementing new routines. Results showed significant time reduction on "Request to Sample Collection" and "Collection to In Lab Delivery" time intervals with less significant improvement on the analytical phase of the turnaround time.

Spin-analyzed SANS for soft matter applications

NASA Astrophysics Data System (ADS)

Chen, W. C.; Barker, J. G.; Jones, R.; Krycka, K. L.; Watson, S. M.; Gagnon, C.; Perevozchivoka, T.; Butler, P.; Gentile, T. R.

2017-06-01

The small angle neutron scattering (SANS) of nearly Q-independent nuclear spin-incoherent scattering from hydrogen present in most soft matter and biology samples may raise an issue in structure determination in certain soft matter applications. This is true at high wave vector transfer Q where coherent scattering is much weaker than the nearly Q-independent spin-incoherent scattering background. Polarization analysis is capable of separating coherent scattering from spin-incoherent scattering, hence potentially removing the nearly Q-independent background. Here we demonstrate SANS polarization analysis in conjunction with the time-of-flight technique for separation of coherent and nuclear spin-incoherent scattering for a sample of silver behenate back-filled with light water. We describe a complete procedure for SANS polarization analysis for separating coherent from incoherent scattering for soft matter samples that show inelastic scattering. Polarization efficiency correction and subsequent separation of the coherent and incoherent scattering have been done with and without a time-of-flight technique for direct comparisons. In addition, we have accounted for the effect of multiple scattering from light water to determine the contribution of nuclear spin-incoherent scattering in both the spin flip channel and non-spin flip channel when performing SANS polarization analysis. We discuss the possible gain in the signal-to-noise ratio for the measured coherent scattering signal using polarization analysis with the time-of-flight technique compared with routine unpolarized SANS measurements.

A real time metabolomic profiling approach to detecting fish fraud using rapid evaporative ionisation mass spectrometry.

PubMed

Black, Connor; Chevallier, Olivier P; Haughey, Simon A; Balog, Julia; Stead, Sara; Pringle, Steven D; Riina, Maria V; Martucci, Francesca; Acutis, Pier L; Morris, Mike; Nikolopoulos, Dimitrios S; Takats, Zoltan; Elliott, Christopher T

2017-01-01

Fish fraud detection is mainly carried out using a genomic profiling approach requiring long and complex sample preparations and assay running times. Rapid evaporative ionisation mass spectrometry (REIMS) can circumvent these issues without sacrificing a loss in the quality of results. To demonstrate that REIMS can be used as a fast profiling technique capable of achieving accurate species identification without the need for any sample preparation. Additionally, we wanted to demonstrate that other aspects of fish fraud other than speciation are detectable using REIMS. 478 samples of five different white fish species were subjected to REIMS analysis using an electrosurgical knife. Each sample was cut 8-12 times with each one lasting 3-5 s and chemometric models were generated based on the mass range m/z 600-950 of each sample. The identification of 99 validation samples provided a 98.99% correct classification in which species identification was obtained near-instantaneously (≈ 2 s) unlike any other form of food fraud analysis. Significant time comparisons between REIMS and polymerase chain reaction (PCR) were observed when analysing 6 mislabelled samples demonstrating how REIMS can be used as a complimentary technique to detect fish fraud. Additionally, we have demonstrated that the catch method of fish products is capable of detection using REIMS, a concept never previously reported. REIMS has been proven to be an innovative technique to help aid the detection of fish fraud and has the potential to be utilised by fisheries to conduct their own quality control (QC) checks for fast accurate results.

Coalescence computations for large samples drawn from populations of time-varying sizes

PubMed Central

Polanski, Andrzej; Szczesna, Agnieszka; Garbulowski, Mateusz; Kimmel, Marek

2017-01-01

We present new results concerning probability distributions of times in the coalescence tree and expected allele frequencies for coalescent with large sample size. The obtained results are based on computational methodologies, which involve combining coalescence time scale changes with techniques of integral transformations and using analytical formulae for infinite products. We show applications of the proposed methodologies for computing probability distributions of times in the coalescence tree and their limits, for evaluation of accuracy of approximate expressions for times in the coalescence tree and expected allele frequencies, and for analysis of large human mitochondrial DNA dataset. PMID:28170404

An enhanced droplet-based liquid microjunction surface sampling system coupled with HPLC-ESI-MS/MS for spatially resolved analysis

DOE PAGES

Van Berkel, Gary J.; Weiskittel, Taylor M.; Kertesz, Vilmos

2014-11-07

Droplet-based liquid microjunction surface sampling coupled with high-performance liquid chromatography (HPLC)-electrospray ionization (ESI)-tandem mass spectrometry (MS/MS) for spatially resolved analysis provides the possibility of effective analysis of complex matrix samples and can provide a greater degree of chemical information from a single spot sample than is typically possible with a direct analysis of an extract. Described here is the setup and enhanced capabilities of a discrete droplet liquid microjunction surface sampling system employing a commercially available CTC PAL autosampler. The system enhancements include incorporation of a laser distance sensor enabling unattended analysis of samples and sample locations of dramatically disparatemore » height as well as reliably dispensing just 0.5 μL of extraction solvent to make the liquid junction to the surface, wherein the extraction spot size was confined to an area about 0.7 mm in diameter; software modifications improving the spatial resolution of sampling spot selection from 1.0 to 0.1 mm; use of an open bed tray system to accommodate samples as large as whole-body rat thin tissue sections; and custom sample/solvent holders that shorten sampling time to approximately 1 min per sample. Lastly, the merit of these new features was demonstrated by spatially resolved sampling, HPLC separation, and mass spectral detection of pharmaceuticals and metabolites from whole-body rat thin tissue sections and razor blade (“crude”) cut mouse tissue.« less

An enhanced droplet-based liquid microjunction surface sampling system coupled with HPLC-ESI-MS/MS for spatially resolved analysis

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

Van Berkel, Gary J.; Weiskittel, Taylor M.; Kertesz, Vilmos

Droplet-based liquid microjunction surface sampling coupled with high-performance liquid chromatography (HPLC)-electrospray ionization (ESI)-tandem mass spectrometry (MS/MS) for spatially resolved analysis provides the possibility of effective analysis of complex matrix samples and can provide a greater degree of chemical information from a single spot sample than is typically possible with a direct analysis of an extract. Described here is the setup and enhanced capabilities of a discrete droplet liquid microjunction surface sampling system employing a commercially available CTC PAL autosampler. The system enhancements include incorporation of a laser distance sensor enabling unattended analysis of samples and sample locations of dramatically disparatemore » height as well as reliably dispensing just 0.5 μL of extraction solvent to make the liquid junction to the surface, wherein the extraction spot size was confined to an area about 0.7 mm in diameter; software modifications improving the spatial resolution of sampling spot selection from 1.0 to 0.1 mm; use of an open bed tray system to accommodate samples as large as whole-body rat thin tissue sections; and custom sample/solvent holders that shorten sampling time to approximately 1 min per sample. Lastly, the merit of these new features was demonstrated by spatially resolved sampling, HPLC separation, and mass spectral detection of pharmaceuticals and metabolites from whole-body rat thin tissue sections and razor blade (“crude”) cut mouse tissue.« less

Changes in dispositional empathy in American college students over time: a meta-analysis.

PubMed

Konrath, Sara H; O'Brien, Edward H; Hsing, Courtney

2011-05-01

The current study examines changes over time in a commonly used measure of dispositional empathy. A cross-temporal meta-analysis was conducted on 72 samples of American college students who completed at least one of the four subscales (Empathic Concern, Perspective Taking, Fantasy, and Personal Distress) of the Interpersonal Reactivity Index (IRI) between 1979 and 2009 (total N = 13,737). Overall, the authors found changes in the most prototypically empathic subscales of the IRI: Empathic Concern was most sharply dropping, followed by Perspective Taking. The IRI Fantasy and Personal Distress subscales exhibited no changes over time. Additional analyses found that the declines in Perspective Taking and Empathic Concern are relatively recent phenomena and are most pronounced in samples from after 2000.

Digital timing: sampling frequency, anti-aliasing filter and signal interpolation filter dependence on timing resolution.

PubMed

Cho, Sanghee; Grazioso, Ron; Zhang, Nan; Aykac, Mehmet; Schmand, Matthias

2011-12-07

The main focus of our study is to investigate how the performance of digital timing methods is affected by sampling rate, anti-aliasing and signal interpolation filters. We used the Nyquist sampling theorem to address some basic questions such as what will be the minimum sampling frequencies? How accurate will the signal interpolation be? How do we validate the timing measurements? The preferred sampling rate would be as low as possible, considering the high cost and power consumption of high-speed analog-to-digital converters. However, when the sampling rate is too low, due to the aliasing effect, some artifacts are produced in the timing resolution estimations; the shape of the timing profile is distorted and the FWHM values of the profile fluctuate as the source location changes. Anti-aliasing filters are required in this case to avoid the artifacts, but the timing is degraded as a result. When the sampling rate is marginally over the Nyquist rate, a proper signal interpolation is important. A sharp roll-off (higher order) filter is required to separate the baseband signal from its replicates to avoid the aliasing, but in return the computation will be higher. We demonstrated the analysis through a digital timing study using fast LSO scintillation crystals as used in time-of-flight PET scanners. From the study, we observed that there is no significant timing resolution degradation down to 1.3 Ghz sampling frequency, and the computation requirement for the signal interpolation is reasonably low. A so-called sliding test is proposed as a validation tool checking constant timing resolution behavior of a given timing pick-off method regardless of the source location change. Lastly, the performance comparison for several digital timing methods is also shown.

Mobile membrane introduction tandem mass spectrometry for on-the-fly measurements and adaptive sampling of VOCs around oil and gas projects in Alberta, Canada

NASA Astrophysics Data System (ADS)

Krogh, E.; Gill, C.; Bell, R.; Davey, N.; Martinsen, M.; Thompson, A.; Simpson, I. J.; Blake, D. R.

2012-12-01

The release of hydrocarbons into the environment can have significant environmental and economic consequences. The evolution of smaller, more portable mass spectrometers to the field can provide spatially and temporally resolved information for rapid detection, adaptive sampling and decision support. We have deployed a mobile platform membrane introduction mass spectrometer (MIMS) for the in-field simultaneous measurement of volatile and semi-volatile organic compounds. In this work, we report instrument and data handling advances that produce geographically referenced data in real-time and preliminary data where these improvements have been combined with high precision ultra-trace VOCs analysis to adaptively sample air plumes near oil and gas operations in Alberta, Canada. We have modified a commercially available ion-trap mass spectrometer (Griffin ICX 400) with an in-house temperature controlled capillary hollow fibre polydimethylsiloxane (PDMS) polymer membrane interface and in-line permeation tube flow cell for a continuously infused internal standard. The system is powered by 24 VDC for remote operations in a moving vehicle. Software modifications include the ability to run continuous, interlaced tandem mass spectrometry (MS/MS) experiments for multiple contaminants/internal standards. All data are time and location stamped with on-board GPS and meteorological data to facilitate spatial and temporal data mapping. Tandem MS/MS scans were employed to simultaneously monitor ten volatile and semi-volatile analytes, including benzene, toluene, ethylbenzene and xylene (BTEX), reduced sulfur compounds, halogenated organics and naphthalene. Quantification was achieved by calibrating against a continuously infused deuterated internal standard (toluene-d8). Time referenced MS/MS data were correlated with positional data and processed using Labview and Matlab to produce calibrated, geographical Google Earth data-visualizations that enable adaptive sampling protocols. This real-time approach has been employed in a moving vehicle to identify and track downwind plumes of fugitive VOC emissions near hydrocarbon upgrading and chemical processing facilities in Fort Saskatchewan, Alberta. This information was relayed to a trailing vehicle, which collected stationary grab samples in evacuated canisters for ultra trace analysis of over seventy VOC analytes. In addition, stationary time series data were collected and compared with grab samples co-located with our sampling line. Spatially and temporally resolved, time referenced MS/MS data for several air contaminants associated with oil and gas processing were processed in real time to produce geospatial data for visualization in Google Earth. This information was used to strategically locate grab samples for high precision, ultra trace analysis.

The active and passive sampling of benzene, toluene, ethyl benzene and xylenes compounds using the inside needle capillary adsorption trap device.

PubMed

Shojania, S; Oleschuk, R D; McComb, M E; Gesser, H D; Chow, A

1999-08-23

A new and simple method of solventless extraction of volatile organic compounds (VOCs) from air is presented. The sampling device has an adsorbing carbon coating on the interior surface of a hollow needle, and is called the inside needle capillary adsorption trap (INCAT). This paper describes a study of the reproducibility in the preparation and sampling of the INCAT device. In addition, this paper examines the effects of sample volume in active sampling and exposure time in passive sampling on the analyte adsorption. Analysis was achieved by sampling the air from an environmental chamber doped with benzene, toluene, ethyl benzene and xylenes (BTEX) compounds. Initial rates of adsorption were found to vary among the different compounds, but ranged from 0.0099 to 0.016 nmol h(-1) for passive sampling and from 2.2 to 10 nmol h(-1) for active sampling. Analysis was done by thermal desorption of the adsorbed compounds directly into a gas chromatograph injection port. Quantification of the analysis was done by comparison to actively sampled activated carbon solid phase extraction (SPE) measurements.

High-performance liquid chromatography with fluorescence detection for the rapid analysis of pheophytins and pyropheophytins in virgin olive oil.

PubMed

Li, Xueqi; Woodman, Michael; Wang, Selina C

2015-08-01

Pheophytins and pyropheophytin are degradation products of chlorophyll pigments, and their ratios can be used as a sensitive indicator of stress during the manufacturing and storage of olive oil. They increase over time depending on the storage condition and if the oil is exposed to heat treatments during the refining process. The traditional analysis method includes solvent- and time-consuming steps of solid-phase extraction followed by analysis by high-performance liquid chromatography with ultraviolet detection. We developed an improved dilute/fluorescence method where multi-step sample preparation was replaced by a simple isopropanol dilution before the high-performance liquid chromatography injection. A quaternary solvent gradient method was used to include a fourth strong solvent wash on a quaternary gradient pump, which avoided the need to premix any solvents and greatly reduced the oil residues on the column from previous analysis. This new method not only reduces analysis cost and time but shows reliability, repeatability, and improved sensitivity, especially important for low-level samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Dust Bowl in the American West: A geochemical record of dust provenance and deposition in the Upper Fremont Glacier ice core

NASA Astrophysics Data System (ADS)

Andrus, C. F. T.; Bassett, C.; Black, H. D.; Payne, T. N.

2016-12-01

Several recent studies demonstrate that nitrogen isotope analysis of the organic fraction of mollusk shells can serve as a proxy for anthropogenic environmental impacts, including sewage input into estuaries. Analysis of δ15N in shells from archaeological sites permits construction of time-series proxy data from the present day to pre-industrial times, yielding insight into the history of some human environmental influences such as waste input and land use changes. Most such studies utilize a single bulk analysis per valve, combining shell material grown over time periods of one or more years. However, large, fast-growing species (e.g. some scallops and abalone) may permit sub-annual sampling, potentially yielding insight into seasonal processes. Such sclerochronological sampling of archaeological shells may enable researchers to detect variation at a finer temporal scale than has been attempted to date, which in turn may facilitate analysis of seasonal resource procurement strategies and related actions. This presentation will incorporate new and published data from the Atlantic, Pacific and Gulf of Mexico coasts of North America to assess how sclerochronological δ15N data can be useful to better understand pre-industrial human-environmental interaction and change, and also address diagenesis and other preservational concerns commonly found in archaeological samples.

Nitrogen Isotope Analyses in Mollusk Shell: Applications to Environmental Sciences and Archaeology.

NASA Astrophysics Data System (ADS)

Andrus, C. F. T.; Bassett, C.; Black, H. D.; Payne, T. N.

2017-12-01

Several recent studies demonstrate that nitrogen isotope analysis of the organic fraction of mollusk shells can serve as a proxy for anthropogenic environmental impacts, including sewage input into estuaries. Analysis of δ15N in shells from archaeological sites permits construction of time-series proxy data from the present day to pre-industrial times, yielding insight into the history of some human environmental influences such as waste input and land use changes. Most such studies utilize a single bulk analysis per valve, combining shell material grown over time periods of one or more years. However, large, fast-growing species (e.g. some scallops and abalone) may permit sub-annual sampling, potentially yielding insight into seasonal processes. Such sclerochronological sampling of archaeological shells may enable researchers to detect variation at a finer temporal scale than has been attempted to date, which in turn may facilitate analysis of seasonal resource procurement strategies and related actions. This presentation will incorporate new and published data from the Atlantic, Pacific and Gulf of Mexico coasts of North America to assess how sclerochronological δ15N data can be useful to better understand pre-industrial human-environmental interaction and change, and also address diagenesis and other preservational concerns commonly found in archaeological samples.

The stability of hydrogen ion and specific conductance in filtered wet-deposition samples stored at ambient temperatures

USGS Publications Warehouse

Gordon, J.D.; Schroder, L.J.; Morden-Moore, A. L.; Bowersox, V.C.

1995-01-01

Separate experiments by the U.S. Geological Survey (USGS) and the Illinois State Water Survey Central Analytical Laboratory (CAL) independently assessed the stability of hydrogen ion and specific conductance in filtered wet-deposition samples stored at ambient temperatures. The USGS experiment represented a test of sample stability under a diverse range of conditions, whereas the CAL experiment was a controlled test of sample stability. In the experiment by the USGS, a statistically significant (?? = 0.05) relation between [H+] and time was found for the composited filtered, natural, wet-deposition solution when all reported values are included in the analysis. However, if two outlying pH values most likely representing measurement error are excluded from the analysis, the change in [H+] over time was not statistically significant. In the experiment by the CAL, randomly selected samples were reanalyzed between July 1984 and February 1991. The original analysis and reanalysis pairs revealed that [H+] differences, although very small, were statistically different from zero, whereas specific-conductance differences were not. Nevertheless, the results of the CAL reanalysis project indicate there appears to be no consistent, chemically significant degradation in sample integrity with regard to [H+] and specific conductance while samples are stored at room temperature at the CAL. Based on the results of the CAL and USGS studies, short-term (45-60 day) stability of [H+] and specific conductance in natural filtered wet-deposition samples that are shipped and stored unchilled at ambient temperatures was satisfactory.

Modifications of the 1H NMR metabolite profile of processed mullet (Mugil cephalus) roes under different storage conditions.

PubMed

Scano, Paola; Rosa, Antonella; Locci, Emanuela; Manzo, Giorgia; Dessì, M Assunta

2012-06-01

(1)H NMR spectroscopy was employed to study the modifications over time of the water-soluble low molecular weight metabolites extracted from samples of salted and dried mullet (Mugil cephalus) roes (mullet bottarga) stored at different conditions. Samples of grated mullet bottarga were stored for 7 months at -20 °C, at 3 °C, and at room temperature in the presence and in the absence of light and then timely extracted and analyzed by NMR. Principal component multivariate data analysis applied to the spectral data indicated that samples stored at -20 °C maintained similar features over time whereas, along PC1, samples stored at room temperature in the presence and in the absence of light showed, over time, marked metabolite modifications. The comparative analysis of the integrated areas of the selected regions of the (1)H NMR spectra indicated that the major compositional changes due to storage conditions were (i) the increase of the derivatives of the breakdown of phosphatidylcholine (choline, phosphorylcholine, and glycerol), (ii) the breakdown of nucleosides, (iii) the decrease of methionine, tryptophan, and tyrosine, and (iv) the cyclization of creatine. These changes were observed at different storage conditions, with more pronounced trends in the samples stored at room temperature. The role of metabolites in food aging is discussed. Copyright © 2012 John Wiley & Sons, Ltd.

Portable Dew Point Mass Spectrometry System for Real-Time Gas and Moisture Analysis

NASA Technical Reports Server (NTRS)

Arkin, C.; Gillespie, Stacey; Ratzel, Christopher

2010-01-01

A portable instrument incorporates both mass spectrometry and dew point measurement to provide real-time, quantitative gas measurements of helium, nitrogen, oxygen, argon, and carbon dioxide, along with real-time, quantitative moisture analysis. The Portable Dew Point Mass Spectrometry (PDP-MS) system comprises a single quadrupole mass spectrometer and a high vacuum system consisting of a turbopump and a diaphragm-backing pump. A capacitive membrane dew point sensor was placed upstream of the MS, but still within the pressure-flow control pneumatic region. Pressure-flow control was achieved with an upstream precision metering valve, a capacitance diaphragm gauge, and a downstream mass flow controller. User configurable LabVIEW software was developed to provide real-time concentration data for the MS, dew point monitor, and sample delivery system pressure control, pressure and flow monitoring, and recording. The system has been designed to include in situ, NIST-traceable calibration. Certain sample tubing retains sufficient water that even if the sample is dry, the sample tube will desorb water to an amount resulting in moisture concentration errors up to 500 ppm for as long as 10 minutes. It was determined that Bev-A-Line IV was the best sample line to use. As a result of this issue, it is prudent to add a high-level humidity sensor to PDP-MS so such events can be prevented in the future.

Analysis of the Precursors, Simulants and Degradation Products of Chemical Warfare Agents.

PubMed

Witkiewicz, Zygfryd; Neffe, Slawomir; Sliwka, Ewa; Quagliano, Javier

2018-09-03

Recent advances in analysis of precursors, simulants and degradation products of chemical warfare agents (CWA) are reviewed. Fast and reliable analysis of precursors, simulants and CWA degradation products is extremely important at a time, when more and more terrorist groups and radical non-state organizations use or plan to use chemical weapons to achieve their own psychological, political and military goals. The review covers the open source literature analysis after the time, when the chemical weapons convention had come into force (1997). The authors stated that during last 15 years increased number of laboratories are focused not only on trace analysis of CWA (mostly nerve and blister agents) in environmental and biological samples, but the growing number of research are devoted to instrumental analysis of precursors and degradation products of these substances. The identification of low-level concentration of CWA degradation products is often more important and difficult than the original CWA, because of lower level of concentration and a very large number of compounds present in environmental and biological samples. Many of them are hydrolysis products and are present in samples in the ionic form. For this reason, two or three instrumental methods are used to perform a reliable analysis of these substances.

Temporal Noise Analysis of Charge-Domain Sampling Readout Circuits for CMOS Image Sensors.

PubMed

Ge, Xiaoliang; Theuwissen, Albert J P

2018-02-27

This paper presents a temporal noise analysis of charge-domain sampling readout circuits for Complementary Metal-Oxide Semiconductor (CMOS) image sensors. In order to address the trade-off between the low input-referred noise and high dynamic range, a Gm-cell-based pixel together with a charge-domain correlated-double sampling (CDS) technique has been proposed to provide a way to efficiently embed a tunable conversion gain along the read-out path. Such readout topology, however, operates in a non-stationery large-signal behavior, and the statistical properties of its temporal noise are a function of time. Conventional noise analysis methods for CMOS image sensors are based on steady-state signal models, and therefore cannot be readily applied for Gm-cell-based pixels. In this paper, we develop analysis models for both thermal noise and flicker noise in Gm-cell-based pixels by employing the time-domain linear analysis approach and the non-stationary noise analysis theory, which help to quantitatively evaluate the temporal noise characteristic of Gm-cell-based pixels. Both models were numerically computed in MATLAB using design parameters of a prototype chip, and compared with both simulation and experimental results. The good agreement between the theoretical and measurement results verifies the effectiveness of the proposed noise analysis models.

