Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

Bismuth molybdate thick films as ethanol sensor

NASA Astrophysics Data System (ADS)

Jain, Kiran; Kumar, Vipin; Gupta, H. P.; Rastogi, A. C.

2003-10-01

Ethanol sensitivity of bismuth molybdate thick films and sintered pellets were investigated. Sintered pellets were prepared by traditional ceramic processing. Thick films were prepared by metallorganic decomposition process. Ethanol gas sensitivity was measured at various temperatures and concentrations. Thick films of alpha phase bismuth molybdate prepared by spray pyrolysis showed a very fast response to ethanol detection. The response time for the bulk samples is about 40 sec which decreased to about 6 sec for thick films at an operating temperature of 300°C. An extremely low level approximately 10 ppm detection and fast response makes this technique ideal for sensor element fabrication for detection and estimation of alcohol in breath-analyzer. Unlike SnO2, the resistance of these sensors is not affected by humidity at the operating temperature.

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope.

PubMed

Fang, Yurui; Zhang, Zhenglong; Sun, Mengtao

2016-03-01

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10(-7) Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 × 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.

Language use affects food behaviours and food values among Mexican-origin adults in the USA.

PubMed

Langellier, Brent A; Brookmeyer, Ron; Wang, May C; Glik, Deborah

2015-02-01

Previous studies have established that acculturation is associated with dietary intake among Mexican immigrants and their offspring, but few studies have investigated whether food purchasing, food preparation or food-related values act as mechanisms of dietary acculturation. We examine the relationship between language use and a wide range of food behaviours and food-related values among Mexican-American adults. Nationally representative probability sample of the US population. 2005-2010 National Health and Nutrition Examination Survey. Mexican-American adults (n 2792) at least 20 years of age. Mexican Americans who speak only or mostly English consume more energy from fast-food and sit-down restaurants and report increased consumption of non-homemade meals, fast-food and pizza meals, frozen meals and ready-to-eat meals relative to Spanish speakers. English speakers prepare one fewer homemade dinner per week and spend less time on meal preparation. English speakers are more likely than Spanish speakers to cite convenience as an important reason why they prefer fast food over cooking at home. There is no relationship between language use and the perceived importance of the nutritional quality, price or taste of fast food. Our results provide evidence that the well-documented relationship between acculturation and diet among Mexican Americans may be just one indicator of a broader pattern characterized by decreased home meal preparation and increased reliance on convenience foods.

Novel method for fast characterization of high-surface-area electrocatalytic materials using carbon fiber microelectrode.

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

Strmcnik, D.; Hodnik, N.; Hocevar, S. B.

2010-02-18

A carbon fiber microelectrode (CFME) was used for characterization of the nanoparticle catalysts as an alternative to the well-established rotating disk electrode (RDE) method. We found that the novel CFME method yielded comparable results to the RDE method when investigating the adsorption/desorption processes as well the specific activity for reactions such as the oxygen reduction reaction. Its major advantage over the RDE method is a fast sample preparation and rapid measurement, reducing significantly the time of a single sample characterization from 2-3 h to a favorable 5-10 min.

Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples - FY17 Year End Report

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

Ticknor, Brian W.; Metzger, Shalina C.; McBay, Eddy H.

Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s Network of Analytical Laboratories (IAEA NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA and UTEVA resins, with a chemical separation method based on the Oakmore » Ridge National Laboratory (ORNL) NWAL chemical procedure. The newly designed prepFAST-SR has had several upgrades compared with the original prepFAST-MC2. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL.« less

DIY Tomography sample holder

NASA Astrophysics Data System (ADS)

Lari, L.; Wright, I.; Boyes, E. D.

2015-10-01

A very simple tomography sample holder at minimal cost was developed in-house. The holder is based on a JEOL single tilt fast exchange sample holder where its exchangeable tip was modified to allow high angle degree tilt. The shape of the tip was designed to retain mechanical stability while minimising the lateral size of the tip. The sample can be mounted on as for a standard 3mm Cu grids as well as semi-circular grids from FIB sample preparation. Applications of the holder on different sample systems are shown.

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope

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

Fang, Yurui; Bionanophotonics, Department of Applied Physics, Chalmers University of Technology, Göteborg, SE 41296; Zhang, Zhenglong

2016-03-15

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10{sup −7} Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 ×more » 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.« less

Sequence-specific sepsis-related DNA capture and fluorescent labeling in monoliths prepared by single-step photopolymerization in microfluidic devices.

PubMed

Knob, Radim; Hanson, Robert L; Tateoka, Olivia B; Wood, Ryan L; Guerrero-Arguero, Israel; Robison, Richard A; Pitt, William G; Woolley, Adam T

2018-05-21

Fast determination of antibiotic resistance is crucial in selecting appropriate treatment for sepsis patients, but current methods based on culture are time consuming. We are developing a microfluidic platform with a monolithic column modified with oligonucleotides designed for sequence-specific capture of target DNA related to the Klebsiella pneumoniae carbapenemase (KPC) gene. We developed a novel single-step monolith fabrication method with an acrydite-modified capture oligonucleotide in the polymerization mixture, enabling fast monolith preparation in a microfluidic channel using UV photopolymerization. These prepared columns had a threefold higher capacity compared to monoliths prepared in a multistep process involving Schiff-base DNA attachment. Conditions for denaturing, capture and fluorescence labeling using hybridization probes were optimized with synthetic 90-mer oligonucleotides. These procedures were applied for extraction of a PCR amplicon from the KPC antibiotic resistance gene in bacterial lysate obtained from a blood sample spiked with E. coli. The results showed similar eluted peak areas for KPC amplicon extracted from either hybridization buffer or bacterial lysate. Selective extraction of the KPC DNA was verified by real time PCR on eluted fractions. These results show great promise for application in an integrated microfluidic diagnostic system that combines upstream blood sample preparation and downstream single-molecule counting detection. Copyright © 2018 Elsevier B.V. All rights reserved.

Physical pretreatment of biogenic-rich trommel fines for fast pyrolysis.

PubMed

Eke, Joseph; Onwudili, Jude A; Bridgwater, Anthony V

2017-12-01

Energy from Waste (EfW) technologies such as fluidized bed fast pyrolysis, are beneficial for both energy generation and waste management. Such technologies, however face significant challenges due to the heterogeneous nature, particularly the high ash contents of some municipal solid waste types e.g. trommel fines. A study of the physical/mechanical and thermal characteristics of these complex wastes is important for two main reasons; (a) to inform the design and operation of pyrolysis systems to handle the characteristics of such waste; (b) to control/modify the characteristics of the waste to fit with existing EFW technologies via appropriate feedstock preparation methods. In this study, the preparation and detailed characterisation of a sample of biogenic-rich trommel fines has been carried out with a view to making the feedstock suitable for fast pyrolysis based on an existing fluidized bed reactor. Results indicate that control of feed particle size was very important to prevent problems of dust entrainment in the fluidizing gas as well as to prevent feeder hardware problems caused by large stones and aggregates. After physical separation and size reduction, nearly 70wt% of the trommel fines was obtained within the size range suitable for energy recovery using the existing fast pyrolysis system. This pyrolyzable fraction could account for about 83% of the energy content of the 'as received' trommel fines sample. Therefore there was no significant differences in the thermochemical properties of the raw and pre-treated feedstocks, indicating that suitably prepared trommel fines samples can be used for energy recovery, with significant reduction in mass and volume of the original waste. Consequently, this can lead to more than 90% reduction in the present costs of disposal of trommel fines in landfills. In addition, the recovered plastics and textile materials could be used as refuse derived fuel. Copyright © 2017 Elsevier Ltd. All rights reserved.

Femtosecond laser machining for characterization of local mechanical properties of biomaterials: a case study on wood

PubMed Central

Jakob, Severin; Pfeifenberger, Manuel J.; Hohenwarter, Anton; Pippan, Reinhard

2017-01-01

Abstract The standard preparation technique for micro-sized samples is focused ion beam milling, most frequently using Ga+ ions. The main drawbacks are the required processing time and the possibility and risks of ion implantation. In contrast, ultrashort pulsed laser ablation can process any type of material with ideally negligible damage to the surrounding volume and provides 4 to 6 orders of magnitude higher ablation rates than the ion beam technique. In this work, a femtosecond laser was used to prepare wood samples from spruce for mechanical testing at the micrometre level. After optimization of the different laser parameters, tensile and compressive specimens were produced from microtomed radial-tangential and longitudinal-tangential sections. Additionally, laser-processed samples were exposed to an electron beam prior to testing to study possible beam damage. The specimens originating from these different preparation conditions were mechanically tested. Advantages and limitations of the femtosecond laser preparation technique and the deformation and fracture behaviour of the samples are discussed. The results prove that femtosecond laser processing is a fast and precise preparation technique, which enables the fabrication of pristine biological samples with dimensions at the microscale. PMID:28970867

Femtosecond laser machining for characterization of local mechanical properties of biomaterials: a case study on wood

NASA Astrophysics Data System (ADS)

Jakob, Severin; Pfeifenberger, Manuel J.; Hohenwarter, Anton; Pippan, Reinhard

2017-12-01

The standard preparation technique for micro-sized samples is focused ion beam milling, most frequently using Ga+ ions. The main drawbacks are the required processing time and the possibility and risks of ion implantation. In contrast, ultrashort pulsed laser ablation can process any type of material with ideally negligible damage to the surrounding volume and provides 4 to 6 orders of magnitude higher ablation rates than the ion beam technique. In this work, a femtosecond laser was used to prepare wood samples from spruce for mechanical testing at the micrometre level. After optimization of the different laser parameters, tensile and compressive specimens were produced from microtomed radial-tangential and longitudinal-tangential sections. Additionally, laser-processed samples were exposed to an electron beam prior to testing to study possible beam damage. The specimens originating from these different preparation conditions were mechanically tested. Advantages and limitations of the femtosecond laser preparation technique and the deformation and fracture behaviour of the samples are discussed. The results prove that femtosecond laser processing is a fast and precise preparation technique, which enables the fabrication of pristine biological samples with dimensions at the microscale.

Large outbreak of salmonella phage type 1 infection with high infection rate and severe illness associated with fast food premises.

PubMed

Giraudon, I; Cathcart, S; Blomqvist, S; Littleton, A; Surman-Lee, S; Mifsud, A; Anaraki, S; Fraser, G

2009-06-01

To describe the epidemiology of an outbreak of Salmonella enteritidis phage type 1 (PT1) infection associated with a fast food premises, and to identify the causative factors leading to an acute outbreak with high attack rate and severe illness including hospital admission. Integrated descriptive study of epidemiology, food and environmental microbiology, and professional environmental health assessment, supplemented by a case-case analytical study. Cases were identified through multiple sources and were interviewed to identify food items consumed. Descriptive epidemiology of all cases and a case-case analytical study of risk factors for severe illness were undertaken. Microbiological investigation included analysis and typing of pathogens from stools, blood and environmental surfaces. Professional environmental heath assessment of the premises was undertaken. S. enteritidis PT1 was recovered from two-thirds of faecal samples. Three cases had dual infection with enterotoxin-producing Clostridium perfringens. S. enteritidis PT1 was isolated from 14 of 40 food samples examined and C. perfringens was isolated from eight food samples. Environmental health inspection of the premises revealed multiple deficiencies, including deficits in food preparation and hygiene consistent with multiple cross-contamination, and time-temperature abuse of sauces widely used across menu items. Severe cases were associated with consumption of chips and salad. Outbreaks from fast food premises have been infrequently described. This outbreak demonstrates the potential for fast food premises, with multiple deficiencies in food preparation and hygiene, to produce large, intense community outbreaks with high attack rates and severe illness, highly confined in space and time.

Language use affects food behaviours and food values among Mexican-origin adults in the USA

PubMed Central

Langellier, Brent A; Brookmeyer, Ron; Wang, May C; Glik, Deborah

2015-01-01

Objectives Previous studies have established that acculturation is associated with dietary intake among Mexican immigrants and their offspring, but few studies have investigated whether food purchasing, food preparation, or food-related values act as mechanisms of dietary acculturation. We examine the relationship between language use and a wide range of food behaviors and food-related values among Mexican American adults. Design Nationally-representative probability sample of the U.S. population. Setting 2005–2010 National Health and Nutrition Examination Survey. Subjects 2,792 Mexican American adults at least 20 years of age. Results Mexican Americans who speak only or mostly English consume more energy from fast food and sit-down restaurants and report increased consumption of non-homemade meals, fast food and pizza meals, frozen meals, and ready-to-eat meals relative to Spanish speakers. English speakers prepare one fewer homemade dinner per week and spend less time on meal preparation. English speakers are more likely than Spanish speakers to cite convenience as an important reason why they prefer fast food over cooking at home. There is no relationship between language use and the perceived importance of the nutritional quality, price, or taste of fast food. Conclusions Our results provide evidence that the well-documented relationship between acculturation and diet among Mexican Americans may be just one indicator of a broader pattern characterized by decreased home meal preparation and increased reliance on convenience foods. PMID:24698136

Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

ERIC Educational Resources Information Center

DiNunzio, James E.

1985-01-01

Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

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.

Fabric phase sorptive extraction followed by UHPLC-MS/MS for the analysis of benzotriazole UV stabilizers in sewage samples.

PubMed

Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

2015-10-01

A fast and sensitive sample preparation strategy using fabric phase sorptive extraction followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection has been developed to analyse benzotriazole UV stabilizer compounds in aqueous samples. Benzotriazole UV stabilizer compounds are a group of compounds added to sunscreens and other personal care products which may present detrimental effects to aquatic ecosystems. Fabric phase sorptive extraction is a novel solvent minimized sample preparation approach that integrates the advantages of sol-gel derived hybrid inorganic-organic nanocomposite sorbents and the flexible, permeable and hydrophobic surface chemistry of polyester fabric. It is a highly sensitive, fast, efficient and inexpensive device that can be reused and does not suffer from coating damage, unlike SPME fibres or stir bars. In this paper, we optimized the extraction of seven benzotriazole UV filters evaluating the majority of the parameters involved in the extraction process, such as sorbent chemistry selection, extraction time, back-extraction solvent, back-extraction time and the impact of ionic strength. Under the optimized conditions, fabric phase sorptive extraction allows enrichment factors of 10 times with detection limits ranging from 6.01 to 60.7 ng L(-1) and intra- and inter-day % RSDs lower than 11 and 30 % for all compounds, respectively. The optimized sample preparation technique followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection was applied to determine the target analytes in sewage samples from wastewater treatment plants with different purification processes of Gran Canaria Island (Spain). Two UV stabilizer compounds were measured in ranges 17.0-60.5 ng mL(-1) (UV 328) and 69.3-99.2 ng mL(-1) (UV 360) in the three sewage water samples analysed.

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to ∼1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had ∼2.5× higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice ∼25 μm cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

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

Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken frommore » the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.« less

Characterization of Neutron Transmutation Doped (NTD) Ge for low temperature sensor development

NASA Astrophysics Data System (ADS)

Mathimalar, S.; Singh, V.; Dokania, N.; Nanal, V.; Pillay, R. G.; Pal, S.; Ramakrishnan, S.; Shrivastava, A.; Maheshwari, Priya; Pujari, P. K.; Ojha, S.; Kanjilal, D.; Jagadeesan, K. C.; Thakare, S. V.

2015-02-01

Development of NTD Ge sensors has been initiated for low temperature (mK) thermometry in The India-based TIN detector (TIN.TIN). NTD Ge sensors are prepared by thermal neutron irradiation of device grade Ge samples at Dhruva reactor, BARC, Mumbai. Detailed measurements have been carried out in irradiated samples for estimating the carrier concentration and fast neutron induced defects. The Positron Annihilation Lifetime Spectroscopy (PALS) measurements indicated monovacancy type defects for all irradiated samples, while Channeling studies employing RBS with 2 MeV alpha particles, revealed no significant defects in the samples exposed to fast neutron fluence of ∼ 4 ×1016 /cm2 . Both PALS and Channeling studies have shown that vacuum annealing at 600 °C for ∼ 2 h is sufficient to recover the damage in the irradiated samples, thereby making them suitable for the sensor development.

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

USDA-ARS?s Scientific Manuscript database

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

Determination of trace metals in spirits by total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Siviero, G.; Cinosi, A.; Monticelli, D.; Seralessandri, L.

2018-06-01

Eight spirituous samples were analyzed for trace metal content with Horizon Total Reflection X-Ray Fluorescence (TXRF) Spectrometer. The expected single metal amount is at the ng/g level in a mixed aqueous/organic matrix, thus requiring a sample preparation method capable of achieving suitable limits of detection. On-site enrichment and Atmospheric Pressure-Vapor Phase Decomposition allowed to detect Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr and Pb with detection limits ranging from 0.1 ng/g to 4.6 ng/g. These results highlight how the synergy between instrument and sample preparation strategy may foster the use of TXRF as a fast and reliable technique for the determination of trace elements in spirituous samples, either for quality control or risk assessment purposes.

Rapid sample preparation and fast GC-MS/MS for the analysis of pesticides and environmental contaminants in fish

USDA-ARS?s Scientific Manuscript database

A rapid high-throughput analytical method for the simultaneous determination of pesticides and environmental contaminants, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs) and flame retardants (FRs) in fish was developed and ...

Trifunctional Epoxy Resin Composites Modified by Soluble Electrospun Veils: Effect on the Viscoelastic and Morphological Properties

PubMed Central

Ognibene, Giulia; Mannino, Salvatore

2018-01-01

Electrospun veils from copolyethersulfones (coPES) were prepared as soluble interlaminar veils for carbon fiber/epoxy composites. Neat, resin samples were impregnated into coPES veils with unmodified resin, while dry carbon fabrics were covered with electrospun veils and then infused with the unmodified epoxy resin to prepare reinforced laminates. The thermoplastic content varied from 10 wt% to 20 wt%. TGAP epoxy monomer showed improved and fast dissolution for all the temperatures tested. The unreinforced samples were cured first at 180 °C for 2 h and then were post-cured at 220 °C for 3 h. These sample showed a high dependence on the curing cycle. Carbon reinforced samples showed significant differences compared to the neat resin samples in terms of both viscoelastic and morphological properties. PMID:29522444

A High-Performance Liquid Chromatography-Based Screening Method for the Analysis of Atrazine, Alachlor, and Ten of Their Transformation Products

USGS Publications Warehouse

Schroyer, B.R.; Capel, P.D.

1996-01-01

A high-performance liquid Chromatography (HPLC) method is presented for the for the fast, quantitative analysis of the target analytes in water and in low organic-carbon, sandy soils that are known to be contaminated with the parent herbicides. Speed and ease of sample preparation was prioritized above minimizing detection limits. Soil samples were extracted using 80:20 methanol:water (volume:volume). Water samples (50 ??L) were injected directly into the HPLC without prior preparation. Method quantification limits for soil samples (10 g dry weight) and water samples ranged from 20 to 110 ng/g and from 20 to 110 ??g/L for atrazine and its transformation products and from 80 to 320 ng/g and from 80 to 320 ??g/L for alachlor and its transformation products, respectively.

Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

PubMed

Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

Influence of Fasting Status and Sample Preparation on Metabolic Biomarker Measurements in Postmenopausal Women.

PubMed

Murphy, Neil; Falk, Roni T; Messinger, Diana B; Pollak, Michael; Xue, Xiaonan; Lin, Juan; Sgueglia, Robin; Strickler, Howard D; Gaudet, Mia M; Gunter, Marc J

2016-01-01

Epidemiologic data linking metabolic markers-such as insulin, insulin-like growth factors (IGFs)-and adipose tissue-derived factors with cancer are inconsistent. Between-study differences in blood collection protocols, in particular participant's fasting status, may influence measurements. We investigated the impact of fasting status and blood sample processing time on components of the insulin/IGF axis and in adipokines in a controlled feeding study of 45 healthy postmenopausal-women aged 50-75 years. Fasting blood samples were drawn (T0), after which subjects ate a standardized breakfast; subsequent blood draws were made at 1 hour (T1), 3 hours (T3), and 6 hours (T6) after breakfast. Serum samples were assayed for insulin, C-peptide, total- and free-IGF-I, IGF-binding protein [BP]-1 and -3, total and high molecular weight (HMW)-adiponectin, retinol binding protein-4, plasminogen activator inhibitor (PAI)-1, and resistin. Insulin and C-peptide levels followed similar postprandial trajectories; intra-class correlation coefficients [ICC] for insulin = 0.75, (95%CI:0.64-0.97) and C-peptide (ICC = 0.66, 95%CI:0.54-0.77) were similarly correlated in fasting (Spearman correlation, r = 0.78, 95%CI:0.64-0.88) and postprandial states (T1, r = 0.77 (95%CI: 0.62-0.87); T3,r = 0.78 (95%CI: 0.63-0.87); T6,r = 0.77 (95%CI: 0.61-0.87)). Free-IGF-I and IGFBP-1 levels were also affected by fasting status, whereas total-IGF-I and IGFBP-3 levels remained unchanged. Levels of adipokines were largely insensitive to fasting status and blood sample processing delays. Several components of the insulin/IGF axis were significantly impacted by fasting state and in particular, C-peptide levels were substantially altered postprandially and in a similar manner to insulin.

A simple and fast method for fixation of cultured cell lines that preserves cellular structures containing gamma-tubulin.

PubMed

Alvarado-Kristensson, Maria

2018-01-01

When using fluorescence microscope techniques to study cells, it is essential that the cell structure and contents are preserved after preparation of the samples, and that the preparation method employed does not create artefacts that can be perceived as cellular structure/components. γ-Tubulin forms filaments that in some cases are immunostained with an anti-γ-tubulin antibody, but this immunostaining is not reproducible [[1], [2

Which food-related behaviours are associated with healthier intakes of fruits and vegetables among women?

PubMed

Crawford, David; Ball, Kylie; Mishra, Gita; Salmon, Jo; Timperio, Anna

2007-03-01

To examine associations between shopping, food preparation, meal and eating behaviours and fruit and vegetable intake among women. Cross-sectional survey. Community-based sample from metropolitan Melbourne, Australia. A sample of 1136 women aged 18-65 years, randomly selected from the electoral roll. Food-related behaviours reflecting organisation and forward-planning, as well as enjoyment of and high perceived value of meal shopping, preparation and consumption were associated with healthier intakes of fruits and vegetables. For example, women who more frequently planned meals before they went shopping, wrote a shopping list, enjoyed food shopping, planned in the morning what they will eat for dinner that night, planned what they will eat for lunch, reported they enjoy cooking, liked trying new recipes and who reported they sometimes prepare dishes ahead of time were more likely to consume two or more servings of vegetables daily. Conversely, women who frequently found cooking a chore, spent less than 15 minutes preparing dinner, decided on the night what they will eat for dinner, ate in a fast-food restaurant, ate takeaway meals from a fast-food restaurant, ate dinner and snacks while watching television and who frequently ate on the run were less likely to eat two or more servings of vegetables daily. Practical strategies based on these behavioural characteristics could be trialled in interventions aimed at promoting fruit and vegetable consumption among women.

Analytical platform for metabolome analysis of microbial cells using methyl chloroformate derivatization followed by gas chromatography-mass spectrometry.

PubMed

Smart, Kathleen F; Aggio, Raphael B M; Van Houtte, Jeremy R; Villas-Bôas, Silas G

2010-09-01

This protocol describes an analytical platform for the analysis of intra- and extracellular metabolites of microbial cells (yeast, filamentous fungi and bacteria) using gas chromatography-mass spectrometry (GC-MS). The protocol is subdivided into sampling, sample preparation, chemical derivatization of metabolites, GC-MS analysis and data processing and analysis. This protocol uses two robust quenching methods for microbial cultures, the first of which, cold glycerol-saline quenching, causes reduced leakage of intracellular metabolites, thus allowing a more reliable separation of intra- and extracellular metabolites with simultaneous stopping of cell metabolism. The second, fast filtration, is specifically designed for quenching filamentous micro-organisms. These sampling techniques are combined with an easy sample-preparation procedure and a fast chemical derivatization reaction using methyl chloroformate. This reaction takes place at room temperature, in aqueous medium, and is less prone to matrix effect compared with other derivatizations. This protocol takes an average of 10 d to complete and enables the simultaneous analysis of hundreds of metabolites from the central carbon metabolism (amino and nonamino organic acids, phosphorylated organic acids and fatty acid intermediates) using an in-house MS library and a data analysis pipeline consisting of two free software programs (Automated Mass Deconvolution and Identification System (AMDIS) and R).

Comparing nutrition environments in bodegas and fast food restaurants

PubMed Central

Lovasi, Laszlo; Yousefzadeh, Paulette; Sheehan, Daniel; Milinkovic, Karla; Baecker, Aileen; Bader, Michael D. M.; Weiss, Christopher; Lovasi, Gina S.; Rundle, Andrew

2015-01-01

Many small grocery stores or “bodegas” sell prepared or ready-to-eat items, filling a similar niche in the food environment as fast food restaurants. However, little comparative information is available about the nutrition environments of bodegas and fast food outlets. This study compared the nutrition environments of bodegas and national chain fast food restaurants using a common audit instrument, the Nutrition Environment Measures Study in Restaurants (NEMS-R) protocol. The analytic sample included 109 bodegas and 107 fast food restaurants located in New York City neighborhoods in the upper third and lower third of the census tract poverty rate distribution. Inter-rater reliability was evaluated in 102 food outlets including 31 from the analytic sample and 71 from a supplementary convenience sample. The analysis compared scores on individual NEMS-R items, a total summary score, and sub-scores indicating healthy food availability, nutrition information, promotions of healthy or unhealthy eating, and price incentives for healthy eating, using t-tests and chi-square statistics to evaluate differences by outlet type and neighborhood poverty. Fast food restaurants were more likely to provide nutritional information, while bodegas scored higher on healthy food availability, promotions, and pricing. Bodegas and fast food restaurants had similar NEMS-R total scores (bodegas: 13.09, fast food: 14.31, p=0.22). NEMS-R total scores were higher (indicating healthier environments) in low- than high-poverty neighborhoods among both bodegas (14.79 vs. 11.54, p=0.01) and fast food restaurants (16.27 vs. 11.60, p<.01). Results imply different policy measures to improve nutrition environments in the two types of food outlets. PMID:24035459

Comparing nutrition environments in bodegas and fast-food restaurants.

PubMed

Neckerman, Kathryn M; Lovasi, Laszlo; Yousefzadeh, Paulette; Sheehan, Daniel; Milinkovic, Karla; Baecker, Aileen; Bader, Michael D M; Weiss, Christopher; Lovasi, Gina S; Rundle, Andrew

2014-04-01

Many small grocery stores or "bodegas" sell prepared or ready-to-eat items, filling a niche in the food environment similar to fast-food restaurants. However, little comparative information is available about the nutrition environments of bodegas and fast-food outlets. This study compared the nutrition environments of bodegas and national chain fast-food restaurants using a common audit instrument, the Nutrition Environment Measures Study in Restaurants (NEMS-R) protocol. The analytic sample included 109 bodegas and 107 fast-food restaurants located in New York City neighborhoods in the upper third and lower third of the census tract poverty rate distribution. Inter-rater reliability was evaluated in 102 food outlets, including 31 from the analytic sample and 71 from a supplementary convenience sample. The analysis compared scores on individual NEMS-R items, a total summary score, and subscores indicating healthy food availability, nutrition information, promotions of healthy or unhealthy eating, and price incentives for healthy eating, using t tests and χ(2) statistics to evaluate differences by outlet type and neighborhood poverty. Fast-food restaurants were more likely to provide nutrition information, and bodegas scored higher on healthy food availability, promotions, and pricing. Bodegas and fast-food restaurants had similar NEMS-R total scores (bodegas 13.09, fast food 14.31; P=0.22). NEMS-R total scores were higher (indicating healthier environments) in low- than high-poverty neighborhoods among both bodegas (14.79 vs 11.54; P=0.01) and fast-food restaurants (16.27 vs 11.60; P<0.01). Results imply different policy measures to improve nutrition environments in the two types of food outlets. Copyright © 2014 Academy of Nutrition and Dietetics. Published by Elsevier Inc. All rights reserved.

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

An ultrahigh vacuum fast-scanning and variable temperature scanning tunneling microscope for large scale imaging.

PubMed

Diaconescu, Bogdan; Nenchev, Georgi; de la Figuera, Juan; Pohl, Karsten

2007-10-01

We describe the design and performance of a fast-scanning, variable temperature scanning tunneling microscope (STM) operating from 80 to 700 K in ultrahigh vacuum (UHV), which routinely achieves large scale atomically resolved imaging of compact metallic surfaces. An efficient in-vacuum vibration isolation and cryogenic system allows for no external vibration isolation of the UHV chamber. The design of the sample holder and STM head permits imaging of the same nanometer-size area of the sample before and after sample preparation outside the STM base. Refractory metal samples are frequently annealed up to 2000 K and their cooldown time from room temperature to 80 K is 15 min. The vertical resolution of the instrument was found to be about 2 pm at room temperature. The coarse motor design allows both translation and rotation of the scanner tube. The total scanning area is about 8 x 8 microm(2). The sample temperature can be adjusted by a few tens of degrees while scanning over the same sample area.

Substrate water exchange in photosystem II depends on the peripheral proteins.

PubMed

Hillier, W; Hendry, G; Burnap, R L; Wydrzynski, T

2001-12-14

The (18)O exchange rates for the substrate water bound in the S(3) state were determined in different photosystem II sample types using time-resolved mass spectrometry. The samples included thylakoid membranes, salt-washed Triton X-100-prepared membrane fragments, and purified core complexes from spinach and cyanobacteria. For each sample type, two kinetically distinct isotopic exchange rates could be resolved, indicating that the biphasic exchange behavior for the substrate water is inherent to the O(2)-evolving catalytic site in the S(3) state. However, the fast phase of exchange became somewhat slower (by a factor of approximately 2) in NaCl-washed membrane fragments and core complexes from spinach in which the 16- and 23-kDa extrinsic proteins have been removed, compared with the corresponding rate for the intact samples. For CaCl(2)-washed membrane fragments in which the 33-kDa manganese stabilizing protein (MSP) has also been removed, the fast phase of exchange slowed down even further (by a factor of approximately 3). Interestingly, the slow phase of exchange was little affected in the samples from spinach. For core complexes prepared from Synechocystis PCC 6803 and Synechococcus elongatus, the fast and slow exchange rates were variously affected. Nevertheless, within the experimental error, nearly the same exchange rates were measured for thylakoid samples made from wild type and an MSP-lacking mutant of Synechocystis PCC 6803. This result could indicate that the MSP has a slightly different function in eukaryotic organisms compared with prokaryotic organisms. In all samples, however, the differences in the exchange rates are relatively small. Such small differences are unlikely to arise from major changes in the metal-ligand structure at the catalytic site. Rather, the observed differences may reflect subtle long range effects in which the exchange reaction coordinates become slightly altered. We discuss the results in terms of solvent penetration into photosystem II and the regional dielectric around the catalytic site.

Evaluation of the antifungal effects of bio-oil prepared with lignocellulosic biomass using fast pyrolysis technology.

PubMed

Kim, Kwang Ho; Jeong, Han Seob; Kim, Jae-Young; Han, Gyu Seong; Choi, In-Gyu; Choi, Joon Weon

2012-10-01

This study was performed to investigate the utility of bio-oil, produced via a fast pyrolysis process, as an antifungal agent against wood-rot fungi. Bio-oil solutions (25-100 wt.%) were prepared by diluting the bio-oil with EtOH. Wood block samples (yellow poplar and pitch pine) were treated with diluted bio-oil solutions and then subjected to a leaching process under hot water (70°C) for 72 h. After the wood block samples were thoroughly dried, they were subjected to a soil block test using Tyromyces palustris and Trametes versicolor. The antifungal effect of the 75% and 100% bio-oil solutions was the highest for both wood blocks. Scanning electron microscopy analysis indicated that some chemical components in the bio-oil solution could agglomerate together to form clusters in the inner part of the wood during the drying process, which could act as a wood preservative against fungal growth. According to GC/MS analysis, the components of the agglomerate were mainly phenolic compounds derived from lignin polymers. Copyright © 2012 Elsevier Ltd. All rights reserved.

Application of PLE for the determination of essential oil components from Thymus vulgaris L.

PubMed

Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

2008-08-15

Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

Detection of Salmonella enterica in Meat in Less than 5 Hours by a Low-Cost and Noncomplex Sample Preparation Method

PubMed Central

Hoorfar, J.; Hansen, F.; Christensen, J.; Mansdal, S.; Josefsen, M. H.

2016-01-01

ABSTRACT Salmonella is recognized as one of the most important foodborne bacteria and has wide health and socioeconomic impacts worldwide. Fresh pork meat is one of the main sources of Salmonella, and efficient and fast methods for detection are therefore necessary. Current methods for Salmonella detection in fresh meat usually include >16 h of culture enrichment, in a few cases <12 h, thus requiring at least two working shifts. Here, we report a rapid (<5 h) and high-throughput method for screening of Salmonella in samples from fresh pork meat, consisting of a 3-h enrichment in standard buffered peptone water and a real-time PCR-compatible sample preparation method based on filtration, centrifugation, and enzymatic digestion, followed by fast-cycling real-time PCR detection. The method was validated in an unpaired comparative study against the Nordic Committee on Food Analysis (NMKL) reference culture method 187. Pork meat samples (n = 140) were either artificially contaminated with Salmonella at 0, 1 to 10, or 10 to 100 CFU/25 g of meat or naturally contaminated. Cohen's kappa for the degree of agreement between the rapid method and the reference was 0.64, and the relative accuracy, sensitivity, and specificity for the rapid method were 81.4, 95.1, and 97.9%, respectively. The 50% limit of detections (LOD50s) were 8.8 CFU/25 g for the rapid method and 7.7 CFU/25 g for the reference method. Implementation of this method will enable faster release of Salmonella low-risk meat, providing savings for meat producers, and it will help contribute to improved food safety. IMPORTANCE While the cost of analysis and hands-on time of the presented rapid method were comparable to those of reference culture methods, the fast product release by this method can provide the meat industry with a competitive advantage. Not only will the abattoirs save costs for work hours and cold storage, but consumers and retailers will also benefit from fresher meat with a longer shelf life. Furthermore, the presented sample preparation might be adjusted for application in the detection of other pathogenic bacteria in different sample types. PMID:27986726

Detection of Salmonella enterica in Meat in Less than 5 Hours by a Low-Cost and Noncomplex Sample Preparation Method.

PubMed

Fachmann, M S R; Löfström, C; Hoorfar, J; Hansen, F; Christensen, J; Mansdal, S; Josefsen, M H

2017-03-01

Salmonella is recognized as one of the most important foodborne bacteria and has wide health and socioeconomic impacts worldwide. Fresh pork meat is one of the main sources of Salmonella , and efficient and fast methods for detection are therefore necessary. Current methods for Salmonella detection in fresh meat usually include >16 h of culture enrichment, in a few cases <12 h, thus requiring at least two working shifts. Here, we report a rapid (<5 h) and high-throughput method for screening of Salmonella in samples from fresh pork meat, consisting of a 3-h enrichment in standard buffered peptone water and a real-time PCR-compatible sample preparation method based on filtration, centrifugation, and enzymatic digestion, followed by fast-cycling real-time PCR detection. The method was validated in an unpaired comparative study against the Nordic Committee on Food Analysis (NMKL) reference culture method 187. Pork meat samples ( n = 140) were either artificially contaminated with Salmonella at 0, 1 to 10, or 10 to 100 CFU/25 g of meat or naturally contaminated. Cohen's kappa for the degree of agreement between the rapid method and the reference was 0.64, and the relative accuracy, sensitivity, and specificity for the rapid method were 81.4, 95.1, and 97.9%, respectively. The 50% limit of detections (LOD 50 s) were 8.8 CFU/25 g for the rapid method and 7.7 CFU/25 g for the reference method. Implementation of this method will enable faster release of Salmonella low-risk meat, providing savings for meat producers, and it will help contribute to improved food safety. IMPORTANCE While the cost of analysis and hands-on time of the presented rapid method were comparable to those of reference culture methods, the fast product release by this method can provide the meat industry with a competitive advantage. Not only will the abattoirs save costs for work hours and cold storage, but consumers and retailers will also benefit from fresher meat with a longer shelf life. Furthermore, the presented sample preparation might be adjusted for application in the detection of other pathogenic bacteria in different sample types. Copyright © 2017 American Society for Microbiology.

Chemical fingerprinting of Arabidopsis using Fourier transform infrared (FT-IR) spectroscopic approaches.

PubMed

Gorzsás, András; Sundberg, Björn

2014-01-01

Fourier transform infrared (FT-IR) spectroscopy is a fast, sensitive, inexpensive, and nondestructive technique for chemical profiling of plant materials. In this chapter we discuss the instrumental setup, the basic principles of analysis, and the possibilities for and limitations of obtaining qualitative and semiquantitative information by FT-IR spectroscopy. We provide detailed protocols for four fully customizable techniques: (1) Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS): a sensitive and high-throughput technique for powders; (2) attenuated total reflectance (ATR) spectroscopy: a technique that requires no sample preparation and can be used for solid samples as well as for cell cultures; (3) microspectroscopy using a single element (SE) detector: a technique used for analyzing sections at low spatial resolution; and (4) microspectroscopy using a focal plane array (FPA) detector: a technique for rapid chemical profiling of plant sections at cellular resolution. Sample preparation, measurement, and data analysis steps are listed for each of the techniques to help the user collect the best quality spectra and prepare them for subsequent multivariate analysis.

Inhomogeneities and superconductivity in poly-phase Fe-Se-Te systems

NASA Astrophysics Data System (ADS)

Hartwig, S.; Schäfer, N.; Schulze, M.; Landsgesell, S.; Abou-Ras, D.; Blum, Ch. G. F.; Wurmehl, S.; Sokolowski, A.; Büchner, B.; Prokeš, K.

2018-02-01

The impact of synthesis conditions, post-preparation heating procedure, aging and influence of pressure on the superconducting properties of FeSe0.4Te0.6 crystals is reported. Two FeSe0.4Te0.6 single crystals were used in the study, prepared from stoichiometric melt but cooled down with very different cooling rates, and investigated using magnetic bulk and electrical-resistivity methods. The fast-cooled crystal contains large inclusions of Fe3Se2.1Te1.8 and exhibits bulk superconductivity in its as-prepared state, while the other is homogeneous and shows only traces of superconductivity. AC susceptibility measurements under hydrostatic pressure show that the superconducting transition temperature of the inhomogeneous crystal increases from 12.3 K at ambient pressure to Tsc = 17.9 K at 9 kbar. On the other hand, neither pressure nor mechanically-induced stress is sufficient to induce superconductivity in the homogeneous crystal. However, an additional heat treatment at 673 K followed by fast cooling down and/or long-term aging at ambient conditions leads to the appearance of bulk superconductivity also in the latter sample. This sample remains homogeneous on a scale down to few μm but shows an additional magnetic phase transition around 130 K suggesting that it must be inhomogeneous. For comparison also Fe3Se2.1Te1.8 polycrystals have been prepared and their magnetic properties have been studied. It appears that this phase is not superconducting by itself. It is concluded that nano-scale inhomogeneities that appear in the FeSexTe1-x system due to a spinodal decomposition in the solid state are necessary for bulk superconductivity, possibly due to minor changes in the crystal structure and microstructure. Macroscopic inclusions quenched by fast cooling from high temperatures lead obviously to strain and hence variations in the lattice constants, an effect that is further supported by application of pressure/stress.

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.

Extraction and derivatization of polar herbicides for GC-MS analyses.

PubMed

Ranz, Andreas; Maier, Eveline; Motter, Herbert; Lankmayr, Ernst

2008-09-01

A sample preparation procedure including a simultaneous microwave-assisted (MA) extraction and derivatization for the determination of chlorophenoxy acids in soil samples is presented. For a selective and sensitive measurement, an analytical technique such as GC coupled with MS needs to be adopted. For GC analyses, chlorophenoxy acids have to be converted into more volatile and thermally stable derivatives. Derivatization by means of microwave radiation offers new alternatives in terms of shorter derivatization time and reduces susceptibility for the formation of artefacts. Extraction and derivatization into methyl esters (ME) were performed with sulphuric acid and methanol. Due to the novelty of the simultaneous extraction and derivatization assisted by means of microwave radiation, a careful investigation and optimization of influential reaction parameters was necessary. It could be shown that the combination of sulphuric acid and methanol provides a fast sample preparation including an efficient clean up procedure. The data obtained by the described method are in good agreement with those published for the reference material. Finally, compared to conventional heating and also to the standard procedure of the EPA, the sample preparation time could be considerably shortened.

Fabrication of a high sensitivity and fast response self-powered photosensor based on a core-shell silicon nanowire homojunction

NASA Astrophysics Data System (ADS)

Abdul-Hameed, Assel A.; Mahdi, M. A.; Ali, Basil; Selman, Abbas M.; Al-Taay, H. F.; Jennings, P.; Lee, Wen-Jen

2018-04-01

Core-shell self-powered SiNWs homojunction photosensors have been fabricated. SiNWs are prepared by a metal assisted chemical etching method using different HF/H2O2 ratios and etching times. The length of the p-SiNWs increased as the H2O2 concentration and etching time increased. All the grown SiNWs show very low (∼0.7%) optical reflectance for the wavelength range of 200-1100 nm. Photoluminescence spectra of all prepared SiNWs show sharp and broad emission bands located in the red region of the light spectrum. Core-shell homojunction photosensors were fabricated by spin coating P2O2 onto the surface of the prepared p-SiNWs and annealed at 900 °C for 1 h. The fabricated devices exhibited photovoltaic behavior and high photosensitivity with fast response speed to the visible light. However, the sample that was fabricated using HF/H2O2 ratio of 1:1 showed the highest photosensitivity value of 3578% while the photosensor prepared using 2:1 ratio of HF/H2O2 gave the faster rise and decay time.

Preparation of Magnetic Hollow Molecularly Imprinted Polymers for Detection of Triazines in Food Samples.

PubMed

Wang, Aixiang; Lu, Hongzhi; Xu, Shoufang

2016-06-22

Novel magnetic hollow molecularly imprinted polymers (M-H-MIPs) were proposed for highly selective recognition and fast enrichment of triazines in food samples. M-H-MIPs were prepared on the basis of multi-step swelling polymerization, followed by in situ growth of magnetic Fe3O4 nanoparticles on the surface of hollow molecularly imprinted polymers (H-MIPs). Transmission electron microscopy and scanning electron microscopy confirmed the successful immobilization of Fe3O4 nanoparticles on the surface of H-MIPs. M-H-MIPs could be separated simply using an external magnet. The binding adsorption results indicated that M-H-MIPs displayed high binding capacity and fast mass transfer property and class selective property for triazines. Langmuir isotherm and pseudo-second-order kinetic models fitted the best adsorption models for M-H-MIPs. M-H-MIPs were used to analyze atrazine, simazine, propazine, and terbuthylazine in corn, wheat, and soybean samples. Satisfactory recoveries were in the range of 80.62-101.69%, and relative standard deviation was lower than 5.2%. Limits of detection from 0.16 to 0.39 μg L(-1) were obtained. When the method was applied to test positive samples that were contaminated with triazines, the results agree well with those obtained from an accredited method. Thus, the M-H-MIP-based dispersive solid-phase extraction method proved to be a convenient and practical platform for detection of triazines in food samples.

Effect of sample preparation method on sensory quality of cooked chicken breast fillets processed for food service

USDA-ARS?s Scientific Manuscript database

Chicken fillets (Pectoralis major) are one of popular items for food service. In the store, especially in fast food service stores, ready-to-cook meat products are commonly stored in freezers before use. The frozen meat can be cooked either directly from a frozen stage or after thawing. However, the...

Anesthesia and bariatric surgery gut preparation alter plasma acylcarnitines reflective of mitochondrial fat and branched-chain amino acid oxidation

USDA-ARS?s Scientific Manuscript database

The period around bariatric surgery offers a unique opportunity to characterize metabolism responds to dynamic shifts in energy, gut function, and anesthesia. We analyzed plasma acylcarnitines in obese women (n=17) sampled in the overnight fasted/postabsorptive state ca. 1-2 weeks prior to surgery ...

Fast quantification of bovine milk proteins employing external cavity-quantum cascade laser spectroscopy.

PubMed

Schwaighofer, Andreas; Kuligowski, Julia; Quintás, Guillermo; Mayer, Helmut K; Lendl, Bernhard

2018-06-30

Analysis of proteins in bovine milk is usually tackled by time-consuming analytical approaches involving wet-chemical, multi-step sample clean-up procedures. The use of external cavity-quantum cascade laser (EC-QCL) based IR spectroscopy was evaluated as an alternative screening tool for direct and simultaneous quantification of individual proteins (i.e. casein and β-lactoglobulin) and total protein content in commercial bovine milk samples. Mid-IR spectra of protein standard mixtures were used for building partial least squares (PLS) regression models. A sample set comprising different milk types (pasteurized; differently processed extended shelf life, ESL; ultra-high temperature, UHT) was analysed and results were compared to reference methods. Concentration values of the QCL-IR spectroscopy approach obtained within several minutes are in good agreement with reference methods involving multiple sample preparation steps. The potential application as a fast screening method for estimating the heat load applied to liquid milk is demonstrated. Copyright © 2018 Elsevier Ltd. All rights reserved.

Direct PCR Offers a Fast and Reliable Alternative to Conventional DNA Isolation Methods for Gut Microbiomes.

PubMed

Videvall, Elin; Strandh, Maria; Engelbrecht, Anel; Cloete, Schalk; Cornwallis, Charlie K

2017-01-01

The gut microbiome of animals is emerging as an important factor influencing ecological and evolutionary processes. A major bottleneck in obtaining microbiome data from large numbers of samples is the time-consuming laboratory procedures required, specifically the isolation of DNA and generation of amplicon libraries. Recently, direct PCR kits have been developed that circumvent conventional DNA extraction steps, thereby streamlining the laboratory process by reducing preparation time and costs. However, the reliability and efficacy of direct PCR for measuring host microbiomes have not yet been investigated other than in humans with 454 sequencing. Here, we conduct a comprehensive evaluation of the microbial communities obtained with direct PCR and the widely used Mo Bio PowerSoil DNA extraction kit in five distinct gut sample types (ileum, cecum, colon, feces, and cloaca) from 20 juvenile ostriches, using 16S rRNA Illumina MiSeq sequencing. We found that direct PCR was highly comparable over a range of measures to the DNA extraction method in cecal, colon, and fecal samples. However, the two methods significantly differed in samples with comparably low bacterial biomass: cloacal and especially ileal samples. We also sequenced 100 replicate sample pairs to evaluate repeatability during both extraction and PCR stages and found that both methods were highly consistent for cecal, colon, and fecal samples ( r s > 0.7) but had low repeatability for cloacal ( r s = 0.39) and ileal ( r s = -0.24) samples. This study indicates that direct PCR provides a fast, cheap, and reliable alternative to conventional DNA extraction methods for retrieving 16S rRNA data, which can aid future gut microbiome studies. IMPORTANCE The microbial communities of animals can have large impacts on their hosts, and the number of studies using high-throughput sequencing to measure gut microbiomes is rapidly increasing. However, the library preparation procedure in microbiome research is both costly and time-consuming, especially for large numbers of samples. We investigated a cheaper and faster direct PCR method designed to bypass the DNA isolation steps during 16S rRNA library preparation and compared it with a standard DNA extraction method. We used both techniques on five different gut sample types collected from 20 juvenile ostriches and sequenced samples with Illumina MiSeq. The methods were highly comparable and highly repeatable in three sample types with high microbial biomass (cecum, colon, and feces), but larger differences and low repeatability were found in the microbiomes obtained from the ileum and cloaca. These results will help microbiome researchers assess library preparation procedures and plan their studies accordingly.

Preparation of improved catalytic materials for water purification

NASA Astrophysics Data System (ADS)

Cherkezova-Zheleva, Z.; Paneva, D.; Tsvetkov, M.; Kunev, B.; Milanova, M.; Petrov, N.; Mitov, I.

2014-04-01

The aim of presented paper was to study preparation of catalytic materials for water purification. Iron oxide (Fe3O4) samples supported on activated carbon were prepared by wet impregnation method and low temperature heating in an inert atmosphere. The as-prepared, activated and samples after catalytic test were characterized by Mössbauer spectroscopy and X-ray diffraction. The obtained X-ray diffraction patterns of prepared samples show broad and low-intensity peaks of magnetite phase and the characteristic peaks of the activated carbon. The average crystallite size of magnetite particles was calculated below 20 nm. The registered Mössbauer spectra of prepared materials show a superposition of doublet lines or doublet and sextet components. The calculated hyperfine parameters after spectra evaluation reveal the presence of magnetite phase with nanosize particles. Relaxation phenomena were registered in both cases, i.e. superparamagnetism or collective magnetic excitation behavior, respectively. Low temperature Mössbauer spectra confirm this observation. Application of materials as photo-Fenton catalysts for organic pollutions degradation was studied. It was obtained high adsorption degree of dye, extremely high reaction rate and fast dye degradation. Photocatalytic behaviour of a more active sample was enhanced using mechanochemical activation (MCA). The nanometric size and high dispersion of photocatalyst particles influence both the adsorption and degradation mechanism of reaction. The results showed that all studied photocatalysts effectively decompose the organic pollutants under UV light irradiation. Partial oxidation of samples after catalytic tests was registered. Combination of magnetic particles with high photocatalytic activity meets both the requirements of photocatalytic degradation of water contaminants and that of recovery for cyclic utilization of material.

Assays for therapeutic drug monitoring of β-lactam antibiotics: A structured review.

PubMed

Carlier, Mieke; Stove, Veronique; Wallis, Steven C; De Waele, Jan J; Verstraete, Alain G; Lipman, Jeffrey; Roberts, Jason A

2015-10-01

In some patient groups, including critically ill patients, the pharmacokinetics of β-lactam antibiotics may be profoundly disturbed due to pathophysiological changes in distribution and elimination. Therapeutic drug monitoring (TDM) is a strategy that may help to optimise dosing. The aim of this review was to identify and analyse the published literature on the methods used for β-lactam quantification in TDM programmes. Sixteen reports described methods for the simultaneous determination of three or more β-lactam antibiotics in plasma/serum. Measurement of these antibiotics, due to low frequency of usage relative to some other tests, is generally limited to in-house chromatographic methods coupled to ultraviolet or mass spectrometric detection. Although many published methods state they are fit for TDM, they are inconvenient because of intensive sample preparation and/or long run times. Ideally, methods used for routine TDM should have a short turnaround time (fast run-time and fast sample preparation), a low limit of quantification and a sufficiently high upper limit of quantification. The published assays included a median of 6 analytes [interquartile range (IQR) 4-10], with meropenem and piperacillin being the most frequently measured β-lactam antibiotics. The median run time was 8 min (IQR 5.9-21.3 min). There is also a growing number of methods measuring free concentrations. An assay that measures antibiotics without any sample preparation would be the next step towards real-time monitoring; no such method is currently available. Copyright © 2015 Elsevier B.V. and the International Society of Chemotherapy. All rights reserved.

Fast determination of diphenhydramine hydrochloride in reconstitutable syrups by CWT, PLS AND PCR methods.

PubMed

Devrim, Burcu; Dinç, Erdal; Bozkir, Asuman

2014-01-01

Diphenhydramine hydrochloride (DPH), a histamine H1-receptor antagonist, is widely used as antiallergic, antiemetic and antitussive drug found in many pharmaceutical preparations. In this study, a new reconstitutable syrup formulation of DPH was prepared because it is more stable in solid form than that in liquid form. The quantitative estimation of the DPH content of a reconstitutable syrup formulation in the presence of pharmaceutical excipients, D-sorbitol, sodium citrate, sodium benzoate and sodium EDTA is not possible by the direct absorbance measurement. Therefore, a signal processing approach based on continuous wavelet transform was used to determine the DPH in the reconstitutable syrup formulations and to eliminate the effect of excipients on the analysis. The absorption spectra of DPH in the range of 5.0-40.0 μg/mL were recorded between 200-300 nm. Various wavelet families were tested and Biorthogonal1.1 continuous wavelet transform (BIOR1.1-CWT) was found to be optimal signal processing family to get fast and desirable determination results and to overcome excipient interference effects. For a comparison of the experimental results obtained by partial least squares (PLS) and principal component regression (PCR) methods were applied to the quantitative prediction of DPH in the mentioned samples. The validity of the proposed BIOR1.1-CWT, PLS and PCR methods were achieved analyzing the prepared samples containing the mentioned excipients and using standard addition technique. It was observed that the proposed graphical and numerical approaches are suitable for the quantitative analysis of DPH in samples including excipients.

Preparation of Low-Input and Ligation-Free ChIP-seq Libraries Using Template-Switching Technology.

PubMed

Bolduc, Nathalie; Lehman, Alisa P; Farmer, Andrew

2016-10-10

Chromatin immunoprecipitation (ChIP) followed by high-throughput sequencing (ChIP-seq) has become the gold standard for mapping of transcription factors and histone modifications throughout the genome. However, for ChIP experiments involving few cells or targeting low-abundance transcription factors, the small amount of DNA recovered makes ligation of adapters very challenging. In this unit, we describe a ChIP-seq workflow that can be applied to small cell numbers, including a robust single-tube and ligation-free method for preparation of sequencing libraries from sub-nanogram amounts of ChIP DNA. An example ChIP protocol is first presented, resulting in selective enrichment of DNA-binding proteins and cross-linked DNA fragments immobilized on beads via an antibody bridge. This is followed by a protocol for fast and easy cross-linking reversal and DNA recovery. Finally, we describe a fast, ligation-free library preparation protocol, featuring DNA SMART technology, resulting in samples ready for Illumina sequencing. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

Fast Lithium-Ion Transportation in Crystalline Polymer Electrolytes.

PubMed

Fu, Xiao-Bin; Yang, Guang; Wu, Jin-Ze; Wang, Jia-Chen; Chen, Qun; Yao, Ye-Feng

2018-01-05

Fast lithium-ion transportation is found in the crystalline polymer electrolytes, α-CD-PEO n /Li + (n=12, 40), prepared by self-assembly of α-cyclodextrin (CD), polyethylene oxide (PEO) and Li + salts. A detailed solid-state NMR study combined with the X-ray diffraction technique reveals the unique structural features of the samples, that is, a) the tunnel structure formed by the assembled CDs, providing the ordered long-range pathway for Li + ion transportation; b) the all-trans conformational sequence of the PEO chains in the tunnels, attenuating significantly the coordination between Li + and the EO segments. The origin of the fast lithium-ion transportation has been attributed to these unique structural features. This work demonstrates the first example in solid polymer electrolytes (SPEs) for "creating" fast ion transportation through material design and will find potential applications in the design of new ionconducting SPE materials. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Atmospheric vs. anaerobic processing of metabolome samples for the metabolite profiling of a strict anaerobic bacterium, Clostridium acetobutylicum.

PubMed

Lee, Sang-Hyun; Kim, Sooah; Kwon, Min-A; Jung, Young Hoon; Shin, Yong-An; Kim, Kyoung Heon

2014-12-01

Well-established metabolome sample preparation is a prerequisite for reliable metabolomic data. For metabolome sampling of a Gram-positive strict anaerobe, Clostridium acetobutylicum, fast filtration and metabolite extraction with acetonitrile/methanol/water (2:2:1, v/v) at -20°C under anaerobic conditions has been commonly used. This anaerobic metabolite processing method is laborious and time-consuming since it is conducted in an anaerobic chamber. Also, there have not been any systematic method evaluation and development of metabolome sample preparation for strict anaerobes and Gram-positive bacteria. In this study, metabolome sampling and extraction methods were rigorously evaluated and optimized for C. acetobutylicum by using gas chromatography/time-of-flight mass spectrometry-based metabolomics, in which a total of 116 metabolites were identified. When comparing the atmospheric (i.e., in air) and anaerobic (i.e., in an anaerobic chamber) processing of metabolome sample preparation, there was no significant difference in the quality and quantity of the metabolomic data. For metabolite extraction, pure methanol at -20°C was a better solvent than acetonitrile/methanol/water (2:2:1, v/v/v) at -20°C that is frequently used for C. acetobutylicum, and metabolite profiles were significantly different depending on extraction solvents. This is the first evaluation of metabolite sample preparation under aerobic processing conditions for an anaerobe. This method could be applied conveniently, efficiently, and reliably to metabolome analysis for strict anaerobes in air. © 2014 Wiley Periodicals, Inc.

Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods

USDA-ARS?s Scientific Manuscript database

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChE...

Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry for ultratrace analysis of pesticide residues in baby food.

PubMed

Hercegová, Andrea; Dömötörová, Milena; Kruzlicová, Dása; Matisová, Eva

2006-05-01

Four sample preparation techniques were compared for the ultratrace analysis of pesticide residues in baby food: (a) modified Schenck's method based on ACN extraction with SPE cleaning; (b) quick, easy, cheap, effective, rugged, and safe (QuEChERS) method based on ACN extraction and dispersive SPE; (c) modified QuEChERS method which utilizes column-based SPE instead of dispersive SPE; and (d) matrix solid phase dispersion (MSPD). The methods were combined with fast gas chromatographic-mass spectrometric analysis. The effectiveness of clean-up of the final extract was determined by comparison of the chromatograms obtained. Time consumption, laboriousness, demands on glassware and working place, and consumption of chemicals, especially solvents, increase in the following order QuEChERS < modified QuEChERS < MSPD < modified Schenck's method. All methods offer satisfactory analytical characteristics at the concentration levels of 5, 10, and 100 microg/kg in terms of recoveries and repeatability. Recoveries obtained for the modified QuEChERS method were lower than for the original QuEChERS. In general the best LOQs were obtained for the modified Schenck's method. Modified QuEChERS method provides 21-72% better LOQs than the original method.

Receptor-based screening assays for the detection of antibiotics residues - A review.

PubMed

Ahmed, Saeed; Ning, Jianan; Cheng, Guyue; Ahmad, Ijaz; Li, Jun; Mingyue, Liu; Qu, Wei; Iqbal, Mujahid; Shabbir, M A B; Yuan, Zonghui

2017-05-01

Consumer and regulatory agencies have a high concern to antibiotic residues in food producing animals, so appropriate screening assays of fast, sensitive, low cost, and easy sample preparation for the identification of these residues are essential for the food-safety insurance. Great efforts in the development of a high-throughput antibiotic screening assay have been made in recent years. Concerning the screening of antibiotic residue, this review elaborate an overview on the availability, advancement and applicability of antibiotic receptor based screening assays for the safety assessment of antibiotics usage (i.e. radio receptor assay, enzyme labeling assays, colloidal gold receptor assay, enzyme colorimetry assay and biosensor assay). This manuscript also tries to shed a light on the selection, preparation and future perspective of receptor protein for antibiotic residue detection. These assays have been introduced for the screening of numerous food samples. Receptor based screening technology for antibiotic detection has high accuracy. It has been concluded that at the same time, it can detect a class of drugs for certain receptor, and realize the multi-residue detection. These assays offer fast, easy and precise detection of antibiotics. Copyright © 2017 Elsevier B.V. All rights reserved.

Microplates in liquid chromatography--new solution in clinical research? A review.

PubMed

Krcmova, Lenka; Solichova, Dagmar; Solich, Petr

2013-10-15

Microplates are routinely used in Radio- or Immuno-assays. Recently, microplates have found use not only in analytical but also in the pre-analytical phase in bioanalyses (sample storage, sample preparation). New connection of this technology to liquid chromatography could be economical, fast and simple solution for many routine laboratories handling large sequences of biological samples. This review summarises the application of microplates in bioanalytical laboratories. Different types of sorbents, materials and shapes of microplates are discussed, and the main advantages and disadvantages of microplates used in clinical research are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Classification of jet fuels by fuzzy rule-building expert systems applied to three-way data by fast gas chromatography--fast scanning quadrupole ion trap mass spectrometry.

PubMed

Sun, Xiaobo; Zimmermann, Carolyn M; Jackson, Glen P; Bunker, Christopher E; Harrington, Peter B

2011-01-30

A fast method that can be used to classify unknown jet fuel types or detect possible property changes in jet fuel physical properties is of paramount interest to national defense and the airline industries. While fast gas chromatography (GC) has been used with conventional mass spectrometry (MS) to study jet fuels, fast GC was combined with fast scanning MS and used to classify jet fuels into lot numbers or origin for the first time by using fuzzy rule-building expert system (FuRES) classifiers. In the process of building classifiers, the data were pretreated with and without wavelet transformation and evaluated with respect to performance. Principal component transformation was used to compress the two-way data images prior to classification. Jet fuel samples were successfully classified with 99.8 ± 0.5% accuracy for both with and without wavelet compression. Ten bootstrapped Latin partitions were used to validate the generalized prediction accuracy. Optimized partial least squares (o-PLS) regression results were used as positively biased references for comparing the FuRES prediction results. The prediction results for the jet fuel samples obtained with these two methods were compared statistically. The projected difference resolution (PDR) method was also used to evaluate the fast GC and fast MS data. Two batches of aliquots of ten new samples were prepared and run independently 4 days apart to evaluate the robustness of the method. The only change in classification parameters was the use of polynomial retention time alignment to correct for drift that occurred during the 4-day span of the two collections. FuRES achieved perfect classifications for four models of uncompressed three-way data. This fast GC/fast MS method furnishes characteristics of high speed, accuracy, and robustness. This mode of measurement may be useful as a monitoring tool to track changes in the chemical composition of fuels that may also lead to property changes. Copyright © 2010 Elsevier B.V. All rights reserved.

Use of CTX-I and PINP as bone turnover markers: National Bone Health Alliance recommendations to standardize sample handling and patient preparation to reduce pre-analytical variability.

PubMed

Szulc, P; Naylor, K; Hoyle, N R; Eastell, R; Leary, E T

2017-09-01

The National Bone Health Alliance (NBHA) recommends standardized sample handling and patient preparation for C-terminal telopeptide of type I collagen (CTX-I) and N-terminal propeptide of type I procollagen (PINP) measurements to reduce pre-analytical variability. Controllable and uncontrollable patient-related factors are reviewed to facilitate interpretation and minimize pre-analytical variability. The IOF and the International Federation of Clinical Chemistry (IFCC) Bone Marker Standards Working Group have identified PINP and CTX-I in blood to be the reference markers of bone turnover for the fracture risk prediction and monitoring of osteoporosis treatment. Although used in clinical research for many years, bone turnover markers (BTM) have not been widely adopted in clinical practice primarily due to their poor within-subject and between-lab reproducibility. The NBHA Bone Turnover Marker Project team aim to reduce pre-analytical variability of CTX-I and PINP measurements through standardized sample handling and patient preparation. Recommendations for sample handling and patient preparations were made based on review of available publications and pragmatic considerations to reduce pre-analytical variability. Controllable and un-controllable patient-related factors were reviewed to facilitate interpretation and sample collection. Samples for CTX-I must be collected consistently in the morning hours in the fasted state. EDTA plasma is preferred for CTX-I for its greater sample stability. Sample collection conditions for PINP are less critical as PINP has minimal circadian variability and is not affected by food intake. Sample stability limits should be observed. The uncontrollable aspects (age, sex, pregnancy, immobility, recent fracture, co-morbidities, anti-osteoporotic drugs, other medications) should be considered in BTM interpretation. Adopting standardized sample handling and patient preparation procedures will significantly reduce controllable pre-analytical variability. The successful adoption of such recommendations necessitates the close collaboration of various stakeholders at the global stage, including the laboratories, the medical community, the reagent manufacturers and the regulatory agencies.

The Successful Diagnosis and Typing of Systemic Amyloidosis Using A Microwave-Assisted Filter-Aided Fast Sample Preparation Method and LC/MS/MS Analysis

PubMed Central

Zou, Lili; Shen, Kaini; Zhong, Dingrong; Zhou, Daobin; Sun, Wei; Li, Jian

2015-01-01

Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove contaminants with a 10-kDa cutoff ultrafiltration unit and can accelerate the digestion process with the assistance of a microwave. Additionally, two parameters (P- and D-scores) based on the exponentially modified protein abundance index were developed to define the existence of amyloid deposits and those causative proteins with the greatest abundance. Using our protocol, twenty cases of systemic amyloidosis that were well-typed according to clinical diagnostic standards (training group) and another twenty-four cases without subtype diagnoses (validation group) were analyzed. Using this approach, sample preparation could be completed within four hours. We successfully subtyped 100% of the cases in the training group, and the diagnostic success rate in the validation group was 91.7%. This maFASP-aided proteomic protocol represents an efficient approach for amyloid diagnosis and subtyping, particularly for serum-contaminated samples. PMID:25984759

Sampling and Homogenization Strategies Significantly Influence the Detection of Foodborne Pathogens in Meat.

PubMed

Rohde, Alexander; Hammerl, Jens Andre; Appel, Bernd; Dieckmann, Ralf; Al Dahouk, Sascha

2015-01-01

Efficient preparation of food samples, comprising sampling and homogenization, for microbiological testing is an essential, yet largely neglected, component of foodstuff control. Salmonella enterica spiked chicken breasts were used as a surface contamination model whereas salami and meat paste acted as models of inner-matrix contamination. A systematic comparison of different homogenization approaches, namely, stomaching, sonication, and milling by FastPrep-24 or SpeedMill, revealed that for surface contamination a broad range of sample pretreatment steps is applicable and loss of culturability due to the homogenization procedure is marginal. In contrast, for inner-matrix contamination long treatments up to 8 min are required and only FastPrep-24 as a large-volume milling device produced consistently good recovery rates. In addition, sampling of different regions of the spiked sausages showed that pathogens are not necessarily homogenously distributed throughout the entire matrix. Instead, in meat paste the core region contained considerably more pathogens compared to the rim, whereas in the salamis the distribution was more even with an increased concentration within the intermediate region of the sausages. Our results indicate that sampling and homogenization as integral parts of food microbiology and monitoring deserve more attention to further improve food safety.

Sampling and Homogenization Strategies Significantly Influence the Detection of Foodborne Pathogens in Meat

PubMed Central

Rohde, Alexander; Hammerl, Jens Andre; Appel, Bernd; Dieckmann, Ralf; Al Dahouk, Sascha

2015-01-01

Efficient preparation of food samples, comprising sampling and homogenization, for microbiological testing is an essential, yet largely neglected, component of foodstuff control. Salmonella enterica spiked chicken breasts were used as a surface contamination model whereas salami and meat paste acted as models of inner-matrix contamination. A systematic comparison of different homogenization approaches, namely, stomaching, sonication, and milling by FastPrep-24 or SpeedMill, revealed that for surface contamination a broad range of sample pretreatment steps is applicable and loss of culturability due to the homogenization procedure is marginal. In contrast, for inner-matrix contamination long treatments up to 8 min are required and only FastPrep-24 as a large-volume milling device produced consistently good recovery rates. In addition, sampling of different regions of the spiked sausages showed that pathogens are not necessarily homogenously distributed throughout the entire matrix. Instead, in meat paste the core region contained considerably more pathogens compared to the rim, whereas in the salamis the distribution was more even with an increased concentration within the intermediate region of the sausages. Our results indicate that sampling and homogenization as integral parts of food microbiology and monitoring deserve more attention to further improve food safety. PMID:26539462

Advances in biological dosimetry

NASA Astrophysics Data System (ADS)

Ivashkevich, A.; Ohnesorg, T.; Sparbier, C. E.; Elsaleh, H.

2017-01-01

Rapid retrospective biodosimetry methods are essential for the fast triage of persons occupationally or accidentally exposed to ionizing radiation. Identification and detection of a radiation specific molecular ‘footprint’ should provide a sensitive and reliable measurement of radiation exposure. Here we discuss conventional (cytogenetic) methods of detection and assessment of radiation exposure in comparison to emerging approaches such as gene expression signatures and DNA damage markers. Furthermore, we provide an overview of technical and logistic details such as type of sample required, time for sample preparation and analysis, ease of use and potential for a high throughput analysis.

Construction of super - hydrophobic copper alloy surface by one - step mixed solution immersion method

NASA Astrophysics Data System (ADS)

Gu, Qiang; Chen, Ying; Chen, Dong; Zhang, Zeting

2018-01-01

This paper presents a method for preparing a super hydrophobic surface with a fast, simple, low-cost, one-step reaction by immersing copper alloy in an ethanol solution containing silver nitrate and myristic acid. The effects of reaction time, reaction temperature, reactant concentration and reaction time on the wettability of the material were studied. The surface wettability, appearance, chemical composition, durability and chemical stability of the prepared samples was measured by water contact angle (CA), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results show that when the reaction time is only 10min, the surface WCA of the prepared material can reach 154.9. This study provides an effective method for the rapid preparation of stable super hydrophobic surfaces.

[Research of preparation craft of Danshen phenolic acid fast release unit in multi-drug delivery system of Tongmai micro-pellets].

PubMed

Chen, Bin; Xiao, Wei; Jia, Xiao-Bin; Huang, Yang

2012-07-01

To prepare Danshen phenolic acid fast release micro-pellets and study its preparation craft. The factors which could impact yield, extrude shaping, dissolution of Danshen phenolic acid micro-pellets such as wetting agent, drug loading dose, adjuvant, lactose dose, disintegrant, CMS-Na dose and wetting agent dose was investigated. The optimum preparation craft of Danshen phenolic acid fast release micro-pellets was screened out by orhogonal design. Formula of Danshen phenolic acid fast release micro-pellets was calculated as volume dose 50 g. The formula was as follows: principal agent 22.5 g, lactose 5 g, CMS-Na 2 g, MCC 20.5 g, 27 mL 30% ethanol as wetting agent. Extrusion-spheronization was applied. The optimum conditions were screened out as follows: extrusion frequency (25 Hz), spheronization machine frequency (50 Hz), spheronization time (4 min). The process was scientific and rational. The preparation is stable settles basis for multi-drug delivery system of Tongmai micro-pellets.

How we eat what we eat: identifying meal routines and practices most strongly associated with healthy and unhealthy dietary factors among young adults.

PubMed

Laska, Melissa N; Hearst, Mary O; Lust, Katherine; Lytle, Leslie A; Story, Mary

2015-08-01

(i) To examine associations between young adults' meal routines and practices (e.g. food preparation, meal skipping, eating on the run) and key dietary indicators (fruit/vegetable, fast-food and sugar-sweetened beverage intakes) and (ii) to develop indices of protective and risky meal practices most strongly associated with diet. Cross-sectional survey. Minneapolis/St. Paul metropolitan area, Minnesota (USA). A diverse sample of community college and public university students (n 1013). Meal routines and practices most strongly associated with healthy dietary patterns were related to home food preparation (i.e. preparing meals at home, preparing meals with vegetables) and meal regularity (i.e. routine consumption of evening meals and breakfast). In contrast, factors most strongly associated with poor dietary patterns included eating on the run, using media while eating and purchasing foods/beverages on campus. A Protective Factors Index, summing selected protective meal routines and practices, was positively associated with fruit/vegetable consumption and negatively associated with fast-food and sugar-sweetened beverage consumption (P<0·001). A Risky Factors Index yielded significant, positive associations with fast-food and sugar-sweetened beverage consumption (P<0·001). The probability test for the association between the Risky Factors Index and fruit/vegetable intake was P=0·05. Meal routines and practices were significantly associated with young adults' dietary patterns, suggesting that ways in which individuals structure mealtimes and contextual characteristics of eating likely influence food choice. Thus, in addition to considering specific food choices, it also may be important to consider the context of mealtimes in developing dietary messaging and guidelines.

How we eat what we eat: Identifying meal routines and practices most strongly associated with healthy and unhealthy dietary factors among young adults

PubMed Central

Laska, Melissa N.; Hearst, Mary O.; Lust, Katherine; Lytle, Leslie; Story, Mary

2017-01-01

Objectives (a) To examine associations between young adult meal routines and practices (e.g., food preparation, meal skipping, eating on the run) and key dietary indicators (fruit/vegetable, fast food and sugar-sweetened beverage intake), and (b) to develop indices of protective and risky meal practices most strongly associated with diet. Design Cross-sectional survey. Setting Minneapolis/St. Paul metropolitan area, Minnesota (USA). Subjects A diverse sample of community college and public university (n=1,013) students. Results Meal routines and practices most strongly associated with healthy dietary patterns were related to home food preparation (i.e., preparing meals at home, preparing meals with vegetables) and meal regularity (i.e., routine consumption of evening meals and breakfast). In contrast, factors most strongly associated with poor dietary patterns included eating on the run, using media while eating, and purchasing foods/beverages on campus. A Protective Factors Index, summing selected protective meal routines and practices, was positively associated with fruit/vegetable consumption, and negatively associated with fast food and sugar-sweetened beverage consumption (p<0.001). A Risky Factors Index yielded significant, positive associations with fast food and sugar sweetened beverage (p<0.001) consumption. The probability test for the association between the Risky Factors Index and fruit/vegetable intake was p=0.05. Conclusions Meal routines and practices were significantly associated with young adult dietary patterns, suggesting that ways in which individuals structure mealtimes and contextual characteristics of eating likely influence food choice. Thus, in addition to considering specific food choices, it also may be important to consider the context of mealtimes in developing dietary messaging and guidelines. PMID:25439511

Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

NASA Astrophysics Data System (ADS)

López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

2007-01-01

A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

Dithizone modified magnetic nanoparticles for fast and selective solid phase extraction of trace elements in environmental and biological samples prior to their determination by ICP-OES.

PubMed

Cheng, Guihong; He, Man; Peng, Hanyong; Hu, Bin

2012-01-15

A fast and simple method for analysis of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II) in environmental and biological samples was developed by combining magnetic solid phase extraction (MSPE) with inductively coupled plasma-optical emission spectrometry (ICP-OES) detection. Dithizone modified silica-coated magnetic Fe(3)O(4) nanoparticles (H(2)Dz-SCMNPs) were prepared and used for MSPE of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II). The prepared magnetic nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The factors affecting the extraction of the target metal ions such as pH, sample volume, eluent, and interfering ions had been investigated and the adsorption mechanism of the target metals on the self-prepared H(2)Dz-SCMNPs was investigated by FT-IR and X-ray photo electron spectroscopy (XPS). Under the optimized conditions, the detection limits of the developed method for Cr(III), Cu(II), Pb(II) and Zn(II) were 35, 11, 62, and 8ngL(-1), respectively, with the enrichment factor of 100. The relative standard deviations (RSDs, c=10μgL(-1), n=7) were in the range of 1.7-3.1% and the linear range was 0.1-100μgL(-1). The proposed method had been validated by two certified reference materials (GSBZ50009-88 environmental water and GBW07601 human hair), and the determined values were in good agreement with the certified values. The method was also applied for the determination of trace metals in real water and human hair samples with recoveries in the range of 85-110% for the spiked samples. The developed MSPE-ICP-OES method has the advantages of simplicity, rapidity, selectivity, high extraction efficiency and is suitable for the analysis of samples with large volume and complex matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

Testing of an automated online EA-IRMS method for fast and simultaneous carbon content and stable isotope measurement of aerosol samples

NASA Astrophysics Data System (ADS)

Major, István; Gyökös, Brigitta; Túri, Marianna; Futó, István; Filep, Ágnes; Hoffer, András; Molnár, Mihály

2016-04-01

Comprehensive atmospheric studies have demonstrated that carbonaceous aerosol is one of the main components of atmospheric particulate matter over Europe. Various methods, considering optical or thermal properties, have been developed for quantification of the accurate amount of both organic and elemental carbon constituents of atmospheric aerosol. The aim of our work was to develop an alternative fast and easy method for determination of the total carbon content of individual aerosol samples collected on prebaked quartz filters whereby the mass and surface concentration becomes simply computable. We applied the conventional "elemental analyzer (EA) coupled online with an isotope ratio mass spectrometer (IRMS)" technique which is ubiquitously used in mass spectrometry. Using this technique we are able to measure simultaneously the carbon stable isotope ratio of the samples, as well. During the developing process, we compared the EA-IRMS technique with an off-line catalytic combustion method worked out previously at Hertelendi Laboratory of Environmental Studies (HEKAL). We tested the combined online total carbon content and stable isotope ratio measurement both on standard materials and real aerosol samples. Regarding the test results the novel method assures, on the one hand, at least 95% of carbon recovery yield in a broad total carbon mass range (between 100 and 3000 ug) and, on the other hand, a good reproducibility of stable isotope measurements with an uncertainty of ± 0.2 per mill. Comparing the total carbon results obtained by the EA-IRMS and the off-line catalytic combustion method we found a very good correlation (R2=0.94) that proves the applicability of both preparation method. Advantages of the novel method are the fast and simplified sample preparation steps and the fully automated, simultaneous carbon stable isotope ratio measurement processes. Furthermore stable isotope ratio results can effectively be applied in the source apportionment investigations of atmospheric carbonaceous aerosol. This research was supported by the European Union and the State of Hungary, co-financed by the European Social Fund in the framework of TÁMOP 4.2.4.A/2-11-1-2012-0001 'National Excellence Program.

Peptide Analysis Using Tandem Mass Spectrometry

DTIC Science & Technology

1989-06-01

to give pyroglutamic acid during storage, eliminating ammonia. It is almost absent in the spectrum of a freshly-prepared sample and is not seen in...USING TANDEM MASS SPECTROMETRY INTRODUCTION S The objective of the project was to determine the complete amino acid sequence of the large polypeptide...Ubiquitin by use of fast atom bombardment (FAB) ionization and tandem mass spectrometry. The peptide containing 76 amino acid residues was available

Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

The “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) approach to sample preparation is widely applied in pesticide residue analysis, but the use of magnesium sulfate for salting out in the method is not ideal for mass spectrometry. In this study we developed and evaluated three new diffe...

A Fast and Effective Microfluidic Spraying-Plunging Method for High-Resolution Single-Particle Cryo-EM.

PubMed

Feng, Xiangsong; Fu, Ziao; Kaledhonkar, Sandip; Jia, Yuan; Shah, Binita; Jin, Amy; Liu, Zheng; Sun, Ming; Chen, Bo; Grassucci, Robert A; Ren, Yukun; Jiang, Hongyuan; Frank, Joachim; Lin, Qiao

2017-04-04

We describe a spraying-plunging method for preparing cryoelectron microscopy (cryo-EM) grids with vitreous ice of controllable, highly consistent thickness using a microfluidic device. The new polydimethylsiloxane (PDMS)-based sprayer was tested with apoferritin. We demonstrate that the structure can be solved to high resolution with this method of sample preparation. Besides replacing the conventional pipetting-blotting-plunging method, one of many potential applications of the new sprayer is in time-resolved cryo-EM, as part of a PDMS-based microfluidic reaction channel to study short-lived intermediates on the timescale of 10-1,000 ms. Published by Elsevier Ltd.

Dietary exposure of Canadians to perfluorinated carboxylates and perfluorooctane sulfonate via consumption of meat, fish, fast foods, and food items prepared in their packaging.

PubMed

Tittlemier, Sheryl A; Pepper, Karen; Seymour, Carol; Moisey, John; Bronson, Roni; Cao, Xu-Liang; Dabeka, Robert W

2007-04-18

Human exposure to perfluorinated compounds is a worldwide phenomenon; however, routes of human exposure to these compounds have not been well-characterized. Fifty-four solid food composite samples collected as part of the Canadian Total Diet Study (TDS) were analyzed for perfluorocarboxylates and perfluorooctanesulfonate (PFOS) using a methanol extraction liquid chromatography tandem mass spectrometry method. Foods analyzed included fish and seafood, meat, poultry, frozen entrées, fast food, and microwave popcorn collected from 1992 to 2004 and prepared as for consumption. Nine composites contained detectable levels of perfluorinated compounds-four meat-containing, three fish and shellfish, one fast food, and one microwave popcorn. PFOS and perfluorooctanoate (PFOA) were detected the most frequently; concentrations ranged from 0.5 to 4.5 ng/g. The average dietary intake of total perfluorocarboxylates and PFOS for Canadians was estimated to be 250 ng/day, using results from the 2004 TDS composites. A comparison with intakes of perfluorocarboxylates and PFOS via other routes (air, water, dust, treated carpeting, and apparel) suggested that diet is an important source of these compounds. There was a substantial margin of exposure between the toxicological points of reference and the magnitude of dietary intake of perfluorinated compounds for Canadians >/= 12 years old.

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

Nieroda, Pawel; Zybala, Rafal; Wojciechowski, Krzysztof T.

The aim of the study was to develop a fast and simple method for preparation of polycrystalline Mg{sub 2}Si. For this purpose a Spark Plasma Sintering (SPS) method was used and synthesis conditions were adjusted in such a manner that no excess Mg was required. Materials were synthesized by the direct reaction of Mg and Si raw powders. To determine the phase and chemical composition, the fabricated samples were studied by X-ray diffraction and SEM microscopy coupled with EDX chemical analysis. Thermoelectric properties of samples (thermal conductivity, electrical conductivity and Seebeck coefficient) were measured all over temperature range of 300-650more » K. The analysis by the scanning thermoelectric microprobe (STM) shows that samples have uniform distribution of Seebeck coefficient with mean value of about -405 {mu}VK{sup -1} and standard deviation of 94 {mu}VK{sup -1}. Prepared materials have intrinsic band gap of 0.45 eV and thermal conductivity {lambda}= 7.5 Wm{sup -1}K{sup -1} at room temperature.« less

Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

PubMed

Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

2017-05-12

A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

Imaging of fullerene-like structures in CNx thin films by electron microscopy; sample preparation artefacts due to ion-beam milling.

PubMed

Czigány, Zs; Neidhardt, J; Brunell, I F; Hultman, L

2003-04-01

The microstructure of CN(x) thin films, deposited by reactive magnetron sputtering, was investigated by transmission electron microscopy (TEM) at 200kV in plan-view and cross-sectional samples. Imaging artefacts arise in high-resolution TEM due to overlap of nm-sized fullerene-like features for specimen thickness above 5nm. The thinnest and apparently artefact-free areas were obtained at the fracture edges of plan-view specimens floated-off from NaCl substrates. Cross-sectional samples were prepared by ion-beam milling at low energy to minimize sample preparation artefacts. The depth of the ion-bombardment-induced surface amorphization was determined by TEM cross sections of ion-milled fullerene-like CN(x) surfaces. The thickness of the damaged surface layer at 5 degrees grazing incidence was 13 and 10nm at 3 and 0.8keV, respectively, which is approximately three times larger than that observed on Si prepared under the same conditions. The shallowest damage depth, observed for 0.25keV, was less than 1nm. Chemical changes due to N loss and graphitization were also observed by X-ray photoelectron spectroscopy. As a consequence of chemical effects, sputtering rates of CN(x) films were similar to that of Si, which enables relatively fast ion-milling procedure compared to carbon compounds. No electron beam damage of fullerene-like CN(x) was observed at 200kV.

Process for preparing phenolic formaldehyde resole resin products derived from fractionated fast-pyrolysis oils

DOEpatents

Chum, Helena L.; Kreibich, Roland E.

1992-01-01

A process for preparing phenol-formaldehyde resole resins and adhesive compositions in which portions of the phenol normally contained in said resins are replaced by a phenol/neutral fractions extract obtained from fractionating fast-pyrolysis oils.

Fast preconcentration of trace rare earth elements from environmental samples by di(2-ethylhexyl)phosphoric acid grafted magnetic nanoparticles followed by inductively coupled plasma mass spectrometry detection

NASA Astrophysics Data System (ADS)

Yan, Ping; He, Man; Chen, Beibei; Hu, Bin

2017-10-01

In this work, di(2-ethylhexyl)phosphoric acid (P204) grafted magnetic nanoparticles were synthesized by fabricating P204 onto Fe3O4@TiO2 nanoparticles based on Lewis acid-base interaction between Ti and phosphate group under weakly acidic condition. The prepared Fe3O4@TiO2@P204 nanoparticles exhibited excellent selectivity for rare earth elements, and good anti-interference ability. Based on it, a method of magnetic solid phase extraction (MSPE) combined with inductively coupled plasma mass spectrometry (ICP-MS) was developed for fast preconcentration and determination of trace rare earth elements in environmental samples. Under the optimal conditions, the detection limits of rare earth elements were in the range of 0.01 (Tm)-0.12 (Nd) ng L- 1 with an enrichment factor of 100-fold, and the relative standard deviations ranged from 4.9 (Pr) to 10.7% (Er). The proposed method was successfully applied to the determination of rare earth elements in environmental samples, including river water, lake water, seawater and sediment.

Fast cholesterol detection using flow injection microfluidic device with functionalized carbon nanotubes based electrochemical sensor.

PubMed

Wisitsoraat, A; Sritongkham, P; Karuwan, C; Phokharatkul, D; Maturos, T; Tuantranont, A

2010-12-15

This work reports a new cholesterol detection scheme using functionalized carbon nanotube (CNT) electrode in a polydimethylsiloxane/glass based flow injection microfluidic chip. CNTs working, silver reference and platinum counter electrode layers were fabricated on the chip by sputtering and low temperature chemical vapor deposition methods. Cholesterol oxidase prepared in polyvinyl alcohol solution was immobilized on CNTs by in-channel flow technique. Cholesterol analysis based on flow injection chronoamperometric measurement was performed in 150-μm-wide and 150-μm-deep microchannels. Fast and sensitive real-time detection was achieved with high throughput of more than 60 samples per hour and small sample volume of 15 μl. The cholesterol sensor had a linear detection range between 50 and 400 mg/dl. In addition, low cross-sensitivities toward glucose, ascorbic acid, acetaminophen and uric acid were confirmed. The proposed system is promising for clinical diagnostics of cholesterol with high speed real-time detection capability, very low sample consumption, high sensitivity, low interference and good stability. Copyright © 2010 Elsevier B.V. All rights reserved.

Rapid, portable, multiplexed detection of bacterial pathogens directly from clinical sample matrices

DOE PAGES

Phaneuf, Christopher R.; Mangadu, Betty Lou Bosano; Piccini, Matthew E.; ...

2016-09-23

Enteric and diarrheal diseases are a major cause of childhood illness and death in countries with developing economies. Each year, more than half of a million children under the age of five die from these diseases. We have developed a portable, microfluidic platform capable of simultaneous, multiplexed detection of several of the bacterial pathogens that cause these diseases. Furthermore, this platform can perform fast, sensitive immunoassays directly from relevant, complex clinical matrices such as stool without extensive sample cleanup or preparation. Using only 1 µL of sample per assay, we demonstrate simultaneous multiplexed detection of four bacterial pathogens implicated inmore » diarrheal and enteric diseases in less than 20 min.« less

Rapid, portable, multiplexed detection of bacterial pathogens directly from clinical sample matrices

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

Phaneuf, Christopher R.; Mangadu, Betty Lou Bosano; Piccini, Matthew E.

Enteric and diarrheal diseases are a major cause of childhood illness and death in countries with developing economies. Each year, more than half of a million children under the age of five die from these diseases. We have developed a portable, microfluidic platform capable of simultaneous, multiplexed detection of several of the bacterial pathogens that cause these diseases. Furthermore, this platform can perform fast, sensitive immunoassays directly from relevant, complex clinical matrices such as stool without extensive sample cleanup or preparation. Using only 1 µL of sample per assay, we demonstrate simultaneous multiplexed detection of four bacterial pathogens implicated inmore » diarrheal and enteric diseases in less than 20 min.« less

Thermal Diffusivity of High-Density Polyethylene Samples of Different Crystallinity Evaluated by Indirect Transmission Photoacoustics

NASA Astrophysics Data System (ADS)

Nesic, M.; Popovic, M.; Rabasovic, M.; Milicevic, D.; Suljovrujic, E.; Markushev, D.; Stojanovic, Z.

2018-02-01

In this work, thermal diffusivity of crystalline high-density polyethylene samples of various thickness, and prepared using different procedures, was evaluated by transmission gas-microphone frequency photoacoustics. The samples' composition analysis and their degree of crystallinity were determined from the wide-angle X-ray diffraction, which confirmed that high-density polyethylene samples, obtained by slow and fast cooling, were equivalent in composition but with different degrees of crystallinity. Structural analysis, performed by differential scanning calorimetry, demonstrated that all of the used samples had different levels of crystallinity, depending not only on the preparing procedure, but also on sample thickness. Therefore, in order to evaluate the samples' thermal diffusivity, it was necessary to modify standard photoacoustic fitting procedures (based on the normalization of photoacoustic amplitude and phase characteristics on two thickness levels) for the interpretation of photoacoustic measurements. The calculated values of thermal diffusivity were in the range of the expected literature values. Besides that, the obtained results indicate the unexpected correlation between the values of thermal diffusivity and thermal conductivity with the degree of crystallinity of the investigated geometrically thin samples. The results indicate the necessity of additional investigation of energy transport in macromolecular systems, as well as the possible employment of the photoacoustic techniques in order to clarify its mechanism.

Reduced detection by Ziehl-Neelsen method of acid-fast bacilli in sputum samples preserved in cetylpyridinium chloride solution.

PubMed

Selvakumar, N; Sudhamathi, S; Duraipandian, M; Frieden, T R; Narayanan, P R

2004-02-01

Twelve health facilities implementing the DOTS strategy, and the Tuberculosis Research Centre (TRC), Chennai, India. To determine the detection rates using Ziehl-Neelsen (ZN) and auramine-phenol to stain acid-fast bacilli (AFB) in sputum samples stored in cetylpyridinium chloride (CPC) solution. Two smears were prepared from each of 988 sputum samples collected in CPC and randomly allocated, one to ZN and the other to auramine-phenol staining. All samples were processed for culture of Mycobacterium tuberculosis. A significantly higher proportion of samples were negative using the ZN method compared to the auramine-phenol method (74.5% vs. 61.8%, McNamara's paired chi2 test; P < 0.001). Among 377 samples that were positive using auramine-phenol, 44% were negative using ZN. There were more culture-positive, smear-negative samples in ZN (52.7%) than in auramine-phenol (30%); the difference attained statistical significance (McNemar's paired chi2 test; P < 0.00004). Using ZN, of the 104 smears made immediately after collection, 52 were positive for AFB, of which only 35 (67.3%) were positive after storage in CPC; the reduction in the number of positive smears attained statistical significance (McNemar's paired chi2 test; P = 0.004). Detection of AFB in sputum samples preserved in CPC is significantly reduced using ZN staining.

Making the practically impossible "Merely difficult"--Cryogenic FIB lift-out for "Damage free" soft matter imaging.

PubMed

Parmenter, Christopher D J; Fay, Michael W; Hartfield, Cheryl; Eltaher, Hoda M

2016-04-01

The preparation of thinned lamellae from bulk samples for transmission electron microscopy (TEM) analysis has been possible in the focussed ion beam scanning electron microscope (FIB-SEM) for over 20 years via the in situ lift-out method. Lift-out offers a fast and site specific preparation method for TEM analysis, typically in the field of materials science. More recently it has been applied to a low-water content biological sample (Rubino 2012). This work presents the successful lift-out of high-water content lamellae, under cryogenic conditions (cryo-FIB lift-out) and using a nanomanipulator retaining its full range of motion, which are advances on the work previously done by Rubino (2012). Strategies are explored for maintaining cryogenic conditions, grid attachment using cryo-condensation of water and protection of the lamella when transferring to the TEM. © 2016 Wiley Periodicals, Inc.

Reducing Time and Increasing Sensitivity in Sample Preparation for Adherent Mammalian Cell Metabolomics

PubMed Central

Lorenz, Matthew A.; Burant, Charles F.; Kennedy, Robert T.

2011-01-01

A simple, fast, and reproducible sample preparation procedure was developed for relative quantification of metabolites in adherent mammalian cells using the clonal β-cell line INS-1 as a model sample. The method was developed by evaluating the effect of different sample preparation procedures on high performance liquid chromatography- mass spectrometry quantification of 27 metabolites involved in glycolysis and the tricarboxylic acid cycle on a directed basis as well as for all detectable chromatographic features on an undirected basis. We demonstrate that a rapid water rinse step prior to quenching of metabolism reduces components that suppress electrospray ionization thereby increasing signal for 26 of 27 targeted metabolites and increasing total number of detected features from 237 to 452 with no detectable change of metabolite content. A novel quenching technique is employed which involves addition of liquid nitrogen directly to the culture dish and allows for samples to be stored at −80 °C for at least 7 d before extraction. Separation of quenching and extraction steps provides the benefit of increased experimental convenience and sample stability while maintaining metabolite content similar to techniques that employ simultaneous quenching and extraction with cold organic solvent. The extraction solvent 9:1 methanol: chloroform was found to provide superior performance over acetonitrile, ethanol, and methanol with respect to metabolite recovery and extract stability. Maximal recovery was achieved using a single rapid (~1 min) extraction step. The utility of this rapid preparation method (~5 min) was demonstrated through precise metabolite measurements (11% average relative standard deviation without internal standards) associated with step changes in glucose concentration that evoke insulin secretion in the clonal β-cell line INS-1. PMID:21456517

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.

Influence of the cooling rate and the blend ratio on the physical stability of co-amorphous naproxen/indomethacin.