Temporal Noise Analysis of Charge-Domain Sampling Readout Circuits for CMOS Image Sensors †

PubMed Central

Theuwissen, Albert J. P.

2018-01-01

This paper presents a temporal noise analysis of charge-domain sampling readout circuits for Complementary Metal-Oxide Semiconductor (CMOS) image sensors. In order to address the trade-off between the low input-referred noise and high dynamic range, a Gm-cell-based pixel together with a charge-domain correlated-double sampling (CDS) technique has been proposed to provide a way to efficiently embed a tunable conversion gain along the read-out path. Such readout topology, however, operates in a non-stationery large-signal behavior, and the statistical properties of its temporal noise are a function of time. Conventional noise analysis methods for CMOS image sensors are based on steady-state signal models, and therefore cannot be readily applied for Gm-cell-based pixels. In this paper, we develop analysis models for both thermal noise and flicker noise in Gm-cell-based pixels by employing the time-domain linear analysis approach and the non-stationary noise analysis theory, which help to quantitatively evaluate the temporal noise characteristic of Gm-cell-based pixels. Both models were numerically computed in MATLAB using design parameters of a prototype chip, and compared with both simulation and experimental results. The good agreement between the theoretical and measurement results verifies the effectiveness of the proposed noise analysis models. PMID:29495496

Assessment of sampling stability in ecological applications of discriminant analysis

USGS Publications Warehouse

Williams, B.K.; Titus, K.

1988-01-01

A simulation study was undertaken to assess the sampling stability of the variable loadings in linear discriminant function analysis. A factorial design was used for the factors of multivariate dimensionality, dispersion structure, configuration of group means, and sample size. A total of 32,400 discriminant analyses were conducted, based on data from simulated populations with appropriate underlying statistical distributions. A review of 60 published studies and 142 individual analyses indicated that sample sizes in ecological studies often have met that requirement. However, individual group sample sizes frequently were very unequal, and checks of assumptions usually were not reported. The authors recommend that ecologists obtain group sample sizes that are at least three times as large as the number of variables measured.

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Sandstrom, Mark W.; Stroppel, Max E.; Foreman, William T.; Schroeder, Michael P.

2001-01-01

A method for the isolation and analysis of 21 parent pesticides and 20 pesticide degradates in natural-water samples is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase-extraction columns that contain octadecyl-bonded porous silica to extract the analytes. The columns are dried by using nitrogen gas, and adsorbed analytes are eluted with ethyl acetate. Extracted analytes are determined by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 2 micrograms per liter (?g/L) for most analytes. Single-operator method detection limits in reagent-water samples range from 0.00 1 to 0.057 ?g/L. Validation data also are presented for 14 parent pesticides and 20 degradates that were determined to have greater bias or variability, or shorter holding times than the other compounds. The estimated maximum holding time for analytes in pesticide-grade water before extraction was 4 days. The estimated maximum holding time for analytes after extraction on the dry solid-phase-extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time. The method complements existing U.S. Geological Survey Method O-1126-95 (NWQL Schedules 2001 and 2010) by using identical sample preparation and comparable instrument analytical conditions so that sample extracts can be analyzed by either method to expand the range of analytes determined from one water sample.

Effect of delayed serum separation and storage temperature on serum glucose concentration in horse, dog, alpaca, and sturgeon.

PubMed

Collicutt, Nancy B; Garner, Bridget; Berghaus, Roy D; Camus, Melinda S; Hart, Kelsey

2015-03-01

Although delays between blood sample collection and analysis are common in veterinary medicine, the effect of prolonged serum-clot contact time on serum glucose concentration is not well established and species differences have not been elucidated. The objective was to investigate the effect of storage time and temperature on serum glucose concentration in stored whole blood samples from horse, dog, alpaca, and sturgeon. Whole blood specimens were divided into 7 no-additive tubes and serum was separated from one sample within one hour, serving as the reference sample. The remaining samples were stored at 4°C and 25°C, then centrifuged and serum glucose measured by automated analysis at 2, 4, and 8 hours postcollection. Glucose concentrations were compared using linear mixed models. The decline in serum glucose concentration for all samples stored at 4°C was not statistically significant, except for the 8-hour samples from sturgeon and dog. At 25°C, serum glucose concentration was comparable to reference values at 2 hours in sturgeon and alpaca, but significantly lower at 4 and 8 hours in those species, and at all time points in equine and canine specimens, being most prominent after 8 hours of storage in canine specimens. Storage at 4°C limits serum glucose decline for at least 4 hours in all species tested and up to 8 hours in specimens of horse and alpaca. At 25°C, serum-clot contact time should not exceed 1 hour in equine and canine samples, and 2 hours in specimens from alpaca and sturgeon. © 2014 American Society for Veterinary Clinical Pathology.

Rapid quality assessment of Radix Aconiti Preparata using direct analysis in real time mass spectrometry.

PubMed

Zhu, Hongbin; Wang, Chunyan; Qi, Yao; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

2012-11-08

This study presents a novel and rapid method to identify chemical markers for the quality control of Radix Aconiti Preparata, a world widely used traditional herbal medicine. In the method, the samples with a fast extraction procedure were analyzed using direct analysis in real time mass spectrometry (DART MS) combined with multivariate data analysis. At present, the quality assessment approach of Radix Aconiti Preparata was based on the two processing methods recorded in Chinese Pharmacopoeia for the purpose of reducing the toxicity of Radix Aconiti and ensuring its clinical therapeutic efficacy. In order to ensure the safety and effectivity in clinical use, the processing degree of Radix Aconiti should be well controlled and assessed. In the paper, hierarchical cluster analysis and principal component analysis were performed to evaluate the DART MS data of Radix Aconiti Preparata samples in different processing times. The results showed that the well processed Radix Aconiti Preparata, unqualified processed and the raw Radix Aconiti could be clustered reasonably corresponding to their constituents. The loading plot shows that the main chemical markers having the most influence on the discrimination amongst the qualified and unqualified samples were mainly some monoester diterpenoid aconitines and diester diterpenoid aconitines, i.e. benzoylmesaconine, hypaconitine, mesaconitine, neoline, benzoylhypaconine, benzoylaconine, fuziline, aconitine and 10-OH-mesaconitine. The established DART MS approach in combination with multivariate data analysis provides a very flexible and reliable method for quality assessment of toxic herbal medicine. Copyright © 2012 Elsevier B.V. All rights reserved.

SOLVENT HOLD TANK SAMPLE RESULTS FOR MCU-14-259/260/261 AND MCU-14-315/316/317: APRIL AND MAY 2014 MONTHLY SAMPLES

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

Fondeur, F.; Taylor-Pashow, K.

2014-08-05

SRNL received two sets of SHT samples (MCU-14-259/260/261 in April 2014 and MCU-14- 315/316/317 in May 2014) for analysis. The samples were analyzed for composition. Both samples have similar chemical composition. As with the previous solvent sample results, these analyses indicate that the solvent does not require Isopar® L trimming at this time. Since an addition of TiDG and MaxCalix to the SHT was added in early July 2014, the solvent does not require TiDG addition at this time. The current TiDG level (1.5 mM) is above the minimum recommended operating level of 1 mM.

Transactional Patterns of Maternal Depressive Symptoms and Mother-Child Mutual Negativity in an Adoption Sample

ERIC Educational Resources Information Center

Roben, Caroline K. P.; Moore, Ginger A.; Cole, Pamela M.; Molenaar, Peter; Leve, Leslie D.; Shaw, Daniel S.; Reiss, David; Neiderhiser, Jenae M.

2015-01-01

Transactional models of analysis can examine both moment-to-moment interactions within a dyad and dyadic patterns of influence across time. This study used data from a prospective adoption study to test a transactional model of parental depressive symptoms and mutual negativity between mother and child over time, utilizing contingency analysis of…

Application of real-time PCR and melting curve analysis in rapid Diego blood group genotyping.

PubMed

Novaretti, M C Z; Ruiz, A S; Dorlhiac-Llacer, P E; Chamone, D A F

2010-01-01

The paucity of appropriate reagents for serologic typing of the Diego blood group antigens has prompted the development of a real-time PCR and melting curve analysis for Diego blood group genotyping. In this study, we phenotyped 4326 donor blood samples for Di(a) using semiautomated equipment. All 157 Di(a+) samples were then genotyped by PCR using sequence-specific primers (PCR-SSP) for DI*02 because of anti-Di(b) scarcity. Of the 4326 samples, we simultaneously tested 160 samples for Di(a) and Di(b) serology, and DI*01 and DI*02 by PCR-SSP and by real-time PCR. We used the same primers for Diego genotyping by real-time PCR and PCR-SSP. Melting curve profiles obtained using the dissociation software of the real-time PCR apparatus enabled the discrimination of Diego alleles. Of the total samples tested, 4169 blood donors, 96.4 percent (95% confidence interval [CI], 95.8-96.9%), were homozygous for DI*02 and 157, 3.6 percent (95% CI, 3.1%-4.2%), were heterozygous DI*01/02. No blood donor was found to be homozygous for DI*01 in this study. The calculated DI*01 and DI*02 allele frequencies were 0.0181 (95% CI, 0.0173-0.0189) and 0.9819 (95% CI, 0.9791-0.9847), respectively, showing a good fit for the Hardy-Weinberg equilibrium. There was full concordance among Diego phenotype results by PCR-SSP and real-time PCR. DI*01 and DI*02 allele determination with SYBR Green I and thermal cycler technology are useful methods for Diego determination. The real-time PCR with SYBR Green I melting temperature protocol can be used as a rapid screening tool for DI*01 and DI*02 blood group genotyping.

Tannin analysis of chestnut bark samples (Castanea sativa Mill.) by HPLC-DAD-MS.

PubMed

Comandini, Patrizia; Lerma-García, María Jesús; Simó-Alfonso, Ernesto Francisco; Toschi, Tullia Gallina

2014-08-15

In the present investigation, an HPLC-DAD/ESI-MS method for the complete analysis of tannins and other phenolic compounds of different commercial chestnut bark samples was developed. A total of seven compounds (vescalin, castalin, gallic acid, vescalagin, 1-O-galloyl castalagin, castalagin and ellagic acid) were separated and quantified, being 1-O-galloyl castalagin tentatively identified and found for the first time in chestnut bark samples. Thus, this method provided information regarding the composition and quality of chestnut bark samples, which is required since these samples are commercialised due to their biochemical properties as ingredients of food supplements. Copyright © 2014 Elsevier Ltd. All rights reserved.

Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

PubMed

Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

2002-07-19

This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

Improved sample preparation of glyphosate and methylphosphonic acid by EPA method 6800A and time-of-flight mass spectrometry using novel solid-phase extraction.

PubMed

Wagner, Rebecca; Wetzel, Stephanie J; Kern, John; Kingston, H M Skip

2012-02-01

The employment of chemical weapons by rogue states and/or terrorist organizations is an ongoing concern in the United States. The quantitative analysis of nerve agents must be rapid and reliable for use in the private and public sectors. Current methods describe a tedious and time-consuming derivatization for gas chromatography-mass spectrometry and liquid chromatography in tandem with mass spectrometry. Two solid-phase extraction (SPE) techniques for the analysis of glyphosate and methylphosphonic acid are described with the utilization of isotopically enriched analytes for quantitation via atmospheric pressure chemical ionization-quadrupole time-of-flight mass spectrometry (APCI-Q-TOF-MS) that does not require derivatization. Solid-phase extraction-isotope dilution mass spectrometry (SPE-IDMS) involves pre-equilibration of a naturally occurring sample with an isotopically enriched standard. The second extraction method, i-Spike, involves loading an isotopically enriched standard onto the SPE column before the naturally occurring sample. The sample and the spike are then co-eluted from the column enabling precise and accurate quantitation via IDMS. The SPE methods in conjunction with IDMS eliminate concerns of incomplete elution, matrix and sorbent effects, and MS drift. For accurate quantitation with IDMS, the isotopic contribution of all atoms in the target molecule must be statistically taken into account. This paper describes two newly developed sample preparation techniques for the analysis of nerve agent surrogates in drinking water as well as statistical probability analysis for proper molecular IDMS. The methods described in this paper demonstrate accurate molecular IDMS using APCI-Q-TOF-MS with limits of quantitation as low as 0.400 mg/kg for glyphosate and 0.031 mg/kg for methylphosphonic acid. Copyright © 2012 John Wiley & Sons, Ltd.

A dryer for rapid response on-line expired gas measurements.

PubMed

Deno, N S; Kamon, E

1979-06-01

A dryer is described for use in on-line breath-by-breath gas analysis systems. The dryer continuously removes water vapor by condensation and controls the sample gas at 2 degrees C dew-point temperature or 5 Torr water vapor partial pressure. It is designed to operate at gas sampling flow rates from 0.5 to 1 1.min-1. The step-response time for the described system including a Beckman LB-2 CO2 analyzer, sampling tubing, and dryer is 120 ms at 1 l.min-1. The time required for gas samples to transport through the dryer is 105 ms at a gas sampling-flow rate of 1 l.min=1.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR COLLECTION OF PERSONAL AIR SAMPLES FOR ANALYSIS OF PESTICIDES OR METALS (UA-F-14.0)

EPA Science Inventory

The purpose of this SOP is to describe the procedure for sampling personal air for metals and pesticides during a predetermined time period. The SOP includes the set up of the samplers for collection of either a metals sample or a pesticides sample, the calibration and initial c...

Collection methods and quality assessment for Esche-richia coli, water quality, and microbial source tracking data within Tumacácori National Historical Park and the upper Santa Cruz River, Arizona, 2015-16

USGS Publications Warehouse

Paretti, Nicholas; Coes, Alissa L.; Kephart, Christopher M.; Mayo, Justine

2018-03-05

Tumacácori National Historical Park protects the culturally important Mission, San José de Tumacácori, while also managing a portion of the ecologically diverse riparian corridor of the Santa Cruz River. This report describes the methods and quality assurance procedures used in the collection of water samples for the analysis of Escherichia coli (E. coli), microbial source tracking markers, suspended sediment, water-quality parameters, turbidity, and the data collection for discharge and stage; the process for data review and approval is also described. Finally, this report provides a quantitative assessment of the quality of the E. coli, microbial source tracking, and suspended sediment data.The data-quality assessment revealed that bias attributed to field and laboratory contamination was minimal, with E. coli detections in only 3 out of 33 field blank samples analyzed. Concentrations in the field blanks were several orders of magnitude lower than environmental concentrations. The microbial source tracking (MST) field blank was below the detection limit for all MST markers analyzed. Laboratory blanks for E. coli at the USGS Arizona Water Science Center and laboratory blanks for MST markers at the USGS Ohio Water Microbiology Laboratory were all below the detection limit. Irreplicate data for E. coli and suspended sediment indicated that bias was not introduced to the data by combining samples collected using discrete sampling methods with samples collected using automatic sampling methods.The split and sequential E. coli replicate data showed consistent analytical variability and a single equation was developed to explain the variability of E. coli concentrations. An additional analysis of analytical variability for E. coli indicated analytical variability around 18 percent relative standard deviation and no trend was observed in the concentration during the processing and analysis of multiple split-replicates. Two replicate samples were collected for MST and individual markers were compared for a base flow and flood sample. For the markers found in common between the two types of samples, the relative standard deviation for the base flow sample was more than 3 times greater than the markers in the flood sample. Sequential suspended sediment replicates had a relative standard deviation of about 1.3 percent, indicating that environmental and analytical variability was minimal.A holding time review and laboratory study analysis supported the extended holding times required for this investigation. Most concentrations for flood and base-flow samples were within the theoretical variability specified in the most probable number approach suggesting that extended hold times did not overly influence the final concentrations reported.

DEVELOPMENT AND PEER REVIEW OF TIME-TO-EFFECT MODELS FOR THE ANALYSIS OF NEUROTOXICITY AND OTHER TIME DEPENDENT DATA

EPA Science Inventory

Neurobehavioral studies pose unique challenges for dose-response modeling, including small sample size and relatively large intra-subject variation, repeated measurements over time, multiple endpoints with both continuous and ordinal scales, and time dependence of risk characteri...

Sub-microsecond-resolution probe microscopy

DOEpatents

Ginger, David; Giridharagopal, Rajiv; Moore, David; Rayermann, Glennis; Reid, Obadiah

2014-04-01

Methods and apparatus are provided herein for time-resolved analysis of the effect of a perturbation (e.g., a light or voltage pulse) on a sample. By operating in the time domain, the provided method enables sub-microsecond time-resolved measurement of transient, or time-varying, forces acting on a cantilever.

The Australian longitudinal study on male health sampling design and survey weighting: implications for analysis and interpretation of clustered data.

PubMed

Spittal, Matthew J; Carlin, John B; Currier, Dianne; Downes, Marnie; English, Dallas R; Gordon, Ian; Pirkis, Jane; Gurrin, Lyle

2016-10-31

The Australian Longitudinal Study on Male Health (Ten to Men) used a complex sampling scheme to identify potential participants for the baseline survey. This raises important questions about when and how to adjust for the sampling design when analyzing data from the baseline survey. We describe the sampling scheme used in Ten to Men focusing on four important elements: stratification, multi-stage sampling, clustering and sample weights. We discuss how these elements fit together when using baseline data to estimate a population parameter (e.g., population mean or prevalence) or to estimate the association between an exposure and an outcome (e.g., an odds ratio). We illustrate this with examples using a continuous outcome (weight in kilograms) and a binary outcome (smoking status). Estimates of a population mean or disease prevalence using Ten to Men baseline data are influenced by the extent to which the sampling design is addressed in an analysis. Estimates of mean weight and smoking prevalence are larger in unweighted analyses than weighted analyses (e.g., mean = 83.9 kg vs. 81.4 kg; prevalence = 18.0 % vs. 16.7 %, for unweighted and weighted analyses respectively) and the standard error of the mean is 1.03 times larger in an analysis that acknowledges the hierarchical (clustered) structure of the data compared with one that does not. For smoking prevalence, the corresponding standard error is 1.07 times larger. Measures of association (mean group differences, odds ratios) are generally similar in unweighted or weighted analyses and whether or not adjustment is made for clustering. The extent to which the Ten to Men sampling design is accounted for in any analysis of the baseline data will depend on the research question. When the goals of the analysis are to estimate the prevalence of a disease or risk factor in the population or the magnitude of a population-level exposure-outcome association, our advice is to adopt an analysis that respects the sampling design.

Literature Reference for Cryptosporidium spp. (Applied and Environmental Microbiology. 2007. 73(13): 4218–4225)

EPA Pesticide Factsheets

Procedures are described for analysis of drinking water samples and may be adapted for assessment of solid, particulate, aerosol, and liquid samples. The method uses real-time PCR for identification of Cryptosporidium spp.

X-Ray Imaging Applied to Problems in Planetary Materials

NASA Technical Reports Server (NTRS)

Jurewicz, A. J. G.; Mih, D. T.; Jones, S. M.; Connolly, H.

2000-01-01

Real-time radiography (X-ray imaging) can be a useful tool for tasks such as (1) the non-destructive, preliminary examination of opaque samples and (2) optimizing how to section opaque samples for more traditional microscopy and chemical analysis.

Attosecond transient absorption instrumentation for thin film materials: Phase transitions, heat dissipation, signal stabilization, timing correction, and rapid sample rotation.

PubMed

Jager, Marieke F; Ott, Christian; Kaplan, Christopher J; Kraus, Peter M; Neumark, Daniel M; Leone, Stephen R

2018-01-01

We present an extreme ultraviolet (XUV) transient absorption apparatus tailored to attosecond and femtosecond measurements on bulk solid-state thin-film samples, specifically when the sample dynamics are sensitive to heating effects. The setup combines methodology for stabilizing sub-femtosecond time-resolution measurements over 48 h and techniques for mitigating heat buildup in temperature-dependent samples. Single-point beam stabilization in pump and probe arms and periodic time-zero reference measurements are described for accurate timing and stabilization. A hollow-shaft motor configuration for rapid sample rotation, raster scanning capability, and additional diagnostics are described for heat mitigation. Heat transfer simulations performed using a finite element analysis allow comparison of sample rotation and traditional raster scanning techniques for 100 Hz pulsed laser measurements on vanadium dioxide, a material that undergoes an insulator-to-metal transition at a modest temperature of 340 K. Experimental results are presented confirming that the vanadium dioxide (VO 2 ) sample cannot cool below its phase transition temperature between laser pulses without rapid rotation, in agreement with the simulations. The findings indicate the stringent conditions required to perform rigorous broadband XUV time-resolved absorption measurements on bulk solid-state samples, particularly those with temperature sensitivity, and elucidate a clear methodology to perform them.

Attosecond transient absorption instrumentation for thin film materials: Phase transitions, heat dissipation, signal stabilization, timing correction, and rapid sample rotation

NASA Astrophysics Data System (ADS)

Jager, Marieke F.; Ott, Christian; Kaplan, Christopher J.; Kraus, Peter M.; Neumark, Daniel M.; Leone, Stephen R.

2018-01-01

We present an extreme ultraviolet (XUV) transient absorption apparatus tailored to attosecond and femtosecond measurements on bulk solid-state thin-film samples, specifically when the sample dynamics are sensitive to heating effects. The setup combines methodology for stabilizing sub-femtosecond time-resolution measurements over 48 h and techniques for mitigating heat buildup in temperature-dependent samples. Single-point beam stabilization in pump and probe arms and periodic time-zero reference measurements are described for accurate timing and stabilization. A hollow-shaft motor configuration for rapid sample rotation, raster scanning capability, and additional diagnostics are described for heat mitigation. Heat transfer simulations performed using a finite element analysis allow comparison of sample rotation and traditional raster scanning techniques for 100 Hz pulsed laser measurements on vanadium dioxide, a material that undergoes an insulator-to-metal transition at a modest temperature of 340 K. Experimental results are presented confirming that the vanadium dioxide (VO2) sample cannot cool below its phase transition temperature between laser pulses without rapid rotation, in agreement with the simulations. The findings indicate the stringent conditions required to perform rigorous broadband XUV time-resolved absorption measurements on bulk solid-state samples, particularly those with temperature sensitivity, and elucidate a clear methodology to perform them.

Introduction and application of the multiscale coefficient of variation analysis.

PubMed

Abney, Drew H; Kello, Christopher T; Balasubramaniam, Ramesh

2017-10-01

Quantifying how patterns of behavior relate across multiple levels of measurement typically requires long time series for reliable parameter estimation. We describe a novel analysis that estimates patterns of variability across multiple scales of analysis suitable for time series of short duration. The multiscale coefficient of variation (MSCV) measures the distance between local coefficient of variation estimates within particular time windows and the overall coefficient of variation across all time samples. We first describe the MSCV analysis and provide an example analytical protocol with corresponding MATLAB implementation and code. Next, we present a simulation study testing the new analysis using time series generated by ARFIMA models that span white noise, short-term and long-term correlations. The MSCV analysis was observed to be sensitive to specific parameters of ARFIMA models varying in the type of temporal structure and time series length. We then apply the MSCV analysis to short time series of speech phrases and musical themes to show commonalities in multiscale structure. The simulation and application studies provide evidence that the MSCV analysis can discriminate between time series varying in multiscale structure and length.