PubMed

Beyer, Andreas; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2016-12-01

Co-amorphization represents a promising approach to increase the physical stability and dissolution rate of amorphous active pharmaceutical ingredients (APIs) as an alternative to polymer glass solutions. For amorphous and co-amorphous systems, it is reported that the preparation method and the blend ratio play major roles with regard to the resulting physical stability. Therefore, in the present study, co-amorphous naproxen-indomethacin (NAP/IND) was prepared by melt-quenching at three different cooling rates and at ten different NAP/IND blend ratios. The samples were analyzed using XRPD and FTIR, both directly after preparation and during storage to investigate their physical stabilities. All cooling methods led to fully amorphous samples, but with significantly different physical stabilities. Samples prepared by fast cooling had a higher degree of crystallinity after 300d of storage than samples prepared by intermediate cooling and slow cooling. Intermediate cooling was subsequently used to prepare co-amorphous NAP/IND at different blend ratios. In a previous study, it was postulated that the equimolar (0.5:0.5) co-amorphous blend of NAP/IND is most stable. However, in the present study the physically most stable blend was found for a NAP/IND ratio of 0.6:0.4, which also represents the eutectic composition of the crystalline NAP/γ-IND system. This indicates that the eutectic point may be of major importance for the stability of binary co-amorphous systems. Slight deviations from the optimal naproxen molar fraction led to significant recrystallization during storage. Either naproxen or γ-indomethacin recrystallized until a naproxen molar fraction of about 0.6 in the residual co-amorphous phase was reached again. In conclusion, the physical stability of co-amorphous NAP/IND may be significantly improved, if suitable preparation conditions and the optimal phase composition are chosen. Copyright © 2016 Elsevier B.V. All rights reserved.

Fast screening of short-chain chlorinated paraffins in indoor dust samples by graphene-assisted laser desorption/ionization mass spectrometry.

PubMed

Huang, Xiu; Liu, Qian; Gao, Wei; Wang, Yawei; Nie, Zhou; Yao, Shouzhuo; Jiang, Guibin

2018-03-01

As an important class of emerging chemical contaminants, short-chain chlorinated paraffins (SCCPs) are considered as one of the most challenging groups of compounds to analyze. In this paper, we report a new method for fast screening of SCCPs based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) with graphene as a matrix and 2,5,6,9-tetrachlorodecane as an internal standard. We found that the use of graphene as MALDI matrix generated high peak intensities for SCCPs while producing few background noises. The ion fragmentation mechanisms of SCCPs in MALDI are discussed in detail. Under the optimized conditions, much lower detection limits of SCCP congeners (0.1-5ng/mL) than those reported previously were obtained. Other distinct advantages such as short analysis time and simplified sample preparation procedures are also demonstrated. The method was successfully applied in fast screening of SCCPs in indoor dust samples and monitoring of human exposure levels to SCCPs, and the results were verified by gas chromatography coupled to negative chemical ionization quadrupole time-of-flight high-resolution mass spectrometry. This work not only offers a new promising tool for SCCP studies, but also further demonstrates the promise of graphene as a new generation of MALDI matrix. Copyright © 2017 Elsevier B.V. All rights reserved.

A new dimethyl labeling-based SID-MRM-MS method and its application to three proteases involved in insulin maturation.

PubMed

Cheng, Dongwan; Zheng, Li; Hou, Junjie; Wang, Jifeng; Xue, Peng; Yang, Fuquan; Xu, Tao

2015-01-01

The absolute quantification of target proteins in proteomics involves stable isotope dilution coupled with multiple reactions monitoring mass spectrometry (SID-MRM-MS). The successful preparation of stable isotope-labeled internal standard peptides is an important prerequisite for the SID-MRM absolute quantification methods. Dimethyl labeling has been widely used in relative quantitative proteomics and it is fast, simple, reliable, cost-effective, and applicable to any protein sample, making it an ideal candidate method for the preparation of stable isotope-labeled internal standards. MRM mass spectrometry is of high sensitivity, specificity, and throughput characteristics and can quantify multiple proteins simultaneously, including low-abundance proteins in precious samples such as pancreatic islets. In this study, a new method for the absolute quantification of three proteases involved in insulin maturation, namely PC1/3, PC2 and CPE, was developed by coupling a stable isotope dimethyl labeling strategy for internal standard peptide preparation with SID-MRM-MS quantitative technology. This method offers a new and effective approach for deep understanding of the functional status of pancreatic β cells and pathogenesis in diabetes.

Preparation of Nickel Aluminum-Manganese Spinel Oxides Ni xAl 1- xMn 2O 4 for Oxygen Electrocatalysis in Alkaline Medium: Comparison of Properties Stemming from Different Preparation Methods

NASA Astrophysics Data System (ADS)

Ponce, Jilberto; Ríos, Edmundo; Rehspringer, Jean-Luc; Poillerat, Gérard; Chartier, Pierre; Gautier, Juan Luis

1999-06-01

Two different procedures were used to prepare spinel-type NixAl1-xMn2O4 (0≤x≤1) compounds to study the effects of solid state properties of mixed oxides on their electrocatalytic properties. The oxalic route, coprecipitation of metal oxalates dissolved in propanol or ethanol, and the propionic route, hydrolysis of metal carboxylates in propionic acid, have been used. In both routes, thermal decomposition produces the corresponding oxides. X-ray diffraction patterns showed that the oxides crystallize in a cubic spinel phase with a unit cell parameter a that increases as aluminum is replaced by nickel. At low x values, compounds prepared by the propionic route showed a larger variation for parameter a than compounds prepared by the oxalic route, probably due to oxygen stoichiometric deficiency. This effect was estimated from the tetrahedral force constant (kt) values, which showed a fast decrease as x varied from 0 to 1. Electrical conductivity, conduction activation energy, hole mobility, and pHz of oxides prepared by the propionic route were also higher than those from oxides prepared by the oxalic route. Crystallinity grade and particle size were nearly 50‧ higher in propionic-route samples than in oxalic-route samples. The apparent and real electrocatalytic activities of both types of oxides were compared for O2 evolution.

Green and Fast Laser Fusion Technique for Bulk Silicate Rock Analysis by Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Zhang, Chenxi; Hu, Zhaochu; Zhang, Wen; Liu, Yongsheng; Zong, Keqing; Li, Ming; Chen, Haihong; Hu, Shenghong

2016-10-18

Sample preparation of whole-rock powders is the major limitation for their accurate and precise elemental analysis by laser ablation inductively-coupled plasma mass spectrometry (ICPMS). In this study, a green, efficient, and simplified fusion technique using a high energy infrared laser was developed for major and trace elemental analysis. Fusion takes only tens of milliseconds for each sample. Compared to the pressed pellet sample preparation, the analytical precision of the developed laser fusion technique is higher by an order of magnitude for most elements in granodiorite GSP-2. Analytical results obtained for five USGS reference materials (ranging from mafic to intermediate to felsic) using the laser fusion technique generally agree with recommended values with discrepancies of less than 10% for most elements. However, high losses (20-70%) of highly volatile elements (Zn and Pb) and the transition metal Cu are observed. The achieved precision is within 5% for major elements and within 15% for most trace elements. Direct laser fusion of rock powders is a green and notably simple method to obtain homogeneous samples, which will significantly accelerate the application of laser ablation ICPMS for whole-rock sample analysis.

Well-defined magnetic surface imprinted nanoparticles for selective enrichment of 2,4-dichlorophenoxyacetic acid in real samples.

PubMed

Sheng, Le; Jin, Yulong; He, Yonghuan; Huang, Yanyan; Yan, Liushui; Zhao, Rui

2017-11-01

Superparamagnetic core-shell molecularly imprinted polymer nanoparticles (MIPs) were prepared via surface initiated reversible-addition fragmentation chain transfer (si-RAFT) polymerization for the selective recognition of 2,4-dichlorophenoxyacetic acid (2,4-D) in real samples. The construction of uniform core-shell structure with a 50nm MIP layer was successfully accomplished, which favored mass transfer and resulted in fast recognition kinetics. The static equilibrium experiments revealed the satisfied adsorption capacity and imprinting efficiency of Fe 3 O 4 @MIP. Moreover, the Fe 3 O 4 @MIP exhibited high selectivity and affinity towards 2,4-D over structural analogues. The prepared Fe 3 O 4 @MIP nanoparticles were used for the selective enrichment of 2,4-D in tap water and Chinese cabbage samples. Combined with RP-HPLC, the recoveries of 2,4-D were calculated from 93.1% to 103.3% with RSD of 1.7-5.4% (n = 3) in Chinese cabbage samples. This work provides a versatile approach for fabricating well-constructed core-shell MIP nanoparticles for rapid enrichment and highly selective separation of target molecules in real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Use of the Falcon assay screening test--enzyme-linked immunosorbent assay (FAST-ELISA) and the enzyme-linked immunoelectrotransfer blot (EITB) to determine the prevalence of human fascioliasis in the Bolivian Altiplano.

PubMed

Hillyer, G V; Soler de Galanes, M; Rodriguez-Perez, J; Bjorland, J; Silva de Lagrava, M; Ramirez Guzman, S; Bryan, R T

1992-05-01

A collaborative study between the University of Puerto Rico School of Medicine, the Centers for Disease Control, the Bolivian Ministry of Health, and private voluntary organizations (Foster Parents Plan International and Danchurchaid) working in Bolivia has identified a region in the northwestern Altiplano of Bolivia near Lake Titicaca as harboring the highest prevalence of human fascioliasis in the world reported to date. Two serologic techniques (the Falcon assay screening test-enzyme-linked immunosorbent assay [FAST-ELISA] and the enzyme-linked immunoelectrotransfer blot [EITB]) were used in the determination of its prevalence. One hundred serum samples and 73 stool samples were obtained from Aymara Indians from Corapata, Bolivia. Antibody absorbance levels to Fasciola hepatica excretion-secretion antigens were compared with EITB banding patterns using the same antigen preparation. A positive FAST-ELISA result was defined as an absorbance value greater than the mean plus three standard deviations of two sets of normal negative controls (Puerto Rican and Bolivian). Using this criterion, 53 of 100 sera tested were found positive by this technique. Within this group, 19 (95%) of 20 individuals who were parasite positive were also positive by FAST-ELISA. An additional 24 individuals who were negative for F. hepatica eggs and 10 individuals for whom no specimens were received were also positive by FAST-ELISA. Among the 53 individuals negative for F. hepatica eggs, 29 were also negative by FAST-ELISA. The EITB analysis of the sera from confirmed infected individuals revealed at least three F. hepatica (Fh) bands with molecular weights of 12, 17, and 63 kD, respectively.(ABSTRACT TRUNCATED AT 250 WORDS)

Fast preparation of ultrafine monolayered transition-metal dichalcogenide quantum dots using electrochemical shock for explosive detection.

PubMed

Chen, Zhigang; Tao, Zhengxu; Cong, Shan; Hou, Junyu; Zhang, Dengsong; Geng, Fengxia; Zhao, Zhigang

2016-09-15

A simple, general and fast method called "electrochemical shock" is developed to prepare monolayered transition-metal dichalcogenide (TMD) QDs with an average size of 2-4 nm and an average thickness of 0.85 ± 0.5 nm with only about 10 min of ultrasonication. Just like nails hammered into a plate, the electrochemical shock with Al 3+ ions and the following extraction with the help of oleic acid can disintegrate bulk TMD crystals into ultrafine TMD QDs. The fast-prepared QDs are then applied to detect highly explosive molecules such as 2,4,6-trinitrophenol (TNP) with a low detection limit of 10 -6 M. Our versatile method could be broadly applicable for the fast production of ultrathin QDs of other materials with great promise for various applications.

Linear Quantitative Profiling Method Fast Monitors Alkaloids of Sophora Flavescens That Was Verified by Tri-Marker Analyses.

PubMed

Hou, Zhifei; Sun, Guoxiang; Guo, Yong

2016-01-01

The present study demonstrated the use of the Linear Quantitative Profiling Method (LQPM) to evaluate the quality of Alkaloids of Sophora flavescens (ASF) based on chromatographic fingerprints in an accurate, economical and fast way. Both linear qualitative and quantitative similarities were calculated in order to monitor the consistency of the samples. The results indicate that the linear qualitative similarity (LQLS) is not sufficiently discriminating due to the predominant presence of three alkaloid compounds (matrine, sophoridine and oxymatrine) in the test samples; however, the linear quantitative similarity (LQTS) was shown to be able to obviously identify the samples based on the difference in the quantitative content of all the chemical components. In addition, the fingerprint analysis was also supported by the quantitative analysis of three marker compounds. The LQTS was found to be highly correlated to the contents of the marker compounds, indicating that quantitative analysis of the marker compounds may be substituted with the LQPM based on the chromatographic fingerprints for the purpose of quantifying all chemicals of a complex sample system. Furthermore, once reference fingerprint (RFP) developed from a standard preparation in an immediate detection way and the composition similarities calculated out, LQPM could employ the classical mathematical model to effectively quantify the multiple components of ASF samples without any chemical standard.

The utility of direct agglutination (DAT) and fast agglutination screening (FAST) tests in serodiagnosis of experimental microsporidiosis.

PubMed

Abou El Naga, Iman F; Gaafar, Maha R; El-Zawawy, Lobna A; El-Said, Doaa; Mossallam, Sherin F

2008-12-01

The present study was designed to evaluate the efficiency of two serodiagnostic tests; the direct agglutination test (DAT) and the fast agglutination screening test (FAST) in the diagnosis of Microsporidia in experimentally infected mice and to differentiate between different species of the parasite. The swiss albino mice were divided into non infected control and infected experimental groups which were further subdivided into ten subgroups. Ten samples of microsporidial spores were isolated from ten human stools and each one was used to infect each subgroup of mice. Stool and sera were collected weekly from each subgroup from the 1st to the 4th week post infection (PI). DAT & FAST tests, using antigen prepared from the different species of microsporidial spores were used to detect antibodies in sera of different mice subgroups. The cross reactivity of microsporidial spores with the antibodies of Cyclospora cyatenensis and Cryptosporidium parvum was investigated by DAT & FAST. The results proved that DAT & FAST were effective in detecting microsporidial antibodies in sera of experimentally infected mice from the 2nd week PI till the end of the study, without cross reactivity with C. cyatenensis or C. parvum. They failed to differentiate between different Microspoiridia species used but, they gave good interpretation and they were specific and sensitive, and did not need sophisticated equipments.

A Fast Solution to NGS Library Prep with Low Nanogram DNA Input

PubMed Central

Liu, Pingfang; Lohman, Gregory J.S.; Cantor, Eric; Langhorst, Bradley W.; Yigit, Erbay; Apone, Lynne M.; Munafo, Daniela B.; Stewart, Fiona J.; Evans, Thomas C.; Nichols, Nicole; Dimalanta, Eileen T.; Davis, Theodore B.; Sumner, Christine

2013-01-01

Next Generation Sequencing (NGS) has significantly impacted human genetics, enabling a comprehensive characterization of the human genome as well as a better understanding of many genomic abnormalities. By delivering massive DNA sequences at unprecedented speed and cost, NGS promises to make personalized medicine a reality in the foreseeable future. To date, library construction with clinical samples has been a challenge, primarily due to the limited quantities of sample DNA available. Our objective here was to overcome this challenge by developing NEBNext® Ultra DNA Library Prep Kit, a fast library preparation method. Specifically, we streamlined the workflow utilizing novel NEBNext reagents and adaptors, including a new DNA polymerase that has been optimized to minimize GC bias. As a result of this work, we have developed a simple method for library construction from an amount of DNA as low as 5 ng, which can be used for both intact and fragmented DNA. Moreover, the workflow is compatible with multiple NGS platforms.

Fingerprinting and characterization of anthocyanins in 94 colored wheat varieties and blue aleurone and purple pericarp wheat crosses.

PubMed

Krüger, Stephanie; Morlock, Gertrud E

2018-02-23

Colored wheat varieties and crosses were analyzed to figure out their anthocyanin profiles, and thus, their potential as health-related food. After method development, the obtained 94 anthocyanin fingerprints allowed the clear differentiation of the blue aleurone and purple pericarp genotypes as well as their breeding lines. The method was trimmed so that the complete analysis of the whole grain flour including sample preparation of up to 20 samples on one plate took less than 3 h (<9 min per sample) and total costs including sample preparation were <1.0 Euro/sample. Sample preparation of the complex wheat matrix was reduced to a minimum (only acidified methanol extraction of the ground whole wheat grain). Separation was well achieved on amino phases with a mixture of ethyl acetate, 2-butanone, water and formic acid. It was superior to the separation on either normal or reversed phases and more robust with regard to intrinsic pH variances of the sample extracts. Pattern recognition of anthocyanins was simply performed by visual detection (the image), a key feature of high-performance thin-layer chromatography. Wheat varieties and crosses with higher anthocyanin contents were easily selectable, and thus, successfully made out. Prominent anthocyanin zones were characterized by electrospray ionization mass spectrometry. Their sugar moiety was characterized via methanolysis and compared with the sugars available freely in the whole wheat grain. The developed profiling is a fast and efficient screening tool with option for quantification or identification on the same HPTLC plate. Copyright © 2018 Elsevier B.V. All rights reserved.

Differences in nutrient and energy contents of commonly consumed dishes prepared in restaurants v. at home in Hunan Province, China.

PubMed

Jia, Xiaofang; Liu, Jiawu; Chen, Bo; Jin, Donghui; Fu, Zhongxi; Liu, Huilin; Du, Shufa; Popkin, Barry M; Mendez, Michelle A

2018-05-01

Eating away from home is associated with poor diet quality, in part due to less healthy food choices and larger portions. However, few studies account for the potential additional contribution of differences in food composition between restaurant- and home-prepared dishes. The present study aimed to investigate differences in nutrients of dishes prepared in restaurants v. at home. Eight commonly consumed dishes were collected in twenty of each of the following types of locations: small and large restaurants, and urban and rural households. In addition, two fast-food items were collected from ten KFC, McDonald's and food stalls. Five samples per dish were randomly pooled from every location. Nutrients were analysed and energy was calculated in composite samples. Differences in nutrients of dishes by preparation location were determined. Hunan Province, China. Na, K, protein, total fat, fatty acids, carbohydrate and energy in dishes. On average, both the absolute and relative fat contents, SFA and Na:K ratio were higher in dishes prepared in restaurants than households (P < 0·05). Protein was 15 % higher in animal food-based dishes prepared in households than restaurants (P<0·05). Quantile regression models found that, at the 90th quantile, restaurant preparation was consistently negatively associated with protein and positively associated with the percentage of energy from fat in all dishes. Moreover, restaurant preparation also positively influenced the SFA content in dishes, except at the highest quantiles. These findings suggest that compared with home preparation, dishes prepared in restaurants in China may differ in concentrations of total fat, SFA, protein and Na:K ratio, which may further contribute, beyond food choices, to less healthy nutrient intakes linked to eating away from home.

Differences in nutrient and energy content of commonly-consumed dishes prepared in restaurants vs. at home in Hunan province, China

PubMed Central

Jia, Xiaofang; Liu, Jiawu; Chen, Bo; Jin, Donghui; Fu, Zhongxi; Liu, Huilin; Du, Shufa; Popkin, Barry M.; Mendez, Michelle A.

2017-01-01

Objective Eating away from home is associated with poor diet quality, in part due to less healthy food choices and larger portions. However, few studies take into account the potential additional contribution of differences in food composition between restaurant- and home-prepared dishes. This study aimed to investigate differences in nutrients of dishes prepared in restaurants vs. at home. Design Eight commonly consumed dishes were collected in 20 of each of the following types of locations: small and large restaurants, and urban and rural households. In addition, two fast-food items were collected from 10 KFC’s, McDonald’s, and food stalls. Five samples per dish were randomly pooled from every location. Nutrients were analyzed and energy was calculated in composite samples. Differences in nutrients of dishes by preparation location were determined. Setting Urban and rural. Subjects Sodium, potassium, protein, total fat, fatty acids, carbohydrate, and energy in dishes. Results On average, both the absolute and relative fat content, saturated fatty acid (SFA) and sodium/potassium ratio were higher in dishes prepared in restaurants than households (P<0.05). Protein was 15% higher in animal food-based dishes prepared in households than restaurants (P <0.05). Quantile regression models found that, at the 90th quantile, restaurant preparation was consistently negatively associated with protein and positively associated with the percentage energy from fat in all dishes. Moreover, restaurant preparation also positively influenced the SFA content in dishes, except at the highest quantiles. Conclusions These findings suggest that compared to home preparation, dishes prepared in restaurants in China may differ in concentrations of total fat, SFA, protein, and sodium/potassium ratio, which may further contribute, beyond food choices, to less healthy nutrient intake linked to eating away from home. PMID:29306339

Online reverse phase-high-performance liquid chromatography-fluorescence detection-electrospray ionization-mass spectrometry separation and characterization of heparan sulfate, heparin, and low-molecular weight-heparin disaccharides derivatized with 2-aminoacridone.

PubMed

Galeotti, Fabio; Volpi, Nicola

2011-09-01

A high-resolution online reverse-phase-high-performance liquid chromatography (RP-HPLC)-fluorescence detector (Fd)-electrospray ionization-mass spectrometry (ESI-MS) separation and structural characterization of disaccharides prepared from heparin (Hep), heparan sulfate (HS), and various low-molecular-weight (LMW)-Hep using heparin lyases and derivatization with 2-aminoacridone (AMAC) are described. A total of 12 commercially available Hep/HS-derived unsaturated disaccharides were separated and unambiguously identified on the basis of their retention times and mass spectra. The constituent disaccharides of various samples, including unfractionated Hep/HS, fast-moving and slow-moving Hep components, and several marketed products, were characterized. Furthermore, for the first time, the saturated trisulfated disaccharide belonging to the nonreducing end of Heps was detected as being approximately 2% in unfractionated samples and ~15-21% in LMW-Heps prepared by nitrous acid depolymerization. No desalting of the commercial products prior to enzymatic digestion or prepurification steps to eliminate any excess of AMAC reagent or interference from proteins, peptides, and other sample impurities before RP-HPLC-Fd-ESI-MS injection were necessary. This method has applicability for the rapid differentiation of pharmaceutical Heps and LMW-Heps prepared by means of different depolymerization processes and for compositional analysis of small amounts of samples derived from biological sources by using the highly sensitive fluorescence detector.

Electromechanical properties of polyamide/lycra fabric treated with PEDOT:PSS

NASA Astrophysics Data System (ADS)

Tadesse, M. G.; Mengistie, D. A.; Loghin, C.; Chen, Y.; Wang, L.; Catalin, D.; Müller, C.; Nierstrasz, V.

2017-10-01

One of the challenges in smart textiles is to develop suitable multifunctional materials that can address simultaneously several characteristics such as durability, stretchability, lightweight, and conductivity. Conductive polymers which showed success in different technological fields like polymer solar cells and light emitting diodes are promising in many smart textile applications. In this work, we treated a common polyamide/lycra knitted fabric with PEDOT:PSS for stretchable e-textiles. PEDOT:PSS, with DMSO as a conductivity enhancer and different ratios of water-based polyurethane dispersions as a binder, was applied to the fabric with simple immersion and coating applications. The effect of different application methods and binder ratio on the surface resistance of the fabric was monitored with four point probe electrical surface resistance measurement systems. Samples prepared by immersion technique are more uniform and have higher conductivity than those prepared by a coating technique. SEM images showed that PEDOT:PSS is incorporated into the structure in the immersion method while in the coating it is majorly present on the surface of the fabric. The tensile measurement showed that the acidic PEDOT:PSS and polyurethane dispersion coating has no adverse effect on the tensile strength of the fabric. The coated samples can be stretched up to 700% while still reasonably conductive. The resistance increases only by a small amount when samples were stretched cyclically by stretching 100%. Generally, samples prepared by the immersion method maintained better conductivity while stretching than those by a coating method. The washing fastness of the samples was also assessed.

Assessment of the characteristics and biocompatibility of gelatin sponge scaffolds prepared by various crosslinking methods.

PubMed

Yang, Gang; Xiao, Zhenghua; Long, Haiyan; Ma, Kunlong; Zhang, Junpeng; Ren, Xiaomei; Zhang, Jiang

2018-01-25

This comparative study aims to identify a biocompatible and effective crosslinker for preparing gelatin sponges. Glutaraldehyde (GTA), genipin (GP), 1-ethyl-3-(3-dimethyl aminopropyl)carbodiimide (EDC), and microbial transglutaminase (mTG) were used as crosslinking agents. The physical properties of the prepared samples were characterized, and material degradation was studied in vitro with various proteases and in vivo through subcutaneous implantation of the sponges in rats. Adipose-derived stromal stem cells (ADSCs) were cultured and inoculated onto the scaffolds to compare the cellular biocompatibility of the sponges. Cellular seeding efficiency and digestion time of the sponges were also evaluated. Cellular viability and proliferation in scaffolds were analyzed by fluorescence staining and MTT assay. All the samples exhibited high porosity, good swelling ratio, and hydrolysis properties; however, material strength, hydrolysis, and enzymolytic properties varied among the samples. GTA-sponge and GP-sponge possessed high compressive moduli, and EDC-sponge exhibited fast degradation performance. GTA and GP sponge implants exerted strong in vivo rejections, and the former showed poor cell growth. mTG-sponge exhibited the optimal comprehensive performance, with good porosity, compressive modulus, anti-degradation ability, and good biocompatibility. Hence, mTG-sponge can be used as a scaffold material for tissue engineering applications.

Optical and electrical studies of cerium mixed oxides

NASA Astrophysics Data System (ADS)

Sherly, T. R.; Raveendran, R.

2014-10-01

The fast development in nanotechnology makes enthusiastic interest in developing nanomaterials having tailor made properties. Cerium mixed oxide materials have received great attention due to their UV absorption property, high reactivity, stability at high temperature, good electrical property etc and these materials find wide applications in solid oxide fuel cells, solar control films, cosmetics, display units, gas sensors etc. In this study cerium mixed oxide compounds were prepared by co-precipitation method. All the samples were doped with Zn (II) and Fe (II). Preliminary characterizations such as XRD, SEM / EDS, TEM were done. UV - Vis, Diffuse reflectance, PL, FT-IR, Raman and ac conductivity studies of the samples were performed.

Laser-based measurements of δ13 C and δ2 H methane isotope signatures: precisions competitive with mass spectrometry methods

NASA Astrophysics Data System (ADS)

Yacovitch, Tara; Shorter, Joanne; Nelson, David; Herndon, Scott; Agnese, Mike; McManus, Barry; Zahniser, Mark

2017-04-01

In order to understand how and why methane (CH4 ) concentrations change over time, it is necessary to understand their sources and sinks. Stable isotope measurements of 13 CH4 :12 CH4 and CH3 D:12 CH4 ratios constrain the inventory of these sinks and sources. Current measurements often depend on Isotope Ratio Mass Spectrometry (IRMS), which requires extensive sample preparation including cryogenic separation of methane from air and subsequent conversion to either CO2 or H2 . Here, we detail improvements to a direct-absorption laser spectrometer that enable fast and precise measurements of methane isotope ratios (δ13 C and δ2 H ) of ambient air samples, without such sample preparation. The measurement system consists of a laser-based direct absorption spectrometer configured with a sample manifold for measurement of discrete samples (as opposed to flow-through measurements). Samples are trapped in the instrument using a rapid sample switching technique that compares each flask sample against a monitor tank sample. This approach reduces instrument drift and results in excellent precision. Precisions of 0.054 o/oo for δ13 C and 1.4 o/oo for δ2 H have been achieved (Allan-Werle deviations). These results are obtained in 20 minutes using 4 replicate comparisons to a monitor tank.

Investigating obesity risk-reduction behaviours and psychosocial factors in Chinese Americans.

PubMed

Liou, Doreen; Bauer, Kathleen; Bai, Yeon

2014-11-01

The purpose of this research was to examine the attitudes, beliefs and behaviours related to obesity risk reduction in Chinese Americans. A questionnaire was administered to a convenience sample of 300 US-born and foreign-born Chinese Americans residing in the New York metropolitan area, ranging from 18 to 40 years of age. Obesity risk reduction behaviours and psychosocial variables derived from the Theory of Planned Behaviour and Health Belief Model were measured. Acculturation was assessed using a modified Suinn-Lew Asian Self-Identity Acculturation Scale. Frequency distributions were delineated and stepwise regression analyses were analysed for different acculturation groups. 65% of the respondents were female and the mean age of the sample was 26 years. Respondents indicated the most commonly practised behaviour to be eating home-cooked meals instead of restaurant-prepared foods. Perceived barriers to adopting obesity risk-reduction behaviours included convenience of consuming fast foods, cost, lack of time to prepare home-cooked meals, and the physical environment of unhealthy foods. In predicting intention to perform obesity risk-reduction behaviours, attitude was significant for 'western-identified' individuals. In 'Asian-identified' individuals, perceived behavioural control, self-efficacy and perceived benefits were salient. Nutrition educators working with Chinese Americans need to address self-efficacy in preparing plant-based, home-cooked meals and making healthy choices at fast-food restaurants with portion control. Concrete and perceived barriers such as lack of time and convenience need to be addressed in nutrition education interventions. Educators need to identify new channels and media outlets to disseminate practical, easy-to-implement behaviours for obesity risk reduction that are socially acceptable. © Royal Society for Public Health 2013.

GRAPPA reconstructed wave-CAIPI MP-RAGE at 7 Tesla.

PubMed

Schwarz, Jolanda M; Pracht, Eberhard D; Brenner, Daniel; Reuter, Martin; Stöcker, Tony

2018-04-16

The aim of this project was to develop a GRAPPA-based reconstruction for wave-CAIPI data. Wave-CAIPI fully exploits the 3D coil sensitivity variations by combining corkscrew k-space trajectories with CAIPIRINHA sampling. It reduces artifacts and limits reconstruction induced spatially varying noise enhancement. The GRAPPA-based wave-CAIPI method is robust and does not depend on the accuracy of coil sensitivity estimations. We developed a GRAPPA-based, noniterative wave-CAIPI reconstruction algorithm utilizing multiple GRAPPA kernels. For data acquisition, we implemented a fast 3D magnetization-prepared rapid gradient-echo wave-CAIPI sequence tailored for ultra-high field application. The imaging results were evaluated by comparing the g-factor and the root mean square error to Cartesian CAIPIRINHA acquisitions. Additionally, to assess the performance of subcortical segmentations (calculated by FreeSurfer), the data were analyzed across five subjects. Sixteen-fold accelerated whole brain magnetization-prepared rapid gradient-echo data (1 mm isotropic resolution) were acquired in 40 seconds at 7T. A clear improvement in image quality compared to Cartesian CAIPIRINHA sampling was observed. For the chosen imaging protocol, the results of 16-fold accelerated wave-CAIPI acquisitions were comparable to results of 12-fold accelerated Cartesian CAIPIRINHA. In comparison to the originally proposed SENSitivity Encoding reconstruction of Wave-CAIPI data, the GRAPPA approach provided similar image quality. High-quality, wave-CAIPI magnetization-prepared rapid gradient-echo images can be reconstructed by means of a GRAPPA-based reconstruction algorithm. Even for high acceleration factors, the noniterative reconstruction is robust and does not require coil sensitivity estimations. By altering the aliasing pattern, ultra-fast whole-brain structural imaging becomes feasible. © 2018 International Society for Magnetic Resonance in Medicine.

Graphene oxide membrane as an efficient extraction and ionization substrate for spray-mass spectrometric analysis of malachite green and its metabolite in fish samples.

PubMed

Wei, Shih-Chun; Fan, Shen; Lien, Chia-Wen; Unnikrishnan, Binesh; Wang, Yi-Sheng; Chu, Han-Wei; Huang, Chih-Ching; Hsu, Pang-Hung; Chang, Huan-Tsung

2018-03-20

A graphene oxide (GO) nanosheet-modified N + -nylon membrane (GOM) has been prepared and used as an extraction and spray-ionization substrate for robust mass spectrometric detection of malachite green (MG), a highly toxic disinfectant in liquid samples and fish meat. The GOM is prepared by self-deposition of GO thin film onto an N + -nylon membrane, which has been used for efficient extraction of MG in aquaculture water samples or homogenized fish meat samples. Having a dissociation constant of 2.17 × 10 -9  M -1 , the GOM allows extraction of approximately 98% of 100 nM MG. Coupling of the GOM-spray with an ion-trap mass spectrometer allows quantitation of MG in aquaculture freshwater and seawater samples down to nanomolar levels. Furthermore, the system possesses high selectivity and sensitivity for the quantitation of MG and its metabolite (leucomalachite green) in fish meat samples. With easy extraction and efficient spray ionization properties of GOM, this membrane spray-mass spectrometry technique is relatively simple and fast in comparison to the traditional LC-MS/MS methods for the quantitation of MG and its metabolite in aquaculture products. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Rapid and reliable determination of the halogenating peroxidase activity in blood samples.

PubMed

Flemmig, Jörg; Schwarz, Pauline; Bäcker, Ingo; Leichsenring, Anna; Lange, Franziska; Arnhold, Jürgen

2014-12-15

By combining easy and fast leukocyte enrichment with aminophenyl-fluorescein (APF) staining we developed a method to quickly and specifically address the halogenating activity of the immunological relevant blood heme peroxidases myeloperoxidase and eosinophil peroxidase, respectively. For leukocyte enrichment a two-fold hypotonic lysis procedure of the blood with Millipore water was chosen which represents a cheap, fast and reliable method to diminish the amount of erythrocytes in the samples. This procedure is shown to be suitable both to human and murine blood micro-samples, making it also applicable to small animal experiments with recurring blood sampling. As all types of leukocytes are kept in the sample during the preparation, they can be analysed separately after discrimination during the flow cytometry analysis. This also holds for all heme peroxidase-containing cells, namely neutrophils, eosinophils and monocytes. Moreover additional parameters (e.g. antibody staining) can be combined with the heme peroxidase activity determination to gain additional information about the different immune cell types. Based on previous results we applied APF for specifically addressing the halogenating activity of leukocyte peroxidases in blood samples. This dye is selectively oxidized by the MPO and EPO halogenation products hypochlorous and hypobromous acid. This approach may provide a suitable tool to gain more insights into the immune-physiological role of the halogenating activity of heme peroxidases. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of Pass/Fail Criteria for Promoted Combustion Testing

NASA Technical Reports Server (NTRS)

Sparks, Kyle M.; Stoltzfus, Joel M.; Steinberg, Theodore A.; Lynn, David

2009-01-01

Promoted ignition testing is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. In these tests, a promoter is used to ignite each metal rod to start the sample burning. Experiments were performed to better understand the promoted ignition test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Various ignition promoters were used to ignite the test samples. The thermocouple measurements and test video was synchronized to determine temperature increase with respect to time and length along each test sample. A recommended length of test sample that must be consumed to be considered a flammable material was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.

Cyclospora cayetanensis in Three Populations at Risk in Guatemala

PubMed Central

Pratdesaba, Rafael A.; González, Mario; Piedrasanta, Evelyn; Mérida, Claudia; Contreras, Karen; Vela, Carlos; Culajay, Francisco; Flores, Luis; Torres, Olga

2001-01-01

In 1996 and 1997, outbreaks of Cyclospora cayetanensis in North America were linked to Guatemalan raspberries. From April 1999 to April 2000, we undertook a survey for C. cayetanensis in raspberry farm workers, malnourished children, and human immunodeficiency virus and AIDS patients in Guatemala. Stool samples were analyzed using ethylacetate-formalin concentration, wet preparation, modified acid-fast staining method, and epifluorescence. Oocysts were found in 1.5% of the subjects, none of whom were raspberry farm workers. PMID:11474019

CoPt/TiN films nanopatterned by RF plasma etching towards dot-patterned magnetic media

NASA Astrophysics Data System (ADS)

Szívós, János; Pothorszky, Szilárd; Soltys, Jan; Serényi, Miklós; An, Hongyu; Gao, Tenghua; Deák, András; Shi, Ji; Sáfrán, György

2018-03-01

CoPt thin films as possible candidates for Bit Patterned magnetic Media (BPM) were prepared and investigated by electron microscopy techniques and magnetic measurements. The structure and morphology of the Direct Current (DC) sputtered films with N incorporation were revealed in both as-prepared and annealed state. Nanopatterning of the samples was carried out by means of Radio Frequency (RF) plasma etching through a Langmuir-Blodgett film of silica nanospheres that is a fast and high throughput technique. As a result, the samples with hexagonally arranged 100 nm size separated dots of fct-phase CoPt were obtained. The influence of the order of nanopatterning and anneling on the nanostructure formation was revealed. The magnetic properties of the nanopatterned fct CoPt films were investigated by Vibrating Sample Magnetometer (VSM) and Magnetic Force Microscopy (MFM). The results show that CoPt thin film nanopatterned by means of the RF plasma etching technique is promising candidate to a possible realization of BPM. Furthermore, this technique is versatile and suitable for scaling up to technological and industrial applications.

Subnanogram determination of aniracetam in pharmaceutical preparations and biofluids by flow injection analysis with chemiluminescence detection based on its enhancement of the myoglobin-luminol reaction.

PubMed

Shao, Xiaodong; Li, Ying; Li, Fagen; Liu, Yangqin; Song, Zhenghua

2011-01-01

A novel flow injection chemiluminescence method with a myoglobin-luminol system is described for determining aniracetam. Myoglobin-bound aniracetam produced a complex that catalyzed the chemiluminescence reaction between luminol and myoglobin, leading to fast chemiluminescence. The chemiluminescence intensity in the presence of aniracetam was remarkably enhanced compared with that in the absence of aniracetam. Under the optimum reaction conditions the chemiluminescence increment produced was proportional to the concentration of aniracetam in the range of 0.1-1000.0 ng/mL (R2 = 0.9992), with a detection limit of 0.03 ng/mL (3delta). At a flow rate of 2.0 mL/min, the whole process, including sampling and washing, could be completed in 0.5 min, offering a sampling efficiency of 120/h; the RSD was less than 3.0% (n = 5). The method was satisfactory for determination of aniracetam in pharmaceutical preparations and human urine and serum samples. A possible mechanism of the reaction is also discussed.

Preparation and evaluation of magnetic core-shell mesoporous molecularly imprinted polymers for selective adsorption of tetrabromobisphenol S.

PubMed

Wang, Xuemei; Huang, Pengfei; Ma, Xiaomin; Wang, Huan; Lu, Xiaoquan; Du, Xinzhen

2017-05-01

Novel magnetic mesoporous molecularly imprinted polymers (MMIPs) with core-shell structure were prepared by simple surface molecular imprinting polymerization using tetrabromobisphenol-S (TBBPS) as the template. The MMIPs-TBBPS were characterized by fourier-transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N 2 adsorption-desorption transmission, and vibrating sample magnetometry. The resultant MMIPs-TBBPS were successfully applied magnetic solid-phase extraction (MSPE) coupled with HPLC determination of TBBPS in spiked real water samples with recoveries of 77.8-88.9%. The adsorption experiments showed that the binding capacity of MMIPs-TBBPS to TBBPS and six structural analogs were significantly higher than that of the magnetic nonimprinted polymers (MNIPs). Meanwhile, the MMIPs-TBBPS possessed rapid binding affinity, excellent magnetic response, specific selectivity and high adsorption capacity toward TBBPS with a maximum adsorption capacity of 1626.8µgg -1 . The analytical results indicate that the MMIPs-TBBPS are promising materials for selective separation and fast enrichment of TBBPS from complicated enviromental samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

PubMed

Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

2017-05-01

Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecularly imprinted polymer online solid-phase extraction coupled with high-performance liquid chromatography-UV for the determination of three sulfonamides in pork and chicken.

PubMed

He, Jinxing; Wang, Shuo; Fang, Guozhen; Zhu, Huaping; Zhang, Yan

2008-05-14

A selective imprinted amino-functionalized silica gel sorbent was prepared by combining a surface molecular imprinting technique with a sol-gel process for online solid-phase extraction-HPLC determination of three trace sulfonamides in pork and chicken muscle. The imprinted functionalized silica gel sorbent exhibited selectivity and fast kinetics for the adsorption and desorption of sulfonamides. With a sample loading flow rate of 4 mL min (-1) for 12.5 min, enhancement factors and detection limits for three sulfonamides ( S/ N = 3) were achieved. The precision (RSD) for nine replicate online sorbent extractions of 5 microg L (-1) sulfonamides was less than 4.5%. The sorbent also offered good linearity ( r (2) > 0.99) for online solid-phase extraction of trace levels of sulfonamides. The method was applied to the determination of sulfonamides in pork and chicken muscle samples. The prepared polymer sorbent shows promise for online solid-phase extraction for HPLC determination of trace levels of sulfonamides in pork and chicken samples.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis.

PubMed

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-05

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p=0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis

NASA Astrophysics Data System (ADS)

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-01

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4 mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p = 0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes.

Quantitative analysis of virgin coconut oil in cream cosmetics preparations using fourier transform infrared (FTIR) spectroscopy.

PubMed

Rohman, A; Man, Yb Che; Sismindari

2009-10-01

Today, virgin coconut oil (VCO) is becoming valuable oil and is receiving an attractive topic for researchers because of its several biological activities. In cosmetics industry, VCO is excellent material which functions as a skin moisturizer and softener. Therefore, it is important to develop a quantitative analytical method offering a fast and reliable technique. Fourier transform infrared (FTIR) spectroscopy with sample handling technique of attenuated total reflectance (ATR) can be successfully used to analyze VCO quantitatively in cream cosmetic preparations. A multivariate analysis using calibration of partial least square (PLS) model revealed the good relationship between actual value and FTIR-predicted value of VCO with coefficient of determination (R2) of 0.998.

Volatility-dependent 2D IR correlation analysis of traditional Chinese medicine ‘Red Flower Oil’ preparation from different manufacturers

NASA Astrophysics Data System (ADS)

Wu, Yan-Wen; Sun, Su-Qin; Zhou, Qun; Tao, Jia-Xun; Noda, Isao

2008-06-01

As a traditional Chinese medicine (TCM), 'Red Flower Oil' preparation is widely used as a household remedy in China and Southeast Asia. Usually, the preparation is a mixture of several plant essential oils with different volatile features, such as wintergreen oil, turpentine oil and clove oil. The proportions of these plant essential oils in 'Red Flower Oil' vary from different manufacturers. Thus, it is important to develop a simple and rapid evaluation method for quality assurance of the preparations. Fourier transform infrared (FT-IR) was applied and two-dimensional correlation infrared spectroscopy (2D IR) based on the volatile characteristic of samples was used to enhance the resolution of FT-IR spectra. 2D IR technique could, not only easily provide the composition and their volatile sequences in 'Red flower Oil' preparations, but also rapidly discriminate the subtle differences in products from different manufacturers. Therefore, FT-IR combined with volatility-dependent 2D IR correlation analysis provides a very fast and effective method for the quality control of essential oil mixtures in TCM.

Preparation of nickel aluminum-manganese spinel oxides Ni{sub x}Al{sub 1{minus}x}Mn{sub 2}O{sub 4} for oxygen electrocatalysis in alkaline medium: Comparison of properties stemming from different preparation methods

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

Ponce, J.; Rios, E.; Gautier, J.L.

Two different procedures were used to prepare spinel-type Ni{sub x}Al{sub 1{minus}x}Mn{sub 2}O{sub 4} (0 {le} x {le} 1) compounds to study the effects of solid state properties of mixed oxides on their electrocatalytic properties. The oxalic route, coprecipitation of metal oxalates dissolved in propanol or ethanol, and the propionic route, hydrolysis of metal carboxylates in propionic acid, have been used. In both routes, thermal decomposition produces the corresponding oxides. X-ray diffraction patterns showed that the oxides crystallize in a cubic spinel phase with a unit cell parameter a that increases as aluminum is replaced by nickel. At low x values,more » compounds prepared by the propionic route showed a larger variation for parameter a than compounds prepared by the oxalic route, probably due to oxygen stoichiometric deficiency. This effect was estimated from the tetrahedral force constant (k{sub 1}) values, which showed a fast decrease as x varied from 0 to 1. Electrical conductivity, conduction activation energy, hole mobility, and pHz of oxides prepared by the propionic route were also higher than those from oxides prepared by the oxalic route. Crystallinity grade and particle size were nearly 50% higher in propionic-route samples than in oxalic-route samples. The apparent and real electrocatalytic activities of both types of oxides were compared for O{sub 2} evolution. 42 refs., 6 figs., 4 tabs.« less

Determination of heat conductivity of waste glass feed and its applicability for modeling the batch-to-glass conversion

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

Hujova, Miroslava; Pokorny, Richard; Klouzek, Jaroslav

The heat conductivity of reacting melter feed affects the heat transfer and conversion process in the cold cap (the reacting feed floating on molten glass). To investigate it, we simulated the feed conditions and morphology in the cold-cap by preparing “fast-dried slurry blocks”, formed by rapidly evaporating water from feed slurry poured onto a 200°C surface. A heat conductivity meter was used to measure heat conductivity of samples cut from the fast-dried slurry blocks, samples of a cold cap retrieved from a laboratory-scale melter, and loose dry powder feed samples. Our study indicates that the heat conductivity of the feedmore » in the cold cap is significantly higher than that of loose dry powder feed, resulting from the feed solidification during the water evaporation from the feed slurry. To assess the heat transfer at higher temperatures when feed turns into foam, we developed a theoretical model that predicts the foam heat conductivity based on morphology data from in-situ X-ray computed tomography. The implications for the mathematical modeling of the cold cap are discussed.« less

Tailoring Co(OH)2 hollow nanostructures via Cu2O template etching for high performance supercapacitors.

PubMed

Yang, Huan; Xie, Jiale; Bao, Shu juan; Li, Chang Ming

2015-11-01

Co(OH)2 hollow nanostructures including cube, octahedron and flower are delicately tailored via a simple and fast one-step Cu2O template etching method. The as-prepared materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscope (FESEM), N2 adsorption-desorption and electrochemical methods and X-ray photoelectron spectroscopy (XPS). In particular, the supercapacitive behaviors of the as-prepared materials were investigated to explore relation of capacitance versus nanostructure. Results indicate that the as-prepared Co(OH)2 samples inherit the size and shape of the Cu2O templates but with an inside hollow, and the differently nanostructured Co(OH)2 exhibits different capacitive behaviors. Among various morphologies, the flower Co(OH)2 has the largest specific capacitance of 1350 F/g, while octahedron Co(OH)2 has the smallest one of 986.4 F/g. This is mainly because the flower Co(OH)2 not only has the largest available surface area, but also offers the fast interfacial electron transfer for higher pseudocapacitance and enhanced electrolyte ion diffusion rate for high power density, which is supported by both theoretical calculation, measured BET data and ac impedance measurements. This work may provide a vivid example to rationally design a nanostructure and further explore its fundamental insights for high performance supercapacitors. Copyright © 2015 Elsevier Inc. All rights reserved.

Large-volume injection of sample diluents not miscible with the mobile phase as an alternative approach in sample preparation for bioanalysis: an application for fenspiride bioequivalence.

PubMed

Medvedovici, Andrei; Udrescu, Stefan; Albu, Florin; Tache, Florentin; David, Victor

2011-09-01

Liquid-liquid extraction of target compounds from biological matrices followed by the injection of a large volume from the organic layer into the chromatographic column operated under reversed-phase (RP) conditions would successfully combine the selectivity and the straightforward character of the procedure in order to enhance sensitivity, compared with the usual approach of involving solvent evaporation and residue re-dissolution. Large-volume injection of samples in diluents that are not miscible with the mobile phase was recently introduced in chromatographic practice. The risk of random errors produced during the manipulation of samples is also substantially reduced. A bioanalytical method designed for the bioequivalence of fenspiride containing pharmaceutical formulations was based on a sample preparation procedure involving extraction of the target analyte and the internal standard (trimetazidine) from alkalinized plasma samples in 1-octanol. A volume of 75 µl from the octanol layer was directly injected on a Zorbax SB C18 Rapid Resolution, 50 mm length × 4.6 mm internal diameter × 1.8 µm particle size column, with the RP separation being carried out under gradient elution conditions. Detection was made through positive ESI and MS/MS. Aspects related to method development and validation are discussed. The bioanalytical method was successfully applied to assess bioequivalence of a modified release pharmaceutical formulation containing 80 mg fenspiride hydrochloride during two different studies carried out as single-dose administration under fasting and fed conditions (four arms), and multiple doses administration, respectively. The quality attributes assigned to the bioanalytical method, as resulting from its application to the bioequivalence studies, are highlighted and fully demonstrate that sample preparation based on large-volume injection of immiscible diluents has an increased potential for application in bioanalysis.

Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

NASA Astrophysics Data System (ADS)

Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

2014-05-01

MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples.

PubMed

Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-10-31

In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Solvent Vapor Annealing of Amorphous Carbamazepine Films for Fast Polymorph Screening and Dissolution Alteration.

PubMed

Schrode, Benedikt; Bodak, Brigitta; Riegler, Hans; Zimmer, Andreas; Christian, Paul; Werzer, Oliver

2017-09-30

Solubility enhancement and thus higher bioavailability are of great importance and a constant challenge in pharmaceutical research whereby polymorph screening and selection is one of the most important tasks. A very promising approach for polymorph screening is solvent vapor annealing where a sample is exposed to an atmosphere saturated with molecules of a specific chemical/solvent. In this work, amorphous carbamazepine thin films were prepared by spin coating, and the transformation into crystalline forms under exposure to solvent vapors was investigated. Employing grazing incidence X-ray diffraction, four distinct carbamazepine polymorphs, a solvate, and hydrates could be identified, while optical microscopy showed mainly spherulitic morphologies. In vitro dissolution experiments revealed different carbamazepine release from the various thin-film samples containing distinct polymorphic compositions: heat treatment of amorphous samples at 80 °C results in an immediate release; samples exposed to EtOH vapors show a drug release about 5 times slower than this immediate one; and all the others had intermediate release profiles. Noteworthy, even the sample of slowest release has a manifold faster release compared to a standard powder sample demonstrating the capabilities of thin-film preparation for faster drug release in general. Despite the small number of samples in this screening experiment, the results clearly show how solvent vapor annealing can assist in identifying potential polymorphs and allows for estimating their impact on properties like bioavailability.

[Research on fast classification based on LIBS technology and principle component analyses].

PubMed

Yu, Qi; Ma, Xiao-Hong; Wang, Rui; Zhao, Hua-Feng

2014-11-01

Laser-induced breakdown spectroscopy (LIBS) and the principle component analysis (PCA) were combined to study aluminum alloy classification in the present article. Classification experiments were done on thirteen different kinds of standard samples of aluminum alloy which belong to 4 different types, and the results suggested that the LIBS-PCA method can be used to aluminum alloy fast classification. PCA was used to analyze the spectrum data from LIBS experiments, three principle components were figured out that contribute the most, the principle component scores of the spectrums were calculated, and the scores of the spectrums data in three-dimensional coordinates were plotted. It was found that the spectrum sample points show clear convergence phenomenon according to the type of aluminum alloy they belong to. This result ensured the three principle components and the preliminary aluminum alloy type zoning. In order to verify its accuracy, 20 different aluminum alloy samples were used to do the same experiments to verify the aluminum alloy type zoning. The experimental result showed that the spectrum sample points all located in their corresponding area of the aluminum alloy type, and this proved the correctness of the earlier aluminum alloy standard sample type zoning method. Based on this, the identification of unknown type of aluminum alloy can be done. All the experimental results showed that the accuracy of principle component analyses method based on laser-induced breakdown spectroscopy is more than 97.14%, and it can classify the different type effectively. Compared to commonly used chemical methods, laser-induced breakdown spectroscopy can do the detection of the sample in situ and fast with little sample preparation, therefore, using the method of the combination of LIBS and PCA in the areas such as quality testing and on-line industrial controlling can save a lot of time and cost, and improve the efficiency of detection greatly.

A review of microdialysis coupled to microchip electrophoresis for monitoring biological events

PubMed Central

Saylor, Rachel A.; Lunte, Susan M.

2015-01-01

Microdialysis is a powerful sampling technique that enables monitoring of dynamic processes in vitro and in vivo. The combination of microdialysis with chromatographic or electrophoretic methods yields along with selective detection methods yields a “separation-based sensor” capable of monitoring multiple analytes in near real time. Analysis of microdialysis samples requires techniques that are fast (<1 min), have low volume requirements (nL–pL), and, ideally, can be employed on-line. Microchip electrophoresis fulfills these requirements and also permits the possibility of integrating sample preparation and manipulation with detection strategies directly on-chip. Microdialysis coupled to microchip electrophoresis has been employed for monitoring biological events in vivo and in vitro. This review discusses technical considerations for coupling microdialysis sampling and microchip electrophoresis, including various interface designs, and current applications in the field. PMID:25637011

Identification of lipid- and protein-based binders in paintings by direct on-plate wet chemistry and matrix-assisted laser desorption ionization mass spectrometry.

PubMed

Calvano, Cosima Damiana; van der Werf, Inez Dorothé; Palmisano, Francesco; Sabbatini, Luigia

2015-01-01

Direct on-target plate processing of small (ca. 100 μg) fragments of paint samples for MALDI-MS identification of lipid- and protein-based binders is described. Fragments were fixed on a conventional stainless steel target plate by colloidal graphite followed by in situ fast tryptic digestion and matrix addition. The new protocol was first developed on paint replicas composed of chicken egg, collagen, and cow milk mixed with inorganic pigments and then successfully applied on historical paint samples taken from a fifteenth century Italian panel painting. The present work contributes a step forward in the simplification of binder identification in very small paint samples since no conventional solvent extraction is required, speeding up the whole sample preparation to 10 min and reducing lipid/protein loss.

Fast trace determination of nine odorant and estrogenic chloro- and bromo-phenolic compounds in real water samples through automated solid-phase extraction coupled with liquid chromatography tandem mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuang-Tao; Lin, Qing; Yin, Hua; Lin, Zhang; Dang, Zhi

2018-02-01

A fast and reliable method was developed for simultaneous trace determination of nine odorous and estrogenic chloro- and bromo-phenolic compounds (CPs and BPs) in water samples using solid-phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS). For sample preparation, the extraction efficiencies of two widely applied cartridges Oasis HLB and Sep-Pak C18 were compared, and the Oasis HLB cartridge showed much better extraction performance; pH of water sample also plays important role on extraction, and pH = 2-3 was found to be most appropriate. For separation of the target compounds, small addition of ammonium hydroxide can obviously improve the detection sensitivity, and the optimized addition concentration was determined as 0.2%. The developed efficient method was validated and showed excellent linearity (R 2  > 0.995), low limit of detection (LOD, 1.9-6.2 ng/L), and good recovery efficiencies of 57-95% in surface and tap water with low relative standard deviation (RSD, 1.3-17.4%). The developed method was finally applied to one tap and one surface water samples and most of these nine targets were detected, but all of them were below their odor thresholds, and their estrogen equivalent (EEQ) were also very low.

Studying the spatial variability of Cr in agricultural field using both particle induced X-ray emission (PIXE) and instrumental neutron activation analysis (INAA) technique

NASA Astrophysics Data System (ADS)

Cruvinel, Paulo E.; Crestana, Sílvio; Artaxo, Paulo; Martins, JoséV.; Armelin, Maria JoséA.

1996-04-01

In the field of soil physics, a technique which permits a non-destructive, accurate and fast elemental analysis with a minimum of sample preparation effort is often desired. Although trace elements are minor components of the solid phase, they play an important role in soil fertility. Cr is of nutritional importance because it is a required element in human and animal nutrition. The immobility of Cr may be responsible for an inadequate Cr supply to plants. This work not only demonstrates the suitability of PIXE as a fast and non-destructive technique, useful to measure Cr content in soil samples, but also outlines a study of spatial variability of that element in agricultural field. To demonstrate the capability of the method soil samples were collected in a 5000 m 2 agricultural field. The soil samples were analyzed using both PIXE and INAA techniques. Besides, a Fourier interpolation technique was used to verify the distribution of Cr along of the sampled field. INAA was carried out by means of the γ-ray emitted by 51Cr(320 keV). Results show that there is a good linear relationship between the elemental concentration of Cr obtained using those techniques, i.e. a correlation coefficient of r2 = 0.82 was achieved.

Linear Quantitative Profiling Method Fast Monitors Alkaloids of Sophora Flavescens That Was Verified by Tri-Marker Analyses

PubMed Central

Hou, Zhifei; Sun, Guoxiang; Guo, Yong

2016-01-01

The present study demonstrated the use of the Linear Quantitative Profiling Method (LQPM) to evaluate the quality of Alkaloids of Sophora flavescens (ASF) based on chromatographic fingerprints in an accurate, economical and fast way. Both linear qualitative and quantitative similarities were calculated in order to monitor the consistency of the samples. The results indicate that the linear qualitative similarity (LQLS) is not sufficiently discriminating due to the predominant presence of three alkaloid compounds (matrine, sophoridine and oxymatrine) in the test samples; however, the linear quantitative similarity (LQTS) was shown to be able to obviously identify the samples based on the difference in the quantitative content of all the chemical components. In addition, the fingerprint analysis was also supported by the quantitative analysis of three marker compounds. The LQTS was found to be highly correlated to the contents of the marker compounds, indicating that quantitative analysis of the marker compounds may be substituted with the LQPM based on the chromatographic fingerprints for the purpose of quantifying all chemicals of a complex sample system. Furthermore, once reference fingerprint (RFP) developed from a standard preparation in an immediate detection way and the composition similarities calculated out, LQPM could employ the classical mathematical model to effectively quantify the multiple components of ASF samples without any chemical standard. PMID:27529425

Performance-based, cost- and time-effective pcb analytical methodology.

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

Alvarado, J. S.

1998-06-11

Laboratory applications for the analysis of PCBs (polychlorinated biphenyls) in environmental matrices such as soil/sediment/sludge and oil/waste oil were evaluated for potential reduction in waste, source reduction, and alternative techniques for final determination. As a consequence, new procedures were studied for solvent substitution, miniaturization of extraction and cleanups, minimization of reagent consumption, reduction of cost per analysis, and reduction of time. These new procedures provide adequate data that meet all the performance requirements for the determination of PCBs. Use of the new procedures reduced costs for all sample preparation techniques. Time and cost were also reduced by combining the newmore » sample preparation procedures with the power of fast gas chromatography. Separation of Aroclor 1254 was achieved in less than 6 min by using DB-1 and SPB-608 columns. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost. With performance-based methodology, the applications presented here can be applied now, without waiting for regulatory approval.« less

Fast determination of pyrethroid pesticides in tobacco by GC-MS-SIM coupled with modified QuEChERS sample preparation procedure.

PubMed

Gao, Yan; Sun, Ying; Jiang, Chunzhu; Yu, Xi; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

2013-01-01

An analytical method was developed for the extraction and determination of pyrethroid pesticide residues in tobacco. The modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was applied for preparing samples. In this study, methyl cyanide (MeCN)-saturated salt aqueous was used as the two-phase extraction solvent for the first time, and a vortex shaker was used for the simultaneous shaking and concentration of the analytes. The effects of experimental parameters on extraction and clean-up efficiency were investigated and optimized. The analytes were determined by gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). The obtained recoveries of the analytes at three different fortification levels were 76.85-114.1% and relative standard deviations (RSDs) were lower than 15.7%. The limits of quantification (LOQs) were from 1.28 to 26.6 μg kg(-1). This method was also applied to the analysis of actual commercial tobacco products and the analytical results were satisfactory.

One-step electrochemical deposition of a graphene-ZrO 2 nanocomposite: Preparation, characterization and application for detection of organophosphorus agents

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

Du, Dan; Liu, Juan; Zhang, Xiao-Yan

2011-04-27

This paper described the preparation, characterization, and electrochemical properties of a graphene-ZrO 2 nanocomposite (GZN) and its application for both the enrichment and detection of methyl parathion (MP). GZN was fabricated using electrochemical deposition and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), which showed the successful formation of nanocomposites. Due to the strong affinity to the phosphoric group and the fast electron-transfer kinetics of GZN, both the extraction and electrochemical detection of organophosphorus (OP) agents at the same GZN modified electrochemical sensor was possible. The combination of solid-phase extractionmore » and stripping voltammetric analysis allowed fast, sensitive, and selective determination of MP in garlic samples. The stripping response was highly linear over the MP concentrations ranging from 0.5 ng mL -1 to 100 ng mL -1, with a detection limit of 0.1 ng mL -1. This new nanocomposite-based electrochemical sensor provides an opportunity to develop a field-deployable, sensitive, and quantitative method for monitoring exposure to OPs.« less

A simplified and efficient method for the analysis of fatty acid methyl esters suitable for large clinical studies.

PubMed

Masood, Athar; Stark, Ken D; Salem, Norman

2005-10-01

Conventional sample preparation for fatty acid analysis is a complicated, multiple-step process, and gas chromatography (GC) analysis alone can require >1 h per sample to resolve fatty acid methyl esters (FAMEs). Fast GC analysis was adapted to human plasma FAME analysis using a modified polyethylene glycol column with smaller internal diameters, thinner stationary phase films, increased carrier gas linear velocity, and faster temperature ramping. Our results indicated that fast GC analyses were comparable to conventional GC in peak resolution. A conventional transesterification method based on Lepage and Roy was simplified to a one-step method with the elimination of the neutralization and centrifugation steps. A robotics-amenable method was also developed, with lower methylation temperatures and in an open-tube format using multiple reagent additions. The simplified methods produced results that were quantitatively similar and with similar coefficients of variation as compared with the original Lepage and Roy method. The present streamlined methodology is suitable for the direct fatty acid analysis of human plasma, is appropriate for research studies, and will facilitate large clinical trials and make possible population studies.

Fast and direct analysis of Cr, Cd and Pb in brown sugar by GF AAS.

PubMed

Dos Santos, Jeferson M; Quináia, Sueli P; Felsner, Maria L

2018-09-15

A simple and fast analytical method for the determination of Cr, Pb and Cd in brown sugar by GF AAS using slurry sampling was developed and in house validated for the first time. Analytical curves were prepared by external standardization for Cr, and by matrix simulation for Pb and Cd and they were linear. Low limits of quantification for Cr (32.8 ng g -1 ), Pb (49.3 ng g -1 ) and Cd (4.5 ng g -1 ) were found. Repeatability and intermediate precision estimates (<10% and <15%, respectively) and recovery rates (95-103%) demonstrated a good precision and accuracy. The levels in brown sugar samples ranged from <32.8 to 160 ng g -1 for Cr, from <49.3 to 211.0 ng g -1 for Pb and from <4.5 to 7.0 ng g -1 for Cd and they may be assigned to anthropogenic activities and the adoption of inadequate practices of production and processing. Copyright © 2018 Elsevier Ltd. All rights reserved.

Fast quantitation of opioid isomers in human plasma by differential mobility spectrometry/mass spectrometry via SPME/open-port probe sampling interface.

PubMed

Liu, Chang; Gómez-Ríos, Germán Augusto; Schneider, Bradley B; Le Blanc, J C Yves; Reyes-Garcés, Nathaly; Arnold, Don W; Covey, Thomas R; Pawliszyn, Janusz

2017-10-23

Mass spectrometry (MS) based quantitative approaches typically require a thorough sample clean-up and a decent chromatographic step in order to achieve needed figures of merit. However, in most cases, such processes are not optimal for urgent assessments and high-throughput determinations. The direct coupling of solid phase microextraction (SPME) to MS has shown great potential to shorten the total sample analysis time of complex matrices, as well as to diminish potential matrix effects and instrument contamination. In this study, we demonstrate the use of the open-port probe (OPP) as a direct and robust sampling interface to couple biocompatible-SPME (Bio-SPME) fibres to MS for the rapid quantitation of opioid isomers (i.e. codeine and hydrocodone) in human plasma. In place of chromatography, a differential mobility spectrometry (DMS) device was implemented to provide the essential selectivity required to quantify these constitutional isomers. Taking advantage of the simplified sample preparation process based on Bio-SPME and the fast separation with DMS-MS coupling via OPP, a high-throughput assay (10-15 s per sample) with limits of detection in the sub-ng/mL range was developed. Succinctly, we demonstrated that by tuning adequate ion mobility separation conditions, SPME-OPP-MS can be employed to quantify non-resolved compounds or those otherwise hindered by co-extracted isobaric interferences without further need of coupling to other separation platforms. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of water-phase derivatization followed by solid-phase microextraction and gas chromatography/mass spectrometry for fast determination of valproic acid in human plasma.

PubMed

Deng, Chunhui; Li, Ning; Ji, Jie; Yang, Bei; Duan, Gengli; Zhang, Xiangmin

2006-01-01

In this study, a simple, rapid, and sensitive method was developed and validated for the quantification of valproic acid (VPA), an antiepileptic drug, in human plasma, which was based on water-phase derivatization followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS). In the proposed method, VPA in plasma was rapidly derivatized with a mixture of isobutyl chloroformate, ethanol and pyridine under mild conditions (room temperature, aqueous medium), and the VPA ethyl ester formed was headspace-extracted and simultaneously concentrated using the SPME technique. Finally, the analyte extracted on SPME fiber was analyzed by GC/MS. The experimental parameters and method validations were studied. The optimal conditions were obtained: PDMS fiber, stirring rate of 1100 rpm, sample temperature of 80 degrees C, extraction time of 20 min, NaCl concentration of 30%. The proposed method had a limit of quantification (0.3 microg/mL), good recovery (89-97%) and precision (RSD value less than 10%). Because the proposed method combined a rapid water-phase derivatization with a fast, simple and solvent-free sample extraction and concentration technique of SPME, the sample preparation time was less than 25 min. This much shortens the whole analysis time of VPA in plasma. The validated method has been successfully used to analyze VPA in human plasma samples for application in pharmacokinetic studies. All these results show that water-phase derivatization followed by HS-SPME and GC/MS is an alternative and powerful method for fast determination of VPA in biological fluids. Copyright 2006 John Wiley & Sons, Ltd.

Heat Effects of Promoters and Determination of Burn Criterion in Promoted Combustion Testing

NASA Technical Reports Server (NTRS)

Sparks, Kyle M.; Stoltzfus, Joel M.; Steinberg, Theodore A.; Lynn, David

2010-01-01

Promoted ignition testing (NASA Test 17) [1] is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. A promoter is used to ignite a metal sample rod, initiating sample burning. If a predetermined length of the sample burns, beyond the promoter, the material is considered flammable at the condition tested. Historically, this burn length has been somewhat arbitrary. Experiments were performed to better understand this test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Thermocouple measurements and test video were synchronized to determine temperature increase with respect to time and length along each test sample. A recommended flammability burn length, based on a sample preheat of 500 F, was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.

Reliability of Serum Metabolites over a Two-Year Period: A Targeted Metabolomic Approach in Fasting and Non-Fasting Samples from EPIC

PubMed Central

Achaintre, David; Sacerdote, Carlotta; Vineis, Paolo; Key, Timothy J.; Onland Moret, N. Charlotte; Scalbert, Augustin; Rinaldi, Sabina; Ferrari, Pietro

2015-01-01

Objective Although metabolic profiles have been associated with chronic disease risk, lack of temporal stability of metabolite levels could limit their use in epidemiological investigations. The present study aims to evaluate the reliability over a two-year period of 158 metabolites and compare reliability over time in fasting and non-fasting serum samples. Methods Metabolites were measured with the AbsolueIDQp180 kit (Biocrates, Innsbruck, Austria) by mass spectrometry and included acylcarnitines, amino acids, biogenic amines, hexoses, phosphatidylcholines and sphingomyelins. Measurements were performed on repeat serum samples collected two years apart in 27 fasting men from Turin, Italy, and 39 non-fasting women from Utrecht, The Netherlands, all participating in the European Prospective Investigation into Cancer and Nutrition (EPIC) study. Reproducibility was assessed by estimating intraclass correlation coefficients (ICCs) in multivariable mixed models. Results In fasting samples, a median ICC of 0.70 was observed. ICC values were <0.50 for 48% of amino acids, 27% of acylcarnitines, 18% of lysophosphatidylcholines and 4% of phosphatidylcholines. In non-fasting samples, the median ICC was 0.54. ICC values were <0.50 for 71% of acylcarnitines, 48% of amino acids, 44% of biogenic amines, 36% of sphingomyelins, 34% of phosphatidylcholines and 33% of lysophosphatidylcholines. Overall, reproducibility was lower in non-fasting as compared to fasting samples, with a statistically significant difference for 19–36% of acylcarnitines, phosphatidylcholines and sphingomyelins. Conclusion A single measurement per individual may be sufficient for the study of 73% and 52% of the metabolites showing ICCs >0.50 in fasting and non-fasting samples, respectively. ICCs were higher in fasting samples that are preferable to non-fasting. PMID:26274920

Recent advances in monolithic columns for protein and peptide separation by capillary liquid chromatography.

PubMed

Liang, Yu; Zhang, Lihua; Zhang, Yukui

2013-03-01

Capillary liquid chromatography (cLC) has great potential for protein and peptide separation, with advantages of high efficiency, high resolution, low sample consumption, and high sensitivity when coupled with mass spectrometry. In recent years, monoliths have been widely used as the stationary phases for capillary columns, owing to easy preparation, high permeability, fast mass transfer, and low backpressure. This review summarizes recent advances (2007-2012) in monolithic columns for protein and peptide separation by cLC. After a brief introduction on the preparation of monolithic capillary columns, the emphasis of this review is focused on the recent application of such columns for protein and peptide separation by cLC. Furthermore, the challenges and potential hot points of monolithic capillary columns in the future are discussed.

Investigation of novel zinc molybdate-graphene nanocomposite for supercapacitor applications

NASA Astrophysics Data System (ADS)

Reddy, B. Joji; Vickraman, P.; Justin, A. Simon

2018-06-01

Novel zinc molybdate-graphene nanocomposite is prepared for the first time in a fast, facile and eco-friendly microwave synthesis route as an electrode material for electrochemical supercapacitors. The as-prepared sample is investigated by X-ray diffraction, FTIR, Raman, scanning electron microscope and transmission electron microscope techniques. The studies have confirmed the formation of ZnMoO4 and its composite with graphene. The synthesized materials are subjected to electrochemical characterization studies in 2M KOH electrolyte solution which prove that ZnMoO4-graphene as an effective electrode material for supercapacitor applications. ZnMoO4 in its composite behavior has exhibited a specific capacitance of 272.93 F g- 1 at 0.5 A g- 1 with good cyclic stability for 1000 cycles.

Purification of pharmaceutical preparations using thin-layer chromatography to obtain mass spectra with Direct Analysis in Real Time and accurate mass spectrometry.

PubMed

Wood, Jessica L; Steiner, Robert R

2011-06-01

Forensic analysis of pharmaceutical preparations requires a comparative analysis with a standard of the suspected drug in order to identify the active ingredient. Purchasing analytical standards can be expensive or unattainable from the drug manufacturers. Direct Analysis in Real Time (DART™) is a novel, ambient ionization technique, typically coupled with a JEOL AccuTOF™ (accurate mass) mass spectrometer. While a fast and easy technique to perform, a drawback of using DART™ is the lack of component separation of mixtures prior to ionization. Various in-house pharmaceutical preparations were purified using thin-layer chromatography (TLC) and mass spectra were subsequently obtained using the AccuTOF™- DART™ technique. Utilizing TLC prior to sample introduction provides a simple, low-cost solution to acquiring mass spectra of the purified preparation. Each spectrum was compared against an in-house molecular formula list to confirm the accurate mass elemental compositions. Spectra of purified ingredients of known pharmaceuticals were added to an in-house library for use as comparators for casework samples. Resolving isomers from one another can be accomplished using collision-induced dissociation after ionization. Challenges arose when the pharmaceutical preparation required an optimized TLC solvent to achieve proper separation and purity of the standard. Purified spectra were obtained for 91 preparations and included in an in-house drug standard library. Primary standards would only need to be purchased when pharmaceutical preparations not previously encountered are submitted for comparative analysis. TLC prior to DART™ analysis demonstrates a time efficient and cost saving technique for the forensic drug analysis community. Copyright © 2011 John Wiley & Sons, Ltd. Copyright © 2011 John Wiley & Sons, Ltd.

Comparing Effects of Feedstock and Run Conditions on Pyrolysis Products Produced at Pilot-Scale

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

Dunning, Timothy C; Gaston, Katherine R; Wilcox, Esther

2018-01-19

Fast pyrolysis is a promising pathway for mass production of liquid transportable biofuels. The Thermochemical Process Development Unit (TCPDU) pilot plant at NREL is conducting research to support the Bioenergy Technologies Office's 2017 goal of a $3 per gallon biofuel. In preparation for down select of feedstock and run conditions, four different feedstocks were run at three different run conditions. The products produced were characterized extensively. Hot pyrolysis vapors and light gasses were analyzed on a slip stream, and oil and char samples were characterized post run.

Assessment of four protocols for rapid bacterial identification from positive blood culture pellets by matrix-assisted laser desorption ionization-time of flight mass spectrometry (Vitek® MS).

PubMed

Thomin, Jean; Aubin, Guillaume Ghislain; Foubert, Fabrice; Corvec, Stéphane

2015-08-01

In this study, we developed and compared four protocols to prepare a bacterial pellet from 944 positive blood cultures for direct MALDI-TOF mass spectrometry Vitek® MS analysis. Protocol 4, tested on 200 monomicrobial samples, allowed 83% of bacterial identification. This easy, fast, cheap and accurate method is promising in daily practice, especially to limit broad range antibiotic treatment. Copyright © 2015 Elsevier B.V. All rights reserved.

Fast filtration sampling protocol for mammalian suspension cells tailored for phosphometabolome profiling by capillary ion chromatography - tandem mass spectrometry.

PubMed

Kvitvang, Hans F N; Bruheim, Per

2015-08-15

Capillary ion chromatography (capIC) is the premium separation technology for low molecular phosphometabolites and nucleotides in biological extracts. Removal of excessive amounts of salt during sample preparation stages is a prerequisite to enable high quality capIC separation in combination with reproducible and sensitive MS detection. Existing sampling protocols for mammalian cells used for GC-MS and LC-MS metabolic profiling can therefore not be directly applied to capIC separations. Here, the development of a fast filtration sampling protocol for mammalian suspension cells tailored for quantitative profiling of the phosphometabolome on capIC-MS/MS is presented. The whole procedure from sampling the culture to transfer of filter to quenching and extraction solution takes less than 10s. To prevent leakage it is critical that a low vacuum pressure is applied, and satisfactorily reproducibility was only obtained by usage of a vacuum pressure controlling device. A vacuum of 60mbar was optimal for filtration of multiple myeloma Jjn-3 cell cultures through 5μm polyvinylidene (PVDF) filters. A quick deionized water (DI-water) rinse step prior to extraction was tested, and significantly higher metabolite yields were obtained during capIC-MS/MS analyses in this extract compared to extracts prepared by saline and reduced saline (25%) washing steps only. In addition, chromatographic performance was dramatically improved. Thus, it was verified that a quick DI-water rinse is tolerated by the cells and can be included as the final stage during filtration. Over 30 metabolites were quantitated in JJN-3 cell extracts by using the optimized sampling protocol with subsequent capIC-MS/MS analysis, and up to 2 million cells can be used in a single filtration step for the chosen filter and vacuum pressure. The technical set-up is also highly advantageous for microbial metabolome filtration protocols after optimization of vacuum pressure and washing solutions, and the reduced salt content of the extract will also improve the quality of LC-MS analysis due to lower salt adduct ion formation. Copyright © 2015 Elsevier B.V. All rights reserved.

A comprehensive high-resolution mass spectrometry approach for characterization of metabolites by combination of ambient ionization, chromatography and imaging methods.

PubMed

Berisha, Arton; Dold, Sebastian; Guenther, Sabine; Desbenoit, Nicolas; Takats, Zoltan; Spengler, Bernhard; Römpp, Andreas

2014-08-30

An ideal method for bioanalytical applications would deliver spatially resolved quantitative information in real time and without sample preparation. In reality these requirements can typically not be met by a single analytical technique. Therefore, we combine different mass spectrometry approaches: chromatographic separation, ambient ionization and imaging techniques, in order to obtain comprehensive information about metabolites in complex biological samples. Samples were analyzed by laser desorption followed by electrospray ionization (LD-ESI) as an ambient ionization technique, by matrix-assisted laser desorption/ionization (MALDI) mass spectrometry imaging for spatial distribution analysis and by high-performance liquid chromatography/electrospray ionization mass spectrometry (HPLC/ESI-MS) for quantitation and validation of compound identification. All MS data were acquired with high mass resolution and accurate mass (using orbital trapping and ion cyclotron resonance mass spectrometers). Grape berries were analyzed and evaluated in detail, whereas wheat seeds and mouse brain tissue were analyzed in proof-of-concept experiments. In situ measurements by LD-ESI without any sample preparation allowed for fast screening of plant metabolites on the grape surface. MALDI imaging of grape cross sections at 20 µm pixel size revealed the detailed distribution of metabolites which were in accordance with their biological function. HPLC/ESI-MS was used to quantify 13 anthocyanin species as well as to separate and identify isomeric compounds. A total of 41 metabolites (amino acids, carbohydrates, anthocyanins) were identified with all three approaches. Mass accuracy for all MS measurements was better than 2 ppm (root mean square error). The combined approach provides fast screening capabilities, spatial distribution information and the possibility to quantify metabolites. Accurate mass measurements proved to be critical in order to reliably combine data from different MS techniques. Initial results on the mycotoxin deoxynivalenol (DON) in wheat seed and phospholipids in mouse brain as a model for mammalian tissue indicate a broad applicability of the presented workflow. Copyright © 2014 John Wiley & Sons, Ltd.

Fast and robust method for the determination of microstructure and composition in butadiene, styrene-butadiene, and isoprene rubber by near-infrared spectroscopy.

PubMed

Vilmin, Franck; Dussap, Claude; Coste, Nathalie

2006-06-01

In the tire industry, synthetic styrene-butadiene rubber (SBR), butadiene rubber (BR), and isoprene rubber (IR) elastomers are essential for conferring to the product its properties of grip and rolling resistance. Their physical properties depend on their chemical composition, i. e., their microstructure and styrene content, which must be accurately controlled. This paper describes a fast, robust, and highly reproducible near-infrared analytical method for the quantitative determination of the microstructure and styrene content. The quantitative models are calculated with the help of pure spectral profiles estimated from a partial least squares (PLS) regression, using (13)C nuclear magnetic resonance (NMR) as the reference method. This versatile approach allows the models to be applied over a large range of compositions, from a single BR to an SBR-IR blend. The resulting quantitative predictions are independent of the sample path length. As a consequence, the sample preparation is solvent free and simplified with a very fast (five minutes) hot filming step of a bulk polymer piece. No precise thickness control is required. Thus, the operator effect becomes negligible and the method is easily transferable. The root mean square error of prediction, depending on the rubber composition, is between 0.7% and 1.3%. The reproducibility standard error is less than 0.2% in every case.

Label-free virus detection using silicon photonic microring resonators

PubMed Central

McClellan, Melinda S.; Domier, Leslie L; Bailey, Ryan C.

2013-01-01

Viruses represent a continual threat to humans through a number of mechanisms, which include disease, bioterrorism, and destruction of both plant and animal food resources. Many contemporary techniques used for the detection of viruses and viral infections suffer from limitations such as the need for extensive sample preparation or the lengthy window between infection and measurable immune response, for serological methods. In order to develop a method that is fast, cost-effective, and features reduced sample preparation compared to many other virus detection methods, we report the application of silicon photonic microring resonators for the direct, label-free detection of intact viruses in both purified samples as well as in a complex, real-world analytical matrix. As a model system, we demonstrate the quantitative detection of Bean pod mottle virus, a pathogen of great agricultural importance, with a limit of detection of 10 ng/mL. By simply grinding a small amount of leaf sample in buffer with a mortar and pestle, infected leaves can be identified over a healthy control with a total analysis time of less than 45 min. Given the inherent scalability and multiplexing capability of the semiconductor-based technology, we feel that silicon photonic microring resonators are well-positioned as a promising analytical tool for a number of viral detection applications. PMID:22138465

Development of a micropulverized extraction method for rapid toxicological analysis of methamphetamine in hair.

PubMed

Miyaguchi, Hajime; Kakuta, Masaya; Iwata, Yuko T; Matsuda, Hideaki; Tazawa, Hidekatsu; Kimura, Hiroko; Inoue, Hiroyuki

2007-09-07

We developed a rapid sample preparation method for the toxicological analysis of methamphetamine and amphetamine (the major metabolite of methamphetamine) in human hair by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), to facilitate fast screening and quantitation. Two milligrams of hair were mechanically micropulverized for 5 min in a 2-ml plastic tube together with 100 microl of an aqueous solvent containing 10% acetonitrile, 100 mM trifluoroacetic acid and the corresponding deuterium analogues as internal standards. The pulverizing highly disintegrated the hair components, simultaneously allowing the extraction of any drugs present in the hair. After filtering the suspension with a membrane-filter unit, the clear filtrate was directly analyzed by HPLC-MS/MS. No evaporation processes were required for sample preparation. Method optimization and validation study were carried out using real-case specimens and fortified samples in which the drugs had been artificially absorbed, respectively. Concentration ranges for quantitation were 0.040-125 and 0.040-25 ng/mg for methamphetamine and amphetamine, respectively. Real-case specimens were analyzed by the method presented here and by conventional ones to verify the applicability of our method to real-world analysis. Our method took less than 30 min for a set of chromatograms to be obtained from a washed hair sample.

Classification of red wine based on its protected designation of origin (PDO) using Laser-induced Breakdown Spectroscopy (LIBS).

PubMed

Moncayo, S; Rosales, J D; Izquierdo-Hornillos, R; Anzano, J; Caceres, J O

2016-09-01

This work reports on a simple and fast classification procedure for the quality control of red wines with protected designation of origin (PDO) by means of Laser Induced Breakdown Spectroscopy (LIBS) technique combined with Neural Networks (NN) in order to increase the quality assurance and authenticity issues. A total of thirty-eight red wine samples from different PDO were analyzed to detect fake wines and to avoid unfair competition in the market. LIBS is well known for not requiring sample preparation, however, in order to increase its analytical performance a new sample preparation treatment by previous liquid-to-solid transformation of the wine using a dry collagen gel has been developed. The use of collagen pellets allowed achieving successful classification results, avoiding the limitations and difficulties of working with aqueous samples. The performance of the NN model was assessed by three validation procedures taking into account their sensitivity (internal validation), generalization ability and robustness (independent external validation). The results of the use of a spectroscopic technique coupled with a chemometric analysis (LIBS-NN) are discussed in terms of its potential use in the food industry, providing a methodology able to perform the quality control of alcoholic beverages. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative multiresidue analysis of antibiotics in milk and milk powder by ultra-performance liquid chromatography coupled to tandem quadrupole mass spectrometry.

PubMed

Tian, He; Wang, Jiaqi; Zhang, Yangdong; Li, Songli; Jiang, Jindou; Tao, Dali; Zheng, Nan

2016-10-15

A simple and fast multiresidue extraction and purification method was developed for the determination of 61 veterinary drugs, belonging to seven classes, in milk and milk powder. The extraction depends on the acetonitrile solvent, followed by a single step to remove lipids with fatty acid chains using a new reversed phase SPE without traditional pre-equilibration and washing steps before eluting SPE. The purifying lipid effect of the present preparation method was evaluated by comparing the response changes of ion peak areas of the milk endogenous metabolites before and after SPE treatment using ultra-fast LC coupled to tandem quadrupole and TOF MS. Subsequently, UPLC coupled to tandem quadrupole MS was performed for the quantitative analysis of milk and milk powder samples spiked with 61 veterinary drugs, including β-lactam, macrolide, amide alcohol, forest amine, sulfanilamide, tetracyclines, and quinolones antibiotics. This method is very simple, fast, sensitive, and selective, and allows the good recoveries of all compounds, with a recovery range of 61.5-118.6%, and coefficients of variation of less than 11.6%. The 61 compounds behave in the dynamic range 0.01-200μgkg(-1), with correlation coefficient >0.99. The limits of quantification for the analytes are in the range 0.01-5.18μgkg(-1). Finally, this method has been successfully applied to the screening of veterinary drugs in 50 commercial bovine milk and milk powder samples, and ceftiofur and ciprofloxacin were detected in some brand samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Combination of nano-material enrichment and dead-end filtration for uniform and rapid sample preparation in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Wu, Zengnan; Khan, Mashooq; Mao, Sifeng; Lin, Ling; Lin, Jin-Ming

2018-05-01

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a fast analysis tool for the detection of a wide range of analytes. However, heterogeneous distribution of matrix/analyte cocrystal, variation in signal intensity and poor experimental reproducibility at different locations of the same spot means difficulty in quantitative analysis. In this work, carbon nanotubes (CNTs) were employed as adsorbent for analyte cum matrix on a conductive porous membrane as a novel mass target plate. The sample pretreatment step was achieved by enrichment and dead-end filtration and dried by a solid-liquid separation. This approach enables the homogeneous distribution of analyte in the matrix, good shot-to-shot reproducibility in signals and quantitative detection of peptide and protein at different concentrations with correlation coefficient (R 2 ) of 0.9920 and 0.9909, respectively. The simple preparation of sample in a short time, uniform distribution of analyte, easy quantitative detection, and high reproducibility makes this technique useful and may diversify the application of MALDI-MS for quantitative detection of a variety of proteins. Copyright © 2018 Elsevier B.V. All rights reserved.

Advantages of automation in plasma sample preparation prior to HPLC/MS/MS quantification: application to the determination of cilazapril and cilazaprilat in a bioequivalence study.

PubMed

Kolocouri, Filomila; Dotsikas, Yannis; Apostolou, Constantinos; Kousoulos, Constantinos; Soumelas, Georgios-Stefanos; Loukas, Yannis L

2011-01-01

An HPLC/MS/MS method characterized by complete automation and high throughput was developed for the determination of cilazapril and its active metabolite cilazaprilat in human plasma. All sample preparation and analysis steps were performed by using 2.2 mL 96 deep-well plates, while robotic liquid handling workstations were utilized for all liquid transfer steps, including liquid-liquid extraction. The whole procedure was very fast compared to a manual procedure with vials and no automation. The method also had a very short chromatographic run time of 1.5 min. Sample analysis was performed by RP-HPLC/MS/MS with positive electrospray ionization using multiple reaction monitoring. The calibration curve was linear in the range of 0.500-300 and 0.250-150 ng/mL for cilazapril and cilazaprilat, respectively. The proposed method was fully validated and proved to be selective, accurate, precise, reproducible, and suitable for the determination of cilazapril and cilazaprilat in human plasma. Therefore, it was applied to a bioequivalence study after per os administration of 2.5 mg tablet formulations of cilazapril.

Preoperative fasting: knowledge and perceptions.

PubMed

Baril, Patrice; Portman, Harriet

2007-10-01

Preoperative patient fasting is an essential element of the patient preparation process, but patients may be fasting for excessive lengths of time. Investigators at one facility used semi-structured interviews to explore the knowledge and beliefs of patients, nurses, and anesthesia care providers regarding the practice of preoperative patient fasting. Findings indicate that some patients had excessive fasting times, and practitioners had erroneous perceptions about patient knowledge regarding the rationale for fasting and compliance with instructions. Clinicians expressed concern about the effects of excessive fasting but were reluctant to relax the policy.

Raman spectroscopy as a tool to understand Kerogen production potential

NASA Astrophysics Data System (ADS)

Khatibi, S.; Ostadhassan, M.; Mohammed, R. A.; Alexeyev, A.

2017-12-01

A lot attention has given to unconventional reservoirs specifically oil shale in North America during the last decades. Understanding Kerogen properties in terms of maturity and production potential are crucial for unconventional reservoir. Since, the amount of hydrocarbon generation is a function of kerogen type and content in the formation, and the magnitude and duration in which heat and pressure were applied. This study presents a non-destructive and fast method to determine Kerogen properties in terms of Rock-Eval parameters by means of Raman Spectroscopy. Samples were gathered from upper and lower Bakken formation, with different maturities at different depth. Raman spectroscopy as a powerful nondestructive analytical tool for molecular reconstruction was employed to find Raman spectra of different samples. In the next step, Rock-Eval was performed for each sample and different measurements were made. Then in an original approach, correlation between Rock-Eval parameters with Raman Spectroscopy results was established to fully understand how kerogen productivity potentials can be reflected on the Raman response. Results showed, maturity related parameters (RO, Tmax), S1 (already generated oil in the rock), S2 (potential hydrocarbon) and OSI (oil saturation index as indication of potential oil flow zones) can be correlated to band separation, D band intensity, G band intensity and G/D intensity, respectively. Proposed method provide a fast nondestructive method to evaluate Kerogen quality even at field without any special sample preparation.

Experiences of Fast Queue health care users in primary health care facilities in eThekwini district, South Africa.

PubMed

Sokhela, Dudu G; Makhanya, Nonhlanhla J; Sibiya, Nokuthula M; Nokes, Kathleen M

2013-07-05

Comprehensive Primary Health Care (PHC), based on the principles of accessibility, availability, affordability, equity and acceptability, was introduced in South Africa to address inequalities in health service provision. Whilst the Fast Queue was instrumental in the promotion of access to health care, a major goal of the PHC approach, facilities were not prepared for the sudden influx of clients. Increased access resulted in long waiting times and queues contributing to dissatisfaction with the service which could lead to missed appointments and non-compliance with established treatment plans. Firstly to describe the experiences of clients using the Fast Queue strategy to access routine healthcare services and secondly, to determine how the clients' experiences led to satisfaction or dissatisfaction with the Fast Queue service. A descriptive qualitative survey using content analysis explored the experiences of the Fast Queue users in a PHC setting. Setting was first identified based on greatest number using the Fast Queue and geographic diversity and then a convenience sample of health care users of the Fast Queue were sampled individually along with one focus group of users who accessed the Queue monthly for medication refills. The same interview guide questions were used for both individual interviews and the one focus group discussion. Five clinics with the highest number of attendees during a three month period and a total of 83 health care users of the Fast Queue were interviewed. The average participant was female, 31 years old, single and unemployed. Two themes with sub-themes emerged: health care user flow and communication, which highlights both satisfaction and dissatisfaction with the fast queue and queue marshals, could assist in directing users to the respective queues, reduce waiting time and keep users satisfied with the use of sign posts where there is a lack of human resources. Effective health communication strategies contribute to positive experiences by health care users and these can be effected by: (1) involvement of health care providers in planning the construction of health facilities to give input about patient flow, infection prevention and control and provision of privacy, (2) effective complaints mechanisms for users to ensure that complaints are followed up and (3)encouraging users to arrive at the facility throughout the day, rather than the present practice where all users arrive at the clinic early in the morning.

Testicular biopsy in psittacine birds (Psittaciformes): comparative evaluation of testicular reproductive status by endoscopic, histologic, and cytologic examination.

PubMed

Hänse, Maria; Krautwald-Junghanns, Maria-Elisabeth; Reitemeier, Susanne; Einspanier, Almuth; Schmidt, Volker

2013-12-01

Knowledge of the reproductive cycle of male parrots is important for examining the male genital tract and for successful breeding, especially of endangered species. To evaluate different diagnostic methods and criteria concerning the classification of reproductive stages, we examined 20 testicular samples obtained at necropsy in psittacine birds of different species and testicular biopsy samples collected from 9 cockatiels (Nymphicus hollandicus) and 7 rose-ringed parakeets (Psittacula krameri) by endoscopy 4 times over a 12-month period. The testicular reproductive status was assessed histologically and then compared with the macroscopic appearance of the testicles and cytologic results. The histologic examination was nondiagnostic in 19 of 59 testicular biopsy samples. By contrast, the cytologic preparations were diagnostic in 57 of 59 biopsy samples. The results of the cytologic examination coincided with the histologic results in 34 of 38 biopsy samples and 18 of 20 necropsy samples. Macroscopic parameters displayed some differences between reproductive stages but provided an unreliable indication of the reproductive status. These results suggest that microscopic examination of a testicular biopsy sample is a reliable method for evaluating the reproductive status of male parrots and is preferable to the macroscopic evaluation of the testicle. Cytologic examination provides fast preliminary results, even when the histologic preparation is not sufficient for evaluation, but results may be erroneous. Thus, a combination of histologic and cytologic examination is recommended for evaluating testicular reproductive status.

Ultrafine Nanocrystalline CeO2@C-Containing NaAlH4 with Fast Kinetics and Good Reversibility for Hydrogen Storage.