Statistical analysis of environmental monitoring data: does a worst case time for monitoring clean rooms exist?

PubMed

Cundell, A M; Bean, R; Massimore, L; Maier, C

1998-01-01

To determine the relationship between the sampling time of the environmental monitoring, i.e., viable counts, in aseptic filling areas and the microbial count and frequency of alerts for air, surface and personnel microbial monitoring, statistical analyses were conducted on 1) the frequency of alerts versus the time of day for routine environmental sampling conducted in calendar year 1994, and 2) environmental monitoring data collected at 30-minute intervals during routine aseptic filling operations over two separate days in four different clean rooms with multiple shifts and equipment set-ups at a parenteral manufacturing facility. Statistical analyses showed, except for one floor location that had significantly higher number of counts but no alert or action level samplings in the first two hours of operation, there was no relationship between the number of counts and the time of sampling. Further studies over a 30-day period at the floor location showed no relationship between time of sampling and microbial counts. The conclusion reached in the study was that there is no worst case time for environmental monitoring at that facility and that sampling any time during the aseptic filling operation will give a satisfactory measure of the microbial cleanliness in the clean room during the set-up and aseptic filling operation.

Note: Four-port microfluidic flow-cell with instant sample switching

NASA Astrophysics Data System (ADS)

MacGriff, Christopher A.; Wang, Shaopeng; Tao, Nongjian

2013-10-01

A simple device for high-speed microfluidic delivery of liquid samples to a surface plasmon resonance sensor surface is presented. The delivery platform is comprised of a four-port microfluidic cell, two ports serve as inlets for buffer and sample solutions, respectively, and a high-speed selector valve to control the alternate opening and closing of the two outlet ports. The time scale of buffer/sample switching (or sample injection rise and fall time) is on the order of milliseconds, thereby minimizing the opportunity for sample plug dispersion. The high rates of mass transport to and from the central microfluidic sensing region allow for SPR-based kinetic analysis of binding events with dissociation rate constants (kd) up to 130 s-1. The required sample volume is only 1 μL, allowing for minimal sample consumption during high-speed kinetic binding measurement.

Petroleomics by Direct Analysis in Real Time-Mass Spectrometry.

PubMed

Romão, Wanderson; Tose, Lilian V; Vaz, Boniek G; Sama, Sara G; Lobinski, Ryszard; Giusti, Pierre; Carrier, Hervé; Bouyssiere, Brice

2016-01-01

The analysis of crude oil and its fractions by applying ambient ionization techniques remains underexplored in mass spectrometry (MS). Direct analysis in real time (DART) in the positive-ion mode was coupled to a linear quadrupole ion trap Orbitrap mass spectrometer (LTQ Orbitrap) to analyze crude oil, paraffin samples, and porphyrin standard compounds. The ionization parameters of DART-MS were optimized for crude oil analysis. DART-MS rendered the optimum conditions of the operation using paper as the substrate, T = 400°C, helium as the carrier gas, and a sample concentration ≥6 mg mL(-1). In the crude oils analysis, the DART(+)-Orbitrap mass spectra detected the typical N, NO, and O-containing compounds. In the paraffin samples, oxidized hydrocarbon species (Ox classes, where x = 1-4) with double-bond equivalent of 1-4 were detected, and their structures and connectivity were confirmed by collision-induced dissociation (CID) experiments. DART(+)-MS has identified the porphyrin standard compounds as [M + H](+) ions of m/z 615.2502 and 680.1763, where M = C44H30N4 and C44H28N4OV, respectively, based on the formula assignment and by phenyl losses observed on CID experiments.

Total coliform and Escherichia coli contamination in rural well water: analysis for passive surveillance.

PubMed

Invik, Jesse; Barkema, Herman W; Massolo, Alessandro; Neumann, Norman F; Checkley, Sylvia

2017-10-01

With increasing stress on our water resources and recent waterborne disease outbreaks, understanding the epidemiology of waterborne pathogens is crucial to build surveillance systems. The purpose of this study was to explore techniques for describing microbial water quality in rural drinking water wells, based on spatiotemporal analysis, time series analysis and relative risk mapping. Tests results for Escherichia coli and coliforms from private and small public well water samples, collected between 2004 and 2012 in Alberta, Canada, were used for the analysis. Overall, 14.6 and 1.5% of the wells were total coliform and E. coli-positive, respectively. Private well samples were more often total coliform or E. coli-positive compared with untreated public well samples. Using relative risk mapping we were able to identify areas of higher risk for bacterial contamination of groundwater in the province not previously identified. Incorporation of time series analysis demonstrated peak contamination occurring for E. coli in July and a later peak for total coliforms in September, suggesting a temporal dissociation between these indicators in terms of groundwater quality, and highlighting the potential need to increase monitoring during certain periods of the year.

Root cause analysis of laboratory turnaround times for patients in the emergency department.

PubMed

Fernandes, Christopher M B; Worster, Andrew; Hill, Stephen; McCallum, Catherine; Eva, Kevin

2004-03-01

Laboratory investigations are essential to patient care and are conducted routinely in emergency departments (EDs). This study reports the turnaround times at an academic, tertiary care ED, using root cause analysis to identify potential areas of improvement. Our objectives were to compare the laboratory turnaround times with established benchmarks and identify root causes for delays. Turnaround and process event times for a consecutive sample of hemoglobin and potassium measurements were recorded during an 8-day study period using synchronized time stamps. A log transformation (ln [minutes + 1]) was performed to normalize the time data, which were then compared with established benchmarks using one-sample t tests. The turnaround time for hemoglobin was significantly less than the established benchmark (n = 140, t = -5.69, p < 0.001) and that of potassium was significantly greater (n = 121, t = 12.65, p < 0.001). The hemolysis rate was 5.8%, with 0.017% of samples needing recollection. Causes of delays included order-processing time, a high proportion (43%) of tests performed on patients who had been admitted but were still in the ED waiting for a bed, and excessive laboratory process times for potassium. The turnaround time for hemoglobin (18 min) met the established benchmark, but that for potassium (49 min) did not. Root causes for delay were order-processing time, excessive queue and instrument times for potassium and volume of tests for admitted patients. Further study of these identified causes of delays is required to see whether laboratory TATs can be reduced.

Chemometric and multivariate statistical analysis of time-of-flight secondary ion mass spectrometry spectra from complex Cu-Fe sulfides.

PubMed

Kalegowda, Yogesh; Harmer, Sarah L

2012-03-20

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) spectra of mineral samples are complex, comprised of large mass ranges and many peaks. Consequently, characterization and classification analysis of these systems is challenging. In this study, different chemometric and statistical data evaluation methods, based on monolayer sensitive TOF-SIMS data, have been tested for the characterization and classification of copper-iron sulfide minerals (chalcopyrite, chalcocite, bornite, and pyrite) at different flotation pulp conditions (feed, conditioned feed, and Eh modified). The complex mass spectral data sets were analyzed using the following chemometric and statistical techniques: principal component analysis (PCA); principal component-discriminant functional analysis (PC-DFA); soft independent modeling of class analogy (SIMCA); and k-Nearest Neighbor (k-NN) classification. PCA was found to be an important first step in multivariate analysis, providing insight into both the relative grouping of samples and the elemental/molecular basis for those groupings. For samples exposed to oxidative conditions (at Eh ~430 mV), each technique (PCA, PC-DFA, SIMCA, and k-NN) was found to produce excellent classification. For samples at reductive conditions (at Eh ~ -200 mV SHE), k-NN and SIMCA produced the most accurate classification. Phase identification of particles that contain the same elements but a different crystal structure in a mixed multimetal mineral system has been achieved.

Direct and comprehensive analysis of dyes based on integrated molecular and structural information via laser desorption laser postionization mass spectrometry.

PubMed

Liu, Rong; Yin, Zhibin; Leng, Yixin; Hang, Wei; Huang, Benli

2018-01-01

Laser desorption laser postionization time-of-flight mass spectrometry (LDPI-TOFMS) was employed for direct analysis and determination of typical basic dyes. It was also used for the analysis and comprehensive understanding of complex materials such as blue ballpoint pen inks. Simultaneous emergences of fragmental and molecular information largely simplify and facilitate unambiguous identification of dyes via variable energy of 266nm postionization laser. More specifically, by optimizing postionization laser energy with the same energy of desorption laser, the structurally significant results show definite differences in the fragmentation patterns, which offer opportunities for discrimination of isomeric species with identical molecular weight. Moreover, relatively high spectra resolution can be acquired without the expense of sensitivity. In contrast to laser desorption/ionization mass spectrometry (LDI-MS), LDPI-MS simultaneously offers valuable molecular information about dyes in traces, solvents and additives about inks, thereby offering direct determination and comprehensive understanding of blue ballpoint inks and giving a high level of confidence to discriminate the complicated evidentiary samples. In addition, direct analysis of the inks not only allows the avoidance of the tedious sample preparation processes, significantly shortening the overall analysis time and improving throughput, but allows minimized sample consumption which is important for rare and precious samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Clinical evaluation of the Abbott RealTime MTB Assay for direct detection of Mycobacterium tuberculosis-complex from respiratory and non-respiratory samples.

PubMed

Hinić, Vladimira; Feuz, Kinga; Turan, Selda; Berini, Andrea; Frei, Reno; Pfeifer, Karin; Goldenberger, Daniel

2017-05-01

Rapid and reliable diagnosis is crucial for correct management of tuberculosis. The Abbott RealTime MTB Assay represents a novel qualitative real-time PCR assay for direct detection of M. tuberculosis-complex (MTB) DNA from respiratory samples. The test targets two highly conserved sequences, the multi-copy insertion element IS6110 and the protein antigen B (PAB) gene of MTB, allowing even the detection of IS6610-deficient strains. We evaluated this commercial diagnostic test by analyzing 200 respiratory and, for the first time, 87 non-respiratory clinical specimens from our tertiary care institution and compared its results to our IS6110-based in-house real-time PCR for MTB as well as MTB culture. Overall sensitivity for Abbott RealTime MTB was 100% (19/19) in smear positive and 87.5% (7/8) in smear negative specimens, while the specificity of the assay was 100% (260/260). For both non-respiratory smear positive and smear negative specimens Abbott RealTime MTB tests showed 100% (8/8) sensitivity and 100% (8/8) specificity. Cycle threshold (Ct) value analysis of 16 MTB positive samples showed a slightly higher Ct value of the Abbott RealTime MTB test compared to our in-house MTB assay (mean delta Ct = 2.55). In conclusion, the performance of the new Abbott RealTime MTB Assay was highly similar to culture and in-house MTB PCR. We document successful analysis of 87 non-respiratory samples with the highly automated Abbott RealTime MTB test with no inhibition observed. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization of compounds by time-of-flight measurement utilizing random fast ions

DOEpatents

Conzemius, R.J.

1989-04-04

An apparatus is described for characterizing the mass of sample and daughter particles, comprising a source for providing sample ions; a fragmentation region wherein a fraction of the sample ions may fragment to produce daughter ion particles; an electrostatic field region held at a voltage level sufficient to effect ion-neutral separation and ion-ion separation of fragments from the same sample ion and to separate ions of different kinetic energy; a detector system for measuring the relative arrival times of particles; and processing means operatively connected to the detector system to receive and store the relative arrival times and operable to compare the arrival times with times detected at the detector when the electrostatic field region is held at a different voltage level and to thereafter characterize the particles. Sample and daughter particles are characterized with respect to mass and other characteristics by detecting at a particle detector the relative time of arrival for fragments of a sample ion at two different electrostatic voltage levels. The two sets of particle arrival times are used in conjunction with the known altered voltage levels to mathematically characterize the sample and daughter fragments. In an alternative embodiment the present invention may be used as a detector for a conventional mass spectrometer. In this embodiment, conventional mass spectrometry analysis is enhanced due to further mass resolving of the detected ions. 8 figs.

Characterization of compounds by time-of-flight measurement utilizing random fast ions

DOEpatents

Conzemius, Robert J.

1989-01-01

An apparatus for characterizing the mass of sample and daughter particles, comprising a source for providing sample ions; a fragmentation region wherein a fraction of the sample ions may fragment to produce daughter ion particles; an electrostatic field region held at a voltage level sufficient to effect ion-neutral separation and ion-ion separation of fragments from the same sample ion and to separate ions of different kinetic energy; a detector system for measuring the relative arrival times of particles; and processing means operatively connected to the detector system to receive and store the relative arrival times and operable to compare the arrival times with times detected at the detector when the electrostatic field region is held at a different voltage level and to thereafter characterize the particles. Sample and daughter particles are characterized with respect to mass and other characteristics by detecting at a particle detector the relative time of arrival for fragments of a sample ion at two different electrostatic voltage levels. The two sets of particle arrival times are used in conjunction with the known altered voltage levels to mathematically characterize the sample and daughter fragments. In an alternative embodiment the present invention may be used as a detector for a conventional mass spectrometer. In this embodiment, conventional mass spectrometry analysis is enhanced due to further mass resolving of the detected ions.

Sample entropy applied to the analysis of synthetic time series and tachograms

NASA Astrophysics Data System (ADS)

Muñoz-Diosdado, A.; Gálvez-Coyt, G. G.; Solís-Montufar, E.

2017-01-01

Entropy is a method of non-linear analysis that allows an estimate of the irregularity of a system, however, there are different types of computational entropy that were considered and tested in order to obtain one that would give an index of signals complexity taking into account the data number of the analysed time series, the computational resources demanded by the method, and the accuracy of the calculation. An algorithm for the generation of fractal time-series with a certain value of β was used for the characterization of the different entropy algorithms. We obtained a significant variation for most of the algorithms in terms of the series size, which could result counterproductive for the study of real signals of different lengths. The chosen method was sample entropy, which shows great independence of the series size. With this method, time series of heart interbeat intervals or tachograms of healthy subjects and patients with congestive heart failure were analysed. The calculation of sample entropy was carried out for 24-hour tachograms and time subseries of 6-hours for sleepiness and wakefulness. The comparison between the two populations shows a significant difference that is accentuated when the patient is sleeping.

Progress toward the determination of correct classification rates in fire debris analysis.

PubMed

Waddell, Erin E; Song, Emma T; Rinke, Caitlin N; Williams, Mary R; Sigman, Michael E

2013-07-01

Principal components analysis (PCA), linear discriminant analysis (LDA), and quadratic discriminant analysis (QDA) were used to develop a multistep classification procedure for determining the presence of ignitable liquid residue in fire debris and assigning any ignitable liquid residue present into the classes defined under the American Society for Testing and Materials (ASTM) E 1618-10 standard method. A multistep classification procedure was tested by cross-validation based on model data sets comprised of the time-averaged mass spectra (also referred to as total ion spectra) of commercial ignitable liquids and pyrolysis products from common building materials and household furnishings (referred to simply as substrates). Fire debris samples from laboratory-scale and field test burns were also used to test the model. The optimal model's true-positive rate was 81.3% for cross-validation samples and 70.9% for fire debris samples. The false-positive rate was 9.9% for cross-validation samples and 8.9% for fire debris samples. © 2013 American Academy of Forensic Sciences.

Rapid identification of Bacillus anthracis spores in suspicious powder samples by using matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS).

PubMed

Dybwad, Marius; van der Laaken, Anton L; Blatny, Janet Martha; Paauw, Armand

2013-09-01

Rapid and reliable identification of Bacillus anthracis spores in suspicious powders is important to mitigate the safety risks and economic burdens associated with such incidents. The aim of this study was to develop and validate a rapid and reliable laboratory-based matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis method for identifying B. anthracis spores in suspicious powder samples. A reference library containing 22 different Bacillus sp. strains or hoax materials was constructed and coupled with a novel classification algorithm and standardized processing protocol for various powder samples. The method's limit of B. anthracis detection was determined to be 2.5 × 10(6) spores, equivalent to a 55-μg sample size of the crudest B. anthracis-containing powder discovered during the 2001 Amerithrax incidents. The end-to-end analysis method was able to successfully discriminate among samples containing B. anthracis spores, closely related Bacillus sp. spores, and commonly encountered hoax materials. No false-positive or -negative classifications of B. anthracis spores were observed, even when the analysis method was challenged with a wide range of other bacterial agents. The robustness of the method was demonstrated by analyzing samples (i) at an external facility using a different MALDI-TOF MS instrument, (ii) using an untrained operator, and (iii) using mixtures of Bacillus sp. spores and hoax materials. Taken together, the observed performance of the analysis method developed demonstrates its potential applicability as a rapid, specific, sensitive, robust, and cost-effective laboratory-based analysis tool for resolving incidents involving suspicious powders in less than 30 min.

Rapid Identification of Bacillus anthracis Spores in Suspicious Powder Samples by Using Matrix-Assisted Laser Desorption Ionization–Time of Flight Mass Spectrometry (MALDI-TOF MS)

PubMed Central

van der Laaken, Anton L.; Blatny, Janet Martha; Paauw, Armand

2013-01-01

Rapid and reliable identification of Bacillus anthracis spores in suspicious powders is important to mitigate the safety risks and economic burdens associated with such incidents. The aim of this study was to develop and validate a rapid and reliable laboratory-based matrix-assisted laser desorption ionization–time of flight mass spectrometry (MALDI-TOF MS) analysis method for identifying B. anthracis spores in suspicious powder samples. A reference library containing 22 different Bacillus sp. strains or hoax materials was constructed and coupled with a novel classification algorithm and standardized processing protocol for various powder samples. The method's limit of B. anthracis detection was determined to be 2.5 × 106 spores, equivalent to a 55-μg sample size of the crudest B. anthracis-containing powder discovered during the 2001 Amerithrax incidents. The end-to-end analysis method was able to successfully discriminate among samples containing B. anthracis spores, closely related Bacillus sp. spores, and commonly encountered hoax materials. No false-positive or -negative classifications of B. anthracis spores were observed, even when the analysis method was challenged with a wide range of other bacterial agents. The robustness of the method was demonstrated by analyzing samples (i) at an external facility using a different MALDI-TOF MS instrument, (ii) using an untrained operator, and (iii) using mixtures of Bacillus sp. spores and hoax materials. Taken together, the observed performance of the analysis method developed demonstrates its potential applicability as a rapid, specific, sensitive, robust, and cost-effective laboratory-based analysis tool for resolving incidents involving suspicious powders in less than 30 min. PMID:23811517

Classification of illicit heroin by UPLC-Q-TOF analysis of acidic and neutral manufacturing impurities.

PubMed

Liu, Cuimei; Hua, Zhendong; Bai, Yanping

2015-12-01

The illicit manufacture of heroin results in the formation of trace levels of acidic and neutral manufacturing impurities that provide valuable information about the manufacturing process used. In this work, a new ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF) method; that features high resolution, mass accuracy and sensitivity for profiling neutral and acidic heroin manufacturing impurities was developed. After the UPLC-Q-TOF analysis, the retention times and m/z data pairs of acidic and neutral manufacturing impurities were detected, and 19 peaks were found to be evidently different between heroin samples from "Golden Triangle" and "Golden Crescent". Based on the data set of these 19 impurities in 150 authentic heroin samples, classification of heroin geographic origins was successfully achieved utilizing partial least squares discriminant analysis (PLS-DA). By analyzing another data set of 267 authentic heroin samples, the developed discrimiant model was validated and proved to be accurate and reliable. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Space X First Entry Sample Analysis

NASA Technical Reports Server (NTRS)

James, John T.

2012-01-01

The toxicological assessment of one sample collected on May 26, 2012 and returned to earth on May 31, 2012 was analyzed for pollutants that had offgassed into the Dragon capsule by the time of first entry operations performed by the ISS crew. The components identified in the first-entry sample and their contributions to the total T-value are shown.

Time resolved fluorescence of cow and goat milk powder

NASA Astrophysics Data System (ADS)

Brandao, Mariana P.; de Carvalho dos Anjos, Virgílio; Bell., Maria José V.

2017-01-01

Milk powder is an international dairy commodity. Goat and cow milk powders are significant sources of nutrients and the investigation of the authenticity and classification of milk powder is particularly important. The use of time-resolved fluorescence techniques to distinguish chemical composition and structure modifications could assist develop a portable and non-destructive methodology to perform milk powder classification and determine composition. This study goal is to differentiate milk powder samples from cows and goats using fluorescence lifetimes. The samples were excited at 315 nm and the fluorescence intensity decay registered at 468 nm. We observed fluorescence lifetimes of 1.5 ± 0.3, 6.4 ± 0.4 and 18.7 ± 2.5 ns for goat milk powder; and 1.7 ± 0.3, 6.9 ± 0.2 and 29.9 ± 1.6 ns for cow's milk powder. We discriminate goat and cow powder milk by analysis of variance using Fisher's method. In addition, we employed quadratic discriminant analysis to differentiate the milk samples with accuracy of 100%. Our results suggest that time-resolved fluorescence can provide a new method to the analysis of powder milk and its composition.

On the elemental analysis of different cigarette brands using laser induced breakdown spectroscopy and laser-ablation time of flight mass spectrometry

NASA Astrophysics Data System (ADS)

Ahmed, Nasar; Umar, Zeshan A.; Ahmed, Rizwan; Aslam Baig, M.

2017-10-01

We present qualitative and quantitative analysis of the trace elements present in different brands of tobacco available in Pakistan using laser induced breakdown spectroscopy (LIBS) and Laser ablation Time of Flight Mass Spectrometer (LA-TOFMS). The compositional analysis using the calibration free LIBS technique is based on the observed emission spectra of the laser produced plasma plume whereas the elemental composition analysis using LA-TOFMS is based on the mass spectra of the ions produced by laser ablation. The optical emission spectra of these samples contain spectral lines of calcium, magnesium, sodium, potassium, silicon, strontium, barium, lithium and aluminum with varying intensities. The corresponding mass spectra of the elements were detected in LA-TOF-MS with their composition concentration. The analysis of different brands of cigarettes demonstrates that LIBS coupled with a LA-TOF-MS is a powerful technique for the elemental analysis of the trace elements in any solid sample.

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

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1363-1364-1365), pulled on 11/15/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1363-1364-1365 indicated the Isopar™L concentration is at its nominal level (100%). The extractant (MaxCalix) and the modifier (CS- 7SB) are 8% and 2 % below their nominal concentrations. The suppressor (TiDG) is 7% below its nominal concentration. This analysis confirms the trim and Isopar™ additions to the solvent in November. This analysis also indicates the solvent did not require further additions. Based on the current monthlymore » sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

Microbial Monitoring of Common Opportunistic Pathogens by Comparing Multiple Real-time PCR Platforms for Potential Space Applications

NASA Technical Reports Server (NTRS)

Roman, Monserrate C.; Jones, Kathy U.; Oubre, Cherie M.; Castro, Victoria; Ott, Mark C.; Birmele, Michele; Venkateswaran, Kasthuri J.; Vaishampayan, Parag A.