PubMed

Zhang, Xin; Liu, Yongfeng; Wang, Ke; Li, You; Gao, Mingxia; Pan, Hongge

2015-12-21

A nanocrystalline CeO2@C-containing NaAlH4 composite is successfully synthesized in situ by hydrogenating a NaH-Al mixture doped with CeO2@C. Compared with NaAlH4 , the as-prepared CeO2@C-containing NaAlH4 composite, with a minor amount of excess Al, exhibits significantly improved hydrogen storage properties. The dehydrogenation onset temperature of the hydrogenated [NaH-Al-7 wt % CeO2@C]-0.04Al sample is 77 °C lower than that of the pristine sample because of a reduced kinetic barrier. More importantly, the dehydrogenated sample absorbs ∼4.7 wt % hydrogen within 35 min at 100°C and 10 MPa of hydrogen. Compositional and structural analyses reveal that CeO2 is converted to CeH2 during ball milling and that the newly formed CeH2 works with the excess of Al to synergistically improve the hydrogen storage properties of NaAlH4. Our findings will aid in the rational design of novel catalyst-doped complex hydride systems with low operating temperatures, fast kinetics, and long-term cyclability. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Centrifugal partition chromatography a first dimension for biomass fast pyrolysis oil analysis.

PubMed

Le Masle, Agnès; Santin, Sandra; Marlot, Léa; Chahen, Ludovic; Charon, Nadège

2018-10-31

Biomass fast pyrolysis oils contain molecules having a large variety of chemical functions and a wide range of molecular weights (from several tens to several thousand grams per mole). The good knowledge of their complex composition is essential for optimizing the conversion of bio-oils to biofuels, thereby requiring powerful separation techniques. In this work, we investigate the interest of centrifugal partition chromatography (CPC) as a first dimension for the analysis of a bio-oil. A CPC method is proposed to separate oxygen containing compounds according to their partition coefficients in the solvent system. This approach is a powerful and easy-to-use technique that enables fractionation of a bio-oil at a semi-preparative scale, without any sample loss related to adsorption on the stationary phase. Collected fractions are then injected in liquid chromatography as a second dimension of separation. Contour plot representations of the CPC × LC separation are established to discuss the potential of this approach. These representations can be used as a veritable fingerprint in the comparison of different samples or samples at different steps of a conversion process but also as a powerful tool to identify new compounds and describe the entire composition of the bio-oil. Copyright © 2018 Elsevier B.V. All rights reserved.

Investigation of hidden periodic structures on SEM images of opal-like materials using FFT and IFFT.

PubMed

Stephant, Nicolas; Rondeau, Benjamin; Gauthier, Jean-Pierre; Cody, Jason A; Fritsch, Emmanuel

2014-01-01

We have developed a method to use fast Fourier transformation (FFT) and inverse fast Fourier transformation (IFFT) to investigate hidden periodic structures on SEM images. We focused on samples of natural, play-of-color opals that diffract visible light and hence are periodically structured. Conventional sample preparation by hydrofluoric acid etch was not used; untreated, freshly broken surfaces were examined at low magnification relative to the expected period of the structural features, and, the SEM was adjusted to get a very high number of pixels in the images. These SEM images were treated by software to calculate autocorrelation, FFT, and IFFT. We present how we adjusted SEM acquisition parameters for best results. We first applied our procedure on an SEM image on which the structure was obvious. Then, we applied the same procedure on a sample that must contain a periodic structure because it diffracts visible light, but on which no structure was visible on the SEM image. In both cases, we obtained clearly periodic patterns that allowed measurements of structural parameters. We also investigated how the irregularly broken surface interfered with the periodic structure to produce additional periodicity. We tested the limits of our methodology with the help of simulated images. © 2014 Wiley Periodicals, Inc.

Automated mineralogy based on micro-energy-dispersive X-ray fluorescence microscopy (µ-EDXRF) applied to plutonic rock thin sections in comparison to a mineral liberation analyzer

NASA Astrophysics Data System (ADS)

Nikonow, Wilhelm; Rammlmair, Dieter

2017-10-01

Recent developments in the application of micro-energy-dispersive X-ray fluorescence spectrometry mapping (µ-EDXRF) have opened up new opportunities for fast geoscientific analyses. Acquiring spatially resolved spectral and chemical information non-destructively for large samples of up to 20 cm length provides valuable information for geoscientific interpretation. Using supervised classification of the spectral information, mineral distribution maps can be obtained. In this work, thin sections of plutonic rocks are analyzed by µ-EDXRF and classified using the supervised classification algorithm spectral angle mapper (SAM). Based on the mineral distribution maps, it is possible to obtain quantitative mineral information, i.e., to calculate the modal mineralogy, search and locate minerals of interest, and perform image analysis. The results are compared to automated mineralogy obtained from the mineral liberation analyzer (MLA) of a scanning electron microscope (SEM) and show good accordance, revealing variation resulting mostly from the limit of spatial resolution of the µ-EDXRF instrument. Taking into account the little time needed for sample preparation and measurement, this method seems suitable for fast sample overviews with valuable chemical, mineralogical and textural information. Additionally, it enables the researcher to make better and more targeted decisions for subsequent analyses.

Scintillation properties of rare-earth doped NaPO3-Al(PO3)3 glasses

NASA Astrophysics Data System (ADS)

Kuro, Tomoaki; Okada, Go; Kawaguchi, Noriaki; Fujimoto, Yutaka; Masai, Hirokazu; Yanagida, Takayuki

2016-12-01

We systematically investigated photoluminescence (PL), scintillation and dosimeter properties of rare-earth (RE) doped NaPO3-Al(PO3)3 (NAP) glasses. The NAP glasses doped with a series of RE ions (La-Yb, except Pm) with a consistent concentration (0.3 wt%) were prepared by the conventional melt-quenching method. The PL and scintillation decay time profiles showed fast (ns) and slow (μs or ms) components: the fast components from 15 to 100 ns were due to the host or 5d-4f transition emission, and the slow components from 15 μs to 5 ms were due to the 4f-4f transitions of RE. The thermally stimulated luminescence (TSL) was evaluated as a dosimeter property, and glow peaks appeared around 400 °C in all the samples. The TSL dose response function was examined in the dose range from 10 mGy to 10 Gy. Among the samples tested, Nd and Tb doped glasses showed higher signal by at least one order of magnitude than those of non-doped and other RE-doped samples. Over the dose range tested, the TSL signals are linearly related with the incident X-ray dose, showing a potential for practical applications.

Heart failure - discharge

MedlinePlus

... Avoid fatty foods. Stay away from fast-food restaurants. Avoid some prepared and frozen foods. Learn fast ... A.D.A.M. follows rigorous standards of quality and accountability. A.D.A.M. is among ...

Cooling rate dependence of structural order in Al90Sm10 metallic glass

NASA Astrophysics Data System (ADS)

Sun, Yang; Zhang, Yue; Zhang, Feng; Ye, Zhuo; Ding, Zejun; Wang, Cai-Zhuang; Ho, Kai-Ming

2016-07-01

The atomic structure of Al90Sm10 metallic glass is studied using molecular dynamics simulations. By performing a long sub-Tg annealing, we developed a glass model closer to the experiments than the models prepared by continuous cooling. Using the cluster alignment method, we found that "3661" cluster is the dominating short-range order in the glass samples. The connection and arrangement of "3661" clusters, which define the medium-range order in the system, are enhanced significantly in the sub-Tg annealed sample as compared with the fast cooled glass samples. Unlike some strong binary glass formers such as Cu64.5Zr35.5, the clusters representing the short-range order do not form an interconnected interpenetrating network in Al90Sm10, which has only marginal glass formability.

A Surface Plasmon Resonance-Based Optical Fiber Probe Fabricated with Electropolymerized Molecular Imprinting Film for Melamine Detection

PubMed Central

Zheng, Yongping; Zhang, Tingwei; Wu, Songjie; Zhang, Jue; Fang, Jing

2018-01-01

Molecularly imprinted polymer (MIP) films prepared by bulk polymerization suffer from numerous deficiencies, including poor mass transfer ability and difficulty in controlling reaction rate and film thickness, which usually result in poor repeatability. However, polymer film synthesized by electropolymerization methods benefit from high reproducibility, simplicity and rapidity of preparation. In the present study, an Au film served as the refractive index-sensitive metal film to couple with the light leaked out from optical fiber core and the electrode for electropolymerizing MIP film simultaneously. The manufactured probe exhibited satisfactory sensitivity and specificity. Furthermore, the surface morphology and functional groups of the synthesized MIP film were characterized by Atomic Force Microscopy (AFM) and Fourier transform infrared microspectroscopy (FTIR) for further insights into the adsorption and desorption processes. Given the low cost, label-free test, simple preparation process and fast response, this method has a potential application to monitor substances in complicated real samples for out-of-lab test in the future. PMID:29522472

Gravimetric method for the determination of diclofenac in pharmaceutical preparations.

PubMed

Tubino, Matthieu; De Souza, Rafael L

2005-01-01

A gravimetric method for the determination of diclofenac in pharmaceutical preparations was developed. Diclofenac is precipitated from aqueous solution with copper(II) acetate in pH 5.3 (acetic acid/acetate buffer). Sample aliquots had approximately the same quantity of the drug content in tablets (50 mg) or in ampules (75 mg). The observed standard deviation was about +/- 2 mg; therefore, the relative standard deviation (RSD) was approximately 4% for tablet and 3% for ampule preparations. The results were compared with those obtained with the liquid chromatography method recommended in the United States Pharmacopoeia using the statistical Student's t-test. Complete agreement was observed. It is possible to obtain more precise results using higher aliquots, for example 200 mg, in which case the RSD falls to 1%. This gravimetric method, contrary to what is expected for this kind of procedure, is relatively fast and simple to perform. The main advantage is the absolute character of the gravimetric analysis.

Synergistic effect of carbon nanofiber/nanotube composite catalyst on carbon felt electrode for high-performance all-vanadium redox flow battery.

PubMed

Park, Minjoon; Jung, Yang-jae; Kim, Jungyun; Lee, Ho il; Cho, Jeaphil

2013-10-09

Carbon nanofiber/nanotube (CNF/CNT) composite catalysts grown on carbon felt (CF), prepared from a simple way involving the thermal decomposition of acetylene gas over Ni catalysts, are studied as electrode materials in a vanadium redox flow battery. The electrode with the composite catalyst prepared at 700 °C (denoted as CNF/CNT-700) demonstrates the best electrocatalytic properties toward the V(2+)/V(3+) and VO(2+)/VO2(+) redox couples among the samples prepared at 500, 600, 700, and 800 °C. Moreover, this composite electrode in the full cell exhibits substantially improved discharge capacity and energy efficiency by ~64% and by ~25% at 40 mA·cm(-2) and 100 mA·cm(-2), respectively, compared to untreated CF electrode. This outstanding performance is due to the enhanced surface defect sites of exposed edge plane in CNF and a fast electron transfer rate of in-plane side wall of the CNT.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection.

PubMed

Alexandrou, Lydon D; Meehan, Barry J; Morrison, Paul D; Jones, Oliver A H

2017-05-15

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid-liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9-9.3 µg/L).

Validation of the RIDASCREEN(®)FAST Milk Kit.

PubMed

Weiss, Thomas; Lacorn, Markus; Flannery, Jonathan; Benzinger, M Joseph; Bird, Patrick; Crowley, Erin S; Goins, Dave; Agin, James R; Gilani, Sarwar; Poepping, Bert; Garber, Eric

2016-01-01

The RIDASCREEN(®)FAST Milk test is a sandwich ELISA for the rapid quantification of milk proteins in various foods. The specific antibodies target casein and β-lactoglobulin. Samples are extracted and can then be analyzed in less than 40 min. The calibration curve covers a range from 2.5 to 67.5 mg/kg milk protein. The assay was validated with cookies, infant formula, chocolate dessert, ice cream, and sausages. All negative samples were found well below the LOQ of 2.5 mg/kg. Recoveries of the spiked samples were mostly in the range of 80-120%. The LOD of the ELISA was found below 1 mg/kg. The analysis of 39 different substances of interest revealed that no cross-reactivity above the LOQ occurred. Ruggedness testing proved that variations in incubation temperature, reagent volume, incubation time, extraction temperature, and extraction time had no significant influence. The stability at 4-8°C of three independent lots was investigated and found to exceed 18 months. Very good lot-to-lot consistency and no significant loss of the analytical capacity over the shelf life were observed. Incurred cookies and chocolate dessert samples were prepared and analyzed by an independent laboratory; mean recoveries of 94.4 and 102.2% and mean SDs of 10.9 and 6.3%, respectively, were found. For the 0 mg/kg level for both materials, all samples tested returned values of <2.5 mg/kg. Therefore, the analytical performance claims of the manufacturer were confirmed.

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.

Surface-enhanced Raman scattering spectroscopy characterization and identification of foodborne bacteria

NASA Astrophysics Data System (ADS)

Liu, Yongliang; Chen, Yud-Ren; Nou, Xiangwu; Chao, Kaunglin

2007-09-01

Rapid and routine identification of foodborne bacteria are considerably important, because of bio- / agro- terrorism threats, public health concerns, and economic loss. Conventional, PCR, and immunoassay methods for the detection of bacteria are generally time-consuming, chemical reagent necessary and multi-step procedures. Fast microbial detection requires minimal sample preparation, permits the routine analysis of large numbers of samples with negligible reagent costs, and is easy to operate. Therefore, we have developed silver colloidal nanoparticle based surface-enhanced Raman scattering (SERS) spectroscopy as a potential tool for the rapid and routine detection of E. coli and L. monocytogenes. This study presents the further results of our examination on S. typhimonium, one of the most commonly outbreak bacteria, for the characteristic bands and subsequent identification.

Preliminary study of neutron absorption by concrete with boron carbide addition

NASA Astrophysics Data System (ADS)

Abdullah, Yusof; Ariffin, Fatin Nabilah Tajul; Hamid, Roszilah; Yusof, Mohd Reusmaazran; Zali, Nurazila Mat; Ahmad, Megat Harun Al Rashid Megat; Yazid, Hafizal; Ahmad, Sahrim; Mohamed, Abdul Aziz

2014-02-01

Concrete has become a conventional material in construction of nuclear reactor due to its properties like safety and low cost. Boron carbide was added as additives in the concrete construction as it has a good neutron absorption property. The sample preparation for concrete was produced with different weight percent of boron carbide powder content. The neutron absorption rate of these samples was determined by using a fast neutron source of Americium-241/Be (Am-Be 241) and detection with a portable backscattering neutron detector. Concrete with 20 wt % of boron carbide shows the lowest count of neutron transmitted and this indicates the most neutrons have been absorbed by the concrete. Higher boron carbide content may affect the concrete strength and other properties.

Fast classification of hazelnut cultivars through portable infrared spectroscopy and chemometrics

NASA Astrophysics Data System (ADS)

Manfredi, Marcello; Robotti, Elisa; Quasso, Fabio; Mazzucco, Eleonora; Calabrese, Giorgio; Marengo, Emilio

2018-01-01

The authentication and traceability of hazelnuts is very important for both the consumer and the food industry, to safeguard the protected varieties and the food quality. This study investigates the use of a portable FTIR spectrometer coupled to multivariate statistical analysis for the classification of raw hazelnuts. The method discriminates hazelnuts from different origins/cultivars based on differences of the signal intensities of their IR spectra. The multivariate classification methods, namely principal component analysis (PCA) followed by linear discriminant analysis (LDA) and partial least square discriminant analysis (PLS-DA), with or without variable selection, allowed a very good discrimination among the groups, with PLS-DA coupled to variable selection providing the best results. Due to the fast analysis, high sensitivity, simplicity and no sample preparation, the proposed analytical methodology could be successfully used to verify the cultivar of hazelnuts, and the analysis can be performed quickly and directly on site.

PALS Free Volume Measurements of Fractionated Hydrido- Silsesquioxane Resin.

NASA Astrophysics Data System (ADS)

Madani, Mahmoud M.; Granata, Richard D.; Pernisz, Udo C.

1997-03-01

Hydrido-Silsesquioxane (HSQ) is a resinous polymer with monomer unit formula (HSiO_3/2)_n. For n=8...16, it forms cages which in turn cross-link to yield a resin with a broad molecular weight distribution. It is soluble and forms thin films that may be converted to low-density silica with excellent dielectric properties. These, and the HSQ solubility, depend on molecular structure and size distribution of the cages. Samples of different molecular weight fractions were prepared from HSQ by SCF and the free volume of several cuts was measured by PALS in a conventional fast-fast system. POSITRONFIT and CONTIN programs were used to analyze the spectra. Three separate lifetime regions were identified with free volume regimes that correlate strongly with the molecular weight. The lowest is identified with the monomer cage unit, the larger values with intramolecular separation.

Fast Estimation of Dietary Fiber Content in Apple.

PubMed

Le Gall, Sophie; Even, Sonia; Lahaye, Marc

2016-02-17

Dietary fibers (DF) are one of the nutritional benefits of fleshy fruit consumption that is becoming a quality criterion for genetic selection by breeders. However, the AOAC total DF content determination is not readily amenable for screening large fruit collections. A new screening method of DF content in an apple collection based on the automated preparation of cell wall material as an alcohol-insoluble residue (AIR) is proposed. The yield of AIR from 27 apple genotypes was compared with DF measured according to AOAC method 985.29. Although residual protein content in AIRs did not affect DF measurement, subtraction of starch content above 3% dry weight in AIRs was needed to agree with AOAC measured DF. A fast colorimetric screening of starch in AIR was developed to detect samples needing correction. The proposed method may prove useful for the rapid determination of DF in collections of other fleshy fruit besides apple.

Polydimethylsiloxane/MIL-100(Fe) coated stir bar sorptive extraction-high performance liquid chromatography for the determination of triazines in environmental water samples.

PubMed

Lei, Yun; Chen, Beibei; You, Linna; He, Man; Hu, Bin

2017-12-01

Polydimethylsiloxane (PDMS)/MIL-100(Fe) coated stir bar was prepared by sol gel technique, and good preparation reproducibility was achieved with relative standard deviations (RSDs) ranging from 2.6% to 7.5% (n=7) and 3.6% to 10.8% (n=7) for bar-to-bar and batch-to-batch, respectively. Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/MIL-100(Fe) stir bar showed better extraction efficiency for target triazines compounds. It also exhibited relatively fast extraction/desorption kinetics and long lifespan. Based on it, a method of PDMS/MIL-100(Fe) coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed for the determination of six triazines (simazine, atrazine, prometon, ametryn, prometryne and prebane) in environmental water samples. Several parameters affecting SBSE of six target triazines including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.021-0.079μgL -1 . The repeatability RSDs were in the range of 2.3-6.3% (n=7, c=0.5μgL -1 ) and the enrichment factors (EFs) ranged from 51.1 to 102-fold (theoretical EF was 200-fold). The proposed method was applied to the analysis of target triazines in environmental water samples, with recoveries of 98.0-118% and 94.0-107% for spiked East Lake water and local pond water samples, respectively. Copyright © 2017. Published by Elsevier B.V.

48 CFR 13.403 - Preparation and execution of orders.

Code of Federal Regulations, 2012 CFR

2012-10-01

... REGULATION CONTRACTING METHODS AND CONTRACT TYPES SIMPLIFIED ACQUISITION PROCEDURES Fast Payment Procedure 13... the fast payment procedure shall include the following: (a) A requirement that the supplies be shipped...

48 CFR 13.403 - Preparation and execution of orders.

Code of Federal Regulations, 2011 CFR

2011-10-01

... REGULATION CONTRACTING METHODS AND CONTRACT TYPES SIMPLIFIED ACQUISITION PROCEDURES Fast Payment Procedure 13... the fast payment procedure shall include the following: (a) A requirement that the supplies be shipped...

48 CFR 13.403 - Preparation and execution of orders.

Code of Federal Regulations, 2014 CFR

2014-10-01

... REGULATION CONTRACTING METHODS AND CONTRACT TYPES SIMPLIFIED ACQUISITION PROCEDURES Fast Payment Procedure 13... the fast payment procedure shall include the following: (a) A requirement that the supplies be shipped...

48 CFR 13.403 - Preparation and execution of orders.

Code of Federal Regulations, 2010 CFR

2010-10-01

... REGULATION CONTRACTING METHODS AND CONTRACT TYPES SIMPLIFIED ACQUISITION PROCEDURES Fast Payment Procedure 13... the fast payment procedure shall include the following: (a) A requirement that the supplies be shipped...

48 CFR 13.403 - Preparation and execution of orders.

Code of Federal Regulations, 2013 CFR

2013-10-01

... REGULATION CONTRACTING METHODS AND CONTRACT TYPES SIMPLIFIED ACQUISITION PROCEDURES Fast Payment Procedure 13... the fast payment procedure shall include the following: (a) A requirement that the supplies be shipped...

Guidelines for Bowel Preparation before Video Capsule Endoscopy

PubMed Central

Song, Hyun Joo; Do, Jae Hyuk; Cha, In Hye; Yang, Chang Hun; Choi, Myung-Gyu; Jeen, Yoon Tae; Kim, Hyun Jung

2013-01-01

The preparation for video capsule endoscopy (VCE) of the bowel suggested by manufacturers of capsule endoscopy systems consists only of a clear liquid diet and an 8-hour fast. While there is evidence for a benefit from bowel preparation for VCE, so far there is no domestic consensus on the preparation regimen in Korea. Therefore, we performed this study to recommend guidelines for bowel preparation before VCE. The guidelines on VCE were developed by the Korean Gut Image Study Group, part of the Korean Society of Gastrointestinal Endoscopy. Four key questions were selected. According to our guidelines, bowel preparation with polyethylene glycol (PEG) solution enhances small bowel visualization quality (SBVQ) and diagnostic yield (DY), but it has no effect on cecal completion rate (CR). Bowel preparation with 2 L of PEG solution is similar to that with 4 L of PEG in terms of the SBVQ, DY, and CR of VCE. Bowel preparation with fasting or PEG solution combined with simethicone enhances the SBVQ, but it does not affect the CR of VCE. Bowel preparation with prokinetics does not enhance the SBVQ, DY, or CR of VCE. PMID:23614124

Microwave-assisted RAFT polymerization of well-constructed magnetic surface molecularly imprinted polymers for specific recognition of benzimidazole residues

NASA Astrophysics Data System (ADS)

Chen, Fangfang; Wang, Jiayu; Chen, Huiru; Lu, Ruicong; Xie, Xiaoyu

2018-03-01

Magnetic nanoparticles have been widely used as support core for fast separation, which could be directly separated from complicated matrices using an external magnet in few minutes. Surface imprinting based on magnetic core has shown favorable adsorption and separation performance, including good adsorption capacity, fast adsorption kinetics and special selectivity adsorption. Reversible addition-fragmentation chain transfer (RAFT) is an ideal choice for producing well-defined complex architecture with mild reaction conditions. We herein describe the preparation of well-constructed magnetic molecularly imprinted polymers (MMIPs) for the recognition of benzimidazole (BMZ) residues via the microwave-assisted RAFT polymerization. The merits of RAFT polymerization assisting with microwave heating allowed successful and more efficient preparation of well-constructed imprinted coats. Moreover, the polymerization time dramatically shortened and was just 1/24th of the time taken by conventional heating. The results indicated that a uniform nanoscale imprinted layer was formed on the Fe3O4 core successfully, and enough saturation magnetization of MMIPs (16.53 emu g-1) was got for magnetic separation. The desirable adsorption capacity (30.18 μmol g-1) and high selectivity toward template molecule with a selectivity coefficient (k) of 13.85 of MMIPs were exhibited by the adsorption isothermal assay and competitive binding assay, respectively. A solid phase extraction enrichment approach was successfully established for the determination of four BMZ residues from apple samples using MMIPs coupled to HPLC. Overall, this study provides a versatile approach for highly efficient fabrication of well-constructed MMIPs for enrichment and determination of target molecules from complicated samples.

Ethanol extraction preparation of American ginseng (Panax quinquefolius L) and Korean red ginseng (Panax ginseng C.A. Meyer): differential effects on postprandial insulinemia in healthy individuals.

PubMed

De Souza, Leanne R; Jenkins, Alexandra L; Jovanovski, Elena; Rahelić, Dario; Vuksan, Vladimir

2015-01-15

Ginsenosides are the proposed bioactive constituent of ginseng, especially for the attenuation of postprandial glycemia (PPG). The efficacious proportion of total and specific ginsenosides, remains unknown. Alcohol extraction of whole ginseng root can be used to selectively manipulate the ginsenoside profile with increasing alcohol concentrations producing high yields of total ginsenosides and varying their individual proportions. We aimed to compare the acute efficacy of different ethanol-extraction preparations of American ginseng (AG) and Korean red ginseng (KRG), with their whole-root origins, on PPG and insulin parameters in healthy adults. Following an overnight fast, 13 healthy individuals (Gender: 5M:8F, with mean ± SD, age: 28.9 ± 9.2 years, BMI: 26.3 ± 2.7 kg/m(2) and fasting plasma glucose: 4.21 ± 0.04 mmol/L) randomly received 3g of each of the following 10 different ginseng treatments on separate visits: whole root KRG and AG; 30%, 50% or 70% ethanol extracts of KRG and AG and 2 cornstarch placebos. Treatments were consumed 40 min prior to a 50 g oral glucose challenge test with capillary blood samples collected at baseline, 15, 30, 45, 60, 90 and 120 min. Insulin samples were collected at 0, 30, 60 and 120 min. There was no difference in attenuation of PPG among the tested ginseng preparations. Measures of Insulin Sensitivity Index (ISI) showed increased insulin sensitivity (IS) with KRG-30% and AG-50% extracts compared to placebo (p<0.05). The insulin sensitizing effects of KRG-30% and AG-50% extracts suggest that other root parts, including other ginsenosides not typically measured, may influence PPG and insulin parameters. There is potential for AG and KRG extracts to modulate IS, an independent predictor of type 2 diabetes. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Eating on the run. A qualitative study of health agency and eating behaviors among fast food employees.

PubMed

Mulvaney-Day, Norah E; Womack, Catherine A; Oddo, Vanessa M

2012-10-01

Understanding the relationship between obesity and fast food consumption encompasses a broad range of individual level and environmental factors. One theoretical approach, the health capability framework, focuses on the complex set of conditions allowing individuals to be healthy. This qualitative study aimed to identify factors that influence individual level health agency with respect to healthy eating choices in uniformly constrained environments (e.g., fast food restaurants). We used an inductive qualitative research design to develop an interview guide, conduct open-ended interviews with a purposive sample of 14 student fast food workers (aged 18-25), and analyze the data. Data analysis was conducted iteratively during the study with multiple coders to identify themes. Emergent themes included environmental influences on eating behaviors (time, cost, restaurant policies, social networks) and internal psychological factors (feelings associated with hunger, food knowledge versus food preparation know-how, reaction to physical experiences, perceptions of food options, delayed gratification, and radical subjectivity). A localized, embedded approach to analyzing the factors driving the obesity epidemic is needed. Addressing contextual interactions between internal psychological and external environmental factors responds to social justice and public health concerns, and may yield more relevant and effective interventions for vulnerable communities. Copyright © 2012 Elsevier Ltd. All rights reserved.

Preparation of high affinity antibody for ribavirin with new haptens and residue analysis in chicken muscle, eggs and duck muscle.

PubMed

Wang, Zhaopeng; Yu, Xuezhi; Ma, Licai; Liu, Hebing; Ding, Shuangyang; Wang, Zhanhui; Zhang, Xiya; Shen, Jianzhong; Wen, Kai

2018-05-23

In this work, high affinity polyclonal antibodies for ribavirin (RBV) from new haptens were prepared and were used to analyse RBV residues in chicken muscle, eggs and duck muscle. The new haptens were synthesised with different spacers, and the best antibody was obtained with an IC 50 value as low as 0.61 ng/mL in indirect competitive enzyme-linked immunosorbent assay (ELISA). The cross-reactivities with another five antiviral drugs including amantadine, rimantadine, moroxydine, zanamivir and oseltamivir were less than 0.1%, which indicated the good specificity of the antibody. An ELISA was developed based on the antibody and applied to detect RBV in multi-food matrices. The sample preparation prior to detection only needed simple dilution after trichloroacetic acid extraction. The limits of detection were 1.07, 1.18 and 1.03 μg/kg in chicken muscle, eggs and duck muscle, respectively. Recoveries ranged from 89.0% to 112.7% with coefficients of variation below 13.0%. Ten blind samples of chicken muscle were analysed simultaneously by ELISA and liquid chromatography-tandem mass spectrometry, and a good correlation between the methods was observed. The results indicated that the high affinity antibody could be applied for the simple and fast detection of RBV in multi-food matrices.

Applicability of refractometry for fast routine checking of hospital preparations.

PubMed

Hendrickx, Stijn; Verón, Aurora Monteagudo; Van Schepdael, Ann; Adams, Erwin

2016-04-30

Quality control of hospital pharmacy formulations is of the utmost importance to ensure constant quality and to avoid potential mistakes before administration to the patient. In this study we investigated the applicability of refractometry as a fast, inexpensive and easy-to-use quality control measurement. Refractive indices (RI) of a multitude of different hospital formulations with varying concentrations of active compound were measured. The samples consisted of a number of binary aqueous solutions (one compound in water), complex aqueous solutions (multiple compounds in water or in a constant matrix), two suspensions and one emulsion. For all these formulations, linear regression analysis was performed, quality control limits determined and accuracy and repeatability were checked. Subsequently, actual hospital pharmacy samples were analyzed to check whether they were within the specified limits. For both binary and complex aqueous formulations, repeatability was good and a linear correlation for all samples could be observed on condition that the concentration of the active compound was sufficiently high. The refractometer was not sensitive enough for solutions of folic acid and levothyroxine, which had too low a concentration of active compound. Due to lack of homogeneity and light scattering, emulsions and suspensions do not seem suitable for quality control by refractometry. A mathematical equation was generated to predict the refractive index of an aqueous solution containing clonidine HCl as active compound. Values calculated from the equation were compared with measured values and deviations of all samples were found to be lower than 1.3%. In order to use refractometry in a hospital pharmacy for quality control of multicomponent samples, additional intermediate measurements would be required, to overcome the fact that refractometry is not compound specific. In conclusion, we found that refractometry could potentially be useful for daily, fast quality measurements of relatively concentrated binary and more complex aqueous solutions in the hospital pharmacy. Copyright © 2016 Elsevier B.V. All rights reserved.

Dietary diversity and associated factors among children of Orthodox Christian mothers/caregivers during the fasting season in Dejen District, North West Ethiopia.

PubMed

Kumera, Gemechu; Tsedal, Endalkachew; Ayana, Mulatu

2018-01-01

Proper feeding practices during early childhood is fundamental for optimal child growth and development. However, scientific evidences on the determinants of dietary diversity are scanty. Particularly, the impact of fasting on children`s dietary diversity is not explored in Ethiopia. The aim of this study was to assess dietary diversity and associated factors among children aged 6-23 months, whose mothers/care-givers were Orthodox Christians during the fasting season (Lent), in Dejen District, North West Ethiopia, 2016. A community based cross-sectional study was conducted during the fasting season from March to April, 2016. The study sample were children aged 6-23 months, whose mothers/care-givers were Orthodox Christians. A systematic random sampling technique was used to select a sample of 967 children proportionally from all selected kebeles. Data was entered using Epi data and statistical analysis were done using logistic regression. P-value < 0.05 at 95% confidence interval was taken as statistically significant. Only 13.6% of children surveyed met the minimum requirement for dietary diversity. Unsatisfactory exposure to media [AOR = 5.22] and low household monthly income [AOR = 2.20] were negatively associated with dietary diversity. As compared to economic related reasons, mothers/caregivers who do not feed diet of animal origin to their children due to fear of utensil contamination for family food preparation were 1.5 times [AOR=1.5; 95% CI (1.05 - 2.53)] less likely to feed the recommended dietary diversity. The findings of this study revealed that the diet of children in the study area lacked diversity. Promoting mass media and socioeconomic empowerment of women have positive contribution to optimal child feeding practice. Sustained nutrition education to mothers regarding proper infant and young child feeding practice in collaboration with the respective religious leaders is highly recommended.

Development of an enzyme free glucose sensor based on copper oxide-graphene composite by using green reducing agent ascorbic acid

NASA Astrophysics Data System (ADS)

Palve, Yogesh Pandit; Jha, Neetu

2018-05-01

In this research work we have developed high sensitive and selective glucose sensor based on copper oxide-graphene composite which is prepared by green synthesis method and used for nonenzymatic glucose sensor. In present paper we report that present method highly selective, simple, efficient, accurate, ecofriendly, less toxic. The prepared composite were characterized by material characterization like SEM, XRD and also by electrochemical characterization like CV, chronoamperometry represents that copper oxide-graphene shows excellent electrocatalytic activity towards glucose, exhibiting a good sensitivity of 103.84 µA mM-1 cm-2, a fast response time 2s, a low detection limit 0.00033µM and linear range from 10 µM-3000 µM. The present sensor can successfully apply for determination of glucose concentration in human blood sample.

Food preparation by young adults is associated with better diet quality.

PubMed

Larson, Nicole I; Perry, Cheryl L; Story, Mary; Neumark-Sztainer, Dianne

2006-12-01

To describe food-preparation behaviors, cooking skills, resources for preparing food, and associations with diet quality among young adults. Cross-sectional analyses were performed in a sample of young adults who responded to the second wave of a population-based longitudinal study. Measures pertaining to food preparation were self-reported and dietary intake was assessed by a food frequency questionnaire, both by a mailed survey. Males (n = 764) and females (n = 946) ages 18 to 23 years. Cross-tabulations and chi2 tests were used to examine associations between food preparation, skills/resources for preparing foods, and characteristics of young adults. Mixed regression models were used to generate expected probabilities of meeting the Healthy People 2010 dietary objectives according to reported behaviors and skills/resources. Food-preparation behaviors were not performed by the majority of young adults even weekly. Sex (male), race (African American), and living situation (campus housing) were significantly related to less frequent food preparation. Lower perceived adequacy of skills and resources for food preparation was related to reported race (African American or Hispanic) and student status (part-time or not in school). The most common barrier to food preparation was lack of time, reported by 36% of young adults. Young adults who reported frequent food preparation reported less frequent fast-food use and were more likely to meet dietary objectives for fat (P < 0.001), calcium (P < 0.001), fruit (P < 0.001), vegetable (P < 0.001), and whole-grain (P = 0.003) consumption. To improve dietary intake, interventions among young adults should teach skills for preparing quick and healthful meals.

MStern Blotting-High Throughput Polyvinylidene Fluoride (PVDF) Membrane-Based Proteomic Sample Preparation for 96-Well Plates.

PubMed

Berger, Sebastian T; Ahmed, Saima; Muntel, Jan; Cuevas Polo, Nerea; Bachur, Richard; Kentsis, Alex; Steen, Judith; Steen, Hanno

2015-10-01

We describe a 96-well plate compatible membrane-based proteomic sample processing method, which enables the complete processing of 96 samples (or multiples thereof) within a single workday. This method uses a large-pore hydrophobic PVDF membrane that efficiently adsorbs proteins, resulting in fast liquid transfer through the membrane and significantly reduced sample processing times. Low liquid transfer speeds have prevented the useful 96-well plate implementation of FASP as a widely used membrane-based proteomic sample processing method. We validated our approach on whole-cell lysate and urine and cerebrospinal fluid as clinically relevant body fluids. Without compromising peptide and protein identification, our method uses a vacuum manifold and circumvents the need for digest desalting, making our processing method compatible with standard liquid handling robots. In summary, our new method maintains the strengths of FASP and simultaneously overcomes one of the major limitations of FASP without compromising protein identification and quantification. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

Estimated content percentages of volatile liquids and fat extractables in ready-to-eat foods.

PubMed

Daft, J L; Cline, J K; Palmer, R E; Sisk, R L; Griffitt, K R

1996-01-01

Content percentages of volatile liquids and fat extractables in 340 samples of ready-to-eat foods were determined gravimetrically. Volatile liquids were determined by drying samples in a microwave oven with a self-contained balance; results were printed out automatically. Fat extractables were extracted from the samples with mixed ethers; extracts were dried and weighed manually. The samples, 191 nonfat and 149 fatty (containing ca 2% or more fat) foods, represent about 5000 different food items and include infant and toddler, ethnic, fast, and imported items. Samples were initially prepared for screening of essential and toxic elements and chemical contamination by chopping and mixing into homogenous composites. Content determinations were then made on separate portions from each composite. Content results were put into a database for evaluation. Overall, mean results from both determinations agree with published data for moisture and fat contents of similar food items. Coefficients of variation, however, were lower for determination of volatile liquids than for that of fat extractables.

Neutron-Irradiated Samples as Test Materials for MPEX

DOE PAGES

Ellis, Ronald James; Rapp, Juergen

2015-10-09

Plasma Material Interaction (PMI) is a major concern in fusion reactor design and analysis. The Material-Plasma Exposure eXperiment (MPEX) will explore PMI under fusion reactor plasma conditions. Samples with accumulated displacements per atom (DPA) damage produced by fast neutron irradiations in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) will be studied in the MPEX facility. This paper presents assessments of the calculated induced radioactivity and resulting radiation dose rates of a variety of potential fusion reactor plasma-facing materials (such as tungsten). The scientific code packages MCNP and SCALE were used to simulate irradiation of themore » samples in HFIR including the generation and depletion of nuclides in the material and the subsequent composition, activity levels, gamma radiation fields, and resultant dose rates as a function of cooling time. A challenge of the MPEX project is to minimize the radioactive inventory in the preparation of the samples and the sample dose rates for inclusion in the MPEX facility.« less

MStern Blotting–High Throughput Polyvinylidene Fluoride (PVDF) Membrane-Based Proteomic Sample Preparation for 96-Well Plates*

PubMed Central

Berger, Sebastian T.; Ahmed, Saima; Muntel, Jan; Cuevas Polo, Nerea; Bachur, Richard; Kentsis, Alex; Steen, Judith; Steen, Hanno

2015-01-01

We describe a 96-well plate compatible membrane-based proteomic sample processing method, which enables the complete processing of 96 samples (or multiples thereof) within a single workday. This method uses a large-pore hydrophobic PVDF membrane that efficiently adsorbs proteins, resulting in fast liquid transfer through the membrane and significantly reduced sample processing times. Low liquid transfer speeds have prevented the useful 96-well plate implementation of FASP as a widely used membrane-based proteomic sample processing method. We validated our approach on whole-cell lysate and urine and cerebrospinal fluid as clinically relevant body fluids. Without compromising peptide and protein identification, our method uses a vacuum manifold and circumvents the need for digest desalting, making our processing method compatible with standard liquid handling robots. In summary, our new method maintains the strengths of FASP and simultaneously overcomes one of the major limitations of FASP without compromising protein identification and quantification. PMID:26223766

AC impedance spectroscopy of NASICON type Na3Fe2(PO4)3 ceramic

NASA Astrophysics Data System (ADS)

Mandal, Biswajit; Thakur, A. K.

2018-05-01

Super ionic conductors (e.g.; A3M2(XO4)3, A=Li, Na) have received attention in applied research due to their interesting electrochemical property and inherently high ionic conductivity [1]. However, structural and compatibility requirements for fast ion transport is stringent and it plays a crucial role. In A3M2(XO4)3, a suitable cage formation in the crystal framework due to corner sharing arrangement of XO4 tetrahedra and MO6 octahedra creates voids that acts as host/guest site for cation transport. In this work, we report Nasicon structure Na3Fe2(PO4)3 (NFP) prepared via sol-gel route mediated by citric acid. Structural analysis confirmed that NFP sample belongs to monoclinic crystal structure having Cc space group (S. G. No 9) with lattice parameters, a=15.106 Å, b=8.722 Å, c=8.775 Å and β=124.96°. Electrical properties of the prepared sample have been studied by AC impedance spectroscopy technique. The AC conductivity results indicated typical signature of ionically conducting system.

Structure and short time degradation studies of sodium zirconium phosphate ceramics loaded with simulated fast breeder (FBR) waste

NASA Astrophysics Data System (ADS)

Ananthanarayanan, A.; Ambashta, R. D.; Sudarsan, V.; Ajithkumar, T.; Sen, D.; Mazumder, S.; Wattal, P. K.

2017-04-01

Sodium zirconium phosphate (NZP) ceramics have been prepared using conventional sintering and hot isostatic pressing (HIP) routes. The structure of NZP ceramics, prepared using the HIP route, has been compared with conventionally sintered NZP using a combination of X-ray diffraction (XRD) and (31P and 23Na) nuclear magnetic resonance (NMR) spectroscopy techniques. It is observed that NZP with no waste loading is aggressive toward the steel HIP-can during hot isostatic compaction and significant fraction of cations from the steel enter the ceramic material. Waste loaded NZP samples (10 wt% simulated FBR waste) show significantly low can-interaction and primary NZP phase is evident in this material. Upon exposure of can-interacted and waste loaded NZP to boiling water and steam, 31P NMR does not detect any major modifications in the network structure. However, the 23Na NMR spectra indicate migration of Na+ ions from the surface and possible re-crystallization. This is corroborated by Small-Angle Neutron Scattering (SANS) data and Scanning Electron Microscopy (SEM) measurements carried out on these samples.

Argonne National Laboratory Expedited Site Characterization: First International Symposium on Integrated Technical Approaches to Site Characterization - Proceedings Volume

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

NONE

1998-06-08

Laboratory applications for the analysis of PCBS (polychlorinated biphenyls) in environmental matrices such as soil/sediment/sludge and oil/waste oil were evaluated for potential reduction in waste, source reduction, and alternative techniques for final determination. As a consequence, new procedures were studied for solvent substitution, miniaturization of extraction and cleanups, minimization of reagent consumption, reduction of cost per analysis, and reduction of time. These new procedures provide adequate data that meet all the performance requirements for the determination of PCBS. Use of the new procedures reduced costs for all sample preparation techniques. Time and cost were also reduced by combining the newmore » sample preparation procedures with the power of fast gas chromatography. Separation of Aroclor 1254 was achieved in less than 6 min by using DB-1 and SPB-608 columns. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost. With performance-based methodology, the applications presented here can be applied now, without waiting for regulatory approval.« less

Preparation and characterisation of core-shell CNTs@MIPs nanocomposites and selective removal of estrone from water samples.

PubMed

Gao, Ruixia; Su, Xiaoqian; He, Xiwen; Chen, Langxing; Zhang, Yukui

2011-01-15

This paper reports the preparation of carbon nanotubes (CNTs) functionalized with molecularly imprinted polymers (MIPs) for advanced removal of estrone. CNTs@Est-MIPs nanocomposites with a well-defined core-shell structure were obtained using a semi-covalent imprinting strategy, which employed a thermally reversible covalent bond at the surface of silica-coated CNTs for a large-scale production. The morphology and structure of the products were characterised by transmission electron microscopy and Fourier transform infrared spectroscopy. The adsorption properties were demonstrated by equilibrium rebinding experiments and Scatchard analysis. The results demonstrate that the imprinted nanocomposites possess favourable selectivity, high capacity and fast kinetics for template molecule uptake, yielding an adsorption capacity of 113.5 μmol/g. The synthetic process is quite simple, and the different batches of synthesized CNTs@Est-MIPs nanocomposites showed good reproducibility in template binding. The feasibility of removing estrogenic compounds from environmental water using the CNTs@Est-MIPs nanocomposites was demonstrated using water samples spiked with estrone. Copyright © 2010 Elsevier B.V. All rights reserved.

Fast quantification of endogenous carbohydrates in plasma using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry.

PubMed

Zhu, Bangjie; Liu, Feng; Li, Xituo; Wang, Yan; Gu, Xue; Dai, Jieyu; Wang, Guiming; Cheng, Yu; Yan, Chao

2015-01-01

Endogenous carbohydrates in biosamples are frequently highlighted as the most differential metabolites in many metabolomics studies. A simple, fast, simultaneous quantitative method for 16 endogenous carbohydrates in plasma has been developed using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry. In order to quantify 16 endogenous carbohydrates in plasma, various conditions, including columns, chromatographic conditions, mass spectrometry conditions, and plasma preparation methods, were investigated. Different conditions in this quantified analysis were performed and optimized. The reproducibility, precision, recovery, matrix effect, and stability of the method were verified. The results indicated that a methanol/acetonitrile (50:50, v/v) mixture could effectively and reproducibly precipitate rat plasma proteins. Cold organic solvents coupled with vortex for 1 min and incubated at -20°C for 20 min were the most optimal conditions for protein precipitation and extraction. The results, according to the linearity, recovery, precision, matrix effect, and stability, showed that the method was satisfactory in the quantification of endogenous carbohydrates in rat plasma. The quantified analysis of endogenous carbohydrates in rat plasma performed excellently in terms of sensitivity, high throughput, and simple sample preparation, which met the requirement of quantification in specific expanded metabolomic studies after the global metabolic profiling research. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Facile and controllable preparation of glucose biosensor based on Prussian blue nanoparticles hybrid composites.

PubMed

Li, Lei; Sheng, Qinglin; Zheng, Jianbin; Zhang, Hongfang

2008-11-01

A glucose biosensor based on polyvinylpyrrolidone (PVP) protected Prussian blue nanoparticles (PBNPs)-polyaniline/multi-walled carbon nanotubes hybrid composites was fabricated by electrochemical method. A novel route for PBNPs preparation was applied in the fabrication with the help of PVP, and from scanning electron microscope images, Prussian blue particles on the electrode were found nanoscaled. The biosensor exhibits fast current response (<6 s) and a linearity in the range from 6.7x10(-6) to 1.9x10(-3) M with a high sensitivity of 6.28 microA mM(-1) and a detection limit of 6x10(-7) M (S/N=3) for the detection of glucose. The apparent activation energy of enzyme-catalyzed reaction and the apparent Michaelis-Menten constant are 23.9 kJ mol(-1) and 1.9 mM respectively, which suggests a high affinity of the enzyme-substrate. This easy and controllable construction method of glucose biosensor combines the characteristics of the components of the hybrid composites, which favors the fast and sensitive detection of glucose with improved analytical capabilities. In addition, the biosensor was examined in human serum samples for glucose determination with a recovery between 95.0 and 104.5%.

Insight into the time-resolved extraction of aroma compounds during espresso coffee preparation: online monitoring by PTR-ToF-MS.

PubMed

Sánchez-López, José A; Zimmermann, Ralf; Yeretzian, Chahan

2014-12-02

Using proton-transfer-reaction time-of-flight mass-spectrometry (PTR-ToF-MS), we investigated the extraction dynamic of 95 ion traces in real time (time resolution = 1 s) during espresso coffee preparation. Fifty-two of these ions were tentatively identified. This was achieved by online sampling of the volatile organic compounds (VOCs) in close vicinity to the coffee flow, at the exit of the extraction hose of the espresso machine (single serve capsules). Ten replicates of six different single serve coffee types were extracted to a final weight between 20-120 g, according to the recommended cup size of the respective coffee capsule (Ristretto, Espresso, and Lungo), and analyzed. The results revealed considerable differences in the extraction kinetics between compounds, which led to a fast evolution of the volatile profiles in the extract flow and consequently to an evolution of the final aroma balance in the cup. Besides exploring the time-resolved extraction dynamics of VOCs, the dynamic data also allowed the coffees types (capsules) to be distinguished from one another. Both hierarchical cluster analysis (HCA) and principal component analysis (PCA) showed full separation between the coffees types. The methodology developed provides a fast and simple means of studying the extraction dynamics of VOCs and differentiating between different coffee types.

Preparation and characterization of fast dissolving pullulan films containing BCS class II drug nanoparticles for bioavailability enhancement.

PubMed

Krull, Scott M; Ma, Zhelun; Li, Meng; Davé, Rajesh N; Bilgili, Ecevit

2016-01-01

The aim of this study is to assess pullulan as a novel steric stabilizer during the wet-stirred media milling (WSMM) of griseofulvin, a model poorly water-soluble drug, and as a film-former in the preparation of strip films via casting-drying the wet-milled drug suspensions for dissolution and bioavailability enhancement. To this end, pullulan films, with xanthan gum (XG) as thickening agent and glycerin as plasticizer, were loaded with griseofulvin nanoparticles prepared by WSMM using pullulan in combination with sodium dodecyl sulfate (SDS) as an ionic stabilizer. The effects of drug loading and milling time on the particle size and suspension stability were investigated, as well as XG concentration and casting thickness on film properties and dissolution rate. The nanosuspensions prepared with pullulan-SDS combination were relatively stable over 7 days; hence, this combination was used for the film preparation. All pullulan-based strip films exhibited excellent content uniformity (most <3% RSD) despite containing only 0.3-1.3 mg drug, which was ensured by the use of precursor suspensions with >5000 cP viscosity. USP IV dissolution tests revealed fast/immediate drug release (t80 < 30 min) from films <120 μm thick. Thinner films, films with lower XG loading, or smaller drug particles led to faster drug dissolution, while drug loading had no discernible effect. Overall, these results suggest that pullulan may serve as an acceptable stabilizer for media milling in combination with surfactant as well as a fast-dissolving film former for the fast release of poorly water-soluble drug nanoparticles.

Software and Hardware System for Fast Processes Study When Preparing Foundation Beds of Oil and Gas Facilities

NASA Astrophysics Data System (ADS)

Gruzin, A. V.; Gruzin, V. V.; Shalay, V. V.

2018-04-01

Analysis of existing technologies for preparing foundation beds of oil and gas buildings and structures has revealed the lack of reasoned recommendations on the selection of rational technical and technological parameters of compaction. To study the nature of the dynamics of fast processes during compaction of foundation beds of oil and gas facilities, a specialized software and hardware system was developed. The method of calculating the basic technical parameters of the equipment for recording fast processes is presented, as well as the algorithm for processing the experimental data. The performed preliminary studies confirmed the accuracy of the decisions made and the calculations performed.

Tandem High-pressure Freezing and Quick Freeze Substitution of Plant Tissues for Transmission Electron Microscopy

PubMed Central

Bobik, Krzysztof; Dunlap, John R.; Burch-Smith, Tessa M.

2014-01-01

Since the 1940s transmission electron microscopy (TEM) has been providing biologists with ultra-high resolution images of biological materials. Yet, because of laborious and time-consuming protocols that also demand experience in preparation of artifact-free samples, TEM is not considered a user-friendly technique. Traditional sample preparation for TEM used chemical fixatives to preserve cellular structures. High-pressure freezing is the cryofixation of biological samples under high pressures to produce very fast cooling rates, thereby restricting ice formation, which is detrimental to the integrity of cellular ultrastructure. High-pressure freezing and freeze substitution are currently the methods of choice for producing the highest quality morphology in resin sections for TEM. These methods minimize the artifacts normally associated with conventional processing for TEM of thin sections. After cryofixation the frozen water in the sample is replaced with liquid organic solvent at low temperatures, a process called freeze substitution. Freeze substitution is typically carried out over several days in dedicated, costly equipment. A recent innovation allows the process to be completed in three hours, instead of the usual two days. This is typically followed by several more days of sample preparation that includes infiltration and embedding in epoxy resins before sectioning. Here we present a protocol combining high-pressure freezing and quick freeze substitution that enables plant sample fixation to be accomplished within hours. The protocol can readily be adapted for working with other tissues or organisms. Plant tissues are of special concern because of the presence of aerated spaces and water-filled vacuoles that impede ice-free freezing of water. In addition, the process of chemical fixation is especially long in plants due to cell walls impeding the penetration of the chemicals to deep within the tissues. Plant tissues are therefore particularly challenging, but this protocol is reliable and produces samples of the highest quality. PMID:25350384

Optimization and validation of a rapid method to determine citrate and inorganic phosphate in milk by capillary electrophoresis.

PubMed

Izco, J M; Tormo, M; Harris, A; Tong, P S; Jimenez-Flores, R

2003-01-01

Quantification of phosphate and citrate compounds is very important because their distribution between soluble and colloidal phases of milk and their interactions with milk proteins influence the stability and some functional properties of dairy products. The aim of this work was to optimize and validate a capillary electrophoresis method for the rapid determination of these compounds in milk. Various parameters affecting analysis have been optimized, including type, composition, and pH of the electrolyte, and sample extraction. Ethanol, acetonitrile, sulfuric acid, water at 50 degrees C or at room temperature were tested as sample buffers (SB). Water at room temperature yielded the best overall results and was chosen for further validation. The extraction time was checked and could be shortened to less than 1 min. Also, sample preparation was simplified to pipet 12 microl of milk into 1 ml of water containing 20 ppm of tartaric acid as an internal standard. The linearity of the method was excellent (R2 > 0.999) with CV values of response factors <3%. The detection limits for phosphate and citrate were 5.1 and 2.4 nM, respectively. The accuracy of the method was calculated for each compound (103.2 and 100.3%). In addition, citrate and phosphate content of several commercial milk samples were analyzed by this method, and the results deviated less than 5% from values obtained when analyzing the samples by official methods. To study the versatility of the technique, other dairy productssuch as cream cheese, yogurt, or Cheddar cheese were analyzed and accuracy was similar to milk in all products tested. The procedure is rapid and offers a very fast and simple sample preparation. Once the sample has arrived at the laboratory, less than 5 min (including handling, preparation, running, integration, and quantification) are necessary to determine the concentration of citric acid and inorganic phosphate. Because of the speed and accuracy of this method, it is promising as an analytical quantitative testing technique.

Gas Sensor for Volatile Anesthetic Agents Based on Raman Scattering

NASA Astrophysics Data System (ADS)

Schlüter, Sebastian; Popovska-Leipertz, Nadejda; Seeger, Thomas; Leipertz, Alfred

Continuous monitoring of respiratory and anesthetic gases during a surgery is of vital importance for the patient safety. Commonly the gas composition is determined by gas chromatography or a combination of IR-spectroscopy and electrochemical sensors. This study presents a concept for an optical sensor based on spontaneous Raman scattering which offers several advantages compared to established systems. All essential components can be detected simultaneously, no sample preparation is necessary and it provides fast response times. To reach the performance of a commonly used gas monitor signal gain has to be increased e.g. by using a multi pass setup.

Fast quantification of short chain fatty acids and ketone bodies by liquid chromatography-tandem mass spectrometry after facile derivatization coupled with liquid-liquid extraction.

PubMed

Zeng, Mingfei; Cao, Huachuan

2018-04-15

Short chain fatty acids (SCFA) and ketone bodies recently emerged as important physiological relevant metabolites because of their association with microbiota, immunology, obesity and other metabolic states. They were commonly analyzed by GC-MS with long run time and laborious sample preparation. In this study we developed a novel LC-MS/MS method using fast derivatization coupled with liquid-liquid extraction to detect SCFA and ketone bodies in plasma and feces. Several different derivatization reagents were evaluated to compare the efficiency, the sensitivity and chromatographic separation of structural isomers. O‑benzylhydroxylamine was selected for its superior overall performance in reaction time and isomeric separation that allowed the measurement of each SCFAs and ketone bodies free from interferences. The derivatization procedure is facile and reproducible in aqueous-organic medium, which abolished the evaporation procedure hampering the analysis of volatile short chain acids. Enhancement in sensitivity remarkably improved the detection limit of SCFA and ketone bodies to sub-fmol level. This novel method was applied to quantify these metabolites in fecal and plasma samples from lean and DIO mouse. Copyright © 2018 Elsevier B.V. All rights reserved.

Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography-tandem mass spectrometry.

PubMed

Sapozhnikova, Yelena; Lehotay, Steven J

2013-01-03

A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS-MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n=5). The measured values for both SRMs agreed with certified/reference values (72-119% accuracy) for the majority of analytes. The detection limits were 0.1-0.5ng g(-1) for PCBs, 0.5-10ng g(-1) for PBDEs, 0.5-5ng g(-1) for select pesticides and PAHs and 1-10ng g(-1) for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market. Published by Elsevier B.V.

Preparation of magnetic core mesoporous shell microspheres with C18-modified interior pore-walls for fast extraction and analysis of phthalates in water samples.

PubMed

Li, Zhongbo; Huang, Danni; Fu, Chinfai; Wei, Biwen; Yu, Wenjia; Deng, Chunhui; Zhang, Xiangmin

2011-09-16

In this study, core-shell magnetic mesoporous microspheres with C18-functionalized interior pore-walls were synthesized through coating Fe(3)O(4) microspheres with a mesoporous inorganic-organic hybrid layer with a n-octadecyltriethoxysilane (C18TES) and tetraethyl orthosilicate (TEOS) as the silica source and cetyltrimethylammonia bromide (CTAB) as a template. The obtained C18-functionalized Fe(3)O(4)@mSiO(2) microspheres possess numerous C18 groups anchored in the interior pore-walls, large surface area (274.7 m(2)/g, high magnetization (40.8 emu/g) and superparamagnetism, uniform mesopores (4.1 nm), which makes them ideal absorbents for simple, fast, and efficient extraction and enrichment of hydrophobic organic compounds in water samples. Several kinds of phthalates were used as the model hydrophobic organic compounds to systematically evaluate the performance of the C18-functionalized Fe(3)O(4)@mSiO(2) microspheres in extracting hydrophobic molecules by using a gas chromatography-mass spectrometry. Various parameters, including eluting solvent, the amounts of absorbents, extraction time and elution time were optimized. Hydrophobic extraction was performed in the interior pore of magnetic mesoporous microspheres, and the materials had the anti-interference ability to macromolecular proteins, which was also investigated in the work. Under the optimized conditions, C18-functionalized Fe(3)O(4)@mSiO(2) microspheres were successfully used to analyze the real water samples. The results indicated that this novel method was fast, convenient and efficient for the target compounds and could avoid being interfered by macromolecules. Copyright © 2011 Elsevier B.V. All rights reserved.

Cooling rate dependence of structural order in Al 90Sm 10 metallic glass

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

Sun, Yang; Zhang, Yue; Zhang, Feng

2016-07-07

Here, the atomic structure of Al 90Sm 10 metallic glass is studied using molecular dynamics simulations. By performing a long sub-T g annealing, we developed a glass model closer to the experiments than the models prepared by continuous cooling. Using the cluster alignment method, we found that “3661” cluster is the dominating short-range order in the glass samples. The connection and arrangement of “3661” clusters, which define the medium-range order in the system, are enhanced significantly in the sub-T g annealed sample as compared with the fast cooled glass samples. Unlike some strong binary glass formers such as Cu 64.5Zrmore » 35.5, the clusters representing the short-range order do not form an interconnected interpenetrating network in Al 90Sm 10, which has only marginal glass formability.« less

Cooling rate dependence of structural order in Al{sub 90}Sm{sub 10} metallic glass

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

Sun, Yang; Ames Laboratory, US Department of Energy, Ames, Iowa 50011; Zhang, Yue

2016-07-07

The atomic structure of Al{sub 90}Sm{sub 10} metallic glass is studied using molecular dynamics simulations. By performing a long sub-T{sub g} annealing, we developed a glass model closer to the experiments than the models prepared by continuous cooling. Using the cluster alignment method, we found that “3661” cluster is the dominating short-range order in the glass samples. The connection and arrangement of “3661” clusters, which define the medium-range order in the system, are enhanced significantly in the sub-T{sub g} annealed sample as compared with the fast cooled glass samples. Unlike some strong binary glass formers such as Cu{sub 64.5}Zr{sub 35.5},more » the clusters representing the short-range order do not form an interconnected interpenetrating network in Al{sub 90}Sm{sub 10,} which has only marginal glass formability.« less

Fast Extraction and Detection of 4-Methylimidazole in Soy Sauce Using Magnetic Molecularly Imprinted Polymer by HPLC.

PubMed

Feng, Zufei; Lu, Yan; Zhao, Yingjuan; Ye, Helin

2017-11-02

On the basis of magnetic molecularly imprinted polymer (MMIP) solid-phase extraction coupled with high performance liquid chromatography, we established a new method for the determination of the 4-methylimidazole (4-MEI) in soy sauce. Scanning electron microscopy (SEM), Fourier transform infrared (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) were used to characterize the synthesized MMIPs. To evaluate the polymers, batch rebinding experiments were carried out. The binding strength and capacity were determined from the derived Freundlich isotherm (FI) equation. The selective recognition capability of MMIPs was investigated with a reference compound and a structurally similar compound. As a selective pre-concentration sorbents for 4-methylimidazole in soy sauce, the MMIPs showed a satisfied recoveries rate of spiked samples, ranged from 97% to 105%. As a result, the prepared MMIPs could be applied to selectively pre-concentrate and determine 4-methylimidazole in soy sauce samples.

Desorption atmospheric pressure photoionization-mass spectrometry in routine analysis of confiscated drugs.

PubMed

Kauppila, Tiina J; Flink, Anu; Haapala, Markus; Laakkonen, Ulla-Maija; Aalberg, Laura; Ketola, Raimo A; Kostiainen, Risto

2011-07-15

A comprehensive study was made, where desorption atmospheric pressure photoionization (DAPPI) was applied to the direct analysis of confiscated drugs and pharmaceuticals of various forms and matrices. The analyzed samples included herbal products [Catha edulis (khat), Psilocybe mushrooms, opium and Spice], designer drugs in tablet and powder form [e.g. meta-chlorophenylpiperazine (mCPP), 3-fluoromethamphetamine (3-FMA), methylenedioxypyrovalerone (MDPV) and methylone], and anabolic steroids in oil and tablets. The analyses were performed with ion trap mass spectrometer in MS and MS(2) modes and the obtained spectra were compared with GC-MS results. Contamination of the mass spectrometer was avoided by careful adjustment of the distance of the sample from the mass spectrometer inlet. DAPPI proved to be a fast and specific analysis technique, which does not require any sample preparation, and which therefore suits well to this type of forensic analysis. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

CVD diamond detectors for ionizing radiation

NASA Astrophysics Data System (ADS)

Friedl, M.; Adam, W.; Bauer, C.; Berdermann, E.; Bergonzo, P.; Bogani, F.; Borchi, E.; Brambilla, A.; Bruzzi, M.; Colledani, C.; Conway, J.; Dabrowski, W.; Delpierre, P.; Deneuville, A.; Dulinski, W.; van Eijk, B.; Fallou, A.; Fizzotti, F.; Foulon, F.; Gan, K. K.; Gheeraert, E.; Grigoriev, E.; Hallewell, G.; Hall-Wilton, R.; Han, S.; Hartjes, F.; Hrubec, J.; Husson, D.; Kagan, H.; Kania, D.; Kaplon, J.; Karl, C.; Kass, R.; Knöpfle, K. T.; Krammer, M.; Logiudice, A.; Lu, R.; Manfredi, P. F.; Manfredotti, C.; Marshall, R. D.; Meier, D.; Mishina, M.; Oh, A.; Pan, L. S.; Palmieri, V. G.; Pernegger, H.; Pernicka, M.; Peitz, A.; Pirollo, S.; Polesello, P.; Pretzl, K.; Re, V.; Riester, J. L.; Roe, S.; Roff, D.; Rudge, A.; Schnetzer, S.; Sciortino, S.; Speziali, V.; Stelzer, H.; Stone, R.; Tapper, R. J.; Tesarek, R.; Thomson, G. B.; Trawick, M.; Trischuk, W.; Vittone, E.; Walsh, A. M.; Wedenig, R.; Weilhammer, P.; Ziock, H.; Zoeller, M.; RD42 Collaboration

1999-10-01

In future HEP accelerators, such as the LHC (CERN), detectors and electronics in the vertex region of the experiments will suffer from extreme radiation. Thus radiation hardness is required for both detectors and electronics to survive in this harsh environment. CVD diamond, which is investigated by the RD42 Collaboration at CERN, can meet these requirements. Samples of up to 2×4 cm2 have been grown and refined for better charge collection properties, which are measured with a β source or in a testbeam. A large number of diamond samples has been irradiated with hadrons to fluences of up to 5×10 15 cm-2 to study the effects of radiation. Both strip and pixel detectors were prepared in various geometries. Samples with strip metallization have been tested with both slow and fast readout electronics, and the first diamond pixel detector proved fully functional with LHC electronics.

A large-strain, fast-response, and easy-to-manufacture electrothermal actuator based on laser-reduced graphene oxide

NASA Astrophysics Data System (ADS)

Zhang, Tian-Yu; Wang, Qian; Deng, Ning-Qin; Zhao, Hai-Ming; Wang, Dan-Yang; Yang, Zhen; Liu, Ying; Yang, Yi; Ren, Tian-Ling

2017-09-01

In this paper, we have developed a high-performance graphene electrothermal actuator (ETA). The fabrication method is easy, fast, environmentally friendly, and suitable for preparing both large-size and miniature graphene ETAs. When applied with the driving voltage of 65 V, the graphene ETA achieves a large bending angle of 270° with a fast response of 8 s and the recovery process costs 19 s. The large bending deformation is reversible and can be precisely controlled by the driving voltage. A simple robotic hand prepared by using a single graphene ETA can hold the object, which is more than ten times the weight of itself. By virtue of its large-strain, fast response, and easy-to-manufacture, we believe that the graphene ETA has tremendous potential in extensive applications involving biomimetic robotics, artificial muscles, switches, and microsensors in both macroscopic and microscopic fields.

Preparation of magnetic ODS-PAN thin-films for microextraction of quetiapine and clozapine in plasma and urine samples followed by HPLC-UV detection.

PubMed

Li, Dan; Zou, Juan; Cai, Pei-Shan; Xiong, Chao-Mei; Ruan, Jin-Lan

2016-06-05

In this study, conventional thin-film microextraction (TFME) was endowed with magnetic by introducing superparamagnetic SiO2@Fe3O4 nanoparticles in thin-films. Novel magnetic octadecylsilane (ODS)-polyacrylonitrile (PAN) thin-films were prepared by spraying, and used for the microextraction of quetiapine and clozapine in plasma and urine samples, followed by the detection of HPLC-UV. The influencing factors on the extraction efficiency of magnetic ODS-PAN TFME, including pH, extraction time, desorption solvent, desorption time, and ion strength were investigated systematically. Under the optimal conditions, both analytes showed good linearity over ranges of 0.070-9.000μgmL(-1) and 0.012-9.000μgmL(-1) in plasma and urine samples, respectively, with correlation coefficients (R(2)) above 0.9990. Limits of detection (LODs) for quetiapine in plasma and urine samples were 0.013 and 0.003μgmL(-1), respectively. LODs for clozapine in plasma and urine samples were 0.015 and 0.003μgmL(-1), respectively. The relative standard deviations (RSDs) for quetiapine and clozapine were less than 9.23%. After the validation, the protocol was successfully applied for the determination of quetiapine and clozapine in patients' plasma and urine samples with satisfactory recoveries between 99-110%. The proposed magnetic ODS-PAN TFME was very simple, fast and easy to handle. It showed high potential as a powerful pretreatment technology for routine therapeutic drug monitoring (TDM) in plasma and urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and property of spinel porous ZnMn2O4 microspheres

NASA Astrophysics Data System (ADS)

Guo, N.; Wei, X. Q.; Deng, X. L.; Xu, X. J.

2015-11-01

Mesoporous ternary zinc manganese oxides on the Ti sheet substrate are prepared by easy and fast hydrothermal method for the first time. The obtained ZnMn2O4 materials with homogenously distributed pores have been characterized by XRD, SEM and Raman spectra, which show the good crystal phase and particles for improving supercapacitive performance. XRD and SEM images show that the as-prepared samples have good crystallinity, and ZnMn2O4 microsphere has an average diameter of 10 μm. In addition, ZnMn2O4 are also characterized in 2 M KOH solution using three-electrode system. In the work, we study that different substrates (Ti, carbon and nickel foam) have an important effect on the electrochemical performance of the samples. The research of cyclic voltammogram (CV) indicates that the obtained specific capacitance (155 F g-1) values on nickel foam substrate for the ZnMn2O4 microspheres are higher than the values reported for some inexpensive oxides. However, the specific capacitance of all ZnMn2O4 samples has almost no change at two different scan rates which shows good long-term cycling stability. The electrochemical impedance spectroscopy with a small resistance reveals that the as-synthesized samples have good frequency response characteristics. These results indicate that the unique ZnMn2O4 electrode would be a promising electrode for high-performance supercapacitor applications.

In vitro synthesis and characterisation of three fenoterol sulfoconjugates detected in fenoterol post-administration urine samples.

PubMed

Orlovius, A K; Guddat, S; Gütschow, M; Thevis, M; Schänzer, W

2013-11-01

Fenoterol, a fast-acting β2-adrenergic agonist, is used in the therapy of obstructive pulmonary diseases and for the inhibition of premature labour obstetrics. Doping control for β2-agonists, which are prohibited in sports by the World Anti-Doping Agency, is commonly performed by liquid chromatography/mass spectrometry after hydrolysis of phase II metabolites. The continuing development of analytical procedures has led to direct injection of urine samples without sample preparation becoming a viable tool. For the detection of substances without sample preparation, including hydrolysis, detailed information of the phase II metabolism of the substances is essential. In this study, human S9 fractions of different tissues and two recombinant sulfotransferases were investigated for their potential to form fenoterol sulfoconjugates, which were characterised in detail. Two mono-sulfoconjugates and one bis-sulfoconjugate were synthesised and their structures confirmed by liquid chromatography–high-resolution/high-accuracy mass spectrometry. All of the metabolites were identified as esterified phenolic compounds. Excretion studies with orally and inhalatively administered fenoterol proved the occurrence of the sulfoconjugates in vivo. Inhalatively administered fenoterol resulted in the detection of the two monosulfoconjugates in low amounts in urine due to the lower inhalation dose of fenoterol compared to the oral dose. After oral uptake of fenoterol, the two mono-sulfoconjugates and a fenoterol bis-sulfoconjugate were detected in urine. This is the first report of the bis-sulfoconjugate.

Label-free virus detection using silicon photonic microring resonators.

PubMed

McClellan, Melinda S; Domier, Leslie L; Bailey, Ryan C

2012-01-15

Viruses represent a continual threat to humans through a number of mechanisms, which include disease, bioterrorism, and destruction of both plant and animal food resources. Many contemporary techniques used for the detection of viruses and viral infections suffer from limitations such as the need for extensive sample preparation or the lengthy window between infection and measurable immune response, for serological methods. In order to develop a method that is fast, cost-effective, and features reduced sample preparation compared to many other virus detection methods, we report the application of silicon photonic microring resonators for the direct, label-free detection of intact viruses in both purified samples as well as in a complex, real-world analytical matrix. As a model system, we demonstrate the quantitative detection of Bean pod mottle virus, a pathogen of great agricultural importance, with a limit of detection of 10 ng/mL. By simply grinding a small amount of leaf sample in buffer with a mortar and pestle, infected leaves can be identified over a healthy control with a total analysis time of less than 45 min. Given the inherent scalability and multiplexing capability of the semiconductor-based technology, we feel that silicon photonic microring resonators are well-positioned as a promising analytical tool for a number of viral detection applications. Copyright © 2011 Elsevier B.V. All rights reserved.

Towards a semiquantitative non invasive characterisation of Tyrian purple dye composition: Convergence of UV-Visible reflectance spectroscopy and fast-high temperature-high performance liquid chromatography with photodiode array detection.

PubMed

Clementi, Catia; Nowik, Witold; Romani, Aldo; Cardon, Dominique; Trojanowicz, Marek; Davantès, Athénaïs; Chaminade, Pierre

2016-07-05

In this paper, partial least square (PLS) regression is innovatively applied for a semi-quantitative non invasive study of the most precious dye of Antiquity: Tyrian purple. This original approach for the study of organic dyes in the cultural heritage field, is based on the correlation of spectrophotometric (UV-Visible) and chromatographic (Fast-HT-HPLC-PDA) data from an extensive set of textiles prepared with different snail species according to historical recipes. A cross-validated PLS model, based on the quantity of 6,6'-dibromoindigotin, displays an excellent correlation factor (R(2)Y = 0.987) between values determined by chromatography and those predicted from reflectance spectra. This indicates that the spectral features of Tyrian purple on textile fibre is strictly related to the amount of this indigoid component whose content may be non invasively predicted from reflectance spectrum. The studied correlation also highlights that, independently of the dyeing method and nature of the textile fibre used, the relative content of 6,6'-dibromindigotin may be used as a parameter to distinguish samples prepared with Hexaplex trunculus L. snails from those prepared with further mollusc species. To validate this model, archaeological textile fragments dating from the Roman period were successfully examined. The results achieved open an absolutely new way in Tyrian purple analysis in cultural heritage by non invasive spectroscopic techniques attesting their convergence with HPLC and giving them a semi-quantitative value. Copyright © 2016 Elsevier B.V. All rights reserved.

Preliminary study of neutron absorption by concrete with boron carbide addition

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

Abdullah, Yusof, E-mail: yusofabd@nuclearmalaysia.gov.my; Yusof, Mohd Reusmaazran; Zali, Nurazila Mat

2014-02-12

Concrete has become a conventional material in construction of nuclear reactor due to its properties like safety and low cost. Boron carbide was added as additives in the concrete construction as it has a good neutron absorption property. The sample preparation for concrete was produced with different weight percent of boron carbide powder content. The neutron absorption rate of these samples was determined by using a fast neutron source of Americium-241/Be (Am-Be 241) and detection with a portable backscattering neutron detector. Concrete with 20 wt % of boron carbide shows the lowest count of neutron transmitted and this indicates themore » most neutrons have been absorbed by the concrete. Higher boron carbide content may affect the concrete strength and other properties.« less

Imprint-coating synthesis of selective functionalized ordered mesoporous sorbents for separation and sensors

DOEpatents

Dai, Sheng; Burleigh, Mark C.; Shin, Yongsoon

2001-01-01

The present invention relates generally to mesoporous sorbent materials having high capacity, high selectivity, fast kinetics, and molecular recognition capability. The invention also relates to a process for preparing these mesoporous substrates through molecular imprinting techniques which differ from convention techniques in that a template molecule is bound to one end of bifunctional ligands to form a complex prior to binding of the bifunctional ligands to the substrate. The present invention also relates to methods of using the mesoporous sorbent materials, for example, in the separation of toxic metals from process effluents, paints, and other samples; detection of target molecules, such as amino acids, drugs, herbicides, fertilizers, and TNT, in samples; separation and/or detection of substances using chromatography; imaging agents; sensors; coatings; and composites.

TEA controllable preparation of magnetite nanoparticles (Fe3O4 NPs) with excellent magnetic properties

NASA Astrophysics Data System (ADS)

Han, Chengliang; Zhu, Dejie; Wu, Hanzhao; Li, Yao; Cheng, Lu; Hu, Kunhong

2016-06-01

A fast and controllable synthesis method for superparamagnetic magnetite nanoparticles (Fe3O4 NPs) was developed in Fe(III)-triethanolamine (TEA) solution. The phase structure, morphology and particle size of the as-synthesized samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the magnetic particles were pure Fe3O4 with mean sizes of approximately 10 nm. The used TEA has key effects on the formation of well dispersing Fe3O4 NPs. Vibrating sample magnetometer (VSM) result indicated that the as-obtained Fe3O4 NPs exhibited superparamagnetic behavior and the saturation magnetization (Ms) was about 70 emu/g, which had potential applications in magnetic science and technology.

Identification of (antioxidative) plants in herbal pharmaceutical preparations and dietary supplements.

PubMed

Deconinck, Eric; Custers, Deborah; De Beer, Jacques Omer

2015-01-01

The standard procedures for the identification, authentication, and quality control of medicinal plants and herbs are nowadays limited to pure herbal products. No guidelines or procedures, describing the detection or identification of a targeted plant or herb in pharmaceutical preparations or dietary supplements, can be found. In these products the targeted plant is often present together with other components of herbal or synthetic origin. This chapter describes a strategy for the fast development of a chromatographic fingerprint approach that allows the identification of a targeted plant in herbal preparations and dietary supplements. The strategy consists of a standard chromatographic gradient that is tested for the targeted plant with different extraction solvents and different mobile phases. From the results obtained, the optimal fingerprint is selected. Subsequently the samples are analyzed according to the selected methodological parameters, and the obtained fingerprints can be compared with the one obtained for the pure herbal product or a standard preparation. Calculation of the dissimilarity between these fingerprints will result in a probability of presence of the targeted plant. Optionally mass spectrometry can be used to improve specificity, to confirm identification, or to identify molecules with a potential medicinal or antioxidant activity.

Control of Energy Flow Dynamics between Tetracene Ligands and PbS Quantum Dots by Size Tuning and Ligand Coverage

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

Kroupa, Daniel M.; Arias, Dylan H.; Blackburn, Jeffrey L.

We have prepared a series of samples with the ligand 6,13-bistri(iso-propyl)silylethynyl tetracene 2-carboxylic acid (TIPS-Tc-COOH) attached to PbS quantum dot (QD) samples of three different sizes in order to monitor and control the extent and time scales of energy flow after photoexcitation. Fast energy transfer (~1 ps) to the PbS QD occurs upon direct excitation of the ligand for all samples. The largest size QD maintains the microsecond exciton lifetime characteristic of the as-prepared oleate terminated PbS QDs. However, two smaller QD sizes with lowest exciton energies similar to or larger than the TIPS-Tc-COO- triplet energy undergo energy transfer betweenmore » QD core and ligand triplet on nanosecond to microsecond timescales. For the intermediate size QDs in particular, energy can be recycled many times between ligand and core, but the triplet remains the dominant excited species at long times, living for ~3 us for fully exchanged QDs and up to 30 us for partial ligand exchange, which is revealed as a method for controlling the triplet lifetime. A unique upconverted luminescence spectrum is observed that results from annihilation of triplets after exclusive excitation of the QD core.« less

Fast preparation of a long chimeric armored RNA as controls for external quality assessment for molecular detection of Zika virus.

PubMed

Lin, Guigao; Zhang, Kuo; Zhang, Dong; Han, Yanxi; Xie, Jiehong; Li, Jinming

2017-03-01

The emergence of Zika virus demands accurate laboratory diagnostics. Nucleic acid testing is currently the definitive method for diagnosis of Zika infection. In 2016, an external quality assurance (EQA) for assessing the quality of molecular testing of Zika virus was carried out in China. A single armored RNA encapsulating a 4942-nucleotides (nt) long specific RNA sequence of Zika virus was prepared and used as positive samples. A pre-tested EQA panel, consisting of 4 negative and 6 positive samples with different concentrations of armored RNA, was distributed to 38 laboratories that perform molecular detection of Zika virus. A total of 39 data sets (1 laboratory used two test kits in parallel), produced by using commercial (n=38) or laboratory developed (n=1) quantitative reverse-transcriptase PCR (qRT-PCR) kits, were received. Of these, 35 (89.7%) had correct results for all 10 samples, and 4 (10.3%) reported at least 1 error (11 in total). The testing errors were all false-negatives, highlighting the need of improvements in detecting sensitivity. The EQA reveals that the majority of participating laboratories are proficient in molecular testing of Zika virus. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of coumarin in seasonal bakery products using QuEChERS and GC-MS.

PubMed

Vetter, F; Müller, C; Stöckelhuber, M; Bracher, F

2017-06-01

Cinnamon is a traditional herbal drug, but more importantly, it is used as a flavor compound in the production of foodstuff. Due to the content of significant concentrations of coumarin in Cassia cinnamon, effective control of the coumarin content in seasonal bakery products like ginger bread and cinnamon biscuits is urgently needed. Here we present a novel, fast and fully validated protocol for the determination of coumarin in marketed bakery products using the QuEChERS sample preparation technique in combination with GC-MS analysis. Ten grams of homogenized sample was mixed with 20 mL acetonitrile/water (1:1) and 5 g magnesium sulfate/sodium chloride mixture (4:1). The organic phase was cleaned by dSPE with 25 mg magnesium sulfate/PSA (5:1). The LOD was 0.15 μg/mL and the LOQ 0.50 μg/mL. We detected a mean coumarin content of 19.5 μg/kg in 9 out of 14 seasonal food products (ranging from 1.45 to 39.4 mg/kg). No coumarin was detected in five cinnamon containing products. With this investigation we demonstrate that the QuEChERS sample preparation, previously applied mainly to the analysis of pesticides in vegetables, is also suitable for other complex matrices.

Control of Energy Flow Dynamics between Tetracene Ligands and PbS Quantum Dots by Size Tuning and Ligand Coverage

DOE PAGES

Kroupa, Daniel M.; Arias, Dylan H.; Blackburn, Jeffrey L.; ...

2018-01-24

We have prepared a series of samples with the ligand 6,13-bistri(iso-propyl)silylethynyl tetracene 2-carboxylic acid (TIPS-Tc-COOH) attached to PbS quantum dot (QD) samples of three different sizes in order to monitor and control the extent and time scales of energy flow after photoexcitation. Fast energy transfer (~1 ps) to the PbS QD occurs upon direct excitation of the ligand for all samples. The largest size QD maintains the microsecond exciton lifetime characteristic of the as-prepared oleate terminated PbS QDs. However, two smaller QD sizes with lowest exciton energies similar to or larger than the TIPS-Tc-COO- triplet energy undergo energy transfer betweenmore » QD core and ligand triplet on nanosecond to microsecond timescales. For the intermediate size QDs in particular, energy can be recycled many times between ligand and core, but the triplet remains the dominant excited species at long times, living for ~3 us for fully exchanged QDs and up to 30 us for partial ligand exchange, which is revealed as a method for controlling the triplet lifetime. A unique upconverted luminescence spectrum is observed that results from annihilation of triplets after exclusive excitation of the QD core.« less

Multiscale dispersion-state characterization of nanocomposites using optical coherence tomography

PubMed Central

Schneider, Simon; Eppler, Florian; Weber, Marco; Olowojoba, Ganiu; Weiss, Patrick; Hübner, Christof; Mikonsaari, Irma; Freude, Wolfgang; Koos, Christian

2016-01-01

Nanocomposite materials represent a success story of nanotechnology. However, development of nanomaterial fabrication still suffers from the lack of adequate analysis tools. In particular, achieving and maintaining well-dispersed particle distributions is a key challenge, both in material development and industrial production. Conventional methods like optical or electron microscopy need laborious, costly sample preparation and do not permit fast extraction of nanoscale structural information from statistically relevant sample volumes. Here we show that optical coherence tomography (OCT) represents a versatile tool for nanomaterial characterization, both in a laboratory and in a production environment. The technique does not require sample preparation and is applicable to a wide range of solid and liquid material systems. Large particle agglomerates can be directly found by OCT imaging, whereas dispersed nanoparticles are detected by model-based analysis of depth-dependent backscattering. Using a model system of polystyrene nanoparticles, we demonstrate nanoparticle sizing with high accuracy. We further prove the viability of the approach by characterizing highly relevant material systems based on nanoclays or carbon nanotubes. The technique is perfectly suited for in-line metrology in a production environment, which is demonstrated using a state-of-the-art compounding extruder. These experiments represent the first demonstration of multiscale nanomaterial characterization using OCT. PMID:27557544

Multiscale dispersion-state characterization of nanocomposites using optical coherence tomography.

PubMed

Schneider, Simon; Eppler, Florian; Weber, Marco; Olowojoba, Ganiu; Weiss, Patrick; Hübner, Christof; Mikonsaari, Irma; Freude, Wolfgang; Koos, Christian

2016-08-25

Nanocomposite materials represent a success story of nanotechnology. However, development of nanomaterial fabrication still suffers from the lack of adequate analysis tools. In particular, achieving and maintaining well-dispersed particle distributions is a key challenge, both in material development and industrial production. Conventional methods like optical or electron microscopy need laborious, costly sample preparation and do not permit fast extraction of nanoscale structural information from statistically relevant sample volumes. Here we show that optical coherence tomography (OCT) represents a versatile tool for nanomaterial characterization, both in a laboratory and in a production environment. The technique does not require sample preparation and is applicable to a wide range of solid and liquid material systems. Large particle agglomerates can be directly found by OCT imaging, whereas dispersed nanoparticles are detected by model-based analysis of depth-dependent backscattering. Using a model system of polystyrene nanoparticles, we demonstrate nanoparticle sizing with high accuracy. We further prove the viability of the approach by characterizing highly relevant material systems based on nanoclays or carbon nanotubes. The technique is perfectly suited for in-line metrology in a production environment, which is demonstrated using a state-of-the-art compounding extruder. These experiments represent the first demonstration of multiscale nanomaterial characterization using OCT.

Fast and accurate determination of K, Ca, and Mg in human serum by sector field ICP-MS.

PubMed

Yu, Lee L; Davis, W Clay; Nuevo Ordonez, Yoana; Long, Stephen E

2013-11-01

Electrolytes in serum are important biomarkers for skeletal and cellular health. The levels of electrolytes are monitored by measuring the Ca, Mg, K, and Na in blood serum. Many reference methods have been developed for the determination of Ca, Mg, and K in clinical measurements; however, isotope dilution thermal ionization mass spectrometry (ID-TIMS) has traditionally been the primary reference method serving as an anchor for traceability and accuracy to these secondary reference methods. The sample matrix must be separated before ID-TIMS measurements, which is a slow and tedious process that hindered the adoption of the technique in routine clinical measurements. We have developed a fast and accurate method for the determination of Ca, Mg, and K in serum by taking advantage of the higher mass resolution capability of the modern sector field inductively coupled plasma mass spectrometry (SF-ICP-MS). Each serum sample was spiked with a mixture containing enriched (44)Ca, (26)Mg, and (41)K, and the (42)Ca(+):(44)Ca(+), (24)Mg(+):(26)Mg(+), and (39)K(+):(41)K(+) ratios were measured. The Ca and Mg ratios were measured in medium resolution mode (m/Δm ≈ 4 500), and the K ratio in high resolution mode (m/Δm ≈ 10 000). Residual (40)Ar(1)H(+) interference was still observed but the deleterious effects of the interference were minimized by measuring the sample at K > 100 ng g(-1). The interferences of Sr(++) at the two Ca isotopes were less than 0.25 % of the analyte signal, and they were corrected with the (88)Sr(+) intensity by using the Sr(++):Sr(+) ratio. The sample preparation involved only simple dilutions, and the measurement using this sample preparation approach is known as dilution-and-shoot (DNS). The DNS approach was validated with samples prepared via the traditional acid digestion approach followed by ID-SF-ICP-MS measurement. DNS and digested samples of SRM 956c were measured with ID-SF-ICP-MS for quality assurance, and the results (mean ± expanded uncertainty in mg dL(-1) unit) for Ca (DNS = 10.14 ± 0.13, digested = 10.11 ± 0.10), Mg (DNS = 2.093 ± 0.008, digested = 2.098 ± 0.007), and K (DNS = 15.48 ± 0.11, digested = 15.50 ± 0.28) were in good agreement with the certified values (Ca = 10.17 ± 0.06, Mg = 2.084 ± 0.023, K = 15.55 ± 0.13). Major sources of uncertainty are sample measurement, spike calibration, and instrument factor including mass discrimination of the spectrometer and the detector deadtime.

Porous metal hydride composite and preparation and uses thereof

DOEpatents

Steyert, W.A.; Olsen, C.E.

1980-03-12

A composite formed from large pieces of aggregate formed from (1) metal hydride (or hydride-former) powder and (2) either metal powder or plastic powder or both is prepared. The composite has large macroscopic interconnected pores (much larger than the sizes of the powders which are used) and will have a very fast heat transfer rate and low windage loss. It will be useful, for example, in heat engines, hydrogen storage devices, and refrigerator components which depend for their utility upon both a fast rate of hydriding and dehydriding. Additionally, a method of preparing the composite and a method of increasing the rates of hydriding and dehydriding of metal hydrides are also given.

Porous metal hydride composite and preparation and uses thereof

DOEpatents

Steyert, William A.; Olsen, Clayton E.

1982-01-01

A composite formed from large pieces of aggregate formed from (1) metal hydride (or hydride-former) powder and (2) either metal powder or plastic powder or both is prepared. The composite has large macroscopic interconnected pores (much larger than the sizes of the powders which are used) and will have a very fast heat transfer rate and low windage loss. It will be useful, for example, in heat engines, hydrogen storage devices, and refrigerator components which depend for their utility upon both a fast rate of hydriding and dehydriding. Additionally, a method of preparing the composite and a method of increasing the rates of hydriding and dehydriding of metal hydrides are also given.

Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole and their determination by ICP-OES.

PubMed

Mashhadizadeh, Mohammad Hossein; Karami, Zahra

2011-06-15

A fast, sensitive, and simple method using magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole, as an adsorbent has been successfully developed for extraction, preconcentration, and determination of trace amounts of Ag, Cd, Cu, and Zn from environmental samples. The prepared nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). These magnetic nanoparticles can be easily dispersed in aqueous samples and retrieved by the application of external magnetic field via a piece of permanent magnet. The main factors affecting the extraction efficiency such as pH value, sample volume, eluent concentration and volume, ultrasonication time, and coexisting ions have been investigated and established. Under the optimal conditions, high concentration factors (194, 190, 170, and 182) were achieved for Ag, Cd, Cu, and Zn with relative standard deviations of 5.31%, 4.03%, 3.62%, and 4.20%, respectively. The limits of detection for Ag, Cd, Cu, and Zn were as low as 0.12, 0.12, 0.13 and 0.11 ng mL(-1). The prepared sorbent was applied for preconcentration of trace amounts of Ag, Cd, Cu, and Zn in the various water samples with satisfactory results. Copyright © 2011 Elsevier B.V. All rights reserved.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection

PubMed Central

Alexandrou, Lydon D.; Meehan, Barry J.; Morrison, Paul D.; Jones, Oliver A. H.

2017-01-01

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid–liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9–9.3 µg/L). PMID:28505068

The effect of processing on the surface physical stability of amorphous solid dispersions.

PubMed

Yang, Ziyi; Nollenberger, Kathrin; Albers, Jessica; Moffat, Jonathan; Craig, Duncan; Qi, Sheng

2014-11-01

The focus of this study was to investigate the effect of processing on the surface crystallization of amorphous molecular dispersions and gain insight into the mechanisms underpinning this effect. The model systems, amorphous molecular dispersions of felodipine-EUDRAGIT® E PO, were processed both using spin coating (an ultra-fast solvent evaporation based method) and hot melt extrusion (HME) (a melting based method). Amorphous solid dispersions with drug loadings of 10-90% (w/w) were obtained by both processing methods. Samples were stored under 75% RH/room temperatures for up to 10months. Surface crystallization was observed shortly after preparation for the HME samples with high drug loadings (50-90%). Surface crystallization was characterized by powder X-ray diffraction (PXRD), ATR-FTIR spectroscopy and imaging techniques (SEM, AFM and localized thermal analysis). Spin coated molecular dispersions showed significantly higher surface physical stability than hot melt extruded samples. For both systems, the progress of the surface crystal growth followed zero order kinetics on aging. Drug enrichment at the surfaces of HME samples on aging was observed, which may contribute to surface crystallization of amorphous molecular dispersions. In conclusion it was found the amorphous molecular dispersions prepared by spin coating had a significantly higher surface physical stability than the corresponding HME samples, which may be attributed to the increased process-related apparent drug-polymer solubility and reduced molecular mobility due to the quenching effect caused by the rapid solvent evaporation in spin coating. Copyright © 2014 Elsevier B.V. All rights reserved.

Simple preparation of Fenton catalyst@bacterial cellulose for waste water treatment

NASA Astrophysics Data System (ADS)

Wibowo, Arie; Febi Indrawan, Radian; Triadhi, Untung; Hasdi Aimon, Akfiny; Iskandar, Ferry; Ardy, Husaini

2018-02-01

Heterogeneous fenton catalyst is one of the attractive technologies for destruction of persistent and non-biodegradable pollutant in wastewater, because it can be used in wide range of pH and recyclable. Herein, commercial bacterial celluloses (BCs) were used as an alternative support of fenton catalyst to improve their catalytic activity. Scanning Electron Microscope (SEM) observations indicated that the presence of BCs and decreasing precursor concentration might promote formation of smaller particle sizes of catalyst from 3.5 μm of bare catalyst to 0.7 μm of catalyst@BC. UV-vis measurement showed that fast degradation of dyes with half-time degradation at around 25 min was observed in sample using catalyst@BCs with precursor concentration of 0.01 M. Successful preparation of heterogeneous fenton catalyst with smaller particle size and better catalytic activity is important for their application in wastewater treatment.

Development of magnetic octadecylsilane particles as solid-phase extraction adsorbent for the determination of fat-soluble vitamins in fruit juice-milk beverage by capillary liquid chromatography.

PubMed

Hu, Chaofan; Jia, Li; Liu, Qingqing; Zhang, Sheng

2010-07-01

A sensitive, fast and simple method based on magnetic octadecylsilane particles was developed for the extraction of three fat-soluble vitamins followed by capillary LC (CLC) analysis with UV detection. Magnetic octadecylsilane particles were prepared based on three-step reactions including co-precipitation, sol-gel polymerization and alkylation. The characterization of the prepared product was studied by scanning electron microscope and Fourier-transform infrared spectrometry. The particles were used as magnetic SPE adsorbent for the extraction of fat-soluble vitamins in fruit juice-milk beverage. The extraction condition and efficiency of the particles for fat-soluble vitamins were investigated. By coupling magnetic SPE with capillary LC with UV detection, low concentrations of fat-soluble vitamins in fruit juice-milk beverage can be detected without the interference from other substances in the sample matrix.