2013-01-01

Current methods for microbial detection: a) Labor & time intensive cultivation-based approaches that can fail to detect or characterize all cells present. b) Requires collection of samples on orbit and transportation back to ground for analysis. Disadvantages to current detection methods: a) Unable to perform quick and reliable detection on orbit. b) Lengthy sampling intervals. c) No microbe identification.

Sintering time optimization on red photoluminescence properties of manganese-doped boron carbon oxynitride (BCNO:Mn) phosphor

NASA Astrophysics Data System (ADS)

Wahid Nuryadin, Bebeh; Suryani, Yayu; Yuliani, Yuli; Setiadji, Soni; Yeti Nuryantini, Ade; Iskandar, Ferry

2018-04-01

The effect of sintering time to the transient nature and optimization of red photoluminescence manganese-doped boron carbon oxynitride (BCNO:Mn) phosphor was investigated. The BCNO:Mn samples were synthesized using a facile urea-assisted combustion route involving boric acid, citric acid, manganese salt and urea. The optimized intensity of the dual peak emission at 420 nm (blue emission) and 630 nm (red emission) in the photoluminescence (PL) spectrum could be achieved by controlling the sintering time of the BCNO:Mn. The BCNO:Mn samples in high-crystalline form was found to be in a cubic and hexagonal structure. Based on the PL analysis, it is suggested that the BCNO:Mn symmetric band at 630 nm can be attributed to the 4T1(4G)—6A1(6S) transition absorption of Mn2+ ions into the hexagonal structure. Microstructure analysis showed an irregular and agglomerated shape of the BCNO:Mn sample.

Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry

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

Maddi, Balakrishna; Panisko, Ellen; Albrecht, Karl

Two-dimensional gas chromatography coupled with time of flight mass spectrometry is a powerful tool for identifying and quantifying components in complex mixtures. It has been used to analyze gasoline, jet fuel, diesel, bio-diesel and organic fraction of bio-crude/bio-oil. In these experiments, the first dimension of separation was non-polar, followed by a polar separation. Aqueous fractions of bio-crude and other aqueous samples have been examined with similar column combinations. However, sample preparation techniques such as derivatization, solvent extraction, and solid-phase extraction were necessary prior to analysis. In this study, aqueous fraction obtained from hydrothermal liquefaction of algae was characterized by two-dimensionalmore » gas chromatography coupled with time of flight mass spectrometry without prior sample preparation techniques using a polar separation in the first dimension followed by a non-polar separation. Two-dimensional plots from this analysis were compared with those obtained from the more traditional column combination. Results from qualitative characterization aqueous fractions of algal bio-crude are discussed in detail. The advantages of using a polar separation followed by a non-polar separation for characterization of organics in aqueous samples by two-dimensional gas chromatography coupled with time of flight mass spectrometry are highlighted.« less

Effect of mobile phone use on metal ion release from fixed orthodontic appliances.

PubMed

Saghiri, Mohammad Ali; Orangi, Jafar; Asatourian, Armen; Mehriar, Peiman; Sheibani, Nader

2015-06-01

The aim of this study was to evaluate the effect of exposure to radiofrequency electromagnetic fields emitted by mobile phones on the level of nickel in saliva. Fifty healthy patients with fixed orthodontic appliances were asked not to use their cell phones for a week, and their saliva samples were taken at the end of the week (control group). The patients recorded their time of mobile phone usage during the next week and returned for a second saliva collection (experimental group). Samples at both times were taken between 8:00 and 10:00 pm, and the nickel levels were measured. Two-tailed paired-samples t test, linear regression, independent t test, and 1-way analysis of variance were used for data analysis. The 2-tailed paired-samples t test showed significant differences between the levels of nickel in the control and experimental groups (t [49] = 9.967; P <0.001). The linear regression test showed a significant relationship between mobile phone usage time and the nickel release (F [1, 48] = 60.263; P <0.001; R(2) = 0.577). Mobile phone usage has a time-dependent influence on the concentration of nickel in the saliva of patients with orthodontic appliances. Copyright © 2015 American Association of Orthodontists. Published by Elsevier Inc. All rights reserved.

Rapid and simple procedure for homogenizing leaf tissues suitable for mini-midi-scale DNA extraction in rice.

PubMed

Yi, Gihwan; Choi, Jun-Ho; Lee, Jong-Hee; Jeong, Unggi; Nam, Min-Hee; Yun, Doh-Won; Eun, Moo-Young

2005-01-01

We describe a rapid and simple procedure for homogenizing leaf samples suitable for mini/midi-scale DNA preparation in rice. The methods used tungsten carbide beads and general vortexer for homogenizing leaf samples. In general, two samples can be ground completely within 11.3+/-1.5 sec at one time. Up to 20 samples can be ground at a time using a vortexer attachment. The yields of the DNA ranged from 2.2 to 7.6 microg from 25-150 mg of young fresh leaf tissue. The quality and quantity of DNA was compatible for most of PCR work and RFLP analysis.

Development Status of the WetLab-2 Project: New Tools for On-orbit Real-time Quantitative Gene Expression.

NASA Technical Reports Server (NTRS)

Jung, Jimmy; Parra, Macarena P.; Almeida, Eduardo; Boone, Travis; Chinn, Tori; Ricco, Antonio; Souza, Kenneth; Hyde, Liz; Rukhsana, Yousuf; Richey, C. Scott

2013-01-01

The primary objective of NASA Ames Research Centers WetLab-2 Project is to place on the ISS a research platform to facilitate gene expression analysis via quantitative real-time PCR (qRT-PCR) of biological specimens grown or cultured on orbit. The WetLab-2 equipment will be capable of processing multiple sample types ranging from microbial cultures to animal tissues dissected on-orbit. In addition to the logistical benefits of in-situ sample processing and analysis, conducting qRT-PCR on-orbit eliminates the confounding effects on gene expression of reentry stresses and shock acting on live cells and organisms. The system can also validate terrestrial analyses of samples returned from ISS by providing quantitative on-orbit gene expression benchmarking prior to sample return. The ability to get on orbit data will provide investigators with the opportunity to adjust experimental parameters for subsequent trials based on the real-time data analysis without need for sample return and re-flight. Finally, WetLab-2 can be used for analysis of air, surface, water, and clinical samples to monitor environmental contaminants and crew health. The verification flight of the instrument is scheduled to launch on SpaceX-5 in Aug. 2014.Progress to date: The WetLab-2 project completed a thorough study of commercially available qRT-PCR systems and performed a downselect based on both scientific and engineering requirements. The selected instrument, the Cepheid SmartCycler, has advantages including modular design (16 independent PCR modules), low power consumption, and rapid ramp times. The SmartCycler has multiplex capabilities, assaying up to four genes of interest in each of the 16 modules. The WetLab-2 team is currently working with Cepheid to modify the unit for housing within an EXPRESS rack locker on the ISS. This will enable the downlink of data to the ground and provide uplink capabilities for programming, commanding, monitoring, and instrument maintenance. The project is currently designing a module that will lyse the cells and extract RNA of sufficient quality for use in qRT-PCR reactions while using a housekeeping gene to normalize RNA concentration and integrity. Current testing focuses on two promising commercial products and chemistries that allow for RNA extraction with minimal complexity and crew time.

Trace analysis of energetic materials via direct analyte-probed nanoextraction coupled to direct analysis in real time mass spectrometry.

PubMed

Clemons, Kristina; Dake, Jeffrey; Sisco, Edward; Verbeck, Guido F

2013-09-10

Direct analysis in real time mass spectrometry (DART-MS) has proven to be a useful forensic tool for the trace analysis of energetic materials. While other techniques for detecting trace amounts of explosives involve extraction, derivatization, solvent exchange, or sample clean-up, DART-MS requires none of these. Typical DART-MS analyses directly from a solid sample or from a swab have been quite successful; however, these methods may not always be an optimal sampling technique in a forensic setting. For example, if the sample were only located in an area which included a latent fingerprint of interest, direct DART-MS analysis or the use of a swab would almost certainly destroy the print. To avoid ruining such potentially invaluable evidence, another method has been developed which will leave the fingerprint virtually untouched. Direct analyte-probed nanoextraction coupled to nanospray ionization-mass spectrometry (DAPNe-NSI-MS) has demonstrated excellent sensitivity and repeatability in forensic analyses of trace amounts of illicit drugs from various types of surfaces. This technique employs a nanomanipulator in conjunction with bright-field microscopy to extract single particles from a surface of interest and has provided a limit of detection of 300 attograms for caffeine. Combining DAPNe with DART-MS provides another level of flexibility in forensic analysis, and has proven to be a sufficient detection method for trinitrotoluene (TNT), RDX, and 1-methylaminoanthraquinone (MAAQ). Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

From Sample to Multi-Omics Conclusions in under 48 Hours

PubMed Central

Navas-Molina, Jose A.; Hyde, Embriette R.; Vázquez-Baeza, Yoshiki; Humphrey, Greg; Gaffney, James; Minich, Jeremiah J.; Melnik, Alexey V.; Herschend, Jakob; DeReus, Jeff; Durant, Austin; Dutton, Rachel J.; Khosroheidari, Mahdieh; Green, Clifford; da Silva, Ricardo; Dorrestein, Pieter C.; Knight, Rob

2016-01-01

ABSTRACT Multi-omics methods have greatly advanced our understanding of the biological organism and its microbial associates. However, they are not routinely used in clinical or industrial applications, due to the length of time required to generate and analyze omics data. Here, we applied a novel integrated omics pipeline for the analysis of human and environmental samples in under 48 h. Human subjects that ferment their own foods provided swab samples from skin, feces, oral cavity, fermented foods, and household surfaces to assess the impact of home food fermentation on their microbial and chemical ecology. These samples were analyzed with 16S rRNA gene sequencing, inferred gene function profiles, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) metabolomics through the Qiita, PICRUSt, and GNPS pipelines, respectively. The human sample microbiomes clustered with the corresponding sample types in the American Gut Project (http://www.americangut.org), and the fermented food samples produced a separate cluster. The microbial communities of the household surfaces were primarily sourced from the fermented foods, and their consumption was associated with increased gut microbial diversity. Untargeted metabolomics revealed that human skin and fermented food samples had separate chemical ecologies and that stool was more similar to fermented foods than to other sample types. Metabolites from the fermented foods, including plant products such as procyanidin and pheophytin, were present in the skin and stool samples of the individuals consuming the foods. Some food metabolites were modified during digestion, and others were detected in stool intact. This study represents a first-of-its-kind analysis of multi-omics data that achieved time intervals matching those of classic microbiological culturing. IMPORTANCE Polymicrobial infections are difficult to diagnose due to the challenge in comprehensively cultivating the microbes present. Omics methods, such as 16S rRNA sequencing, metagenomics, and metabolomics, can provide a more complete picture of a microbial community and its metabolite production, without the biases and selectivity of microbial culture. However, these advanced methods have not been applied to clinical or industrial microbiology or other areas where complex microbial dysbioses require immediate intervention. The reason for this is the length of time required to generate and analyze omics data. Here, we describe the development and application of a pipeline for multi-omics data analysis in time frames matching those of the culture-based approaches often used for these applications. This study applied multi-omics methods effectively in clinically relevant time frames and sets a precedent toward their implementation in clinical medicine and industrial microbiology. PMID:27822524

Micropowder collecting technique for stable isotope analysis of carbonates.

PubMed

Sakai, Saburo; Kodan, Tsuyoshi

2011-05-15

Micromilling is a conventional technique used in the analysis of the isotopic composition of geological materials, which improves the spatial resolution of sample collection for analysis. However, a problem still remains concerning the recovery ratio of the milled sample. We constructed a simple apparatus consisting of a vacuum pump, a sintered metal filter, electrically conductive rubber stopper and a stainless steel tube for transferring the milled powder into a reaction vial. In our preliminary experiments on carbonate powder, we achieved a rapid recovery of 5 to 100 µg of carbonate with a high recovery ratio (>90%). This technique shortens the sample preparation time, improves the recovery ratio, and homogenizes the sample quantity, which, in turn, improves the analytical reproducibility. Copyright © 2011 John Wiley & Sons, Ltd.

Quantitative Digital Autoradiography for Environmental Swipe Sample Prioritization: System design, Characterization, and Initial Measurements

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

McDonald, Benjamin S.; Zalavadia, Mital A.; Miller, Brian W.

Environmental sampling and sample analyses by the International Atomic Energy Agency’s (IAEA) Network of Analytical Laboratories (NWAL) is a critical technical tool used to detect facility misuse under a Comprehensive Safeguards Agreement and to verify the absence of undeclared nuclear material activities under an Additional Protocol. Currently all environmental swipe samples (ESS) are screened using gamma spectrometry and x-ray fluorescence to estimate the amount of U and/or Pu in the ESS, to guide further analysis, and to assist in the shipment of ESS to the NWAL. Quantitative Digital Autoradiography for Environmental Samples (QDARES) is being developed to complement existing techniquesmore » through the use of a portable, real-time, high-spatial-resolution camera called the Ionizing-radiation Quantum Imaging Detector (iQID). The iQID constructs a spatial map of radionuclides within a sample or surface in real-time as charged particles (betas) and photons (gamma/x-rays) are detected and localized on an event-by-event basis. Knowledge of the location and nature of radioactive hot spots on the ESS could provide information for subsequent laboratory analysis. As a nondestructive technique, QDARES does not compromise the ESS chain of custody or subsequent laboratory analysis. In this paper we will present the system design and construction, characterization measurements with calibration sources, and initial measurements of ESS.« less

A novel quality by design approach for developing an HPLC method to analyze herbal extracts: A case study of sugar content analysis.

PubMed

Shao, Jingyuan; Cao, Wen; Qu, Haibin; Pan, Jianyang; Gong, Xingchu

2018-01-01

The aim of this study was to present a novel analytical quality by design (AQbD) approach for developing an HPLC method to analyze herbal extracts. In this approach, critical method attributes (CMAs) and critical method parameters (CMPs) of the analytical method were determined using the same data collected from screening experiments. The HPLC-ELSD method for separation and quantification of sugars in Codonopsis Radix extract (CRE) samples and Astragali Radix extract (ARE) samples was developed as an example method with a novel AQbD approach. Potential CMAs and potential CMPs were found with Analytical Target Profile. After the screening experiments, the retention time of the D-glucose peak of CRE samples, the signal-to-noise ratio of the D-glucose peak of CRE samples, and retention time of the sucrose peak in ARE samples were considered CMAs. The initial and final composition of the mobile phase, flow rate, and column temperature were found to be CMPs using a standard partial regression coefficient method. The probability-based design space was calculated using a Monte-Carlo simulation method and verified by experiments. The optimized method was validated to be accurate and precise, and then it was applied in the analysis of CRE and ARE samples. The present AQbD approach is efficient and suitable for analysis objects with complex compositions.

Fast and accurate determination of arsenobetaine in fish tissues using accelerated solvent extraction and HPLC-ICP-MS determination.

PubMed

Wahlen, Raimund

2004-04-01

A high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method has been developed for the fast and accurate analysis of arsenobetaine (AsB) in fish samples extracted by accelerated solvent extraction. The combined extraction and analysis approach is validated using certified reference materials for AsB in fish and during a European intercomparison exercise with a blind sample. Up to six species of arsenic (As) can be separated and quantitated in the extracts within a 10-min isocratic elution. The method is optimized so as to minimize time-consuming sample preparation steps and allow for automated extraction and analysis of large sample batches. A comparison of standard addition and external calibration show no significant difference in the results obtained, which indicates that the LC-ICP-MS method is not influenced by severe matrix effects. The extraction procedure can process up to 24 samples in an automated manner, yet the robustness of the developed HPLC-ICP-MS approach is highlighted by the capability to run more than 50 injections per sequence, which equates to a total run-time of more than 12 h. The method can therefore be used to rapidly and accurately assess the proportion of nontoxic AsB in fish samples with high total As content during toxicological screening studies.

Studies in astronomical time series analysis. III - Fourier transforms, autocorrelation functions, and cross-correlation functions of unevenly spaced data

NASA Technical Reports Server (NTRS)

Scargle, Jeffrey D.

1989-01-01

This paper develops techniques to evaluate the discrete Fourier transform (DFT), the autocorrelation function (ACF), and the cross-correlation function (CCF) of time series which are not evenly sampled. The series may consist of quantized point data (e.g., yes/no processes such as photon arrival). The DFT, which can be inverted to recover the original data and the sampling, is used to compute correlation functions by means of a procedure which is effectively, but not explicitly, an interpolation. The CCF can be computed for two time series not even sampled at the same set of times. Techniques for removing the distortion of the correlation functions caused by the sampling, determining the value of a constant component to the data, and treating unequally weighted data are also discussed. FORTRAN code for the Fourier transform algorithm and numerical examples of the techniques are given.

Onsite Gaseous Centrifuge Enrichment Plant UF6 Cylinder Destructive Analysis

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

Anheier, Norman C.; Cannon, Bret D.; Qiao, Hong

2012-07-17

The IAEA safeguards approach for gaseous centrifuge enrichment plants (GCEPs) includes measurements of gross, partial, and bias defects in a statistical sampling plan. These safeguard methods consist principally of mass and enrichment nondestructive assay (NDA) verification. Destructive assay (DA) samples are collected from a limited number of cylinders for high precision offsite mass spectrometer analysis. DA is typically used to quantify bias defects in the GCEP material balance. Under current safeguards measures, the operator collects a DA sample from a sample tap following homogenization. The sample is collected in a small UF6 sample bottle, then sealed and shipped under IAEAmore » chain of custody to an offsite analytical laboratory. Current practice is expensive and resource intensive. We propose a new and novel approach for performing onsite gaseous UF6 DA analysis that provides rapid and accurate assessment of enrichment bias defects. DA samples are collected using a custom sampling device attached to a conventional sample tap. A few micrograms of gaseous UF6 is chemically adsorbed onto a sampling coupon in a matter of minutes. The collected DA sample is then analyzed onsite using Laser Ablation Absorption Ratio Spectrometry-Destructive Assay (LAARS-DA). DA results are determined in a matter of minutes at sufficient accuracy to support reliable bias defect conclusions, while greatly reducing DA sample volume, analysis time, and cost.« less

Automated liver sampling using a gradient dual-echo Dixon-based technique.

PubMed

Bashir, Mustafa R; Dale, Brian M; Merkle, Elmar M; Boll, Daniel T

2012-05-01

Magnetic resonance spectroscopy of the liver requires input from a physicist or physician at the time of acquisition to insure proper voxel selection, while in multiecho chemical shift imaging, numerous regions of interest must be manually selected in order to ensure analysis of a representative portion of the liver parenchyma. A fully automated technique could improve workflow by selecting representative portions of the liver prior to human analysis. Complete volumes from three-dimensional gradient dual-echo acquisitions with two-point Dixon reconstruction acquired at 1.5 and 3 T were analyzed in 100 subjects, using an automated liver sampling algorithm, based on ratio pairs calculated from signal intensity image data as fat-only/water-only and log(in-phase/opposed-phase) on a voxel-by-voxel basis. Using different gridding variations of the algorithm, the average correct liver volume samples ranged from 527 to 733 mL. The average percentage of sample located within the liver ranged from 95.4 to 97.1%, whereas the average incorrect volume selected was 16.5-35.4 mL (2.9-4.6%). Average run time was 19.7-79.0 s. The algorithm consistently selected large samples of the hepatic parenchyma with small amounts of erroneous extrahepatic sampling, and run times were feasible for execution on an MRI system console during exam acquisition. Copyright © 2011 Wiley Periodicals, Inc.

Literature Reference for Noroviruses (Journal of Clinical Microbiology. 2004. 42(10): 4679–4685)

EPA Pesticide Factsheets

Procedures are described for analysis of clinical samples and may be adapted for of solid, particulate, aerosol, and water samples. This method is an assay for detection and quantitation of norovirus using real-time reverse transcription-PCR.

Literature Reference for Influenza H5N1 (Emerging Infectious Diseases. 2005. 11(8): 1303–1305)

EPA Pesticide Factsheets

Procedures are described for analysis of clinical samples and may be adapted for assessment of solid, particulate, aerosol, liquid and water samples. This is a two-step, real-time reverse transcriptase-PCR multiplex assay.

The Stability and Validity of Automated Vocal Analysis in Preverbal Preschoolers With Autism Spectrum Disorder

PubMed Central

Woynaroski, Tiffany; Oller, D. Kimbrough; Keceli-Kaysili, Bahar; Xu, Dongxin; Richards, Jeffrey A.; Gilkerson, Jill; Gray, Sharmistha; Yoder, Paul

2017-01-01

Theory and research suggest that vocal development predicts “useful speech” in preschoolers with autism spectrum disorder (ASD), but conventional methods for measurement of vocal development are costly and time consuming. This longitudinal correlational study examines the reliability and validity of several automated indices of vocalization development relative to an index derived from human coded, conventional communication samples in a sample of preverbal preschoolers with ASD. Automated indices of vocal development were derived using software that is presently “in development” and/or only available for research purposes and using commercially available Language ENvironment Analysis (LENA) software. Indices of vocal development that could be derived using the software available for research purposes: (a) were highly stable with a single day-long audio recording, (b) predicted future spoken vocabulary to a degree that was nonsignificantly different from the index derived from conventional communication samples, and (c) continued to predict future spoken vocabulary even after controlling for concurrent vocabulary in our sample. The score derived from standard LENA software was similarly stable, but was not significantly correlated with future spoken vocabulary. Findings suggest that automated vocal analysis is a valid and reliable alternative to time intensive and expensive conventional communication samples for measurement of vocal development of preverbal preschoolers with ASD in research and clinical practice. PMID:27459107

Carbon isotopic analysis of atmospheric methane by isotope-ratio-monitoring gas chromatography-mass spectrometry

NASA Technical Reports Server (NTRS)

Merritt, Dawn A.; Hayes, J. M.; Des Marais, David J.

1995-01-01

Less than 15 min are required for the determination of delta C(sub PDB)-13 with a precision of 0.2 ppt(1 sigma, single measurement) in 5-mL samples of air containing CH4 at natural levels (1.7 ppm). An analytical system including a sample-introduction unit incorporating a preparative gas chromatograph (GC) column for separation of CH4 from N2, O2, and Ar is described. The 15-min procedure includes time for operation of that system, high-resolution chromatographic separation of the CH4, on-line combustion and purification of the products, and isotopic calibration. Analyses of standards demonstrate that systematic errors are absent and that there is no dependence of observed values of delta on sample size. For samples containing 100 ppm or more CH4, preconcentration is not required and the analysis time is less than 5 min. The system utilizes a commercially available, high-sensitivity isotope-ratio mass spectrometer. For optimal conditions of smaple handling and combustion, performance of the system is within a factor of 2 of the shot-noise limit. The potential exists therefore for analysis of samples as small as 15 pmol CH4 with a standard deviation of less than 1 ppt.

Classification of time-of-flight secondary ion mass spectrometry spectra from complex Cu-Fe sulphides by principal component analysis and artificial neural networks.