Does involvement in food preparation track from adolescence to young adulthood and is it associated with better dietary quality? Findings from a ten-year longitudinal study

PubMed Central

Larson, Nicole I.; Neumark-Sztainer, Dianne; Story, Mary

2012-01-01

Objectives To examine whether involvement in food preparation tracks over time, between adolescence (15–18 years), emerging adulthood (19–23 years), and the mid-to-late twenties (24–28 years), as well as examine 10-year longitudinal associations between home food preparation, dietary quality and meal patterning. Design Population-based, longitudinal cohort study. Setting Participants were originally sampled from Minnesota public secondary schools (USA). Subjects Participants enrolled in Project EAT (Eating Among Teens)-I, EAT-II, and EAT-III (n=1,321). Results Most participants in their mid-to-late twenties reported an enjoyment of cooking (73% of males, 80% of females); however, few prepared meals including vegetables most days of the week (24% males, 41% females). Participants in their mid-to-late twenties who enjoyed cooking were more likely to have engaged in food preparation as adolescents and emerging adults (p<0.01); those who frequently prepared meals including vegetables were more likely to have engaged in food preparation as emerging adults (p<0.001), but not adolescents. Emerging adult food preparation predicted better dietary quality five years later in the mid-to-late twenties, including higher intakes of fruit, vegetables, dark green/orange vegetables, and less sugar sweetened beverage and fast food consumption. Associations between adolescent food preparation and later dietary quality yielded few significant results. Conclusions Food preparation behaviors appeared to track over time, and engagement in food preparation during emerging adulthood, but not adolescence, was associated with healthier dietary intake during the mid-to-late twenties. Intervention studies are needed to understand whether promoting healthy food preparation results in improvements in eating patterns during the transition to adulthood. PMID:22124458

Does involvement in food preparation track from adolescence to young adulthood and is it associated with better dietary quality? Findings from a 10-year longitudinal study.

PubMed

Laska, Melissa N; Larson, Nicole I; Neumark-Sztainer, Dianne; Story, Mary

2012-07-01

To examine whether involvement in food preparation tracks over time, between adolescence (15-18 years), emerging adulthood (19-23 years) and the mid-to-late twenties (24-28 years), as well as 10-year longitudinal associations between home food preparation, dietary quality and meal patterning. Population-based, longitudinal cohort study. Participants were originally sampled from Minnesota public secondary schools (USA). Participants enrolled in Project EAT (Eating Among Teens and Young Adults)-I, EAT-II and EAT-III (n 1321). Most participants in their mid-to-late twenties reported an enjoyment of cooking (73 % of males, 80 % of females); however, few prepared meals including vegetables most days of the week (24 % of males, 41 % of females). Participants in their mid-to-late twenties who enjoyed cooking were more likely to have engaged in food preparation as adolescents and emerging adults (P < 0·01); those who frequently prepared meals including vegetables were more likely to have engaged in food preparation as emerging adults (P < 0·001), but not as adolescents. Emerging adult food preparation predicted better dietary quality five years later in the mid-to-late twenties, including higher intakes of fruit, vegetables and dark green/orange vegetables, and less sugar-sweetened beverage and fast-food consumption. Associations between adolescent food preparation and later dietary quality yielded few significant results. Food preparation behaviours appeared to track over time and engagement in food preparation during emerging adulthood, but not adolescence, was associated with healthier dietary intake during the mid-to-late twenties. Intervention studies are needed to understand whether promoting healthy food preparation results in improvements in eating patterns during the transition to adulthood.

Effect of liquid immersion of PEDOT: PSS-coated polyester fabric on surface resistance and wettability

NASA Astrophysics Data System (ADS)

Getnet Tadesse, Melkie; Loghin, Carmen; Chen, Yan; Wang, Lichuan; Catalin, Dumitras; Nierstrasz, Vincent

2017-06-01

Coating of textile fabrics with poly (3, 4-ethylenedioxythiophene): poly (styrene sulfonate) (PEDOT:PSS) is one of the methods used for obtaining functional or smart applications. In this work, we prepared PEDOT:PSS polymer with certain additives such as polyethylene glycol, methanol (MeOH), and ethylene glycol on polyester fabric substrates by a simple immersion process. Surface resistance was measured and analyzed with analysis of variance to determine the coating parameters at 95% confidence level. Fourier transform infrared (FTIR) analysis and scanning electron microscopy (SEM) study of the samples were performed. Contact angle and washing fastness measurements were conducted, to observe the wettability and washing fastness of the samples, respectively. Surface resistance values were decreased by a factor of 100, due to conductive enhancers. As the immersion time and temperature condition varies, surface resistance showed no difference, statistically. FTIR analysis supports the idea that the mechanism responsible for the conductivity enhancement is the partial replacement of PSS from PEDOT chain by forming a hydrogen bond with hydroxyl ion (OH) of the conductive enhancers. A SEM images showed that PEDOT:PSS is well distributed to the surface of the fabrics. Contact angle measurements showed morphology change in the samples. The conductivity was reasonably stable after 10 washing cycles. Altogether, an effective simple immersion of coated polyester fabric is presented to achieve functional textiles that offer a broad range of possible applications.

Facile preparation of magnetic molecularly imprinted polymers for the selective extraction and determination of dexamethasone in skincare cosmetics using HPLC.

PubMed

Du, Wei; Zhang, Bilin; Guo, Pengqi; Chen, Guoning; Chang, Chun; Fu, Qiang

2018-03-15

Dexamethasone-imprinted polymers were fabricated by reversible addition-fragmentation chain transfer polymerization on the surface of magnetic nanoparticles under mild polymerization conditions, which exhibited a narrow polydispersity and high selectivity for dexamethasone extraction. The dexamethasone-imprinted polymers were characterized by scanning electron microscopy, transmission electron microscope, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive spectrometry, and vibrating sample magnetometry. The adsorption performance was evaluated by static adsorption, kinetic adsorption and selectivity tests. The results confirmed the successful construction of an imprinted polymer layer on the surface of the magnetic nanoparticles, which benefits the characteristics of high adsorption capacity, fast mass transfer, specific molecular recognition, and simple magnetic separation. Combined with high-performance liquid chromatography, molecularly imprinted polymers as magnetic extraction sorbents were used for the rapid and selective extraction and determination of dexamethasone in skincare cosmetic samples, with the accuracies of the spiked samples ranging from 93.8 to 97.6%. The relative standard deviations were less than 2.7%. The limit of detection and limit of quantification were 0.05 and 0.20 μg/mL, respectively. The developed method was simple, fast and highly selective and could be a promising method for dexamethasone monitoring in cosmetic products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fast Gas Chromatography with Tandem Mass Spectrometry Analysis of Selected Persistent Organic Pollutants and Organophosphorus and Synthetic Pyrethroid Pesticides in Indian Prawn (Fenneropenaeus indicus) in Compliance with the EU-MRLs.

PubMed

Sawant, Durvesh; Kelkar, Jitendra; Rasam, Pratap; Datar, Ajit; Hase, Prashant; Handique, Dheeraj; Bhone, Ankush; Chiplunkar, Sanket; Hate, Manish

2017-05-01

A fast GC with tandem MS method was developed and validated for multiresidue determination of 95 chemical contaminants (24 synthetic pyrethroids, 17 organochlorines, 17 organophosphorus compounds, 18 polycyclic aromatic hydrocarbons, and 19 polychlorinated biphenyls) in Indian prawns (Fenneropenaeus indicus) as per the European Union maximum residual limit requirements. Chromatographic separation and MS determination were achieved within a short run time of 18 min, without compromising sensitivity and specificity. Our findings revealed a 2.5× reduction in the run time compared with conventional GC methods. Sample preparation involved a QuEChERS-based extraction of 10 g sample with 10 mL acidified acetonitrile (1% acetic acid) and phase separation with 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. The extract was cleaned in two steps, first by dispersive cleanup with primary secondary amine and then by C18 SPE cartridge. The regression coefficients of linearity (r2) for the concentration range of 5-50 ng/mL were >0.99 for all the compounds. Recoveries at 5 and 10 ng/g levels were within the acceptable range of 70-120%. The repeatability (RSDr) and within-laboratory reproducibility (RSDwR) precisions were ≤20%. The method was successfully applied for analysis of the real world samples for incurred residues.

Determination of methylmercury in marine biota samples with advanced mercury analyzer: method validation.

PubMed

Azemard, Sabine; Vassileva, Emilia

2015-06-01

In this paper, we present a simple, fast and cost-effective method for determination of methyl mercury (MeHg) in marine samples. All important parameters influencing the sample preparation process were investigated and optimized. Full validation of the method was performed in accordance to the ISO-17025 (ISO/IEC, 2005) and Eurachem guidelines. Blanks, selectivity, working range (0.09-3.0ng), recovery (92-108%), intermediate precision (1.7-4.5%), traceability, limit of detection (0.009ng), limit of quantification (0.045ng) and expanded uncertainty (15%, k=2) were assessed. Estimation of the uncertainty contribution of each parameter and the demonstration of traceability of measurement results was provided as well. Furthermore, the selectivity of the method was studied by analyzing the same sample extracts by advanced mercury analyzer (AMA) and gas chromatography-atomic fluorescence spectrometry (GC-AFS). Additional validation of the proposed procedure was effectuated by participation in the IAEA-461 worldwide inter-laboratory comparison exercises. Copyright © 2014 Elsevier Ltd. All rights reserved.

Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

2013-06-01

Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bioprocess automation on a Mini Pilot Plant enables fast quantitative microbial phenotyping.

PubMed

Unthan, Simon; Radek, Andreas; Wiechert, Wolfgang; Oldiges, Marco; Noack, Stephan

2015-03-11

The throughput of cultivation experiments in bioprocess development has drastically increased in recent years due to the availability of sophisticated microliter scale cultivation devices. However, as these devices still require time-consuming manual work, the bottleneck was merely shifted to media preparation, inoculation and finally the analyses of cultivation samples. A first step towards solving these issues was undertaken in our former study by embedding a BioLector in a robotic workstation. This workstation already allowed for the optimization of heterologous protein production processes, but remained limited when aiming for the characterization of small molecule producer strains. In this work, we extended our workstation to a versatile Mini Pilot Plant (MPP) by integrating further robotic workflows and microtiter plate assays that now enable a fast and accurate phenotyping of a broad range of microbial production hosts. A fully automated harvest procedure was established, which repeatedly samples up to 48 wells from BioLector cultivations in response to individually defined trigger conditions. The samples are automatically clarified by centrifugation and finally frozen for subsequent analyses. Sensitive metabolite assays in 384-well plate scale were integrated on the MPP for the direct determination of substrate uptake (specifically D-glucose and D-xylose) and product formation (specifically amino acids). In a first application, we characterized a set of Corynebacterium glutamicum L-lysine producer strains and could rapidly identify a unique strain showing increased L-lysine titers, which was subsequently confirmed in lab-scale bioreactor experiments. In a second study, we analyzed the substrate uptake kinetics of a previously constructed D-xylose-converting C. glutamicum strain during cultivation on mixed carbon sources in a fully automated experiment. The presented MPP is designed to face the challenges typically encountered during early-stage bioprocess development. Especially the bottleneck of sample analyses from fast and parallelized microtiter plate cultivations can be solved using cutting-edge robotic automation. As robotic workstations become increasingly attractive for biotechnological research, we expect our setup to become a template for future bioprocess development.

Time spent on home food preparation and indicators of healthy eating.

PubMed

Monsivais, Pablo; Aggarwal, Anju; Drewnowski, Adam

2014-12-01

The amount of time spent on food preparation and cooking may have implications for diet quality and health. However, little is known about how food-related time use relates to food consumption and spending, either at restaurants or for food consumed at home. To quantitatively assess the associations among the amount of time habitually spent on food preparation and patterns of self-reported food consumption, food spending, and frequency of restaurant use. This was a cross-sectional study of 1,319 adults in a population-based survey conducted in 2008-2009. The sample was stratified into those who spent <1 hour/day, 1-2 hours/day, and >2 hours/day on food preparation and cleanup. Descriptive statistics and multivariable regression models examined differences between time-use groups. Analyses were conducted in 2011-2013. Individuals who spent the least amount of time on food preparation tended to be working adults who placed a high priority on convenience. Greater amount of time spent on home food preparation was associated with indicators of higher diet quality, including significantly more frequent intake of vegetables, salads, fruits, and fruit juices. Spending <1 hour/day on food preparation was associated with significantly more money spent on food away from home and more frequent use of fast food restaurants compared to those who spent more time on food preparation. The findings indicate that time might be an essential ingredient in the production of healthier eating habits among adults. Further research should investigate the determinants of spending time on food preparation. Copyright © 2014 American Journal of Preventive Medicine. Published by Elsevier Inc. All rights reserved.

Formaldehyde preparation methods for pressure and temperature dependent laser-induced fluorescence measurements

NASA Astrophysics Data System (ADS)

Burkert, A.; Müller, D.; Rieger, S.; Schmidl, G.; Triebel, W.; Paa, W.

2015-12-01

Formaldehyde is an excellent tracer for the early phase of ignition of hydrocarbon fuels and can be used, e.g., for characterization of single droplet ignition. However, due to its fast thermal decomposition at elevated temperatures and pressures, the determination of concentration fields from laser-induced fluorescence (LIF) measurements is difficult. In this paper, we address LIF measurements of this important combustion intermediate using a calibration cell. Here, formaldehyde is created from evaporation of paraformaldehyde. We discuss three setups for preparation of formaldehyde/air mixtures with respect to their usability for well-defined heating of formaldehyde/air mixtures. The "basic setup" uses a resist heater around the measurement cell for investigation of formaldehyde near vacuum conditions or formaldehyde/air samples after sequential admixing of air. The second setup, described for the first time in detail here, takes advantage of a constant flow formaldehyde/air regime which uses preheated air to reduce the necessary time for gas heating. We used the constant flow system to measure new pressure dependent LIF excitation spectra in the 343 nm spectral region (414 absorption band of formaldehyde). The third setup, based on a novel concept for fast gas heating via excitation of SF6 (chemically inert gas) using a TEA (transverse excitation at atmospheric pressure) CO2 laser, allows to further minimize both gas heating time and thermal decomposition. Here, an admixture of CO2 is served for real time temperature measurement based on Raman scattering. The applicability of the fast laser heating system has been demonstrated with gas mixtures of SF6 + air, SF6 + N2, as well as SF6 + N2 + CO2 at 1 bar total pressure.

Effects of zinc and multimineral vitamin supplementation on glycemic and lipid control in adult diabetes.

PubMed

Gunasekara, Priyanka; Hettiarachchi, Manjula; Liyanage, Chandrani; Lekamwasam, Sarath

2011-01-26

To evaluate the effects of zinc with or without other antioxidants on blood glucose, lipid profile, and serum creatinine in adult diabetics on long-term follow-up. Patients (n = 96) were randomly allocated to three groups: group A (n = 29) was supplemented with oral zinc sulfate (22 mg/day) and multivitamin/mineral (zinc+MVM) preparation; group B (n = 31) was given the same preparation without zinc (MVM); and group C (n = 36) was given a matching placebo for a period of 4 months in a single-blinded study. Blood samples were taken at baseline and after 4 months of supplementation to assess blood glucose (fasting and postprandial) and glycosylated hemoglobin (Hb(A1C)%) and serum levels of zinc, creatinine, and lipids. The zinc+MVM group had a mean change of fasting blood sugar -0.33 mmol/L (standard error of the mean 0.21 mmol/L) and was significant (P = 0.05) when compared with the other two groups (mean change in the MVM group +0.19 (0.31) mmol/L and +0.43 (0.23) mmol/L in the control group, respectively). The Hb(A1C)% level reduced significantly, irrespective of the baseline level, in zinc+MVM-supplemented individuals. In the other two groups, the change of Hb(A1C)% level was not significant. Serum lipid levels reduced significantly in the zinc+MVM and MVM groups. Zinc+MVM supplementation showed beneficial effects in the metabolic control of adult diabetics in addition to elevating their serum zinc level. Zinc supplementation improved glycemic control measured by Hb(A1C)% and fasting and postprandial glucose. Furthermore, zinc supplementation lowered serum cholesterol and cholesterol/high-density lipoprotein ratio.

Legume consumption and its association with fasting glucose, insulin resistance and type 2 diabetes in the Indian Migration Study.

PubMed

Dhillon, Preet K; Bowen, Liza; Kinra, Sanjay; Bharathi, Ankalmadugu Venkatsubbareddy; Agrawal, Sutapa; Prabhakaran, Dorairaj; Reddy, Kolli Srinath; Ebrahim, Shah

2016-11-01

Legume consumption is associated with lower fasting glucose (FG) and insulin levels in nutrition trials and lower CVD mortality in large-scale epidemiological studies. In India, legumes are widely consumed in various preparations, yet no epidemiological study has evaluated the association of legumes with FG levels, insulin resistance and diabetes risk. The present study aimed to fill this gap. Fasting blood samples, in-person interviews to obtain information on demographic/socio-economic factors, physical activity, alcohol and tobacco use, and anthropometric measurements were collected. Dietary intakes were assessed by an interviewer-administered, validated, semi-quantitative FFQ. Lucknow, Nagpur, Hyderabad and Bangalore, India. Men and women (n 6367) aged 15-76 years - urban residents, urban migrants and their rural siblings. In multivariate random-effects models adjusted for age, BMI, total energy intake, macronutrients, physical activity and rural/migration status, daily legume consumption was not associated with FG (P-for-trend=0·78), insulin resistance (homeostasis model assessment score; P-for-trend=0·73) or the prevalence of type 2 diabetes mellitus (P-for-trend=0·41). Stratified analyses by vegetarian diet and migration status did not change the findings. Inverse associations between legumes and FG emerged for participants with lower BMI and higher carbohydrate, protein, fat and sugar intakes. Although legumes are essential in traditional Indian diets, as well as in prudent and Mediterranean diets in the West, we did not find an association between legumes and markers of glycaemic control, insulin resistance or diabetes, except for subgroups based on BMI and macronutrient intake. The ubiquitous presence and complexity of legume preparations in Indian diets may contribute to these findings.

Large-Scale Low-Cost NGS Library Preparation Using a Robust Tn5 Purification and Tagmentation Protocol

PubMed Central

Hennig, Bianca P.; Velten, Lars; Racke, Ines; Tu, Chelsea Szu; Thoms, Matthias; Rybin, Vladimir; Besir, Hüseyin; Remans, Kim; Steinmetz, Lars M.

2017-01-01

Efficient preparation of high-quality sequencing libraries that well represent the biological sample is a key step for using next-generation sequencing in research. Tn5 enables fast, robust, and highly efficient processing of limited input material while scaling to the parallel processing of hundreds of samples. Here, we present a robust Tn5 transposase purification strategy based on an N-terminal His6-Sumo3 tag. We demonstrate that libraries prepared with our in-house Tn5 are of the same quality as those processed with a commercially available kit (Nextera XT), while they dramatically reduce the cost of large-scale experiments. We introduce improved purification strategies for two versions of the Tn5 enzyme. The first version carries the previously reported point mutations E54K and L372P, and stably produces libraries of constant fragment size distribution, even if the Tn5-to-input molecule ratio varies. The second Tn5 construct carries an additional point mutation (R27S) in the DNA-binding domain. This construct allows for adjustment of the fragment size distribution based on enzyme concentration during tagmentation, a feature that opens new opportunities for use of Tn5 in customized experimental designs. We demonstrate the versatility of our Tn5 enzymes in different experimental settings, including a novel single-cell polyadenylation site mapping protocol as well as ultralow input DNA sequencing. PMID:29118030

Assessment of glutathione levels in model solution and grape ferments supplemented with glutathione-enriched inactive dry yeast preparations using a novel UPLC-MS/MS method.

PubMed

Kritzinger, E C; Stander, M A; Du Toit, W J

2013-01-01

A novel, robust and fast ultra-high performance liquid chromatography-MS method has been developed for the simultaneous quantification of reduced glutathione (GSH) and oxidised glutathione (GSSG) in grape juice, wine and model wine solution. Sample preparation is minimal and does not require derivatisation. The method has very good performance in terms of sensitivity and selectivity. The limit of detection was 0.002 and 0.001 mg L(-1) for GSH and GSSG, respectively. The amount of GSH and GSSG released by commercial glutathione-enriched inactivated dry yeast preparations (GSH-IDYs) into a model solution was assessed. Significant differences in the amount of GSH and/or GSSG released into a model wine by different GSH-IDYs were observed, with ethanol influencing this release under certain conditions. The GSH and GSSG levels in grape juice fermentations supplemented with GSH-IDY were also assessed in relation to different addition times during fermentation. GSH-IDY addition can lead to elevated wine GSH levels, provided the supplementation is done early during alcoholic fermentation.

Highly ordered, accessible and nanocrystalline mesoporous TiO₂ thin films on transparent conductive substrates.

PubMed

Violi, Ianina L; Perez, M Dolores; Fuertes, M Cecilia; Soler-Illia, Galo J A A

2012-08-01

Highly porous (V(mesopore) = 25-50%) and ordered mesoporous titania thin films (MTTF) were prepared on ITO (indium tin oxide)-covered glass by a fast two-step method. The effects of substrate surface modification and thermal treatment on pore order, accessibility and crystallinity of the MTTF were systematically studied for MTTF deposited onto bare and titania-modified ITO. MTTF exposed briefly to 550 °C resulted in highly ordered films with grid-like structures, enlarged pore size, and increased accessible pore volume when prepared onto the modified ITO substrate. Mesostructure collapse and no significant change in pore volume were observed for MTTF deposited on bare ITO substrates. Highly crystalline anatase was obtained for MTTF prepared on the modified-ITO treated at high temperatures, establishing the relationship between grid-like structures and titania crystallization. Photocatalytic activity was maximized for samples with increased crystallization and high accessible pore volume. In this manner, a simple way of designing materials with optimized characteristics for optoelectronic applications was achieved through the modification of the ITO surface and a controlled thermal treatment.

Using colloidal silica as isolator, diverter and blocking agent for subsurface geological applications

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

Bourcier, William L.; Roberts, Sarah K.; Roberts, Jeffery J.

A system for blocking fast flow paths in geological formations includes preparing a solution of colloidal silica having a nonviscous phase and a solid gel phase. The solution of colloidal silica is injected into the geological formations while the solution of colloidal silica is in the nonviscous phase. The solution of colloidal silica is directed into the fast flow paths and reaches the solid gel phase in the fast flow paths thereby blocking flow of fluid in the fast paths.

Nutritional deficiency during colonoscopy preparation: the forgotten iatrogeny.

PubMed

Nunes, Gonçalo; Barata, Ana Teresa; Santos, Carla Adriana; Patita, Marta; Fonseca, Jorge

2018-05-01

bowel preparation for colonoscopy induces a semi-fasting state, with a potential negative impact on fragile patients. The present study aims to quantify nutritional deficiency during colonoscopy preparation. this was an observational and cross-sectional study. A convenience sample was obtained that included adults that underwent colonoscopy after bowel preparation with Klean-Prep® according to the center protocol. Anthropometric evaluation was performed and nutritional deficiency was calculated via the quantification of energy and protein intake during the 48 hours prior to the examination which was compared with the individuals' needs. The association between nutritional deficiency with the quality of bowel preparation, age and status (hospitalized/ambulatory) was evaluated. the study included 131 patients aged 21-91 years (mean 63.6 ± 13.2 years); 73 cases were male. Malnutrition reached 67.2% using specific anthropometric tools. A median preparation quality of six points was found when the Boston Bowel Preparation Scale was considered. The mean intake 48 hours prior to the procedure was 1,795 kcal and 100 g of protein. A daily energy intake of less than 50% of the individual needs was observed in 88 patients and less than 25% in 29 cases. The mean energy and protein deficiency were 59% (p < 0.01) and 45% (p < 0.01), and there was no correlation with preparation quality (p > 0.05). Nutritional defiency is similar in hospitalized and ambulatory patients (p > 0.05), but higher in older individuals (p = 0.04). nutritional deficiency during colonoscopy preparation was significant, more so in older patients, and there was no correlation with the quality of bowel preparation. We conclude that bowel preparation regimens should be reformulated with an improved nutritional intake and the inclusion of nutritional supplements without residues.

Protein Chips Compatible with MALDI Mass Spectrometry Prepared by Ambient Ion Landing.

PubMed

Pompach, Petr; Benada, Oldřich; Rosůlek, Michal; Darebná, Petra; Hausner, Jiří; Růžička, Viktor; Volný, Michael; Novák, Petr

2016-09-06

We present a technology that allows the preparation of matrix-assisted laser desorption/ionization (MALDI)-compatible protein chips by ambient ion landing of proteins and successive utilization of the resulting protein chips for the development of bioanalytical assays. These assays are based on the interaction between the immobilized protein and the sampled analyte directly on the protein chip and subsequent in situ analysis by MALDI mass spectrometry. The electrosprayed proteins are immobilized on dry metal and metal oxide surfaces, which are nonreactive under normal conditions. The ion landing of electrosprayed protein molecules is performed under atmospheric pressure by an automated ion landing apparatus that can manufacture protein chips with a predefined array of sample positions or any other geometry of choice. The protein chips prepared by this technique are fully compatible with MALDI ionization because the metal-based substrates are conductive and durable enough to be used directly as MALDI plates. Compared to other materials, the nonreactive surfaces show minimal nonspecific interactions with chemical species in the investigated sample and are thus an ideal substrate for selective protein chips. Three types of protein chips were used in this report to demonstrate the bioanalytical applications of ambient ion landing. The protein chips with immobilized proteolytic enzymes showed the usefulness for fast in situ peptide MALDI sequencing; the lectin-based protein chips showed the ability to enrich glycopeptides from complex mixtures with subsequent MALDI analysis, and the protein chips with immobilized antibodies were used for a novel immunoMALDI workflow that allowed the enrichment of antigens from the serum followed by highly specific MALDI detection.

Robust DNA Isolation and High-throughput Sequencing Library Construction for Herbarium Specimens.

PubMed

Saeidi, Saman; McKain, Michael R; Kellogg, Elizabeth A

2018-03-08

Herbaria are an invaluable source of plant material that can be used in a variety of biological studies. The use of herbarium specimens is associated with a number of challenges including sample preservation quality, degraded DNA, and destructive sampling of rare specimens. In order to more effectively use herbarium material in large sequencing projects, a dependable and scalable method of DNA isolation and library preparation is needed. This paper demonstrates a robust, beginning-to-end protocol for DNA isolation and high-throughput library construction from herbarium specimens that does not require modification for individual samples. This protocol is tailored for low quality dried plant material and takes advantage of existing methods by optimizing tissue grinding, modifying library size selection, and introducing an optional reamplification step for low yield libraries. Reamplification of low yield DNA libraries can rescue samples derived from irreplaceable and potentially valuable herbarium specimens, negating the need for additional destructive sampling and without introducing discernible sequencing bias for common phylogenetic applications. The protocol has been tested on hundreds of grass species, but is expected to be adaptable for use in other plant lineages after verification. This protocol can be limited by extremely degraded DNA, where fragments do not exist in the desired size range, and by secondary metabolites present in some plant material that inhibit clean DNA isolation. Overall, this protocol introduces a fast and comprehensive method that allows for DNA isolation and library preparation of 24 samples in less than 13 h, with only 8 h of active hands-on time with minimal modifications.

The diabetic patient in Ramadan.

PubMed

Chamsi-Pasha, Hassan; Aljabri, Khalid S

2014-04-01

During the month of Ramadan, all healthy, adult Muslims are required to fast from dawn to sunset. Fasting during Ramadan involves abstaining from food, water, beverages, smoking, oral drugs, and sexual intercourse. Although the Quran exempts chronically ill from fasting, many Muslims with diabetes still fast during Ramadan. Patients with diabetes who fast during the month of Ramadan can have acute complications. The risk of complications in fasting individuals with diabetes increases with longer periods of fasting. All patients with diabetes who wish to fast during Ramadan should be prepared by undergoing a medical assessment and engaging in a structured education program to undertake the fast as safely as possible. Although some guidelines do exist, there is an overwhelming need for better designed clinical trials which could provide us with evidence-based information and guidance in the management of patients with diabetes fasting Ramadan.

Fasting Might Not Be Necessary Before Lipid Screening: A Nationally Representative Cross-sectional Study

PubMed Central

Skinner, Asheley Cockrell; Perrin, Eliana M.

2011-01-01

BACKGROUND: There are barriers to fasting lipid screening for at-risk children. Results of studies in adults have suggested that lipid testing might be reliably performed without fasting. OBJECTIVE: To examine population-level differences in pediatric lipid values based on length of fast before testing. METHODS: We used the National Health and Nutrition Examination Survey (1999–2008) to examine total cholesterol (TC), HDL (high-density lipoprotein), LDL (low-density lipoprotein), and triglyceride cholesterol components on the basis of the period of fasting. Young children fasted for varying times before being tested, and children older than 12 years were asked to fast; however, adherence was variable. We used ordinary least-squares regression to test for differences in lipid values that were based on fasting times, controlling for weight status, age, race, ethnicity, and gender. RESULTS: TC, HDL, LDL, or triglyceride values were available for 12 744 children. Forty-eight percent of the TC and HDL samples and 80% of the LDL and triglyceride samples were collected from children who had fasted ≥8 hours. Fasting had a small positive effect for TC, HDL, and LDL, resulting in a mean value for the sample that was 2 to 5 mg/dL higher with a 12-hour fast compared with a no-fast sample. Fasting time had a negative effect on triglycerides (β = −0.859; P = .02), which resulted in values in the fasting group that were 7 mg/dL lower. DISCUSSION: Comparison of cholesterol screening results for a nonfasting group of children compared with results for a similar fasting group resulted in small differences that are likely not clinically important. Physicians might be able to decrease the burden of childhood cholesterol screening by not requiring prescreening fasting for these components. PMID:21807697

Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

PubMed Central

Matisová, Eva; Hrouzková, Svetlana

2012-01-01

Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC) and fast CGC with mass spectrometric detection (MS) has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP) residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important. PMID:23202677

Simultaneous measurement and quantitation of 4-hydroxyphenylacetic acid and dopamine with fast-scan cyclic voltammetry.

PubMed

Shin, Mimi; Kaplan, Sam V; Raider, Kayla D; Johnson, Michael A

2015-05-07

Caged compounds have been used extensively to investigate neuronal function in a variety of preparations, including cell culture, ex vivo tissue samples, and in vivo. As a first step toward electrochemically measuring the extent of caged compound photoactivation while also measuring the release of the catecholamine neurotransmitter, dopamine, fast-scan cyclic voltammetry at carbon-fiber microelectrodes (FSCV) was used to electrochemically characterize 4-hydroxyphenylacetic acid (4HPAA) in the absence and presence of dopamine. 4HPAA is a by-product formed during the process of photoactivation of p-hydroxyphenacyl-based caged compounds, such as p-hydroxyphenylglutamate (pHP-Glu). Our data suggest that the oxidation of 4HPAA occurs through the formation of a conjugated species. Moreover, we found that a triangular waveform of -0.4 V to +1.3 V to -0.4 V at 600 V s(-1), repeated every 100 ms, provided an oxidation current of 4HPAA that was enhanced with a limit of detection of 100 nM, while also allowing the detection and quantitation of dopamine within the same scan. Along with quantifying 4HPAA in biological preparations, the results from this work will allow the electrochemical measurement of photoactivation reactions that generate 4HPAA as a by-product as well as provide a framework for measuring the photorelease of electroactive by-products from caged compounds that incorporate other chromophores.

Simultaneous Measurement and Quantitation of 4-Hydroxyphenylacetic acid and Dopamine with Fast-Scan Cyclic Voltammetry

PubMed Central

Shin, Mimi; Kaplan, Sam V.; Raider, Kayla D.; Johnson, Michael A.

2015-01-01

Caged compounds have been used extensively to investigate neuronal function in a variety of preparations, including cell culture, ex vivo tissue samples, and in vivo. As a first step toward electrochemically measuring the extent of caged compound photoactivation while also measuring the release of the catecholamine neurotransmitter, dopamine, fast-scan cyclic voltammetry at carbon-fiber microelectrodes (FSCV) was used to electrochemically characterize 4-hydroxyphenylacetic acid (4HPAA) in the absence and presence of dopamine. 4HPAA is a by-product formed during the process of photoactivation of p-hydroxyphenylacyl-based caged compounds, such as p-hydroxyphenylglutamate (pHP-Glu). Our data suggest that the oxidation of 4HPAA occurs through the formation of a conjugated species. Moreover, we found that a triangular waveform of −0.4 V to +1.3 V to −0.4 V at 600 V/s, repeated every 100 ms, provided an oxidation current of 4HPAA that was enhanced with a limit of detection of 100 nM, while also allowing the detection and quantitation of dopamine within the same scan. Along with quantifying 4HPAA in biological preparations, the results from this work will allow the electrochemical measurement of photoactivation reactions that generate 4HPAA as a by-product as well as provide a framework for measuring the photorelease of electroactive by-products from caged compounds that incorporate other chromophores. PMID:25785694

What Teacher Preparation Programs Can Do to Better Prepare Teachers to Meet the Challenges of Educating Students Living in Poverty

ERIC Educational Resources Information Center

Hughes, Jacqueline A.

2010-01-01

Because of the present, increasing economic circumstances, poverty is fast becoming a crisis, and teacher preparation programs must begin to prepare teachers to explicitly address the needs of poor children. The inclusion of poverty in this discourse is in no way intended to discount the issues of race, ethnicity, and gender. The intention here is…

Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

PubMed

Magiera, Sylwia; Kwietniowska, Ewelina

2016-11-15

In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of experimental and sample factors on dehydration kinetics of mildronate dihydrate: mechanism of dehydration and determination of kinetic parameters.

PubMed

Bērziņš, Agris; Actiņš, Andris

2014-06-01

The dehydration kinetics of mildronate dihydrate [3-(1,1,1-trimethylhydrazin-1-ium-2-yl)propionate dihydrate] was analyzed in isothermal and nonisothermal modes. The particle size, sample preparation and storage, sample weight, nitrogen flow rate, relative humidity, and sample history were varied in order to evaluate the effect of these factors and to more accurately interpret the data obtained from such analysis. It was determined that comparable kinetic parameters can be obtained in both isothermal and nonisothermal mode. However, dehydration activation energy values obtained in nonisothermal mode showed variation with conversion degree because of different rate-limiting step energy at higher temperature. Moreover, carrying out experiments in this mode required consideration of additional experimental complications. Our study of the different sample and experimental factor effect revealed information about changes of the dehydration rate-limiting step energy, variable contribution from different rate limiting steps, as well as clarified the dehydration mechanism. Procedures for convenient and fast determination of dehydration kinetic parameters were offered. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Comparative bioavailability of two novel coenzyme Q10 preparations in humans.

PubMed

Joshi, S S; Sawant, S V; Shedge, A; Halpner, A D

2003-01-01

To determine the absorptive properties of 2 novel coenzyme Q10 preparations, a fast-melting tablet and an effervescent tablet, compared with currently available formulations. In the first trial, the absorptive properties of 4 different coenzyme Q10 preparations (fast-melting, effervescent, soft gelatin, and powder-filled hard shell) were studied in a randomized, single-dose, crossover study. Twenty-four male subjects were given a 60 mg dose of coenzyme Q10 and plasma coenzyme Q10 was measured over the next 12 hours. Pharmacokinetic properties including area under the curve (AUC), maximum plasma concentration (Cmax), time to maximum plasma concentration (Tmax) and elimination half-life (t 1/2) were measured. In a separate single-dose study, the absorptive characteristics of a different coenzyme Q10 soft gel (Q-Gel) were studied in 6 male subjects. Area under the curve (microg/ml x h) for the fast-melting and effervescent formulations, while marginally greater, was not significantly different when compared to the soft gelatin and powder-filled preparations, 5.4 +/- 1.04 (110%) and 5.5 +/- 0.589 (112%) versus 5.0 +/- 0.859 (102%) and 4.9 +/- 0.812 (100%), respectively. Cmax for the 2 novel formulations was also not statistically different from the soft gelatin or powder-filled preparations, 0.87 +/- 0.14 and 0.86 +/- 0.074 versus 0.70 +/- 0.010 and 0.81 +/- 0.159 (microg/ml). Tmax however, was significantly shorter for the fast-melting and effervescent formulations compared with the soft gel and powder-filled forms, 1.3 +/- 0.348 and 2.0 +/- 0.552 versus 3.7 +/- 0.702 and 4.1 +/- 0.993 (h), respectively. The results of the second trial were similar to those of the powder-filled and soft gel formulations from the first study. The novel fast-melting and effervescent formulations provide a more rapid delivery of CoQ10 to the blood while exhibiting a similar AUC compared with current formulations. The potential clinical significance of this finding should be further evaluated.

Dietary Consumption Practices and Cancer Risk In African Americans in the Rural South

PubMed Central

Bovell-Benjamin, Adelia; Dawkins, Norma; Pace, Ralphenia; Shikany, James M.

2017-01-01

This study describes the dietary consumption practices of a sample of African Americans in the rural South. A qualitative research design involving a cross-sectional food diary was utilized. Complete datasets were collected from 114 participants, 66% female, between the ages of 19 and 79 years. The consumption of a variety of fruits, non-starchy vegetables and unprocessed cereals in daily meals was low in this sample. Frequent consumption of fried foods; fast foods; sugary, carbonated beverages; processed, high-fat and high-sodium foods; and low fruit and non-starchy vegetable intake were evident. The findings are crucial to the development for culturally-specific nutrition education intervention programs for African Americans in the rural South targeted at the modification of not only diet, but food preparation methods to reduce cancer risk. PMID:20675946

Understanding and comparisons of different sampling approaches for the Fourier Amplitudes Sensitivity Test (FAST)

PubMed Central

Xu, Chonggang; Gertner, George

2013-01-01

Fourier Amplitude Sensitivity Test (FAST) is one of the most popular uncertainty and sensitivity analysis techniques. It uses a periodic sampling approach and a Fourier transformation to decompose the variance of a model output into partial variances contributed by different model parameters. Until now, the FAST analysis is mainly confined to the estimation of partial variances contributed by the main effects of model parameters, but does not allow for those contributed by specific interactions among parameters. In this paper, we theoretically show that FAST analysis can be used to estimate partial variances contributed by both main effects and interaction effects of model parameters using different sampling approaches (i.e., traditional search-curve based sampling, simple random sampling and random balance design sampling). We also analytically calculate the potential errors and biases in the estimation of partial variances. Hypothesis tests are constructed to reduce the effect of sampling errors on the estimation of partial variances. Our results show that compared to simple random sampling and random balance design sampling, sensitivity indices (ratios of partial variances to variance of a specific model output) estimated by search-curve based sampling generally have higher precision but larger underestimations. Compared to simple random sampling, random balance design sampling generally provides higher estimation precision for partial variances contributed by the main effects of parameters. The theoretical derivation of partial variances contributed by higher-order interactions and the calculation of their corresponding estimation errors in different sampling schemes can help us better understand the FAST method and provide a fundamental basis for FAST applications and further improvements. PMID:24143037

Understanding and comparisons of different sampling approaches for the Fourier Amplitudes Sensitivity Test (FAST).

PubMed

Xu, Chonggang; Gertner, George

2011-01-01

Fourier Amplitude Sensitivity Test (FAST) is one of the most popular uncertainty and sensitivity analysis techniques. It uses a periodic sampling approach and a Fourier transformation to decompose the variance of a model output into partial variances contributed by different model parameters. Until now, the FAST analysis is mainly confined to the estimation of partial variances contributed by the main effects of model parameters, but does not allow for those contributed by specific interactions among parameters. In this paper, we theoretically show that FAST analysis can be used to estimate partial variances contributed by both main effects and interaction effects of model parameters using different sampling approaches (i.e., traditional search-curve based sampling, simple random sampling and random balance design sampling). We also analytically calculate the potential errors and biases in the estimation of partial variances. Hypothesis tests are constructed to reduce the effect of sampling errors on the estimation of partial variances. Our results show that compared to simple random sampling and random balance design sampling, sensitivity indices (ratios of partial variances to variance of a specific model output) estimated by search-curve based sampling generally have higher precision but larger underestimations. Compared to simple random sampling, random balance design sampling generally provides higher estimation precision for partial variances contributed by the main effects of parameters. The theoretical derivation of partial variances contributed by higher-order interactions and the calculation of their corresponding estimation errors in different sampling schemes can help us better understand the FAST method and provide a fundamental basis for FAST applications and further improvements.

High-speed, random-access fluorescence microscopy: I. High-resolution optical recording with voltage-sensitive dyes and ion indicators.

PubMed

Bullen, A; Patel, S S; Saggau, P

1997-07-01

The design and implementation of a high-speed, random-access, laser-scanning fluorescence microscope configured to record fast physiological signals from small neuronal structures with high spatiotemporal resolution is presented. The laser-scanning capability of this nonimaging microscope is provided by two orthogonal acousto-optic deflectors under computer control. Each scanning point can be randomly accessed and has a positioning time of 3-5 microseconds. Sampling time is also computer-controlled and can be varied to maximize the signal-to-noise ratio. Acquisition rates up to 200k samples/s at 16-bit digitizing resolution are possible. The spatial resolution of this instrument is determined by the minimal spot size at the level of the preparation (i.e., 2-7 microns). Scanning points are selected interactively from a reference image collected with differential interference contrast optics and a video camera. Frame rates up to 5 kHz are easily attainable. Intrinsic variations in laser light intensity and scanning spot brightness are overcome by an on-line signal-processing scheme. Representative records obtained with this instrument by using voltage-sensitive dyes and calcium indicators demonstrate the ability to make fast, high-fidelity measurements of membrane potential and intracellular calcium at high spatial resolution (2 microns) without any temporal averaging.

High-speed, random-access fluorescence microscopy: I. High-resolution optical recording with voltage-sensitive dyes and ion indicators.

PubMed Central

Bullen, A; Patel, S S; Saggau, P

1997-01-01

The design and implementation of a high-speed, random-access, laser-scanning fluorescence microscope configured to record fast physiological signals from small neuronal structures with high spatiotemporal resolution is presented. The laser-scanning capability of this nonimaging microscope is provided by two orthogonal acousto-optic deflectors under computer control. Each scanning point can be randomly accessed and has a positioning time of 3-5 microseconds. Sampling time is also computer-controlled and can be varied to maximize the signal-to-noise ratio. Acquisition rates up to 200k samples/s at 16-bit digitizing resolution are possible. The spatial resolution of this instrument is determined by the minimal spot size at the level of the preparation (i.e., 2-7 microns). Scanning points are selected interactively from a reference image collected with differential interference contrast optics and a video camera. Frame rates up to 5 kHz are easily attainable. Intrinsic variations in laser light intensity and scanning spot brightness are overcome by an on-line signal-processing scheme. Representative records obtained with this instrument by using voltage-sensitive dyes and calcium indicators demonstrate the ability to make fast, high-fidelity measurements of membrane potential and intracellular calcium at high spatial resolution (2 microns) without any temporal averaging. Images FIGURE 6 PMID:9199810

Optimizations of packed sorbent and inlet temperature for large volume-direct aqueous injection-gas chromatography to determine high boiling volatile organic compounds in water.

PubMed

Yu, Bofan; Song, Yonghui; Han, Lu; Yu, Huibin; Liu, Yang; Liu, Hongliang

2014-08-22

For the expanded application area, fast trace analysis of certain high boiling point (i.e., 150-250 °C) volatile organic compounds (HVOCs) in water, a large volume-direct aqueous injection-gas chromatography (LV-DAI-GC) method was optimized for the following parameters: packed sorbent for sample on-line pretreatment, inlet temperature and detectors configuration. Using the composite packed sorbent self-prepared with lithium chloride and a type of diatomite, the method enabled safe injection of an approximately 50-100 μL sample at an inlet temperature of 150 °C in the splitless mode and separated HVOCs from water matrix in 2 min. Coupled with a flame ionization detector (FID), an electron capture detector (ECD) and a flame photometric detector (FPD), the method could simultaneously quantify 27 HVOCs that belong to seven subclasses (i.e., halogenated aliphatic hydrocarbons, chlorobenzenes, nitrobenzenes, anilines, phenols, polycyclic aromatic hydrocarbons and organic sulfides) in 26 min. Injecting a 50 μL sample without any enrichment step, such as cryotrap focusing, the limits of quantification (LOQs) for the 27 HVOCs was 0.01-3 μg/L. Replicate analyses of the 27 HVOCs spiked source and river water samples exhibited good precision (relative standard deviations ≤ 11.3%) and accuracy (relative errors ≤ 17.6%). The optimized LV-DAI-GC was robust and applicable for fast determination and automated continuous monitoring of HVOCs in surface water. Copyright © 2014 Elsevier B.V. All rights reserved.

A simplified protocol for molecular identification of Eimeria species in field samples.

PubMed

Haug, Anita; Thebo, Per; Mattsson, Jens G

2007-05-15

This study aimed to find a fast, sensitive and efficient protocol for molecular identification of chicken Eimeria spp. in field samples. Various methods for each of the three steps of the protocol were evaluated: oocyst wall rupturing methods, DNA extraction methods, and identification of species-specific DNA sequences by PCR. We then compared and evaluated five complete protocols. Three series of oocyst suspensions of known number of oocysts from Eimeria mitis, Eimeria praecox, Eimeria maxima and Eimeria tenella were prepared and ground using glass beads or mini-pestle. DNA was extracted from ruptured oocysts using commercial systems (GeneReleaser, Qiagen Stoolkit and Prepman) or phenol-chloroform DNA extraction, followed by identification of species-specific ITS-1 sequences by optimised single species PCR assays. The Stoolkit and Prepman protocols showed insufficient repeatability, and the former was also expensive and relatively time-consuming. In contrast, both the GeneReleaser protocol and phenol-chloroform protocols were robust and sensitive, detecting less than 0.4 oocysts of each species per PCR. Finally, we evaluated our new protocol on 68 coccidia positive field samples. Our data suggests that rupturing the oocysts by mini-pestle grinding, preparing the DNA with GeneReleaser, followed by optimised single species PCR assays, makes a robust and sensitive procedure for identifying chicken Eimeria species in field samples. Importantly, it also provides minimal hands-on-time in the pre-PCR process, lower contamination risk and no handling of toxic chemicals.

Comparison of the recovery of Mycobacterium bovis isolates using the BACTEC MGIT 960 system, BACTEC 460 system, and Middlebrook 7H10 and 7H11 solid media.