PubMed

Kalegowda, Yogesh; Harmer, Sarah L

2013-01-08

Artificial neural network (ANN) and a hybrid principal component analysis-artificial neural network (PCA-ANN) classifiers have been successfully implemented for classification of static time-of-flight secondary ion mass spectrometry (ToF-SIMS) mass spectra collected from complex Cu-Fe sulphides (chalcopyrite, bornite, chalcocite and pyrite) at different flotation conditions. ANNs are very good pattern classifiers because of: their ability to learn and generalise patterns that are not linearly separable; their fault and noise tolerance capability; and high parallelism. In the first approach, fragments from the whole ToF-SIMS spectrum were used as input to the ANN, the model yielded high overall correct classification rates of 100% for feed samples, 88% for conditioned feed samples and 91% for Eh modified samples. In the second approach, the hybrid pattern classifier PCA-ANN was integrated. PCA is a very effective multivariate data analysis tool applied to enhance species features and reduce data dimensionality. Principal component (PC) scores which accounted for 95% of the raw spectral data variance, were used as input to the ANN, the model yielded high overall correct classification rates of 88% for conditioned feed samples and 95% for Eh modified samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Revisiting the incidence of Mg II absorbers along the blazar sightlines

NASA Astrophysics Data System (ADS)

Mishra, Sapna; Chand, Hum; Gopal-Krishna; Joshi, Ravi

2018-04-01

It is believed that the cool gas clouds traced by Mg II absorption, within a velocity offset of 5000 km/s from the background quasar, are associated with the quasar itself, whereas the absorbers seen at larger velocity offsets towards us are intervening systems and hence their existence is completely independent of the background quasar. Recent evidence by Bergeron et al. 2011 (hereafter BBM), however, seriously questions this canonical view, by showing that the number density of intervening Mg II absorbers along the sightlines towards 45 blazars is, on average, 2 times the expectation based on the Mg II absorption systems seen on the sightlines to normal QSOs. Given the serious implications of this finding, it becomes important to revisit this issue by enlarging the source sample and subjecting it to an independent analysis. Here, we first report our results based on a re-analysis of the spectroscopic data for the BBM sample; this has reproduced their factor 2 excess in dN/dz along blazar sightlines, vis-a-vis the normal QSOs. Next, we assemble a 6 times larger sample of blazar sightlines, albeit with lower SNR. Using this enlarged sample together with the BBM sample, our analysis shows that the dN/dz of Mg II absorbers statistically matches that known for normal QSO sightlines.

Direct Analysis of Low-Volatile Molecular Marker Extract from Airborne Particulate Matter Using Sensitivity Correction Method

PubMed Central

Irei, Satoshi

2016-01-01

Molecular marker analysis of environmental samples often requires time consuming preseparation steps. Here, analysis of low-volatile nonpolar molecular markers (5-6 ring polycyclic aromatic hydrocarbons or PAHs, hopanoids, and n-alkanes) without the preseparation procedure is presented. Analysis of artificial sample extracts was directly conducted by gas chromatography-mass spectrometry (GC-MS). After every sample injection, a standard mixture was also analyzed to make a correction on the variation of instrumental sensitivity caused by the unfavorable matrix contained in the extract. The method was further validated for the PAHs using the NIST standard reference materials (SRMs) and then applied to airborne particulate matter samples. Tests with the SRMs showed that overall our methodology was validated with the uncertainty of ~30%. The measurement results of airborne particulate matter (PM) filter samples showed a strong correlation between the PAHs, implying the contributions from the same emission source. Analysis of size-segregated PM filter samples showed that their size distributions were found to be in the PM smaller than 0.4 μm aerodynamic diameter. The observations were consistent with our expectation of their possible sources. Thus, the method was found to be useful for molecular marker studies. PMID:27127511

Electro-focusing liquid extractive surface analysis (EF-LESA) coupled to mass spectrometry.

PubMed

Brenton, A Gareth; Godfrey, A Ruth

2014-04-01

Analysis of the chemical composition of surfaces by liquid sampling devices interfaced to mass spectrometry is attractive as the sample stream can be continuously monitored at good sensitivity and selectivity. A sampling probe has been constructed that takes discrete liquid samples (typically <100 nL) of a surface. It incorporates an electrostatic lens system, comprising three electrodes, to which static and pulsed voltages are applied to form a conical "liquid tip", employed to dissolve analytes at a surface. A prototype system demonstrates spatial resolution of 0.093 mm(2). Time of contact between the liquid tip and the surface is controlled to standardize extraction. Calibration graphs of different analyte concentrations on a stainless surface have been measured, together with the probe's reproducibility, carryover, and recovery. A leucine enkephalin-coated surface demonstrated good linearity (R(2) = 0.9936), with a recovery of 90% and a limit of detection of 38 fmol per single spot sampled. The probe is compact and can be fitted into automated sample analysis equipment having potential for rapid analysis of surfaces at a good spatial resolution.

Electro-Focusing Liquid Extractive Surface Analysis (EF-LESA) Coupled to Mass Spectrometry

PubMed Central

2014-01-01

Analysis of the chemical composition of surfaces by liquid sampling devices interfaced to mass spectrometry is attractive as the sample stream can be continuously monitored at good sensitivity and selectivity. A sampling probe has been constructed that takes discrete liquid samples (typically <100 nL) of a surface. It incorporates an electrostatic lens system, comprising three electrodes, to which static and pulsed voltages are applied to form a conical “liquid tip”, employed to dissolve analytes at a surface. A prototype system demonstrates spatial resolution of 0.093 mm2. Time of contact between the liquid tip and the surface is controlled to standardize extraction. Calibration graphs of different analyte concentrations on a stainless surface have been measured, together with the probe’s reproducibility, carryover, and recovery. A leucine enkephalin-coated surface demonstrated good linearity (R2 = 0.9936), with a recovery of 90% and a limit of detection of 38 fmol per single spot sampled. The probe is compact and can be fitted into automated sample analysis equipment having potential for rapid analysis of surfaces at a good spatial resolution. PMID:24597530

Two modulator generalized ellipsometer for complete mueller matrix measurement

DOEpatents

Jellison, Jr., Gerald E.; Modine, Frank A.

1999-01-01

A two-modulator generalized ellipsometer (2-MGE) comprising two polarizer-photoelastic modulator (PEM) pairs, an optical light source, an optical detection system, and associated data processing and control electronics, where the PEMs are free-running. The input light passes through the first polarizer-PEM pair, reflects off the sample surface or passes through the sample, passes through the second PEM-polarizer pair, and is detected. Each PEM is free running and operates at a different resonant frequency, e.g., 50 and 60 kHz. The resulting time-dependent waveform of the light intensity is a complicated function of time, and depends upon the exact operating frequency and phase of each PEM, the sample, and the azimuthal angles of the polarizer-PEM pairs, but can be resolved into a dc component and eight periodic components. In one embodiment, the waveform is analyzed using a new spectral analysis technique that is similar to Fourier analysis to determine eight sample Mueller matrix elements (normalized to the m.sub.00 Mueller matrix element). The other seven normalized elements of the general 4.times.4 Mueller matrix can be determined by changing the azimuthal angles of the PEM-polarizer pairs with respect to the plane of incidence. Since this instrument can measure all elements of the sample Mueller matrix, it is much more powerful than standard ellipsometers.

Atmospheric CO2 Concentrations from Aircraft for 1972-1981, CSIRO Monitoring Program

DOE Data Explorer

Beardsmore, David J. [Commonwealth Scientific and Industrial Research Organization (CSIRO), Victoria, Australia; Pearman, Graeme I. [Commonwealth Scientific and Industrial Research Organization (CSIRO), Victoria, Australia

2012-01-01

From 1972 through 1981, air samples were collected in glass flasks from aircraft at a variety of latitudes and altitudes over Australia, New Zealand, and Antarctica. The samples were analyzed for CO2 concentrations with nondispersive infrared gas analysis. The resulting data contain the sampling dates, type of aircraft, flight number, flask identification number, sampling time, geographic sector, distance in kilometers from the listed distance measuring equipment (DME) station, station number of the radio navigation distance measuring equipment, altitude of the aircraft above mean sea level, sample analysis date, flask pressure, tertiary standards used for the analysis, analyzer used, and CO2 concentration. These data represent the first published record of CO2 concentrations in the Southern Hemisphere expressed in the WMO 1981 CO2 Calibration Scale and provide a precise record of atmospheric CO2 concentrations in the troposphere and lower stratosphere over Australia and New Zealand.

[Standard sample preparation method for quick determination of trace elements in plastic].

PubMed

Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

2011-08-01

Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

Poisoning: fact or fiction?

PubMed

Flanagan, Robert J

2012-01-01

Analytical toxicology is a complex discipline. Simply detecting a poison in a biological sample does not necessarily mean that the individual from whom the sample was obtained had been poisoned. An analysis can prove exposure and perhaps give an indication of the magnitude of exposure, but the results have to be placed in proper context. Even if sampling was ante-mortem an analysis does not necessarily prove the effects that the drug or poison had on the victim immediately before or at the time of sampling. Tolerance is one big issue, the mechanism of exposure (how the drug got into the body) is another, and of course with post-mortem work there are always additional considerations such as site of sample collection and the possibility of post-mortem change in analyte concentration. There are also questions of quality and reliability, and whether a particular analysis and the interpretation placed upon the result are appropriate in a particular case.

Application of imaging spectrometer in gas analysis by Raman scattering

NASA Astrophysics Data System (ADS)

Zuo, Duluo; Yu, Anlan; Li, Zhe; Wang, Xingbing; Xiong, Youhui

2015-09-01

Spontaneous Raman scattering is an effective technique in gas analysis, but the detection of minor constituents is difficult because of the low signal level and the usually existed background. Imaging spectrometer can provide highly spatial resolved spectra, so it should be much easier to pick up Raman signal of minor constituents from the Raman/fluorescence background of the sample cell and transporting optics compared with the widely used fiber-coupled spectrometers. For this reason, an imaging spectrometer was constructed from transmitting volume phase holographic grating, camera lenses and CCD detector. When it was used to analyze the gas sample in metal-lined capillary, which is a sample cell believed with great enhancement of Raman signal, the background was compressed obviously. When it was used to analyze the gas in a sample cell including a parabolic reflector, only weak background signal was observed, as the wide separation between the collecting zone (the focus point of the parabolic surface) and the wall of sample cell benefitted to the analysis by imaging spectrometer. By using the last sample cell, the signal from CO2 in ambient air was able to be found by an exposure time about 20 sec, and limits of detection for H2, CO2 and CO were estimated as 60 ppm, 100 ppm and 300 ppm respectively by the results of a longer exposure time. These results show that an imaging spectrometer paired with a well-arranged sample cell will lower the detecting limit effectively.

Experimental Investigations of Non-Stationary Properties In Radiometer Receivers Using Measurements of Multiple Calibration References

NASA Technical Reports Server (NTRS)

Racette, Paul; Lang, Roger; Zhang, Zhao-Nan; Zacharias, David; Krebs, Carolyn A. (Technical Monitor)

2002-01-01

Radiometers must be periodically calibrated because the receiver response fluctuates. Many techniques exist to correct for the time varying response of a radiometer receiver. An analytical technique has been developed that uses generalized least squares regression (LSR) to predict the performance of a wide variety of calibration algorithms. The total measurement uncertainty including the uncertainty of the calibration can be computed using LSR. The uncertainties of the calibration samples used in the regression are based upon treating the receiver fluctuations as non-stationary processes. Signals originating from the different sources of emission are treated as simultaneously existing random processes. Thus, the radiometer output is a series of samples obtained from these random processes. The samples are treated as random variables but because the underlying processes are non-stationary the statistics of the samples are treated as non-stationary. The statistics of the calibration samples depend upon the time for which the samples are to be applied. The statistics of the random variables are equated to the mean statistics of the non-stationary processes over the interval defined by the time of calibration sample and when it is applied. This analysis opens the opportunity for experimental investigation into the underlying properties of receiver non stationarity through the use of multiple calibration references. In this presentation we will discuss the application of LSR to the analysis of various calibration algorithms, requirements for experimental verification of the theory, and preliminary results from analyzing experiment measurements.

Full-Time versus Part-Time Employees: Understanding the Links between Work Status, the Psychological Contract, and Attitudes.

ERIC Educational Resources Information Center

Conway, Neil; Briner, Rob B.

2002-01-01

Analysis of psychological contract variables (affective and continuance commitment, intention to quit, well-being, job satisfaction, organizational citizenship behavior)was conducted on two samples: 1,608 banking employees (71% part time) and 366 supermarket employees (65% part time). Part- and full-time workers had different attitudes; fulfilment…

Spatial-dependence recurrence sample entropy

NASA Astrophysics Data System (ADS)

Pham, Tuan D.; Yan, Hong

2018-03-01

Measuring complexity in terms of the predictability of time series is a major area of research in science and engineering, and its applications are spreading throughout many scientific disciplines, where the analysis of physiological signals is perhaps the most widely reported in literature. Sample entropy is a popular measure for quantifying signal irregularity. However, the sample entropy does not take sequential information, which is inherently useful, into its calculation of sample similarity. Here, we develop a method that is based on the mathematical principle of the sample entropy and enables the capture of sequential information of a time series in the context of spatial dependence provided by the binary-level co-occurrence matrix of a recurrence plot. Experimental results on time-series data of the Lorenz system, physiological signals of gait maturation in healthy children, and gait dynamics in Huntington's disease show the potential of the proposed method.

Simultaneous multi-beam planar array IR (pair) spectroscopy

DOEpatents

Elmore, Douglas L.; Rabolt, John F.; Tsao, Mei-Wei

2005-09-13

An apparatus and method capable of providing spatially multiplexed IR spectral information simultaneously in real-time for multiple samples or multiple spatial areas of one sample using IR absorption phenomena requires no moving parts or Fourier Transform during operation, and self-compensates for background spectra and degradation of component performance over time. IR spectral information and chemical analysis of the samples is determined by using one or more IR sources, sampling accessories for positioning the samples, optically dispersive elements, a focal plane array (FPA) arranged to detect the dispersed light beams, and a processor and display to control the FPA, and display an IR spectrograph. Fiber-optic coupling can be used to allow remote sensing. Portability, reliability, and ruggedness is enhanced due to the no-moving part construction. Applications include determining time-resolved orientation and characteristics of materials, including polymer monolayers. Orthogonal polarizers may be used to determine certain material characteristics.

Analysis of acrylamide in food products by in-line preconcentration capillary zone electrophoresis.

PubMed

Bermudo, Elisabet; Núñez, Oscar; Puignou, Luis; Galceran, Maria Teresa

2006-09-29

Two in-line preconcentration capillary zone electrophoresis (CZE) methods (field amplified sample injection (FASI) and stacking with sample matrix removal (LVSS)) have been evaluated for the analysis of acrylamide (AA) in foodstuffs. To allow the determination of AA by CZE, it was derivatized using 2-mercaptobenzoic acid. For FASI, the optimum conditions were water at pH > or = 10 adjusted with NH3 as sample solvent, 35 s hydrodynamic injection (0.5 psi) of a water plug, 35 s of electrokinetic injection (-10 kV) of the sample, and 6s hydrodynamic injection (0.5 psi) of another water plug to prevent AA removal by EOF. In stacking with sample matrix removal, the reversal time was found to be around 3.3 min. A 40 mM phosphate buffer (pH 8.5) was used as carrier electrolyte for CZE separation in both cases. For both FASI and LVSS methods, linear calibration curves over the range studied (10-1000 microg L(-1) and 25-1000 microg L(-1), respectively), limit of detection (LOD) on standards (1 microg L(-1) for FASI and 7 microg L(-1) for LVSS), limit of detection on samples (3 ng g(-1) for FASI and 20 ng g(-1) for LVSS) and both run-to-run (up to 14% for concentration and 0.8% for time values) and day-to-day precisions (up to 16% and 5% for concentration and time values, respectively) were established. Due to the lower detection limits obtained with the FASI-CZE this method was applied to the analysis of AA in different foodstuffs such as biscuits, cereals, crisp bread, snacks and coffee, and the results were compared with those obtained by LC-MS/MS.

Thermal/optical methods for elemental carbon quantification in soils and urban dusts: equivalence of different analysis protocols.

PubMed

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method.

A new strategy for accelerated extraction of target compounds using molecularly imprinted polymer particles embedded in a paper-based disk.

PubMed

Zarejousheghani, Mashaalah; Schrader, Steffi; Möder, Monika; Schmidt, Matthias; Borsdorf, Helko

2018-03-01

In this study, a general simple and inexpensive method is introduced for the preparation of a paper-based selective disk-type solid phase extraction (SPE) technique, appropriate for fast and high throughput monitoring of target compounds. An ion exchange molecularly imprinted polymer (MIP) was synthesized for the extraction and analysis of acesulfame, an anthropogenic water quality marker. Acesulfame imprinting was used as an example for demonstrating the benefits of a nanosized, swellable MIP extraction sorbents integrated in an on-site compatible concept for water quality monitoring. Compared with an 8 mL standard SPE cartridge, the paper-based MIP disk (47 mm ø) format allowed (1) high sample flow rates up to 30 mL•min -1 without losing extraction efficiency (2) extracting sample volumes up to 500 mL in much shorter times than with standard SPE, (3) the reuse of the disks (up to 3 times more than SPE cartridge) due to high robustness and an efficient post-cleaning, and (4) reducing the sampling time from 100 minutes (using the standard SPE format) to about 2 minutes with the MIP paper disk for 50 mL water sample. Different parameters like cellulose fiber/polymer ratios, sample volume, sample flow-rate, washing, and elution conditions were evaluated and optimized. Using developed extraction technique with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, a new protocol was established that provides detection and quantification limits of 0.015 μg•L -1 and 0.05 μg•L -1 , respectively. The developed paper disks were used in-field for the selective extraction of target compounds and transferred to the laboratory for further analysis. Copyright © 2017 John Wiley & Sons, Ltd.

Off-line real-time FTIR analysis of a process step in imipenem production

NASA Astrophysics Data System (ADS)

Boaz, Jhansi R.; Thomas, Scott M.; Meyerhoffer, Steven M.; Staskiewicz, Steven J.; Lynch, Joseph E.; Egan, Richard S.; Ellison, Dean K.

1992-08-01

We have developed an FT-IR method, using a Spectra-Tech Monit-IR 400 systems, to monitor off-line the completion of a reaction in real-time. The reaction is moisture-sensitive and analysis by more conventional methods (normal-phase HPLC) is difficult to reproduce. The FT-IR method is based on the shift of a diazo band when a conjugated beta-diketone is transformed into a silyl enol ether during the reaction. The reaction mixture is examined directly by IR and does not require sample workup. Data acquisition time is less than one minute. The method has been validated for specificity, precision and accuracy. The results obtained by the FT-IR method for known mixtures and in-process samples compare favorably with those from a normal-phase HPLC method.

Smart Sampling and HPC-based Probabilistic Look-ahead Contingency Analysis Implementation and its Evaluation with Real-world Data

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

Chen, Yousu; Etingov, Pavel V.; Ren, Huiying

This paper describes a probabilistic look-ahead contingency analysis application that incorporates smart sampling and high-performance computing (HPC) techniques. Smart sampling techniques are implemented to effectively represent the structure and statistical characteristics of uncertainty introduced by different sources in the power system. They can significantly reduce the data set size required for multiple look-ahead contingency analyses, and therefore reduce the time required to compute them. High-performance-computing (HPC) techniques are used to further reduce computational time. These two techniques enable a predictive capability that forecasts the impact of various uncertainties on potential transmission limit violations. The developed package has been tested withmore » real world data from the Bonneville Power Administration. Case study results are presented to demonstrate the performance of the applications developed.« less

Detection of halogenated flame retardants in polyurethane foam by particle induced X-ray emission

NASA Astrophysics Data System (ADS)

Maley, Adam M.; Falk, Kyle A.; Hoover, Luke; Earlywine, Elly B.; Seymour, Michael D.; DeYoung, Paul A.; Blum, Arlene; Stapleton, Heather M.; Peaslee, Graham F.

2015-09-01

A novel application of particle-induced X-ray emission (PIXE) has been developed to detect the presence of chlorinated and brominated flame retardant chemicals in polyurethane foams. Traditional Gas Chromatography-Mass Spectrometry (GC-MS) methods for the detection and identification of halogenated flame retardants in foams require extensive sample preparation and data acquisition time. The elemental analysis of the halogens in polyurethane foam performed by PIXE offers the opportunity to identify the presence of halogenated flame retardants in a fraction of the time and sample preparation cost. Through comparative GC-MS and PIXE analysis of 215 foam samples, excellent agreement between the two methods was obtained. These results suggest that PIXE could be an ideal rapid screening method for the presence of chlorinated and brominated flame retardants in polyurethane foams.

Differentiating Organic and Conventional Sage by Chromatographic and Mass Spectrometry Flow-Injection Fingerprints Combined with Principal Component Analysis

PubMed Central

Gao, Boyan; Lu, Yingjian; Sheng, Yi; Chen, Pei; Yu, Liangli (Lucy)

2013-01-01

High performance liquid chromatography (HPLC) and flow injection electrospray ionization with ion trap mass spectrometry (FIMS) fingerprints combined with the principal component analysis (PCA) were examined for their potential in differentiating commercial organic and conventional sage samples. The individual components in the sage samples were also characterized with an ultra-performance liquid chromatography with a quadrupole-time of flight mass spectrometer (UPLC Q-TOF MS). The results suggested that both HPLC and FIMS fingerprints combined with PCA could differentiate organic and conventional sage samples effectively. FIMS may serve as a quick test capable of distinguishing organic and conventional sages in 1 min, and could potentially be developed for high-throughput applications; whereas HPLC fingerprints could provide more chemical composition information with a longer analytical time. PMID:23464755

Fast electrophoretic analysis of individual mitochondria using microchip capillary electrophoresis with laser induced fluorescence detection.

PubMed

Duffy, Ciarán F; MacCraith, Brian; Diamond, Dermot; O'Kennedy, Richard; Arriaga, Edgar A

2006-08-01

The analysis of mitochondria by capillary electrophoresis usually takes longer than 20 min per replicate which may compromise the quality of the mitochondria due to degradation. In addition, low sample consumption may be beneficial in the analysis of rare or difficult samples. In this report, we demonstrate the ability to analyze individual mitochondrial events in picoliter-volume samples (approximately 80 pL) taken from a bovine liver preparation using microchip capillary electrophoresis with laser-induced fluorescence detection (micro-chip CE-LIF). Using a commercial "double-T" glass microchip, the sample was electrokinetically loaded in the "double-T" intersection and then subjected to electrophoretic separation along the main separation channel. In order to decrease interactions of mitochondria with channel walls during the analysis, poly(vinyl alcohol) was used as a dynamic coating. This procedure eliminates the need for complicated covalent surface modifications within the channels that were previously used in capillary electrophoresis methods. For analysis, mitochondria, isolated from bovine liver tissue, were selectively labelled using 10-nonyl acridine orange (NAO). The results consist of electropherograms where each mitochondrial event is a narrow spike (240 +/- 44 ms). While the spike intensity is representative of its NAO content, its migration time is used to calculate and describe its electrophoretic mobility, which is a property still largely unexplored for intracellular organelles. The five-fold decrease in separation time (4 min for microchip versus 20 min for capillary electrophoresis) makes microchip electrophoretic separations of organelles a faster, sensitive, low-sample volume alternative for the characterization of individual organelle properties and for investigations of subcellular heterogeneity.

Power spectrum analysis for defect screening in integrated circuit devices

DOEpatents

Tangyunyong, Paiboon; Cole Jr., Edward I.; Stein, David J.

2011-12-01

A device sample is screened for defects using its power spectrum in response to a dynamic stimulus. The device sample receives a time-varying electrical signal. The power spectrum of the device sample is measured at one of the pins of the device sample. A defect in the device sample can be identified based on results of comparing the power spectrum with one or more power spectra of the device that have a known defect status.

Sampling and analyte enrichment strategies for ambient mass spectrometry.

PubMed

Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

2018-01-01

Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

Characterisation of volatile profile and sensory analysis of fresh-cut "Radicchio di Chioggia" stored in air or modified atmosphere.

PubMed

Cozzolino, Rosaria; Martignetti, Antonella; Pellicano, Mario Paolo; Stocchero, Matteo; Cefola, Maria; Pace, Bernardo; De Giulio, Beatrice

2016-02-01

The volatile profile of two hybrids of "Radicchio di Chioggia", Corelli and Botticelli, stored in air or passive modified atmosphere (MAP) during 12 days of cold storage, was monitored by solid phase micro-extraction (SPME) GC-MS. Botticelli samples were also subjected to sensory analysis. Totally, 61 volatile organic compounds (VOCs) were identified in the headspace of radicchio samples. Principal component analysis (PCA) showed that fresh product possessed a metabolic content similar to that of the MAP samples after 5 and 8 days of storage. Projection to latent structures by partial least squares (PLS) regression analysis showed the volatiles content of the samples varied depending only on the packaging conditions. Specifically, 12 metabolites describing the time evolution and explaining the effects of the different storage conditions were highlighted. Finally, a PCA analysis revealed that VOCs profile significantly correlated with sensory attributes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Comparison of nested-multiplex, Taqman & SYBR Green real-time PCR in diagnosis of amoebic liver abscess in a tertiary health care institute in India.

PubMed

Dinoop, K P; Parija, Subhash Chandra; Mandal, Jharna; Swaminathan, R P; Narayanan, P

2016-01-01

Amoebiasis is a common parasitic infection caused by Entamoeba histolytica and amoebic liver abscess (ALA) is the most common extraintestinal manifestation of amoebiasis. The aim of this study was to standardise real-time PCR assays (Taqman and SYBR Green) to detect E. histolytica from liver abscess pus and stool samples and compare its results with nested-multiplex PCR. Liver abscess pus specimens were subjected to DNA extraction. The extracted DNA samples were subjected to amplification by nested-multiplex PCR, Taqman (18S rRNA) and SYBR Green real-time PCR (16S-like rRNA assays to detect E. histolytica/E. dispar/E. moshkovskii). The amplification products were further confirmed by DNA sequence analysis. Receiver operator characteristic (ROC) curve analysis was done for nested-multiplex and SYBR Green real-time PCR and the area under the curve was calculated for evaluating the accuracy of the tests to dignose ALA. In all, 17, 19 and 25 liver abscess samples were positive for E. histolytica by nested-multiplex PCR, SYBR Green and Taqman real-time PCR assays, respectively. Significant differences in detection of E. histolytica were noted in the real-time PCR assays evaluated ( P<0.0001). The nested-multiplex PCR, SYBR Green real-time PCR and Taqman real-time PCR evaluated showed a positivity rate of 34, 38 and 50 per cent, respectively. Based on ROC curve analysis (considering Taqman real-time PCR as the gold standard), it was observed that SYBR Green real-time PCR was better than conventional nested-multiplex PCR for the diagnosis of ALA. Taqman real-time PCR targeting the 18S rRNA had the highest positivity rate evaluated in this study. Both nested multiplex and SYBR Green real-time PCR assays utilized were evaluated to give accurate results. Real-time PCR assays can be used as the gold standard in rapid and reliable diagnosis, and appropriate management of amoebiasis, replacing the conventional molecular methods.

New microfluidic-based sampling procedure for overcoming the hematocrit problem associated with dried blood spot analysis.

PubMed

Leuthold, Luc Alexis; Heudi, Olivier; Déglon, Julien; Raccuglia, Marc; Augsburger, Marc; Picard, Franck; Kretz, Olivier; Thomas, Aurélien

2015-02-17

Hematocrit (Hct) is one of the most critical issues associated with the bioanalytical methods used for dried blood spot (DBS) sample analysis. Because Hct determines the viscosity of blood, it may affect the spreading of blood onto the filter paper. Hence, accurate quantitative data can only be obtained if the size of the paper filter extracted contains a fixed blood volume. We describe for the first time a microfluidic-based sampling procedure to enable accurate blood volume collection on commercially available DBS cards. The system allows the collection of a controlled volume of blood (e.g., 5 or 10 μL) within several seconds. Reproducibility of the sampling volume was examined in vivo on capillary blood by quantifying caffeine and paraxanthine on 5 different extracted DBS spots at two different time points and in vitro with a test compound, Mavoglurant, on 10 different spots at two Hct levels. Entire spots were extracted. In addition, the accuracy and precision (n = 3) data for the Mavoglurant quantitation in blood with Hct levels between 26% and 62% were evaluated. The interspot precision data were below 9.0%, which was equivalent to that of a manually spotted volume with a pipet. No Hct effect was observed in the quantitative results obtained for Hct levels from 26% to 62%. These data indicate that our microfluidic-based sampling procedure is accurate and precise and that the analysis of Mavoglurant is not affected by the Hct values. This provides a simple procedure for DBS sampling with a fixed volume of capillary blood, which could eliminate the recurrent Hct issue linked to DBS sample analysis.

Characterization of the March 2017 Tank 15 Waste Removal Slurry Sample (Combination of Slurry Samples HTF-15-17-28 and HTF-15-17-29)

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

Reboul, S. H.; King, W. D.; Coleman, C. J.

2017-05-09

Two March 2017 Tank 15 slurry samples (HTF-15-17-28 and HTF-15-17-29) were collected during the second bulk waste removal campaign and submitted to SRNL for characterization. At SRNL, the two samples were combined and then characterized by a series of physical, elemental, radiological, and ionic analysis methods. Sludge settling as a function of time was also quantified. The characterization results reported in this document are consistent with expectations based upon waste type, process knowledge, comparisons between alternate analysis techniques, and comparisons with the characterization results obtained for the November 2016 Tank 15 slurry sample (the sample collected during the first bulkmore » waste removal campaign).« less

[High Precision Identification of Igneous Rock Lithology by Laser Induced Breakdown Spectroscopy].

PubMed

Wang, Chao; Zhang, Wei-gang; Yan, Zhi-quan

2015-09-01

In the field of petroleum exploration, lithology identification of finely cuttings sample, especially high precision identification of igneous rock with similar property, has become one of the geological problems. In order to solve this problem, a new method is proposed based on element analysis of Laser-Induced Breakdown Spectroscopy (LIBS) and Total Alkali versus Silica (TAS) diagram. Using independent LIBS system, factors influencing spectral signal, such as pulse energy, acquisition time delay, spectrum acquisition method and pre-ablation are researched through contrast experiments systematically. The best analysis conditions of igneous rock are determined: pulse energy is 50 mJ, acquisition time delay is 2 μs, the analysis result is integral average of 20 different points of sample's surface, and pre-ablation has been proved not suitable for igneous rock sample by experiment. The repeatability of spectral data is improved effectively. Characteristic lines of 7 elements (Na, Mg, Al, Si, K, Ca, Fe) commonly used for lithology identification of igneous rock are determined, and igneous rock samples of different lithology are analyzed and compared. Calibration curves of Na, K, Si are generated by using national standard series of rock samples, and all the linearly dependent coefficients are greater than 0.9. The accuracy of quantitative analysis is investigated by national standard samples. Element content of igneous rock is analyzed quantitatively by calibration curve, and its lithology is identified accurately by the method of TAS diagram, whose accuracy rate is 90.7%. The study indicates that LIBS can effectively achieve the high precision identification of the lithology of igneous rock.

Impact of proto-oncogene mutation detection in cytological specimens from thyroid nodules improves the diagnostic accuracy of cytology.

PubMed

Cantara, Silvia; Capezzone, Marco; Marchisotta, Stefania; Capuano, Serena; Busonero, Giulia; Toti, Paolo; Di Santo, Andrea; Caruso, Giuseppe; Carli, Anton Ferdinando; Brilli, Lucia; Montanaro, Annalisa; Pacini, Furio

2010-03-01

Fine-needle aspiration cytology (FNAC) is the gold standard for the differential diagnosis of thyroid nodules but has the limitation of inadequate sampling or indeterminate lesions. We aimed to verify whether search of thyroid cancer-associated protooncogene mutations in cytological samples may improve the diagnostic accuracy of FNAC. One hundred seventy-four consecutive patients undergoing thyroid surgery were submitted to FNAC (on 235 thyroid nodules) that was used for cytology and molecular analysis of BRAF, RAS, RET, TRK, and PPRgamma mutations. At surgery these nodules were sampled to perform the same molecular testing. Mutations were found in 67 of 235 (28.5%) cytological samples. Of the 67 mutated samples, 23 (34.3%) were mutated by RAS, 33 (49.3%) by BRAF, and 11 (16.4%) by RET/PTC. In 88.2% of the cases, the mutation was confirmed in tissue sample. The presence of mutations at cytology was associated with cancer 91.1% of the times and follicular adenoma 8.9% of the time. BRAF or RET/PTC mutations were always associated with cancer, whereas RAS mutations were mainly associated with cancer (74%) but also follicular adenoma (26%). The diagnostic performance of molecular analysis was superior to that of traditional cytology, with better sensitivity and specificity, and the combination of the two techniques further contributed to improve the total accuracy (93.2%), compared with molecular analysis (90.2%) or traditional cytology (83.0%). Our findings demonstrate that molecular analysis of cytological specimens is feasible and that its results in combination with cytology improves the diagnostic performance of traditional cytology.

Comparative analysis of techniques for evaluating the effectiveness of aircraft computing systems

NASA Technical Reports Server (NTRS)

Hitt, E. F.; Bridgman, M. S.; Robinson, A. C.

1981-01-01

Performability analysis is a technique developed for evaluating the effectiveness of fault-tolerant computing systems in multiphase missions. Performability was evaluated for its accuracy, practical usefulness, and relative cost. The evaluation was performed by applying performability and the fault tree method to a set of sample problems ranging from simple to moderately complex. The problems involved as many as five outcomes, two to five mission phases, permanent faults, and some functional dependencies. Transient faults and software errors were not considered. A different analyst was responsible for each technique. Significantly more time and effort were required to learn performability analysis than the fault tree method. Performability is inherently as accurate as fault tree analysis. For the sample problems, fault trees were more practical and less time consuming to apply, while performability required less ingenuity and was more checkable. Performability offers some advantages for evaluating very complex problems.

Statistical Symbolic Execution with Informed Sampling

NASA Technical Reports Server (NTRS)

Filieri, Antonio; Pasareanu, Corina S.; Visser, Willem; Geldenhuys, Jaco

2014-01-01

Symbolic execution techniques have been proposed recently for the probabilistic analysis of programs. These techniques seek to quantify the likelihood of reaching program events of interest, e.g., assert violations. They have many promising applications but have scalability issues due to high computational demand. To address this challenge, we propose a statistical symbolic execution technique that performs Monte Carlo sampling of the symbolic program paths and uses the obtained information for Bayesian estimation and hypothesis testing with respect to the probability of reaching the target events. To speed up the convergence of the statistical analysis, we propose Informed Sampling, an iterative symbolic execution that first explores the paths that have high statistical significance, prunes them from the state space and guides the execution towards less likely paths. The technique combines Bayesian estimation with a partial exact analysis for the pruned paths leading to provably improved convergence of the statistical analysis. We have implemented statistical symbolic execution with in- formed sampling in the Symbolic PathFinder tool. We show experimentally that the informed sampling obtains more precise results and converges faster than a purely statistical analysis and may also be more efficient than an exact symbolic analysis. When the latter does not terminate symbolic execution with informed sampling can give meaningful results under the same time and memory limits.

Determination of delorazepam in urine by solid-phase microextraction coupled to high performance liquid chromatography.

PubMed

Aresta, Antonella; Monaci, Linda; Zambonin, Carlo Giorgio

2002-06-01

An SPME-HPLC-UV method for the determination of delorazepam, a representative benzodiazepine, in spiked human urine samples was developed for the first time. The performances of two commercially available fibers, a carbowax/templated resin (Carbowax/TPR-100) and a polydimethylsiloxane/divinylbenzene (PDMS/DVB), were compared, indicating the latter as the most suitable for urine samples analysis. All the aspects influencing adsorption (extraction time, pH, temperature, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analyte on the fiber have been investigated. In particular, short extraction times were necessary to reach the equilibrium and very short desorption times were employed. The procedure required simple sample pre-treatment and was able to detect 5 ng/ml in spiked urine, regardless of the complexity of the matrix.

Isolation–By–Distance–and–Time in a stepping–stone model

PubMed Central

Duforet-Frebourg, Nicolas; Slatkin, Montgomery

2015-01-01

With the great advances in ancient DNA extraction, genetic data are now obtained from geographically separated individuals from both present and past. However, population genetics theory about the joint effect of space and time has not been thoroughly studied. Based on the classical stepping–stone model, we develop the theory of Isolation by Distance and Time. We derive the correlation of allele frequencies between demes in the case where ancient samples are present, and investigate the impact of edge effects with forward–in–time simulations. We also derive results about coalescent times in circular and toroidal models. As one of the most common ways to investigate population structure is principal components analysis (PCA), we evaluate the impact of our theory on PCA plots. Our results demonstrate that time between samples is an important factor. Ancient samples tend to be drawn to the center of a PCA plot. PMID:26592162

Cold-Curing Structural Epoxy Resins: Analysis of the Curing Reaction as a Function of Curing Time and Thickness

PubMed Central

Esposito Corcione, Carola; Freuli, Fabrizio; Frigione, Mariaenrica

2014-01-01

The curing reaction of a commercial cold-curing structural epoxy resin, specifically formulated for civil engineering applications, was analyzed by thermal analysis as a function of the curing time and the sample thickness. Original and remarkable results regarding the effects of curing time on the glass transition temperature and on the residual heat of reaction of the cold-cured epoxy were obtained. The influence of the sample thickness on the curing reaction of the cold-cured resin was also deeply investigated. A highly exothermal reaction, based on a self-activated frontal polymerization reaction, was supposed and verified trough a suitable temperature signal acquisition system, specifically realized for this measurement. This is one of the first studies carried out on the curing behavior of these peculiar cold-cured epoxy resins as a function of curing time and thickness. PMID:28788215

Cold-Curing Structural Epoxy Resins: Analysis of the Curing Reaction as a Function of Curing Time and Thickness.

PubMed

Corcione, Carola Esposito; Freuli, Fabrizio; Frigione, Mariaenrica

2014-09-22

The curing reaction of a commercial cold-curing structural epoxy resin, specifically formulated for civil engineering applications, was analyzed by thermal analysis as a function of the curing time and the sample thickness. Original and remarkable results regarding the effects of curing time on the glass transition temperature and on the residual heat of reaction of the cold-cured epoxy were obtained. The influence of the sample thickness on the curing reaction of the cold-cured resin was also deeply investigated. A highly exothermal reaction, based on a self-activated frontal polymerization reaction, was supposed and verified trough a suitable temperature signal acquisition system, specifically realized for this measurement. This is one of the first studies carried out on the curing behavior of these peculiar cold-cured epoxy resins as a function of curing time and thickness.

Laboratory heterogeneity of the lupus anticoagulant: a multicentre study using different clotting assays on a panel of 78 samples. Hemostasis Committee of the "Société Française de Biologie Clinique".

PubMed

1992-05-15

The laboratory heterogeneity of the lupus anticoagulant (LA) was investigated in a multicentre study using a panel of 78 plasma samples diagnosed as containing a LA. Consecutive samples were collected by 12 participants using various screening tests, and sent to 7 laboratories which performed one or more clotting assays among the following: activated partial thromboplastin time (APTT), dilute Russell viper venom time, kaolin clotting time (KCT), dilute tissue thromboplastin time (dTTI) and a platelet neutralization test. For APTT and dTTI, 10 versions of these tests including standard and mixing procedures were carried out. They varied by reagents, phospholipid concentration or methodology. Cut-off times were determined for each test by comparing the results of the panel to those of a control population. When the data of all clotting assays were pooled, 70 of the 78 selected plasmas were considered to contain LA, 15 of them having a low-titer inhibitor. Sensitivity, defined as the proportion of positive results among LA-containing plasmas, varied from 62 to 100% and was positively related to responsiveness (defined as the mean ratio of clotting time to cut-off time). Laboratory heterogeneity of LA-containing plasma was illustrated by a star symbol plot analysis. Different populations of samples, with LA preferentially recognized by one assay (or group of assays) irrespective of the overall sensitivity of this assay, were identified. Multiple component analysis demonstrated the heterogeneity of low-titer inhibitors, which complicates their recognition in routine laboratory investigation.

Clinical Usefulness of Real-Time Polymerase Chain Reaction for the Diagnosis of Vibrio vulnificus Infection Using Skin and Soft Tissues.

PubMed

Lee, Jun-Young; Kim, Seok Won; Kim, Dong-Min; Yun, Na Ra; Kim, Choon-Mee; Lee, Sang-Hong

2017-08-01

Vibrio vulnificus is a halophilic gram-negative bacillus isolated in seawater, fish, and shellfish. Infection by V. vulnificus is the most severe food-borne infection reported in the United States of America. Here, we aimed to examine the clinical usefulness of polymerase chain reaction (PCR) using tissue specimens other than blood samples as a diagnostic tool for V. vulnificus infection. A retrospective study was conducted with patients who underwent real-time PCR of toxR in both blood and skin tissues, including serum, bullae, swab, and operation room specimens, between 2006 and 2009. The median V. vulnificus DNA load of 14 patients in real-time PCR analysis of serum at the time of admission was 638.5 copies/mL blood, which was within the interquartile range (IQR: 37-3,225). In contrast, the median value by real-time PCR using the first tissue specimen at the time of admission was 16,650 copies/mL tissue fluid (IQR: 4,419-832,500). This difference was statistically significant ( P = 0.022). DNA copy numbers in tissues were less affected by short-term antibiotic administration than that in blood samples, and antibiotic administration increased the DNA copy number in some patients. We found, for the first time, that DNA copy numbers in tissues of patients infected by V. vulnificus were higher than those in blood samples. Additionally, skin lesions were more useful than blood samples as specimens for PCR analysis in patients administered antibiotics for V. vulnificus infection before admission.

[Matrix effect and application of field-amplified sample injection in the analysis of four tetracyclines in waters by capillary electrohoresis].

PubMed

2014-08-01

The system abilities of two chromatographic techniques, capillary electrophoresis (CE) and high performance liquid chromatography (HPLC), were compared for the analysis of four tetracyclines (tetracycline, chlorotetracycline, oxytetracycline and doxycycline). The pH, concentration of background electrolyte (BGE) were optimized for the analysis of the standard mixture sample, meanwhile, the effects of separation voltage and water matrix (pH value and hardness) effects were investigated. In hydrodynamic injection (HDI) mode, a good quantitative linearity and baseline separation within 9. 0 min were obtained for the four tetracyclines at the optimal conditions; the analytical time was about half of that of HPLC. The limits of detection (LODs) were in the range of 0. 28 - 0. 62 mg/L, and the relative standard deviations (RSDs) (n= 6) of migration time and peak area were 0. 42% - 0. 56% and 2. 24% - 2. 95%, respectively. The obtained recoveries spiked in tap water and fishpond water were at the ranges of 96. 3% - 107. 2% and 87. 1% - 105. 2%, respectively. In addition, the stacking method, field-amplified sample injection (FASI), was employed to improve the sensitivity, and the LOD was down to the range of 17.8-35.5 μg/L. With FASI stacking, the RSDs (n=6) of migration time and peak area were 0. 85%-0. 95% and 1. 69%-3.43%, respectively. Due to the advantages of simple sample pretreatment and fast speed, CE is promising in the analysis of the antibiotics in environmental water.

Evaluation and recommendation of sensitivity analysis methods for application to Stochastic Human Exposure and Dose Simulation models.

PubMed

Mokhtari, Amirhossein; Christopher Frey, H; Zheng, Junyu

2006-11-01

Sensitivity analyses of exposure or risk models can help identify the most significant factors to aid in risk management or to prioritize additional research to reduce uncertainty in the estimates. However, sensitivity analysis is challenged by non-linearity, interactions between inputs, and multiple days or time scales. Selected sensitivity analysis methods are evaluated with respect to their applicability to human exposure models with such features using a testbed. The testbed is a simplified version of a US Environmental Protection Agency's Stochastic Human Exposure and Dose Simulation (SHEDS) model. The methods evaluated include the Pearson and Spearman correlation, sample and rank regression, analysis of variance, Fourier amplitude sensitivity test (FAST), and Sobol's method. The first five methods are known as "sampling-based" techniques, wheras the latter two methods are known as "variance-based" techniques. The main objective of the test cases was to identify the main and total contributions of individual inputs to the output variance. Sobol's method and FAST directly quantified these measures of sensitivity. Results show that sensitivity of an input typically changed when evaluated under different time scales (e.g., daily versus monthly). All methods provided similar insights regarding less important inputs; however, Sobol's method and FAST provided more robust insights with respect to sensitivity of important inputs compared to the sampling-based techniques. Thus, the sampling-based methods can be used in a screening step to identify unimportant inputs, followed by application of more computationally intensive refined methods to a smaller set of inputs. The implications of time variation in sensitivity results for risk management are briefly discussed.

Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography-mass spectrometry analyses.

PubMed

Bicchi, Carlo; Liberto, Erica; Cagliero, Cecilia; Cordero, Chiara; Sgorbini, Barbara; Rubiolo, Patrizia

2008-11-28

The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host-guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm d(f)) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.

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

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ~10 3–10 4-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering andmore » analysis of phenylalanine hydroxylase fromChromobacterium violaceumcPAH,Trichinella spiralisdeubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied.« less

Analysis, fate studies and monitoring of the antifungal agent clotrimazole in the aquatic environment.

PubMed

Peschka, Manuela; Roberts, Paul H; Knepper, Thomas P

2007-10-01

The analysis and presence of clotrimazole, an antifungal agent with logK(OW) > 4, was thoroughly studied in the aquatic environment. For that reason analytical methods based on gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry were developed and validated to quantify clotrimazole with limits of quantification down to 5 and 1 ng/L, respectively. Both methods were compared in an intercalibration exercise. The complete mass-spectrometric fragmentation pattern could be elucidated with the aid of quadrupole time of flight mass spectrometry. Since clotrimazole tends to adsorb to laboratory glassware, studies on its adsorption behaviour were made to ensure the appropriate handling of water samples, e.g. pH, storage time, pretreatment of sampling vessels or material of the vials used for final extracts. The phenomena of adsorption to suspended matter were investigated while analysing different waste-water samples. Application of the methods in various investigated wastewater and surface water samples demonstrated that clotrimazole could only be detected in the low nanogram per litre range of anthropogenic influenced unfiltered water samples after acidification to pH 2.

High-throughput microcoil NMR of compound libraries using zero-dispersion segmented flow analysis.

PubMed

Kautz, Roger A; Goetzinger, Wolfgang K; Karger, Barry L

2005-01-01

An automated system for loading samples into a microcoil NMR probe has been developed using segmented flow analysis. This approach enhanced 2-fold the throughput of the published direct injection and flow injection methods, improved sample utilization 3-fold, and was applicable to high-field NMR facilities with long transfer lines between the sample handler and NMR magnet. Sample volumes of 2 microL (10-30 mM, approximately 10 microg) were drawn from a 96-well microtiter plate by a sample handler, then pumped to a 0.5-microL microcoil NMR probe as a queue of closely spaced "plugs" separated by an immiscible fluorocarbon fluid. Individual sample plugs were detected by their NMR signal and automatically positioned for stopped-flow data acquisition. The sample in the NMR coil could be changed within 35 s by advancing the queue. The fluorocarbon liquid wetted the wall of the Teflon transfer line, preventing the DMSO samples from contacting the capillary wall and thus reducing sample losses to below 5% after passage through the 3-m transfer line. With a wash plug of solvent between samples, sample-to-sample carryover was <1%. Significantly, the samples did not disperse into the carrier liquid during loading or during acquisitions of several days for trace analysis. For automated high-throughput analysis using a 16-second acquisition time, spectra were recorded at a rate of 1.5 min/sample and total deuterated solvent consumption was <0.5 mL (1 US dollar) per 96-well plate.

Direct quantification of lipopeptide biosurfactants in biological samples via HPLC and UPLC-MS requires sample modification with an organic solvent.

PubMed

Biniarz, Piotr; Łukaszewicz, Marcin

2017-06-01

The rapid and accurate quantification of biosurfactants in biological samples is challenging. In contrast to the orcinol method for rhamnolipids, no simple biochemical method is available for the rapid quantification of lipopeptides. Various liquid chromatography (LC) methods are promising tools for relatively fast and exact quantification of lipopeptides. Here, we report strategies for the quantification of the lipopeptides pseudofactin and surfactin in bacterial cultures using different high- (HPLC) and ultra-performance liquid chromatography (UPLC) systems. We tested three strategies for sample pretreatment prior to LC analysis. In direct analysis (DA), bacterial cultures were injected directly and analyzed via LC. As a modification, we diluted the samples with methanol and detected an increase in lipopeptide recovery in the presence of methanol. Therefore, we suggest this simple modification as a tool for increasing the accuracy of LC methods. We also tested freeze-drying followed by solvent extraction (FDSE) as an alternative for the analysis of "heavy" samples. In FDSE, the bacterial cultures were freeze-dried, and the resulting powder was extracted with different solvents. Then, the organic extracts were analyzed via LC. Here, we determined the influence of the extracting solvent on lipopeptide recovery. HPLC methods allowed us to quantify pseudofactin and surfactin with run times of 15 and 20 min per sample, respectively, whereas UPLC quantification was as fast as 4 and 5.5 min per sample, respectively. Our methods provide highly accurate measurements and high recovery levels for lipopeptides. At the same time, UPLC-MS provides the possibility to identify lipopeptides and their structural isoforms.

Comparative research of effectiveness of cellulose and fiberglass porous membrane carriers for bio sampling in veterinary and food industry monitoring

NASA Astrophysics Data System (ADS)

Gusev, Alexander; Vasyukova, Inna; Zakharova, Olga; Altabaeva, Yuliya; Saushkin, Nikolai; Samsonova, Jeanne; Kondakov, Sergey; Osipov, Alexander; Snegin, Eduard

2017-11-01

The aim of proposed research is to study the applicability of fiberglass porous membrane materials in a new strip format for dried blood storage in food industry monitoring. A comparative analysis of cellulosic and fiberglass porous membrane materials was carried out to obtain dried samples of serum or blood and the possibility of further species-specific analysis. Blood samples of Sus scrofa were used to study the comparative effectiveness of cellulose and fiberglass porous membrane carriers for long-term biomaterial storage allowing for further DNA detection by real-time polymerase chain reaction (PCR) method. Scanning electron microscopy of various membranes - native and with blood samples - indicate a fundamental difference in the form of dried samples. Membranes based on cellulosic materials sorb the components of the biological fluid on the surface of the fibers of their structure, partially penetrating the cellulose fibers, while in the case of glass fiber membranes the components of the biological fluid dry out as films in the pores of the membrane between the structural filaments. This fundamental difference in the retention mechanisms affects the rate of dissolution of the components of dry samples and contributes to an increase in the efficiency of the desorption process of the sample before subsequent analysis. Detecting of pig DNA in every analyzed sample under the performed Real-time PCR as well as good state of the biomaterial preservation on the glass fiber membranes was clearly demonstrated. Good biomaterials preservation has been revealed on the test cards for 4 days as well as for 1 hour.

[Application of fingerprint chromatogram in quality assessment of apple cider].

PubMed

Xu, Kangzhen; Song, Jirong; Ren, Yinghui; Ma, Haixia; Huang, Jie; Du, Xiaodan

2007-01-01

Fingerprints of 14 apple cider samples from different manufacturers were studied using high performance liquid chromatography (HPLC) with an electrochemical detector (ECD). The analysis was carried out on a Zorbax SB-C18 column at 30 degrees C with 2% (v/v) methanol aqueous solution-4% (v/v) acetic acid aqueous solution as mobile phase at a flow rate of 0.8 mL/min. The electrochemical detector was set at 0.7 V. By calculating the relative retention times of certain peaks with chlorogenic acid as the reference standard, 8 common peaks in the samples were analyzed. Relative retention times for the common peaks of various samples were calculated, and the similarities of all the samples were figured out through each peak area with the vectorial angle cosine method and correlative coefficient method. The results indicated that apple cider products of the same manufacturer have good similarity, with the similarities greater than 92.7%. According to this experiment, effectual microcosmic information for apple cider analysis was gained through HPLC and ECD. Moreover, this test method will help the analysis and the control of product quality, the development of new products and the establishment of trade standard.

Metagenomic analysis of bat guano samples revealed the presence of viruses potentially carried by insects, among others by Apis mellifera in Hungary.

PubMed

Zana, Brigitta; Kemenesi, Gábor; Urbán, Péter; Földes, Fanni; Görföl, Tamás; Estók, Péter; Boldogh, Sándor; Kurucz, Kornélia; Jakab, Ferenc

2018-03-01

The predominance of dietary viruses in bat guano samples had been described recently, suggesting a new opportunity to survey the prevalence and to detect new viruses of arthropods or even plant-infecting viruses circulating locally in the ecosystem. Here we describe the diversity of viruses belonging to the order Picornavirales in Hungarian insectivorous bat guano samples. The metagenomic analysis conducted on our samples has revealed the significant predominance of aphid lethal paralysis virus (ALPV) and Big Sioux River virus (BSRV) in Hungary for the first time. Phylogenetic analysis was used to clarify the relationship to previously identified ALPV strains infecting honey bees, showing that our strain possesses a close genetic relationship with the strains that have already been described as pathogenic to honey bees. Furthermore, studies have previously confirmed the ability of these viruses to replicate in adult honey bees; however, no signs related to these viruses have been revealed yet. With the identification of two recently described possibly honey bee infecting viruses for the first time in Hungary, our results might have importance for the health conditions of Hungarian honey bee colonies in the future.

Global analysis of microscopic fluorescence lifetime images using spectral segmentation and a digital micromirror spatial illuminator.

PubMed

Bednarkiewicz, Artur; Whelan, Maurice P

2008-01-01

Fluorescence lifetime imaging (FLIM) is very demanding from a technical and computational perspective, and the output is usually a compromise between acquisition/processing time and data accuracy and precision. We present a new approach to acquisition, analysis, and reconstruction of microscopic FLIM images by employing a digital micromirror device (DMD) as a spatial illuminator. In the first step, the whole field fluorescence image is collected by a color charge-coupled device (CCD) camera. Further qualitative spectral analysis and sample segmentation are performed to spatially distinguish between spectrally different regions on the sample. Next, the fluorescence of the sample is excited segment by segment, and fluorescence lifetimes are acquired with a photon counting technique. FLIM image reconstruction is performed by either raster scanning the sample or by directly accessing specific regions of interest. The unique features of the DMD illuminator allow the rapid on-line measurement of global good initial parameters (GIP), which are supplied to the first iteration of the fitting algorithm. As a consequence, a decrease of the computation time required to obtain a satisfactory quality-of-fit is achieved without compromising the accuracy and precision of the lifetime measurements.

SaDA: From Sampling to Data Analysis-An Extensible Open Source Infrastructure for Rapid, Robust and Automated Management and Analysis of Modern Ecological High-Throughput Microarray Data.

PubMed

Singh, Kumar Saurabh; Thual, Dominique; Spurio, Roberto; Cannata, Nicola

2015-06-03

One of the most crucial characteristics of day-to-day laboratory information management is the collection, storage and retrieval of information about research subjects and environmental or biomedical samples. An efficient link between sample data and experimental results is absolutely important for the successful outcome of a collaborative project. Currently available software solutions are largely limited to large scale, expensive commercial Laboratory Information Management Systems (LIMS). Acquiring such LIMS indeed can bring laboratory information management to a higher level, but most of the times this requires a sufficient investment of money, time and technical efforts. There is a clear need for a light weighted open source system which can easily be managed on local servers and handled by individual researchers. Here we present a software named SaDA for storing, retrieving and analyzing data originated from microorganism monitoring experiments. SaDA is fully integrated in the management of environmental samples, oligonucleotide sequences, microarray data and the subsequent downstream analysis procedures. It is simple and generic software, and can be extended and customized for various environmental and biomedical studies.

Contamination Analysis Tools

NASA Technical Reports Server (NTRS)

Brieda, Lubos

2015-01-01

This talk presents 3 different tools developed recently for contamination analysis:HTML QCM analyzer: runs in a web browser, and allows for data analysis of QCM log filesJava RGA extractor: can load in multiple SRS.ana files and extract pressure vs. time dataC++ Contamination Simulation code: 3D particle tracing code for modeling transport of dust particulates and molecules. Uses residence time to determine if molecules stick. Particulates can be sampled from IEST-STD-1246 and be accelerated by aerodynamic forces.

Volatile organic compounds: sampling methods and their worldwide profile in ambient air.

PubMed

Kumar, Anuj; Víden, Ivan

2007-08-01

The atmosphere is a particularly difficult analytical system because of the very low levels of substances to be analysed, sharp variations in pollutant levels with time and location, differences in wind, temperature and humidity. This makes the selection of an efficient sampling technique for air analysis a key step to reliable results. Generally, methods for volatile organic compounds sampling include collection of the whole air or preconcentration of samples on adsorbents. All the methods vary from each other according to the sampling technique, type of sorbent, method of extraction and identification technique. In this review paper we discuss various important aspects for sampling of volatile organic compounds by the widely used and advanced sampling methods. Characteristics of various adsorbents used for VOCs sampling are also described. Furthermore, this paper makes an effort to comprehensively review the concentration levels of volatile organic compounds along with the methodology used for analysis, in major cities of the world.

Literature Reference for Toxoplasma gondii (Applied and Environmental Microbiology. 2004. 70(7): 4035–4039)

EPA Pesticide Factsheets

Procedures are described for analysis of water samples and may be adapted for assessment of solid, particulate and liquid samples. The method uses real-time PCR assay for detecting Toxoplasma gondii DNA using gene-specific primers and probe.

Parallel replica dynamics method for bistable stochastic reaction networks: Simulation and sensitivity analysis

NASA Astrophysics Data System (ADS)

Wang, Ting; Plecháč, Petr

2017-12-01

Stochastic reaction networks that exhibit bistable behavior are common in systems biology, materials science, and catalysis. Sampling of stationary distributions is crucial for understanding and characterizing the long-time dynamics of bistable stochastic dynamical systems. However, simulations are often hindered by the insufficient sampling of rare transitions between the two metastable regions. In this paper, we apply the parallel replica method for a continuous time Markov chain in order to improve sampling of the stationary distribution in bistable stochastic reaction networks. The proposed method uses parallel computing to accelerate the sampling of rare transitions. Furthermore, it can be combined with the path-space information bounds for parametric sensitivity analysis. With the proposed methodology, we study three bistable biological networks: the Schlögl model, the genetic switch network, and the enzymatic futile cycle network. We demonstrate the algorithmic speedup achieved in these numerical benchmarks. More significant acceleration is expected when multi-core or graphics processing unit computer architectures and programming tools such as CUDA are employed.

Wetlab-2 - Quantitative PCR Tools for Spaceflight Studies of Gene Expression Aboard the International Space Station

NASA Technical Reports Server (NTRS)

Schonfeld, Julie E.

2015-01-01

Wetlab-2 is a research platform for conducting real-time quantitative gene expression analysis aboard the International Space Station. The system enables spaceflight genomic studies involving a wide variety of biospecimen types in the unique microgravity environment of space. Currently, gene expression analyses of space flown biospecimens must be conducted post flight after living cultures or frozen or chemically fixed samples are returned to Earth from the space station. Post-flight analysis is limited for several reasons. First, changes in gene expression can be transient, changing over a timescale of minutes. The delay between sampling on Earth can range from days to months, and RNA may degrade during this period of time, even in fixed or frozen samples. Second, living organisms that return to Earth may quickly re-adapt to terrestrial conditions. Third, forces exerted on samples during reentry and return to Earth may affect results. Lastly, follow up experiments designed in response to post-flight results must wait for a new flight opportunity to be tested.

Modeling and optimization of red currants vacuum drying process by response surface methodology (RSM).

PubMed

Šumić, Zdravko; Vakula, Anita; Tepić, Aleksandra; Čakarević, Jelena; Vitas, Jasmina; Pavlić, Branimir

2016-07-15

Fresh red currants were dried by vacuum drying process under different drying conditions. Box-Behnken experimental design with response surface methodology was used for optimization of drying process in terms of physical (moisture content, water activity, total color change, firmness and rehydratation power) and chemical (total phenols, total flavonoids, monomeric anthocyanins and ascorbic acid content and antioxidant activity) properties of dried samples. Temperature (48-78 °C), pressure (30-330 mbar) and drying time (8-16 h) were investigated as independent variables. Experimental results were fitted to a second-order polynomial model where regression analysis and analysis of variance were used to determine model fitness and optimal drying conditions. The optimal conditions of simultaneously optimized responses were temperature of 70.2 °C, pressure of 39 mbar and drying time of 8 h. It could be concluded that vacuum drying provides samples with good physico-chemical properties, similar to lyophilized sample and better than conventionally dried sample. Copyright © 2016 Elsevier Ltd. All rights reserved.

Evaluation of magnetic nanoparticle samples made from biocompatible ferucarbotran by time-correlation magnetic particle imaging reconstruction method

PubMed Central

2013-01-01

Background Molecular imaging using magnetic nanoparticles (MNPs)—magnetic particle imaging (MPI)—has attracted interest for the early diagnosis of cancer and cardiovascular disease. However, because a steep local magnetic field distribution is required to obtain a defined image, sophisticated hardware is required. Therefore, it is desirable to realize excellent image quality even with low-performance hardware. In this study, the spatial resolution of MPI was evaluated using an image reconstruction method based on the correlation information of the magnetization signal in a time domain and by applying MNP samples made from biocompatible ferucarbotran that have adjusted particle diameters. Methods The magnetization characteristics and particle diameters of four types of MNP samples made from ferucarbotran were evaluated. A numerical analysis based on our proposed method that calculates the image intensity from correlation information between the magnetization signal generated from MNPs and the system function was attempted, and the obtained image quality was compared with that using the prototype in terms of image resolution and image artifacts. Results MNP samples obtained by adjusting ferucarbotran showed superior properties to conventional ferucarbotran samples, and numerical analysis showed that the same image quality could be obtained using a gradient magnetic field generator with 0.6 times the performance. However, because image blurring was included theoretically by the proposed method, an algorithm will be required to improve performance. Conclusions MNP samples obtained by adjusting ferucarbotran showed magnetizing properties superior to conventional ferucarbotran samples, and by using such samples, comparable image quality (spatial resolution) could be obtained with a lower gradient magnetic field intensity. PMID:23734917

High throughput integrated thermal characterization with non-contact optical calorimetry

NASA Astrophysics Data System (ADS)

Hou, Sichao; Huo, Ruiqing; Su, Ming

2017-10-01

Commonly used thermal analysis tools such as calorimeter and thermal conductivity meter are separated instruments and limited by low throughput, where only one sample is examined each time. This work reports an infrared based optical calorimetry with its theoretical foundation, which is able to provide an integrated solution to characterize thermal properties of materials with high throughput. By taking time domain temperature information of spatially distributed samples, this method allows a single device (infrared camera) to determine the thermal properties of both phase change systems (melting temperature and latent heat of fusion) and non-phase change systems (thermal conductivity and heat capacity). This method further allows these thermal properties of multiple samples to be determined rapidly, remotely, and simultaneously. In this proof-of-concept experiment, the thermal properties of a panel of 16 samples including melting temperatures, latent heats of fusion, heat capacities, and thermal conductivities have been determined in 2 min with high accuracy. Given the high thermal, spatial, and temporal resolutions of the advanced infrared camera, this method has the potential to revolutionize the thermal characterization of materials by providing an integrated solution with high throughput, high sensitivity, and short analysis time.

Selected Physical Properties of 2-Chloroethyl-3-Chloropropyl Sulfide (CECPRS)

DTIC Science & Technology

2010-10-01

Analysis * For this work, a TA Instruments 910 Differential Scanning Calorimeter and 2200 Controller were used. Prior to sample measurements, the DSC...controlled mass flow rate over a known time, concentrated, and the mass quantified by GC-FID analysis . This step enables vapor pressure measurements for low...Bellefonte, PA), with a 1.0 (im RTx-1 ( polydimethylsiloxane ) stationary phase, was maintained at 40 °C for 2 min following sample introduction, then heated

Test plan for evaluating the operational performance of the prototype nested, fixed-depth fluidic sampler

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

REICH, F.R.

The PHMC will provide Low Activity Wastes (LAW) tank wastes for final treatment by a privatization contractor from two double-shell feed tanks, 241-AP-102 and 241-AP-104. Concerns about the inability of the baseline ''grab'' sampling to provide large volume samples within time constraints has led to the development of a nested, fixed-depth sampling system. This sampling system will provide large volume, representative samples without the environmental, radiation exposure, and sample volume impacts of the current base-line ''grab'' sampling method. A plan has been developed for the cold testing of this nested, fixed-depth sampling system with simulant materials. The sampling system willmore » fill the 500-ml bottles and provide inner packaging to interface with the Hanford Sites cask shipping systems (PAS-1 and/or ''safe-send''). The sampling system will provide a waste stream that will be used for on-line, real-time measurements with an at-tank analysis system. The cold tests evaluate the performance and ability to provide samples that are representative of the tanks' content within a 95 percent confidence interval, to sample while mixing pumps are operating, to provide large sample volumes (1-15 liters) within a short time interval, to sample supernatant wastes with over 25 wt% solids content, to recover from precipitation- and settling-based plugging, and the potential to operate over the 20-year expected time span of the privatization contract.« less

Isotopic composition analysis and age dating of uranium samples by high resolution gamma ray spectrometry

NASA Astrophysics Data System (ADS)

Apostol, A. I.; Pantelica, A.; Sima, O.; Fugaru, V.

2016-09-01

Non-destructive methods were applied to determine the isotopic composition and the time elapsed since last chemical purification of nine uranium samples. The applied methods are based on measuring gamma and X radiations of uranium samples by high resolution low energy gamma spectrometric system with planar high purity germanium detector and low background gamma spectrometric system with coaxial high purity germanium detector. The ;Multigroup γ-ray Analysis Method for Uranium; (MGAU) code was used for the precise determination of samples' isotopic composition. The age of the samples was determined from the isotopic ratio 214Bi/234U. This ratio was calculated from the analyzed spectra of each uranium sample, using relative detection efficiency. Special attention is paid to the coincidence summing corrections that have to be taken into account when performing this type of analysis. In addition, an alternative approach for the age determination using full energy peak efficiencies obtained by Monte Carlo simulations with the GESPECOR code is described.

The Laser Ablation Ion Funnel: Sampling for in situ Mass Spectrometry on Mars

NASA Technical Reports Server (NTRS)

Johnson, Paul V.; Hodyss, Robert; Tang, Keqi; Brinckerhoff, William B.; Smith, Richard D.

2011-01-01

A considerable investment has been made by NASA and other space agencies to develop instrumentation suitable for in situ analytical investigation of extra terrestrial bodies including various mass spectrometers (time-of-flight, quadrupole ion trap, quadrupole mass filters, etc.). However, the front-end sample handling that is needed to collect and prepare samples for interrogation by such instrumentation remains underdeveloped. Here we describe a novel approach tailored to the exploration of Mars where ions are created in the ambient atmosphere via laser ablation and then efficiently transported into a mass spectrometer for in situ analysis using an electrodynamic ion funnel. This concept would enable elemental and isotopic analysis of geological samples with the analysis of desorbed organic material a possibility as well. Such an instrument would be suitable for inclusion on all potential missions currently being considered such as the Mid-Range Rover, the Astrobiology Field Laboratory, and Mars Sample Return (i.e., as a sample pre-selection triage instrument), among others.

Comparative analysis of laparoscopic and ultrasound-guided biopsy methods for gene expression analysis in transgenic goats.

PubMed

Melo, C H; Sousa, F C; Batista, R I P T; Sanchez, D J D; Souza-Fabjan, J M G; Freitas, V J F; Melo, L M; Teixeira, D I A

2015-07-31

The present study aimed to compare laparoscopic (LP) and ultrasound-guided (US) biopsy methods to obtain either liver or splenic tissue samples for ectopic gene expression analysis in transgenic goats. Tissue samples were collected from human granulocyte colony stimulating factor (hG-CSF)-transgenic bucks and submitted to real-time PCR for the endogenous genes (Sp1, Baff, and Gapdh) and the transgene (hG-CSF). Both LP and US biopsy methods were successful in obtaining liver and splenic samples that could be analyzed by PCR (i.e., sufficient sample sizes and RNA yield were obtained). Although the number of attempts made to obtain the tissue samples was similar (P > 0.05), LP procedures took considerably longer than the US method (P = 0.03). Finally, transgene transcripts were not detected in spleen or liver samples. Thus, for the phenotypic characterization of a transgenic goat line, investigation of ectopic gene expression can be made successfully by LP or US biopsy, avoiding the traditional approach of euthanasia.

The use of wavelength dispersive X-ray fluorescence in the identification of the elemental composition of vanilla samples and the determination of the geographic origin by discriminant function analysis.

PubMed

Hondrogiannis, Ellen; Rotta, Kathryn; Zapf, Charles M

2013-03-01

Sixteen elements found in 37 vanilla samples from Madagascar, Uganda, India, Indonesia (all Vanilla planifolia species), and Papa New Guinea (Vanilla tahitensis species) were measured by wavelength dispersive X-ray fluorescence (WDXRF) spectroscopy for the purpose of determining the elemental concentrations to discriminate among the origins. Pellets were prepared of the samples and elemental concentrations were calculated based on calibration curves created using 4 Natl. Inst. of Standards and Technology (NIST) standards. Discriminant analysis was used to successfully classify the vanilla samples by their species and their geographical region. Our method allows for higher throughput in the rapid screening of vanilla samples in less time than analytical methods currently available. Wavelength dispersive X-ray fluorescence spectroscopy and discriminant function analysis were used to classify vanilla from different origins resulting in a model that could potentially serve to rapidly validate these samples before purchasing from a producer. © 2013 Institute of Food Technologists®

Real-time PCR detection of Plasmodium directly from whole blood and filter paper samples

PubMed Central

2011-01-01

Background Real-time PCR is a sensitive and specific method for the analysis of Plasmodium DNA. However, prior purification of genomic DNA from blood is necessary since PCR inhibitors and quenching of fluorophores from blood prevent efficient amplification and detection of PCR products. Methods Reagents designed to specifically overcome PCR inhibition and quenching of fluorescence were evaluated for real-time PCR amplification of Plasmodium DNA directly from blood. Whole blood from clinical samples and dried blood spots collected in the field in Colombia were tested. Results Amplification and fluorescence detection by real-time PCR were optimal with 40× SYBR® Green dye and 5% blood volume in the PCR reaction. Plasmodium DNA was detected directly from both whole blood and dried blood spots from clinical samples. The sensitivity and specificity ranged from 93-100% compared with PCR performed on purified Plasmodium DNA. Conclusions The methodology described facilitates high-throughput testing of blood samples collected in the field by fluorescence-based real-time PCR. This method can be applied to a broad range of clinical studies with the advantages of immediate sample testing, lower experimental costs and time-savings. PMID:21851640

Multicapillary Gas Chromatography-Temperature Modulated Metal Oxide Semiconductor Sensors Array Detector for Monitoring of Volatile Organic Compounds in Closed Atmosphere Using Gaussian Apodization Factor Analysis.

PubMed

Alinoori, Amir Hossein; Masoum, Saeed

2018-05-22

A unique metal oxide semiconductor sensor (MOS) array detector with eight sensors was designed and fabricated in a PTFE chamber as an interface for coupling with multicapillary gas chromatography. This design consists of eight transfer lines with equal length between the multicapillary columns (MCC) and sensors. The deactivated capillary columns were passed through each transfer line and homemade flow splitter to distribute the same gas flow on each sensor. Using the eight ports flow splitter design helps us to equal the length of carrier gas path and flow for each sensor, minimizing the dead volume of the sensor's chamber and increasing chromatographic resolution. In addition to coupling of MCC to MOS array detector and other considerations in hardware design, modulation of MOS temperature was used to increase sensitivity and selectivity, and data analysis was enhanced with adapted Gaussian apodization factor analysis (GAFA) as a multivariate curve resolution algorithm. Continues air sampling and injecting system (CASI) design provides a fast and easily applied method for continues injection of air sample with no additional sample preparation. The analysis cycle time required for each run is less than 300 s. The high sample load and sharp injection with the fast separation by MCC decrease the peak widths and improve detection limits. This homemade customized instrument is an alternative to other time-consuming and expensive technologies for continuous monitoring of outgassing in air samples.

Agreement in DNA methylation levels from the Illumina 450K array across batches, tissues, and time

PubMed Central

Forest, Marie; O'Donnell, Kieran J.; Voisin, Greg; Gaudreau, Helene; MacIsaac, Julia L.; McEwen, Lisa M.; Silveira, Patricia P.; Steiner, Meir; Kobor, Michael S.; Meaney, Michael J.; Greenwood, Celia M.T.

2018-01-01

ABSTRACT Epigenome-wide association studies (EWAS) have focused primarily on DNA methylation as a chemically stable and functional epigenetic modification. However, the stability and accuracy of the measurement of methylation in different tissues and extraction types is still being actively studied, and the longitudinal stability of DNA methylation in commonly studied peripheral tissues is of great interest. Here, we used data from two studies, three tissue types, and multiple time points to assess the stability of DNA methylation measured with the Illumina Infinium HumanMethylation450 BeadChip array. Redundancy analysis enabled visual assessment of agreement of replicate samples overall and showed good agreement after removing effects of tissue type, age, and sex. At the probe level, analysis of variance contrasts separating technical and biological replicates clearly showed better agreement between technical replicates versus longitudinal samples, and suggested increased stability for buccal cells versus blood or blood spots. Intraclass correlations (ICCs) demonstrated that inter-individual variability is of similar magnitude to within-sample variability at many probes; however, as inter-individual variability increased, so did ICC. Furthermore, we were able to demonstrate decreasing agreement in methylation levels with time, despite a maximal sampling interval of only 576 days. Finally, at 6 popular candidate genes, there was a large range of stability across probes. Our findings highlight important sources of technical and biological variation in DNA methylation across different tissues over time. These data will help to inform longitudinal sampling strategies of future EWAS. PMID:29381404

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.

Research of mine water source identification based on LIF technology

NASA Astrophysics Data System (ADS)

Zhou, Mengran; Yan, Pengcheng

2016-09-01

According to the problem that traditional chemical methods to the mine water source identification takes a long time, put forward a method for rapid source identification system of mine water inrush based on the technology of laser induced fluorescence (LIF). Emphatically analyzes the basic principle of LIF technology. The hardware composition of LIF system are analyzed and the related modules were selected. Through the fluorescence experiment with the water samples of coal mine in the LIF system, fluorescence spectra of water samples are got. Traditional water source identification mainly according to the ion concentration representative of the water, but it is hard to analysis the ion concentration of the water from the fluorescence spectra. This paper proposes a simple and practical method of rapid identification of water by fluorescence spectrum, which measure the space distance between unknown water samples and standard samples, and then based on the clustering analysis, the category of the unknown water sample can be get. Water source identification for unknown samples verified the reliability of the LIF system, and solve the problem that the current coal mine can't have a better real-time and online monitoring on water inrush, which is of great significance for coal mine safety in production.

13C cell wall enrichment and ionic liquid NMR analysis: progress towards a high-throughput detailed chemical analysis of the whole plant cell wall.

PubMed

Foston, Marcus; Samuel, Reichel; Ragauskas, Arthur J

2012-09-07

The ability to accurately and rapidly measure plant cell wall composition, relative monolignol content and lignin-hemicellulose inter-unit linkage distributions has become essential to efforts centered on reducing the recalcitrance of biomass by genetic engineering. Growing (13)C enriched transgenic plants is a viable route to achieve the high-throughput, detailed chemical analysis of whole plant cell wall before and after pretreatment and microbial or enzymatic utilization by (13)C nuclear magnetic resonance (NMR) in a perdeuterated ionic liquid solvent system not requiring component isolation. 1D (13)C whole cell wall ionic liquid NMR of natural abundant and (13)C enriched corn stover stem samples suggest that a high level of uniform labeling (>97%) can significantly reduce the total NMR experiment times up to ~220 times. Similarly, significant reduction in total NMR experiment time (~39 times) of the (13)C enriched corn stover stem samples for 2D (13)C-(1)H heteronuclear single quantum coherence NMR was found.

Ultra-high-performance supercritical fluid chromatography with quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS) for analysis of lignin-derived monomeric compounds in processed lignin samples.

PubMed

Prothmann, Jens; Sun, Mingzhe; Spégel, Peter; Sandahl, Margareta; Turner, Charlotta

2017-12-01

The conversion of lignin to potentially high-value low molecular weight compounds often results in complex mixtures of monomeric and oligomeric compounds. In this study, a method for the quantitative and qualitative analysis of 40 lignin-derived compounds using ultra-high-performance supercritical fluid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS) has been developed. Seven different columns were explored for maximum selectivity. Makeup solvent composition and ion source settings were optimised using a D-optimal design of experiment (DoE). Differently processed lignin samples were analysed and used for the method validation. The new UHPSFC/QTOF-MS method showed good separation of the 40 compounds within only 6-min retention time, and out of these, 36 showed high ionisation efficiency in negative electrospray ionisation mode. Graphical abstract A rapid and selective method for the quantitative and qualitative analysis of 40 lignin-derived compounds using ultra-high-performance supercritical fluid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS).

Risk profiles and peer violence in the context of school and leisure time.

PubMed

Pulido Valero, Rosa; Martín Seoane, Gema; Lucas Molina, Beatriz

2011-11-01

Though violence at school is by no means a new phenomenon, there has been growing social and scientific concern about this issue in recent years. The present study builds on prior analysis of the roles adolescents play in peer harassment, and the relationship between violence occurring at school and during free time. A representative sample of students between the ages of 14 and 18 was selected in the Community of Madrid (N = 1622) through random cluster sampling (school was the unit of analysis). Participants completed the C.E.V.E.O. questionnaire, which presents fifteen situations involving peer violence. The results reveal a relationship between violent situations occurring at school and during free time, and between the roles of aggressor and victim during free time. A profile analysis yielded three different categories: the "minimal violence exposure" type (1126 adolescents), the "psychological violence exposure" type (413 adolescents), and the "high risk of violence" type (83 adolescents). Judging from these results, we posit that interventions must be designed which tailor to each group and their respective risk situations.

Comparative study of two protocols for quantitative image-analysis of serotonin transporter clustering in lymphocytes, a putative biomarker of therapeutic efficacy in major depression.

PubMed

Romay-Tallon, Raquel; Rivera-Baltanas, Tania; Allen, Josh; Olivares, Jose M; Kalynchuk, Lisa E; Caruncho, Hector J

2017-01-01

The pattern of serotonin transporter clustering on the plasma membrane of lymphocytes extracted from human whole blood samples has been identified as a putative biomarker of therapeutic efficacy in major depression. Here we evaluated the possibility of performing a similar analysis using blood smears obtained from rats, and from control human subjects and depression patients. We hypothesized that we could optimize a protocol to make the analysis of serotonin protein clustering in blood smears comparable to the analysis of serotonin protein clustering using isolated lymphocytes. Our data indicate that blood smears require a longer fixation time and longer times of incubation with primary and secondary antibodies. In addition, one needs to optimize the image analysis settings for the analysis of smears. When these steps are followed, the quantitative analysis of both the number and size of serotonin transporter clusters on the plasma membrane of lymphocytes is similar using both blood smears and isolated lymphocytes. The development of this novel protocol will greatly facilitate the collection of appropriate samples by eliminating the necessity and cost of specialized personnel for drawing blood samples, and by being a less invasive procedure. Therefore, this protocol will help us advance the validation of membrane protein clustering in lymphocytes as a biomarker of therapeutic efficacy in major depression, and bring it closer to its clinical application.

Evaluation of PLS, LS-SVM, and LWR for quantitative spectroscopic analysis of soils

USDA-ARS?s Scientific Manuscript database

Soil testing requires the analysis of large numbers of samples in laboratory that are often time consuming and expensive. Mid-infrared spectroscopy (mid-IR) and near-infrared spectroscopy (NIRS) are fast, non-destructive, and inexpensive analytical methods that have been used for soil analysis, in l...

Spatially resolved δ13C analysis using laser ablation isotope ratio mass spectrometry

NASA Astrophysics Data System (ADS)

Moran, J.; Riha, K. M.; Nims, M. K.; Linley, T. J.; Hess, N. J.; Nico, P. S.

2014-12-01

Inherent geochemical, organic matter, and microbial heterogeneity over small spatial scales can complicate studies of carbon dynamics through soils. Stable isotope analysis has a strong history of helping track substrate turnover, delineate rhizosphere activity zones, and identifying transitions in vegetation cover, but most traditional isotope approaches are limited in spatial resolution by a combination of physical separation techniques (manual dissection) and IRMS instrument sensitivity. We coupled laser ablation sampling with isotope measurement via IRMS to enable spatially resolved analysis over solid surfaces. Once a targeted sample region is ablated the resulting particulates are entrained in a helium carrier gas and passed through a combustion reactor where carbon is converted to CO2. Cyrotrapping of the resulting CO2 enables a reduction in carrier gas flow which improves overall measurement sensitivity versus traditional, high flow sample introduction. Currently we are performing sample analysis at 50 μm resolution, require 65 ng C per analysis, and achieve measurement precision consistent with other continuous flow techniques. We will discuss applications of the laser ablation IRMS (LA-IRMS) system to microbial communities and fish ecology studies to demonstrate the merits of this technique and how similar analytical approaches can be transitioned to soil systems. Preliminary efforts at analyzing soil samples will be used to highlight strengths and limitations of the LA-IRMS approach, paying particular attention to sample preparation requirements, spatial resolution, sample analysis time, and the types of questions most conducive to analysis via LA-IRMS.

Analysis of active ricin and castor bean proteins in a ricin preparation, castor bean extract, and surface swabs from a public health investigation.

PubMed

Schieltz, David M; McGrath, Sara C; McWilliams, Lisa G; Rees, Jon; Bowen, Michael D; Kools, John J; Dauphin, Leslie A; Gomez-Saladin, Eduardo; Newton, Bruce N; Stang, Heather L; Vick, Michael J; Thomas, Jerry; Pirkle, James L; Barr, John R

2011-06-15

In late February 2008, law enforcement officials in Las Vegas, Nevada, discovered in a hotel room, a copy of The Anarchist Cookbook, suspected castor beans and a "white powder" thought to be a preparation of ricin. Ricin is a deadly toxin from the seed of the castor bean plant (Ricinus communis). The United States regulates the possession, use, and transfer of ricin and it is the only substance considered a warfare agent in both the Chemical and the Biological Weapons Conventions. Six samples obtained from the hotel room were analyzed by laboratories at the Centers for Disease Control and Prevention using a panel of biological and mass spectrometric assays. The biological assays (real time-PCR, time resolved fluorescence and cytotoxicity) provided presumptive evidence of active ricin in each of the samples. This initial screen was followed by an in-depth analysis using a novel, state-of-the-art mass spectrometry-based ricin functional assay and high sensitivity tandem mass spectrometry for protein identification. Mass spectrometric analysis positively identified ricin and confirmed that in each of the samples it was enzymatically active. The tandem mass spectrometry analysis used here is the most selective method available to detect ricin toxin. In each sample, ricin was unequivocally identified along with other R. communis plant proteins, including the highly homologous protein RCA120. Although database searches using tandem mass spectra acquired from the samples indicated that additional controlled substances were not present in these samples, the mass spectrometric results did provide extensive detail about the sample contents. To the best of our knowledge following a review of the available literature, this report describes the most detailed analysis of a white powder for a public health or forensic investigation involving ricin. Published by Elsevier Ireland Ltd.

RAPID ON-SITE METHODS OF CHEMICAL ANALYSIS

EPA Science Inventory

The analysis of potentially hazardous air, water and soil samples collected and shipped to service laboratories off-site is time consuming and expensive. This Chapter addresses the practical alternative of performing the requisite analytical services on-site. The most significant...

Time of flight secondary ion mass spectrometry of bone—Impact of sample preparation and measurement conditions

PubMed Central

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-01-01

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein. PMID:26253108

Time of flight secondary ion mass spectrometry of bone-Impact of sample preparation and measurement conditions.

PubMed

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-06-07

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein.

Statistical analysis of hydrological response in urbanising catchments based on adaptive sampling using inter-amount times

NASA Astrophysics Data System (ADS)

ten Veldhuis, Marie-Claire; Schleiss, Marc

2017-04-01

Urban catchments are typically characterised by a more flashy nature of the hydrological response compared to natural catchments. Predicting flow changes associated with urbanisation is not straightforward, as they are influenced by interactions between impervious cover, basin size, drainage connectivity and stormwater management infrastructure. In this study, we present an alternative approach to statistical analysis of hydrological response variability and basin flashiness, based on the distribution of inter-amount times. We analyse inter-amount time distributions of high-resolution streamflow time series for 17 (semi-)urbanised basins in North Carolina, USA, ranging from 13 to 238 km2 in size. We show that in the inter-amount-time framework, sampling frequency is tuned to the local variability of the flow pattern, resulting in a different representation and weighting of high and low flow periods in the statistical distribution. This leads to important differences in the way the distribution quantiles, mean, coefficient of variation and skewness vary across scales and results in lower mean intermittency and improved scaling. Moreover, we show that inter-amount-time distributions can be used to detect regulation effects on flow patterns, identify critical sampling scales and characterise flashiness of hydrological response. The possibility to use both the classical approach and the inter-amount-time framework to identify minimum observable scales and analyse flow data opens up interesting areas for future research.

Evaluation of two commercial real-time PCR assays for detecting Campylobacter in broiler carcass rinses.

USDA-ARS?s Scientific Manuscript database

Traditional plating methods are reliable means for Campylobacter identification from poultry samples but automated gene-based detection systems now available can reduce assay time, data collection and analysis. Bio-Rad and DuPont Qualicon recently introduced Campylobacter assays for their real-time ...

A novel strategy to obtain quantitative data for modelling: combined enrichment and real-time PCR for enumeration of salmonellae from pig carcasses.

PubMed

Krämer, Nadine; Löfström, Charlotta; Vigre, Håkan; Hoorfar, Jeffrey; Bunge, Cornelia; Malorny, Burkhard

2011-03-01

Salmonella is a major zoonotic pathogen which causes outbreaks and sporadic cases of gastroenteritis in humans worldwide. The primary sources for Salmonella are food-producing animals such as pigs and poultry. For risk assessment and hazard analysis and critical control point (HACCP) concepts, it is essential to produce large amounts of quantitative data, which is currently not achievable with the standard cultural based methods for enumeration of Salmonella. This study presents the development of a novel strategy to enumerate low numbers of Salmonella in cork borer samples taken from pig carcasses as a first concept and proof of principle for a new sensitive and rapid quantification method based on combined enrichment and real-time PCR. The novelty of the approach is in the short pre-enrichment step, where for most bacteria, growth is in the log phase. The method consists of an 8h pre-enrichment of the cork borer sample diluted 1:10 in non-selective buffered peptone water, followed by DNA extraction, and Salmonella detection and quantification by real-time PCR. The limit of quantification was 1.4 colony forming units (CFU)/20 cm(2) (approximately 10 g) of artificially contaminated sample with 95% confidence interval of ± 0.7 log CFU/sample. The precision was similar to the standard reference most probable number (MPN) method. A screening of 200 potentially naturally contaminated cork borer samples obtained over seven weeks in a slaughterhouse resulted in 25 Salmonella-positive samples. The analysis of salmonellae within these samples showed that the PCR method had a higher sensitivity for samples with a low contamination level (<6.7 CFU/sample), where 15 of the samples negative with the MPN method was detected with the PCR method and 5 were found to be negative by both methods. For the samples with a higher contamination level (6.7-310 CFU/sample) a good agreement between the results obtained with the PCR and MPN methods was obtained. The quantitative real-time PCR method can easily be applied to other food and environmental matrices by adaptation of the pre-enrichment time and media. Copyright © 2010 Elsevier B.V. All rights reserved.

Using high resolution measurements of gas tracers to determine metabolic rates in streams

NASA Astrophysics Data System (ADS)

Knapp, J. L.; Osenbrück, K.; Brennwald, M. S.; Cirpka, O. A.

2017-12-01

Hyporheic exchange and other hyporheic processes are strongly linked to stream respiration, as the majority of a streams' microorganisms are located within the streambed. Directly estimating these respiration rates on the reach scale is usually not possible, but they can indirectly be inferred from measurements of dissolved oxygen. This, however, requires determining stream reaeration rates with high precision. Conducting gas-tracer tests has been found to be the most reliable method to estimate stream reaeration, but the majority of field-based sampling techniques for tracer gases are either costly in time and materials, or imprecise. By contrast, on-site gas analysis using gas-equilibrium membrane-inlet mass spectrometers (miniRUEDI, Gasometrix GmbH [1]) avoid the errors caused by sampling, storage, and analysis in the standard sampling techniques. Furthermore, the high analytical frequency of the on-site mass-spectrometer provides concentration data exhibiting a low uncertainty. We present results from gas-tracer tests with a continuous injection of propane and noble gases as tracers in a number of small streams. The concentrations of the tracer gases are recorded continuously over time at the first measurement station to account for fluctuations of the input signal, whereas shorter sample sets are collected at all further measurement stations. Reaeration rate constants are calculated from gas measurements for individual stream sections. These rates are then used to estimate metabolic rates of respiration and primary production based on time series of oxygen measurements. To demonstrate the advancement of the method provided by the on-site analysis, results from measurements performed by on-site mass spectroscopy are compared to those from traditional headspace sampling with gas chromatography analysis. Additionally, differences in magnitude and uncertainty of the obtained reaeration rates of oxygen and calculated metabolic rates from both methods highlight the usefulness of the high-frequency on-site analysis. [1] Brennwald, M. S., Schmidt, M., Oser, J., and Kipfer, R. (2016). A portable and autonomous mass spectrometric system for on-site environmental gas analysis. Environ. Sci. Technol., 50(24):13455-13463. Doi: 10.1021/acs.est.6b03669

Time and expected value of sample information wait for no patient.

PubMed

Eckermann, Simon; Willan, Andrew R

2008-01-01

The expected value of sample information (EVSI) from prospective trials has previously been modeled as the product of EVSI per patient, and the number of patients across the relevant time horizon less those "used up" in trials. However, this implicitly assumes the eligible patient population to which information from a trial can be applied across a time horizon are independent of time for trial accrual, follow-up and analysis. This article demonstrates that in calculating the EVSI of a trial, the number of patients who benefit from trial information should be reduced by those treated outside as well as within the trial over the time until trial evidence is updated, including time for accrual, follow-up and analysis. Accounting for time is shown to reduce the eligible patient population: 1) independent of the size of trial in allowing for time of follow-up and analysis, and 2) dependent on the size of trial for time of accrual, where the patient accrual rate is less than incidence. Consequently, the EVSI and expected net gain (ENG) at any given trial size are shown to be lower when accounting for time, with lower ENG reinforced in the case of trials undertaken while delaying decisions by additional opportunity costs of time. Appropriately accounting for time reduces the EVSI of trial design and increase opportunity costs of trials undertaken with delay, leading to lower likelihood of trialing being optimal and smaller trial designs where optimal.

Falcon: Visual analysis of large, irregularly sampled, and multivariate time series data in additive manufacturing

DOE PAGES

Steed, Chad A.; Halsey, William; Dehoff, Ryan; ...

2017-02-16

Flexible visual analysis of long, high-resolution, and irregularly sampled time series data from multiple sensor streams is a challenge in several domains. In the field of additive manufacturing, this capability is critical for realizing the full potential of large-scale 3D printers. Here, we propose a visual analytics approach that helps additive manufacturing researchers acquire a deep understanding of patterns in log and imagery data collected by 3D printers. Our specific goals include discovering patterns related to defects and system performance issues, optimizing build configurations to avoid defects, and increasing production efficiency. We introduce Falcon, a new visual analytics system thatmore » allows users to interactively explore large, time-oriented data sets from multiple linked perspectives. Falcon provides overviews, detailed views, and unique segmented time series visualizations, all with adjustable scale options. To illustrate the effectiveness of Falcon at providing thorough and efficient knowledge discovery, we present a practical case study involving experts in additive manufacturing and data from a large-scale 3D printer. The techniques described are applicable to the analysis of any quantitative time series, though the focus of this paper is on additive manufacturing.« less