PubMed

Hines, Nichole; Payeur, Janet B; Hoffman, Lorraine J

2006-05-01

The BACTEC Microbacteria Growth Indicator Tube (MGIT) 960 system was evaluated to determine how it compares with the BACTEC 460 radiometric system and solid media for recovery of Mycobacterium bovis from tissue samples. A total of 506 bovine lymph node samples were collected from abattoirs in the United States and Mexico between November 2003 and September 2004. Processed samples were inoculated into an MGIT 960 tube, BACTEC 460 vial, and Middlebrook 7H10 and Middlebrook 7H11 solid media. Ziehl-Neelsen slides were prepared to check for contaminants and confirm the presence of acid-fast positive bacilli. Samples containing acid-fast bacilli were confirmed as members of the Mycobacterium tuberculosis complex by a nucleic acid assay. Niacin and nitrate biochemical tests were used to distinguish M. bovis from M. tuberculosis isolates. Statistical analyses were performed to compare recovery rate, mean time to detection, contamination rates, as well as pair-wise comparisons in each category. The results showed that the MGIT 960 system had a higher recovery rate of M. bovis (122/129) than did the BACTEC 460 (102/129) and solid media system (96/129). The average time to detection was 15.8 days for the MGIT 960 system, 28.2 days for the BACTEC 460 system, and 43.4 days for solid media. Contamination rates were 6.9% for the MGIT 960 system, 3.4% for the BACTEC 460 system, and 21.7% for solid media. These results indicate the MGIT 960 system can be used as an alternative to the BACTEC 460 system for recovering M. bovis from tissue samples.

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

Fast assembling microarrays of superparamagnetic Fe3O4@Au nanoparticle clusters as reproducible substrates for surface-enhanced Raman scattering

NASA Astrophysics Data System (ADS)

Ye, Min; Wei, Zewen; Hu, Fei; Wang, Jianxin; Ge, Guanglu; Hu, Zhiyuan; Shao, Mingwang; Lee, Shuit-Tong; Liu, Jian

2015-08-01

It is currently a very active research area to develop new types of substrates which integrate various nanomaterials for surface-enhanced Raman scattering (SERS) techniques. Here we report a unique approach to prepare SERS substrates with reproducible performance. It features silicon mold-assisted magnetic assembling of superparamagnetic Fe3O4@Au nanoparticle clusters (NCs) into arrayed microstructures on a wafer scale. This approach enables the fabrication of both silicon-based and hydrogel-based substrates in a sequential manner. We have demonstrated that strong SERS signals can be harvested from these substrates due to an efficient coupling effect between Fe3O4@Au NCs, with enhancement factors >106. These substrates have been confirmed to provide reproducible SERS signals, with low variations in different locations or batches of samples. We investigate the spatial distributions of electromagnetic field enhancement around Fe3O4@Au NCs assemblies using finite-difference-time-domain (FDTD) simulations. The procedure to prepare the substrates is straightforward and fast. The silicon mold can be easily cleaned out and refilled with Fe3O4@Au NCs assisted by a magnet, therefore being re-useable for many cycles. Our approach has integrated microarray technologies and provided a platform for thousands of independently addressable SERS detection, in order to meet the requirements of a rapid, robust, and high throughput performance.It is currently a very active research area to develop new types of substrates which integrate various nanomaterials for surface-enhanced Raman scattering (SERS) techniques. Here we report a unique approach to prepare SERS substrates with reproducible performance. It features silicon mold-assisted magnetic assembling of superparamagnetic Fe3O4@Au nanoparticle clusters (NCs) into arrayed microstructures on a wafer scale. This approach enables the fabrication of both silicon-based and hydrogel-based substrates in a sequential manner. We have demonstrated that strong SERS signals can be harvested from these substrates due to an efficient coupling effect between Fe3O4@Au NCs, with enhancement factors >106. These substrates have been confirmed to provide reproducible SERS signals, with low variations in different locations or batches of samples. We investigate the spatial distributions of electromagnetic field enhancement around Fe3O4@Au NCs assemblies using finite-difference-time-domain (FDTD) simulations. The procedure to prepare the substrates is straightforward and fast. The silicon mold can be easily cleaned out and refilled with Fe3O4@Au NCs assisted by a magnet, therefore being re-useable for many cycles. Our approach has integrated microarray technologies and provided a platform for thousands of independently addressable SERS detection, in order to meet the requirements of a rapid, robust, and high throughput performance. Electronic supplementary information (ESI) available: XRD, reflection spectra, zeta potential, TEM images, evaluations of reproducibility, EDS, tables of EF and RSD values of different substrates. See DOI: 10.1039/c5nr02491a

Multicommuted flow injection method for fast photometric determination of phenolic compounds in commercial virgin olive oil samples.

PubMed

Lara-Ortega, Felipe J; Sainz-Gonzalo, Francisco J; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2016-01-15

A multicommuted flow injection method has been developed for the determination of phenolic species in virgin olive oil samples. The method is based on the inhibitory effect of antioxidants on a stable and colored radical cation formation from the colorless compound N,N-dimethyl-p-phenylenediamine (DMPD(•+)) in acidic medium in the presence of Fe(III) as oxidant. The signal inhibition by phenolic species and other antioxidants is proportional to their concentration in the olive oil sample. Absorbance was recorded at 515nm by means of a modular fiber optic spectrometer. Oleuropein was used as the standard for phenols determination and 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (trolox) was the reference standard used for total antioxidant content calculation. Linear response was observed within the range of 250-1000mg/kg oleuropein, which was in accordance with phenolic contents observed in commercial extra virgin olive oil in the present study. Fast and low-volume liquid-liquid extraction of the samples using 60% MeOH was made previous to their insertion in the flow multicommuted system. The five three-way solenoid valves used for multicommuted liquid handling were controlled by a homemade electronic interface and Java-written software. The proposed approach was applied to different commercial extra virgin olive oil samples and the results were consistent with those obtained by the Folin Ciocalteu (FC) method. Total time for the sample preparation and the analysis required in the present approach can be drastically reduced: the throughput of the present analysis is 8 samples/h in contrast to 1sample/h of the conventional FC method. The present method is easy to implement in routine analysis and can be regarded as a feasible alternative to FC method. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparative Evaluation of Marginal Discrepancy in Tooth Colored Self Cure Acrylic Provisional Restorations With and Without Reinforcement of Glass Beads: An In-Vitro Study.

PubMed

Yasangi, Manoj Kumar; Mannem, Dhanalakshmi; Bommireddy, Vikram Simha; Neturi, Sirisha; Ravoori, Srinivas; Jyothi

2015-05-01

This invitro study was conducted to compare and evaluate marginal discrepancy in two types of tooth colored self cure provisional restorative materials {DPI&UNIFAST TRAD} before and after reinforcement of glass beads. The aim of the present study was to evaluate and compare marginal discrepancy in two types of provisional restorative materials (DPI and UNI FAST TRAD) before and after reinforcement with Glass beads. Tooth shaped resin copings were fabricated on custom made brass metal die. A total of 60 resin copings were fabricated in which 30 samples were prepared with DPI and 30 samples with UNIFAST material. Each group of 30 samples were divided in to two sub groups in which 15 samples were prepared with glass bead reinforcement and 15 samples without reinforcement. The marginal discrepancy was evaluated with photomicroscope {Reichet Polyvar 2 met} by placing the resin copings on custom made brass resin coping holder. Measurements obtained were statistically analysed by unpaired t-test to know any significance between two variables. Unreinforced DPI specimens had shown lower marginal discrepancy (442.82) than reinforced specimens (585.77). Unreinforced UNIFAST specimens have shown high values of marginal discrepancy (592.83) than reinforced specimens (436.35). p-value between reinforced and unreinforced specimens of DPI (p=0.0013) and UNIFAST (p= 0.0038) has shown statistical significance. This in-vitro study revealed that unreinforced DPI specimens have shown lower marginal discrepancy than reinforced specimens and unreinforced UNIFAST specimens have shown higher values of marginal discrepancy than reinforced specimens.

[Preparation of a kind of SERS-active substrates for spot fast analysis].

PubMed

Ji, Nan; Li, Zhi-Shi; Zhao, Bing; Zou, Bo

2013-02-01

A kind of SERS-active substrates was prepared using chemical self-assembly method, aiming at spot fast analysis using portable Raman spectrometer. PDDA was first absorbed on the inner wall of vials, and then Ag colloids were assembled on the inner wall. UV-Vis spectra and Raman spectra of two kinds of blank vials were investigated and the transparent vials were thought to be better for SERS-vials. UV-Vis spectra were used to monitor the assembly process of Ag colloids. SERS activity of our substrates was characterized using p-ATP as probing molecules.

Discovery of a New Photometric Sub-class of Faint and Fast Classical Novae

NASA Astrophysics Data System (ADS)

Kasliwal, M. M.; Cenko, S. B.; Kulkarni, S. R.; Ofek, E. O.; Quimby, R.; Rau, A.

2011-07-01

We present photometric and spectroscopic follow-up of a sample of extragalactic novae discovered by the Palomar 60 inch telescope during a search for "Fast Transients In Nearest Galaxies" (P60-FasTING). Designed as a fast cadence (1 day) and deep (g < 21 mag) survey, P60-FasTING was particularly sensitive to short-lived and faint optical transients. The P60-FasTING nova sample includes 10 novae in M 31, 6 in M 81, 3 in M 82, 1 in NGC 2403, and 1 in NGC 891. This significantly expands the known sample of extragalactic novae beyond the Local Group, including the first discoveries in a starburst environment. Surprisingly, our photometry shows that this sample is quite inconsistent with the canonical maximum-magnitude-rate-of-decline (MMRD) relation for classical novae. Furthermore, the spectra of the P60-FasTING sample are indistinguishable from classical novae. We suggest that we have uncovered a sub-class of faint and fast classical novae in a new phase space in luminosity-timescale of optical transients. Thus, novae span two orders of magnitude in both luminosity and time. Perhaps the MMRD, which is characterized only by the white dwarf mass, was an oversimplification. Nova physics appears to be characterized by a relatively rich four-dimensional parameter space in white dwarf mass, temperature, composition, and accretion rate.

Submicron magnetic core conducting polypyrrole polymer shell: Preparation and characterization.

PubMed

Tenório-Neto, Ernandes Taveira; Baraket, Abdoullatif; Kabbaj, Dounia; Zine, Nadia; Errachid, Abdelhamid; Fessi, Hatem; Kunita, Marcos Hiroiuqui; Elaissari, Abdelhamid

2016-04-01

Magnetic particles are of great interest in various biomedical applications, such as, sample preparation, in vitro biomedical diagnosis, and both in vivo diagnosis and therapy. For in vitro applications and especially in labs-on-a-chip, microfluidics, microsystems, or biosensors, the needed magnetic dispersion should answer various criteria, for instance, submicron size in order to avoid a rapid sedimentation rate, fast separations under an applied magnetic field, and appreciable colloidal stability (stable dispersion under shearing process). Then, the aim of this work was to prepare highly magnetic particles with a magnetic core and conducting polymer shell particles in order to be used not only as a carrier, but also for the in vitro detection step. The prepared magnetic seed dispersions were functionalized using pyrrole and pyrrole-2-carboxylic acid. The obtained core-shell particles were characterized in terms of particle size, size distribution, magnetization properties, FTIR analysis, surface morphology, chemical composition, and finally, the conducting property of those particles were evaluated by cyclic voltammetry. The obtained functional submicron highly magnetic particles are found to be conducting material bearing function carboxylic group on the surface. These promising conducting magnetic particles can be used for both transport and lab-on-a-chip detection. Copyright © 2015. Published by Elsevier B.V.

Preparation of Fe2O3-Clorprenaline/Tetraphenylborate Nanospheres and Their Application as Ion Selective Electrode for Determination of Clorprenaline in Pork

NASA Astrophysics Data System (ADS)

Shao, Xintian; Zhang, Jing; Li, Donghui; Yue, Jingli; Chen, Zhenhua

2016-04-01

A novel modified ion selective electrode based on Fe2O3-clorprenaline/tetraphenylborate nanospheres (Fe2O3-CLPT NSs) as electroactive materials for the determination of clorprenaline hydrochloride (CLP) is described. The α-Fe2O3 nanoparticles (NPs) were prepared by hydrothermal synthesis, then self-assembled on CLP/tetraphenylborate (TPB) to form Fe2O3-CLPT NSs, which were used as a potentiometric electrode for analyte determination innovatively. The Fe2O3-CLPT NSs modified electrode exhibited a wider concentration range from 1.0 × 10-7 to 1.0 × 10-1 mol/L and a lower detection limit of 3.7 × 10-8 mol/L compared with unmodified electrodes. The selectivity of the modified electrode was evaluated by fixed interference method. The good performance of the modified electrode such as wide pH range (2.4-6.7), fast response time (15 s), and adequate lifetime (14 weeks) indicate the utility of the modified electrode for evaluation of CLP content in various real samples. Finally, the modified electrode was successfully employed to detect CLP in pork samples with satisfactory results. These results demonstrated the Fe2O3-CLPT NSs modified electrode to be a functional and convenient method to the field of potentiometry determination of CLP in real samples.

Laser-induced breakdown spectroscopy (LIBS) technique for the determination of the chemical composition of complex inorganic materials

NASA Astrophysics Data System (ADS)

Łazarek, Łukasz; Antończak, Arkadiusz J.; Wójcik, Michał R.; Kozioł, Paweł E.; Stepak, Bogusz; Abramski, Krzysztof M.

2014-08-01

Laser-induced breakdown spectroscopy (LIBS) is a fast, fully optical method, that needs little or no sample preparation. In this technique qualitative and quantitative analysis is based on comparison. The determination of composition is generally based on the construction of a calibration curve namely the LIBS signal versus the concentration of the analyte. Typically, to calibrate the system, certified reference materials with known elemental composition are used. Nevertheless, such samples due to differences in the overall composition with respect to the used complex inorganic materials can influence significantly on the accuracy. There are also some intermediate factors which can cause imprecision in measurements, such as optical absorption, surface structure, thermal conductivity etc. This paper presents the calibration procedure performed with especially prepared pellets from the tested materials, which composition was previously defined. We also proposed methods of post-processing which allowed for mitigation of the matrix effects and for a reliable and accurate analysis. This technique was implemented for determination of trace elements in industrial copper concentrates standardized by conventional atomic absorption spectroscopy with a flame atomizer. A series of copper flotation concentrate samples was analyzed for contents of three elements, that is silver, cobalt and vanadium. It has been shown that the described technique can be used to qualitative and quantitative analyses of complex inorganic materials, such as copper flotation concentrates.

Effective Enrichment and Detection of Trace Polycyclic Aromatic Hydrocarbons in Food Samples based on Magnetic Covalent Organic Framework Hybrid Microspheres.

PubMed

Li, Ning; Wu, Di; Hu, Na; Fan, Guangsen; Li, Xiuting; Sun, Jing; Chen, Xuefeng; Suo, Yourui; Li, Guoliang; Wu, Yongning

2018-04-04

The present study reported a facile, sensitive, and efficient method for enrichment and determination of trace polycyclic aromatic hydrocarbons (PAHs) in food samples by employing new core-shell nanostructure magnetic covalent organic framework hybrid microspheres (Fe 3 O 4 @COF-(TpBD)) as the sorbent followed by HPLC-DAD. Under mild synthetic conditions, the Fe 3 O 4 @COF-(TpBD) were prepared with the retention of colloidal nanosize, larger specific surface area, higher porosity, uniform morphology, and supermagnetism. The as-prepared materials showed an excellent adsorption ability for PAHs, and the enrichment efficiency of the Fe 3 O 4 @COF-(TpBD) could reach 99.95%. The obtained materials also had fast adsorption kinetics and realized adsorption equilibrium within 12 min. The eluent was further analyzed by HPLC-DAD, and good linearity was observed in the range of 1-100 ng/mL with the linear correlation being above 0.9990. The limits of detection (S/N = 3) and limits of quantitation (S/N = 10) for 15 PAHs were in the range of 0.83-11.7 ng/L and 2.76-39.0 ng/L, respectively. For the application, the obtained materials were employed for the enrichment of trace PAHs in food samples and exhibited superior enrichment capacity and excellent applicability.

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

NASA Astrophysics Data System (ADS)

Melo, B. M. G.; Graça, M. P. F.; Prezas, P. R.; Valente, M. A.; Almeida, A. F.; Freire, F. N. A.; Bih, L.

2016-08-01

In this work, phosphate-borate based glasses with molar composition 20.7P2O5-17.2Nb2O5-13.8WO3-34.5A2O-13.8B2O3, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric, and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σac and σdc, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz-1 MHz.

Nutrition labeling and value size pricing at fast-food restaurants: a consumer perspective.

PubMed

O'Dougherty, Maureen; Harnack, Lisa J; French, Simone A; Story, Mary; Oakes, J Michael; Jeffery, Robert W

2006-01-01

This pilot study examined nutrition-related attitudes that may affect food choices at fast-food restaurants, including consumer attitudes toward nutrition labeling of fast foods and elimination of value size pricing. A convenience sample of 79 fast-food restaurant patrons aged 16 and above (78.5% white, 55% female, mean age 41.2 [17.1]) selected meals from fast-food restaurant menus that varied as to whether nutrition information was provided and value pricing included and completed a survey and interview on nutrition-related attitudes. Only 57.9% of participants rated nutrition as important when buying fast food. Almost two thirds (62%) supported a law requiring nutrition labeling on restaurant menus. One third (34%) supported a law requiring restaurants to offer lower prices on smaller instead of bigger-sized portions. This convenience sample of fast-food patrons supported nutrition labels on menus. More research is needed with larger samples on whether point-of-purchase nutrition labeling at fast-food restaurants raises perceived importance of nutrition when eating out.

Fast and efficient detection of tuberculosis antigens using liposome encapsulated secretory proteins of Mycobacterium tuberculosis.

PubMed

Tiwari, Dileep; Haque, Shafiul; Tiwari, Ram P; Jawed, Arshad; Govender, Thavendran; Kruger, Hendrik G

2017-04-01

A rapid and efficient diagnostic test was developed for the detection of Mycobacterium tuberculosis antigens in serum samples of active tuberculosis (TB) and extrapulmonary TB patients via a liposomal agglutination-based method. A rapid card test has been developed to facilitate the recognition of high-affinity binding rabbit raised purified culture filtrate protein antibodies coupled on the surface of activated liposomal preparation. In the presence of TB antigens, the polyclonal antibodies bound to the liposomal particles demonstrate a visible agglutination reaction. The developed assay was simple, rapid, reliable, sensitive, and specific as a diagnostic test for the detection of antigens in serum samples of clinically confirmed cases of TB within 4-5 minutes' duration. The test was evaluated at different hospitals, medical colleges, and pathology centers, and involved 1483 participants. This investigation was conducted to detect the presence of these antigens during the period of active growth of the microorganism in serum samples for pulmonary TB and processed tissue biopsy for other extrapulmonary TB. Results obtained using this test were compared with acid-fast bacilli smear and culture results. Our study demonstrated that the newly developed liposome tuberculosis antigen card test detected antigens in our study population with approximately 97.48% sensitivity and 95.79% specificity. This is the first study to report the liposomal encapsulation of culture filtrate proteins from M. tuberculosis for diagnostic application. Copyright © 2015. Published by Elsevier B.V.

Immunohistochemical evidence for expression of fast-twitch type sarco(endo)plasmic reticulum Ca2+ ATPase (SERCA1) in German shepherd dogs with dilated cardiomyopathy myocardium.

PubMed

Summerfield, Nuala; Peters, Mary E; Hercock, Carol A; Mobasheri, Ali; Young, Iain S

2010-04-01

Dilated cardiomyopathy (DCM) is one of the most common acquired canine heart diseases. It is particularly common in large and giant breed dogs. Although a great deal is known about the clinical progression and manifestations of the disease, the underlying cellular and molecular mechanisms remain poorly understood. One widely held belief is that calcium-handling abnormalities are critically involved in the disease process. This study investigates the changes in expression of the sarco(endo)plasmic reticulum calcium ATPase (SERCA) isoforms in DCM myocardium from German shepherd dogs. Affected tissue samples were obtained from German shepherd dogs with DCM, euthanized for intractable congestive heart failure while normal myocardial tissue samples were obtained from German shepherd dogs, euthanized for non-cardiovascular reasons. Tissue microarrays containing normal and DCM myocardium samples were prepared, immunostained with SERCA1 and SERCA2 antibodies and analyzed. We were able to demonstrate, for the first time, that while there is little change in the expression of the cardiac isoform (SERCA2), there is clear expression of the fast-twitch skeletal muscle isoform SERCA1 in the myocardium of dogs diagnosed with DCM. We propose that SERCA1 expression is evidence of a natural adaptive response to the impaired Ca2+ handling thought to occur in German shepherd dogs with DCM and heart failure. Copyright 2010 Elsevier B.V. All rights reserved.

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.

Microwave-assisted hydrothermal synthesis of marigold-like ZnIn{sub 2}S{sub 4} microspheres and their visible light photocatalytic activity

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

Chen Zhixin, E-mail: czx@fzu.edu.cn; Analysis and Test Center, Fuzhou University, Fuzhou 350002; Li Danzhen

Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 Degree-Sign C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn{sub 2}S{sub 4}, which shows that the ZnIn{sub 2}S{submore » 4} sample synthesized at 195 Degree-Sign C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a fast microwave-assisted hydrothermal method at 80-195 Degree-Sign C with a very short reaction time of 10 min. The as-prepared ZnIn{sub 2}S{sub 4} sample can be used as visible light photocatalyst for degradation of organic dyes. Highlights: Black-Right-Pointing-Pointer ZnIn{sub 2}S{sub 4} microspheres were synthesized by microwave-assisted hydrothermal method. Black-Right-Pointing-Pointer The crystal structure and optical property of the products were almost the same. Black-Right-Pointing-Pointer Increment of the temperature renders high surface area due to the bubbling effect. Black-Right-Pointing-Pointer The ZnIn{sub 2}S{sub 4} synthesized at 195 Degree-Sign C shows the best visible catalytic activity for MO.« less

Screening of TiO2 and Au nanoparticles in cosmetics and determination of elemental impurities by multiple techniques (DLS, SP-ICP-MS, ICP-MS and ICP-OES).

PubMed

de la Calle, Inmaculada; Menta, Mathieu; Klein, Marlène; Séby, Fabienne

2017-08-15

Cosmetics are part of the daily life of most of the people. Thus, a complete characterization of the products we applied in our skin is necessary. In this work, an analytical investigation of a wide variety of cosmetics from the point of view of total element content and metallic nanoparticles (NPs) has been performed. Firstly, we analyzed the total element content by ICP-MS and ICP-OES after acid digestion as an assessment of the presence of metal impurities. Prohibited elements in cosmetics, according to the European Commission regulation No 1223/2009, were not detected, and only elements mentioned in the label were found (e.g. Al, Fe, Ti and Si). Secondly, a screening of the presence of NPs has been performed by Dynamic Light Scattering (DLS) and Single Particle Inductively-Coupled Plasma Mass Spectrometry (SP-ICP-MS). Two sample preparation procedures were applied. The first protocol consisted in the preparation of suspensions in 0.1% w/v SDS and the second based on defatting with hexane followed by resuspension in water. DLS was employed as a routine method for a fast analysis of NPs, but this technique showed limitations due to the lack of specificity. SP-ICP-MS analyses were then performed, first as a screening technique to evaluate the presence of TiO 2 and Au NPs in cosmetics suspensions prepared in SDS; and second, when a positive answer was obtained about the presence of NPs from the screening, SP-ICP-MS was used for particle size determination. Results showed that only TiO 2 NPs were present in two sunscreens, one anti-wrinkle day cream, one lip balm protector labeled as 'nano' and in one brand of toothpaste not labeled as 'nano'. Sizes obtained for both sample preparations were compared and ranged from 30 to 120nm in most of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Matrix-assisted laser desorption-ionization time-of-flight mass spectrometry in the subunit stoichiometry study of high-mass non-covalent complexes

NASA Astrophysics Data System (ADS)

Moniatte, M.; Lesieur, C.; Vecsey-Semjen, B.; Buckley, J. T.; Pattus, F.; van der Goot, F. G.; van Dorsselaer, A.

1997-12-01

This study explores the potential of MALDI-TOF MS for the mass measurement of large non-covalent protein complexes. The following non-covalent complexes have been investigated: aerolysin from Aeromonas hydrophila (335 kDa) and [alpha]-haemolysin from Staphylococcus aureus (233 kDa) which are both cytolytic toxins, three enzymes known to be homotetramers in solution: bovine liver catalase (235 kDa), rabbit muscle pyruvate kinase (232 kDa), yeast alcohol dehydrogenase (147 kDa) and finally a lectin, concanavalin A (102 kDa). Three different matrix preparations were systematically tested under various conditions: ferulic acid dissolved in THF, 2,6-dihydroxyacetophenone in 20 mM aqueous ammonium citrate and a two-step sample preparation with sinapinic acid. It was possible to find a suitable combination of matrix and preparation type which allowed the molecularity of all complexes tested to be deduced from the MALDI mass spectrum. Trimeric and tetrameric intermediates accumulating during the formation of the active heptameric aerolysin complex were also identified, this allowing a formation mechanism to be proposed. The observation of large specific non-covalent complexes has been found to be dependent on the choice of matrix, the type of sample preparation used, the solvent evaporation speed, the pH of the resulting matrix-sample mixture and the number of shots acquired on a given area. From this set of experiments, some useful guidelines for the observation of large complexes by MALDI could therefore be deduced. Fast evaporation of the solvent is particularly necessary in the case of pH sensitive complexes. An ESMS study on the same non-covalent complexes indicated that, rather surprisingly, reliable results could be obtained by MALDI-TOF MS on several very large complexes (above 200 kDa) for which ESMS yielded no clear spectra.

"Two-dimensional" molecularly imprinted solid-phase extraction coupled with crystallization and high performance liquid chromatography for fast semi-preparative purification of tannins from pomegranate husk extract.

PubMed

Sun, Guangying; Liu, Yanfang; Ahat, Hasanjan; Shen, Aijin; Liang, Xinmiao; Xue, Xingya; Luo, Yuqin; Yang, Jian; Liu, Zhao-Sheng; Aisa, Haji Akber

2017-07-07

In this study, "two dimensional" molecularly imprinted solid-phase extraction (2D-MIP-SPE) of semi-preparative grade was constructed to fast purify ellagitannins in pomegranate husk extract with the help of crystallization and reverse-phase liquid chromatgoraphy (RPLC). Ellagic acid and punicalagin imprinted polymers were synthesized in batch mode and two semi-preparative MIP-SPE columns were individually packed. After investigaing "functional complementation", 2D-MIP-SPE was constructed using ellagic acid MIP and punicalagin MIP-SPE as the first and second dimension, respectively. Then, pomegranate husk extract was fast divided into four fractions individually enriching in ellagic acid, granatin A, punicalagin and ellagic acid glucoside by 2D-MIP-SPE. With the aid of crystallization and RPLC, ellagic acid (13.5mg) and punicalagin (53.4mg) were fast obtained in 30min. Ellagic acid glucoside was purified to the purity near 100% with a recovery of 86.1%. Granatin A (92%) was directly obtained by 2D-MIP-SPE with the recovery of 81.8%. All above indicated that 2D-MIP-SPE was highly efficient in natural product purification. The concept of "functional complementation" was expected to be a useful tool in the construction of 2D-MIP-SPE. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2018-02-12

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

Remarkable photo-catalytic degradation of malachite green by nickel doped bismuth selenide under visible light irradiation

NASA Astrophysics Data System (ADS)

Kulsi, Chiranjit; Ghosh, Amrita; Mondal, Anup; Kargupta, Kajari; Ganguly, Saibal; Banerjee, Dipali

2017-01-01

Bismuth selenide (Bi2Se3) and nickel (Ni) doped Bi2Se3 were prepared by a solvothermal approach to explore the photo-catalytic performance of the materials in degradation of malachite green (MG). The presence of nickel was confirmed by X-ray photoelectron spectroscopy (XPS) measurement in doped Bi2Se3. The results showed that the nickel doping played an important role in microstructure and photo-catalytic activity of the samples. Nickel doped Bi2Se3 sample exhibited higher photo-catalytic activity than that of the pure Bi2Se3 sample under visible-light irradiation. The photo-catalytic degradation followed first-order reaction kinetics. Fast degradation kinetics and complete (100% in 5 min of visible light irradiation) removal of MG was achieved by nickel doped Bi2Se3 in presence of hydrogen peroxide (H2O2) due to modification of band gap energies leading to suppression of photo-generated electron-hole recombination.

Recrystallization texture in nickel heavily deformed by accumulative roll bonding

NASA Astrophysics Data System (ADS)

Mishin, O. V.; Zhang, Y. B.; Godfrey, A.

2017-07-01

The recrystallization behavior of Ni processed by accumulative roll bonding to a total accumulated von Mises strain of 4.8 has been examined, and analyzed with respect to heterogeneity in the deformation microstructure. The regions near the bonding interface are found to be more refined and contain particle deformation zones around fragments of the steel wire brush used to prepare the surface for bonding. Sample-scale gradients are also observed, manifested as differences between the subsurface, intermediate and central layers, where the distributions of texture components are different. These heterogeneities affect the progress of recrystallization. While the subsurface and near-interface regions typically contain lower frequencies of cube-oriented grains than anywhere else in the sample, a strong cube texture forms in the sample during recrystallization, attributed to both a high nucleation rate and fast growth rate of cube-oriented grains. The observations highlight the sensitivity of recrystallization to heterogeneity in the deformation microstructure and demonstrate the importance of characterizing this heterogeneity over several length scales.

Free-breathing black-blood CINE fast-spin echo imaging for measuring abdominal aortic wall distensibility: a feasibility study

NASA Astrophysics Data System (ADS)

Lin, Jyh-Miin; Patterson, Andrew J.; Chao, Tzu-Cheng; Zhu, Chengcheng; Chang, Hing-Chiu; Mendes, Jason; Chung, Hsiao-Wen; Gillard, Jonathan H.; Graves, Martin J.

2017-05-01

The paper reports a free-breathing black-blood CINE fast-spin echo (FSE) technique for measuring abdominal aortic wall motion. The free-breathing CINE FSE includes the following MR techniques: (1) variable-density sampling with fast iterative reconstruction; (2) inner-volume imaging; and (3) a blood-suppression preparation pulse. The proposed technique was evaluated in eight healthy subjects. The inner-volume imaging significantly reduced the intraluminal artifacts of respiratory motion (p  =  0.015). The quantitative measurements were a diameter of 16.3  ±  2.8 mm and wall distensibility of 2.0  ±  0.4 mm (12.5  ±  3.4%) and 0.7  ±  0.3 mm (4.1  ±  1.0%) for the anterior and posterior walls, respectively. The cyclic cross-sectional distensibility was 35  ±  15% greater in the systolic phase than in the diastolic phase. In conclusion, we developed a feasible CINE FSE method to measure the motion of the abdominal aortic wall, which will enable clinical scientists to study the elasticity of the abdominal aorta.

Effects of Ramadan upon fluid and food intake, fatigue, and physical, mental, and social activities: a comparison between the UK and Libya.

PubMed

Waterhouse, Jim; Alkib, Lotfia; Reilly, Thomas

2008-09-01

Two studies were performed during Ramadan, one in the UK (N=31) and the other in Libya (N=33). The aims were to assess some changes to lifestyle that are produced by fasting as well as effects due to culture. Subjects were studied on eight separate occasions: four control days (two before and two after Ramadan) and four days during the four weeks of Ramadan itself. A questionnaire was answered that asked about naps and fluid and food intake. The questions elicited if an individual had slept, drank, or eaten, plus the reasons for doing or not doing so. Also, subjects were asked to describe their physical, mental, and social activities, their fatigue, and their perceived abilities to perform physical or mental work. The questionnaire was answered five times per day: at sunrise, at 10:00 h, at 14:00 h, at sunset, and on retiring to sleep at night. Urine samples were collected at sunset and measured for osmolality. Differences between control and Ramadan days, as well as between subjects studied in UK and Libya, were assessed by analysis of variance. Correlations between fatigue and physical, mental, and social activities were also assessed, as were differences in urine osmolality. Fasting during Ramadan resulted in fewer activities and increased fatigue and frequency of napping during daytime. Changes in fluid and food intake indicated some degree of preparation for fasting before sunrise and a marked "recuperation" from fasting after sunset. The reasons given for napping in the daytime, for drinking or not drinking, and for eating or not eating, changed during Ramadan compared with control days; as a result, links between fatigue and activities, and fatigue and fluid and food intake, were all altered during Ramadan, particularly after sunset. Subjects become dehydrated during the daytime, but this was not reduced when females who were menstruating drank during this time. Several differences between the two studies were found. There was a greater frequency of napping during the daytime in the Libya study, and evidence for the conservation of energy during the daytime and reduced physical, mental, and social activities. Subjects' preparations for fasting and recovering from it--their fluid and food intakes and associated reasons for these--also differed. Possible explanations of these differences are discussed.

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

Kasliwal, M. M.; Kulkarni, S. R.; Ofek, E. O.

We present photometric and spectroscopic follow-up of a sample of extragalactic novae discovered by the Palomar 60 inch telescope during a search for 'Fast Transients In Nearest Galaxies' (P60-FasTING). Designed as a fast cadence (1 day) and deep (g < 21 mag) survey, P60-FasTING was particularly sensitive to short-lived and faint optical transients. The P60-FasTING nova sample includes 10 novae in M 31, 6 in M 81, 3 in M 82, 1 in NGC 2403, and 1 in NGC 891. This significantly expands the known sample of extragalactic novae beyond the Local Group, including the first discoveries in a starburstmore » environment. Surprisingly, our photometry shows that this sample is quite inconsistent with the canonical maximum-magnitude-rate-of-decline (MMRD) relation for classical novae. Furthermore, the spectra of the P60-FasTING sample are indistinguishable from classical novae. We suggest that we have uncovered a sub-class of faint and fast classical novae in a new phase space in luminosity-timescale of optical transients. Thus, novae span two orders of magnitude in both luminosity and time. Perhaps the MMRD, which is characterized only by the white dwarf mass, was an oversimplification. Nova physics appears to be characterized by a relatively rich four-dimensional parameter space in white dwarf mass, temperature, composition, and accretion rate.« less

Surface enhanced Raman spectroscopy (SERS) from a molecule adsorbed on a nanoscale silver particle cluster in a holographic plate

NASA Astrophysics Data System (ADS)

Jusinski, Leonard E.; Bahuguna, Ramen; Das, Amrita; Arya, Karamjeet

2006-02-01

Surface enhanced Raman spectroscopy has become a viable technique for the detection of single molecules. This highly sensitive technique is due to the very large (up to 14 orders in magnitude) enhancement in the Raman cross section when the molecule is adsorbed on a metal nanoparticle cluster. We report here SERS (Surface Enhanced Raman Spectroscopy) experiments performed by adsorbing analyte molecules on nanoscale silver particle clusters within the gelatin layer of commercially available holographic plates which have been developed and fixed. The Ag particles range in size between 5 - 30 nanometers (nm). Sample preparation was performed by immersing the prepared holographic plate in an analyte solution for a few minutes. We report here the production of SERS signals from Rhodamine 6G (R6G) molecules of nanomolar concentration. These measurements demonstrate a fast, low cost, reproducible technique of producing SERS substrates in a matter of minutes compared to the conventional procedure of preparing Ag clusters from colloidal solutions. SERS active colloidal solutions require up to a full day to prepare. In addition, the preparations of colloidal aggregates are not consistent in shape, contain additional interfering chemicals, and do not generate consistent SERS enhancement. Colloidal solutions require the addition of KCl or NaCl to increase the ionic strength to allow aggregation and cluster formation. We find no need to add KCl or NaCl to create SERS active clusters in the holographic gelatin matrix. These holographic plates, prepared using simple, conventional procedures, can be stored in an inert environment and preserve SERS activity after several weeks subsequent to preparation.

Experimental and analytical variation in human urine in 1H NMR spectroscopy-based metabolic phenotyping studies.

PubMed

Maher, Anthony D; Zirah, Séverine F M; Holmes, Elaine; Nicholson, Jeremy K

2007-07-15

1H NMR spectroscopy potentially provides a robust approach for high-throughput metabolic screening of biofluids such as urine and plasma, but sample handling and preparation need careful optimization to ensure that spectra accurately report biological status or disease state. We have investigated the effects of storage temperature and time on the 1H NMR spectral profiles of human urine from two participants, collected three times a day on four different days. These were analyzed using modern chemometric methods. Analytical and preparation variation (tested between -40 degrees C and room temperature) and time of storage (to 24 h) were found to be much less influential than biological variation in sample classification. Statistical total correlation spectroscopy and discriminant function methods were used to identify the specific metabolites that were hypervariable due to preparation and biology. Significant intraindividual variation in metabolite profiles were observed even for urine collected on the same day and after at least 6 h fasting. The effect of long-term storage at different temperatures was also investigated, showing urine is stable if frozen for at least 3 months and that storage at room temperature for long periods (1-3 months) results in a metabolic profile explained by bacterial activity. Presampling (e.g., previous day) intake of food and medicine can also strongly influence the urinary metabolic profiles indicating that collective detailed participant historical meta data are important for interpretation of metabolic phenotypes and for avoiding false biomarker discovery.

Fabrication of a Novel Highly Sensitive and Selective Immunosensor for Botulinum Neurotoxin Serotype A Based on an Effective Platform of Electrosynthesized Gold Nanodendrites/Chitosan Nanoparticles.

PubMed

Sorouri, Rahim; Bagheri, Hasan; Afkhami, Abbas; Salimian, Jafar

2017-05-09

In this work, a novel nanocomposite consisting of electrosynthesized gold nanodendrites and chitosan nanoparticles (AuNDs/CSNPs) has been prepared to fabricate an impedimetric immunosensor based on a screen printed carbon electrode (SPCE) for the rapid and sensitive immunoassay of botulinum neurotoxin A (BoNT/A). BoNT/A polyclonal antibody was immobilized on the nanocomposite-modified SPCE for the signal amplification. The structure of the prepared nanocomposite was investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The charge transfer resistance (R CT ) changes were used to detect BoNT/A as the specific immuno-interactions at the immunosensor surface that efficiently limited the electron transfer of Fe(CN)₆ 3-/4- as a redox probe at pH = 7.4. A linear relationship was observed between the %∆ R CT and the concentration logarithm of BoNT/A within the range of 0.2 to 230 pg·mL -1 with a detection limit (S/N = 3) of 0.15 pg·mL -1 . The practical applicability of the proposed sensor was examined by evaluating the detection of BoNT/A in milk and serum samples with satisfactory recoveries. Therefore, the prepared immunosensor holds great promise for the fast, simple and sensitive detection of BoNT/A in various real samples.

Fabrication of a Novel Highly Sensitive and Selective Immunosensor for Botulinum Neurotoxin Serotype A Based on an Effective Platform of Electrosynthesized Gold Nanodendrites/Chitosan Nanoparticles

PubMed Central

Sorouri, Rahim; Bagheri, Hasan; Afkhami, Abbas; Salimian, Jafar

2017-01-01

In this work, a novel nanocomposite consisting of electrosynthesized gold nanodendrites and chitosan nanoparticles (AuNDs/CSNPs) has been prepared to fabricate an impedimetric immunosensor based on a screen printed carbon electrode (SPCE) for the rapid and sensitive immunoassay of botulinum neurotoxin A (BoNT/A). BoNT/A polyclonal antibody was immobilized on the nanocomposite-modified SPCE for the signal amplification. The structure of the prepared nanocomposite was investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The charge transfer resistance (RCT) changes were used to detect BoNT/A as the specific immuno-interactions at the immunosensor surface that efficiently limited the electron transfer of Fe(CN)63−/4− as a redox probe at pH = 7.4. A linear relationship was observed between the %∆RCT and the concentration logarithm of BoNT/A within the range of 0.2 to 230 pg·mL−1 with a detection limit (S/N = 3) of 0.15 pg·mL−1. The practical applicability of the proposed sensor was examined by evaluating the detection of BoNT/A in milk and serum samples with satisfactory recoveries. Therefore, the prepared immunosensor holds great promise for the fast, simple and sensitive detection of BoNT/A in various real samples. PMID:28486408

Single-hole hollow molecularly imprinted polymer embedded carbon dot for fast detection of tetracycline in honey.

PubMed

Li, Huiyu; Zhao, Li; Xu, Yuan; Zhou, Tianyu; Liu, Haochi; Huang, Ning; Ding, Jie; Li, Yi; Ding, Lan

2018-08-01

It is difficult to detect tetracycline (TC) in honey sample by using carbon dots (CDs) because the autofluorescence of the matrix of honey sample overlaps with the fluorescence emission spectrum of the large majority of CDs. Herein, single-hole hollow molecularly imprinted polymers embedded carbon dots (HMIP@CD) was prepared via microwave-assisted method. TC in diluted honey sample was adsorbed by the HMIP@CD within 3 min, after which the HMIP@CD absorbed with TC was separated by centrifugation from honey sample and redispersed into phosphate buffer solution. The autofluorescence of honey that interferes with the fluorescence signal of HMIP@CD was avoided. The method exhibited an excellent linearity within 10-200 μg L -1 and a low detection limit of 3.1 μg L -1 . At three spiking levels of TC, the recoveries ranged from 93% to 105% with precisions below 1.6%. This method provides an effective strategy for detecting analyte in complex matrix with autofluorescence interference. Copyright © 2018. Published by Elsevier B.V.

Disposable pipette extraction for gas chromatographic determination of codeine, morphine, and 6-monoacetylmorphine in vitreous humor.

PubMed

Kovatsi, Leda; Rentifis, Konstantinos; Giannakis, Dimitrios; Njau, Samuel; Samanidou, Victoria

2011-07-01

The availability of a sensitive and rapid analytical method for the determination of opiates, and other substances of forensic interest, in a variety of biological specimens is of utmost importance to forensic laboratories. Solid-phase extraction is very popular in the pre-treatment of forensic samples. Nevertheless, a new approach, disposable pipette extraction (DPX), is gaining increasing interest in sample preparation. DPX has already been applied to the analysis of drugs of abuse in common biological matrices, such as urine and blood, but has not yet been evaluated on alternative biological samples, such as vitreous humor. The objective of this study was to evaluate the applicability of DPX on the analysis of opiates in vitreous humor. The currently developed method is fast, reliable, and easy to perform. The sensitivity, precision, and accuracy are satisfactory. Recoveries obtained are within the range of 72-91%, whereas the sample volume of vitreous humor required is only 100 μL. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Note: A fast pneumatic sample-shuttle with attenuated shocks

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

Biancalana, Valerio; Dancheva, Yordanka; Stiaccini, Leonardo

2014-03-15

We describe a home-built pneumatic shuttle suitable for the fast displacement of samples in the vicinity of a highly sensitive atomic magnetometer. The samples are magnetized at 1 T using a Halbach assembly of magnets. The device enables the remote detection of free-induction-decay in ultra-low-field and zero-field nuclear magnetic resonance (NMR) experiments, in relaxometric measurements and in other applications involving the displacement of magnetized samples within time intervals as short as a few tens of milliseconds. Other possible applications of fast sample shuttling exist in radiological studies, where samples have to be irradiated and then analyzed in a cold environment.

Quantitation of sugar content in pyrolysis liquids after acid hydrolysis using high-performance liquid chromatography without neutralization.

PubMed

Johnston, Patrick A; Brown, Robert C

2014-08-13

A rapid method for the quantitation of total sugars in pyrolysis liquids using high-performance liquid chromatography (HPLC) was developed. The method avoids the tedious and time-consuming sample preparation required by current analytical methods. It is possible to directly analyze hydrolyzed pyrolysis liquids, bypassing the neutralization step usually required in determination of total sugars. A comparison with traditional methods was used to determine the validity of the results. The calibration curve coefficient of determination on all standard compounds was >0.999 using a refractive index detector. The relative standard deviation for the new method was 1.13%. The spiked sugar recoveries on the pyrolysis liquid samples were between 104 and 105%. The research demonstrates that it is possible to obtain excellent accuracy and efficiency using HPLC to quantitate glucose after acid hydrolysis of polymeric and oligomeric sugars found in fast pyrolysis bio-oils without neutralization.

Immunoanalysis Methods for the Detection of Dioxins and Related Chemicals

PubMed Central

Tian, Wenjing; Xie, Heidi Qunhui; Fu, Hualing; Pei, Xinhui; Zhao, Bin

2012-01-01

With the development of biotechnology, approaches based on antibodies, such as enzyme-linked immunosorbent assay (ELISA), active aryl hydrocarbon immunoassay (Ah-I) and other multi-analyte immunoassays, have been utilized as alternatives to the conventional techniques based on gas chromatography and mass spectroscopy for the analysis of dioxin and dioxin-like compounds in environmental and biological samples. These screening methods have been verified as rapid, simple and cost-effective. This paper provides an overview on the development and application of antibody-based approaches, such as ELISA, Ah-I, and multi-analyte immunoassays, covering the sample extraction and cleanup, antigen design, antibody preparation and immunoanalysis. However, in order to meet the requirements for on-site fast detection and relative quantification of dioxins in the environment, further optimization is needed to make these immuno-analytical methods more sensitive and easy to use. PMID:23443395

Tissue diagnosis by means of endogenous fluorophores

NASA Astrophysics Data System (ADS)

Lohmann, Wolfgang; Dreyer, Thomas; Nilles, M.; Bohle, Rainer M.; Schill, Wolf-Bernhard; Glanz, Hiltrud; Fryen, Andreas; Horn, Gisela; Pollich, Beate

1995-01-01

In vitro or in situ single spot or area excitation of human tissue with either 337 nm or 365 nm results in a fluorescence spectrum at about 470 nm. Since in most tissue samples the spectra obtained look alike and differ in intensity only, the 2D tomographical distribution of the fluorescence intensity was also investigated. It could be shown that the fluorescence images of unfixed and unstained cryosections match the histological images (HE stained cryosections). They exhibit a fluorescence pattern unique for the different types of diseases investigated (basalioma, melanoma, nevi, psoriasis, seborrheic keratosis). Additional information can be obtained by elastica van Gieson stained images and by illuminating the HE stained cryosections with 365 nm. Since the cryosections can be prepared and evaluated in less than 5 minutes, this technique might be used as a fast cut technique for determining e.g. the diagnosis of a biopsy sample, also during surgery.

Leaf Protein and Mineral Concentrations across the “Miracle Tree” Genus Moringa

PubMed Central

Sankaran, Renuka P.; Fahey, Jed W.; Grusak, Michael A.; Odee, David; Nouman, Wasif

2016-01-01

The moringa tree Moringa oleifera is a fast-growing, drought-resistant tree cultivated across the lowland dry tropics worldwide for its nutritious leaves. Despite its nutritious reputation, there has been no systematic survey of the variation in leaf nutritional quality across M. oleifera grown worldwide, or of the other species of the genus. To guide informed use of moringa, we surveyed protein, macro-, and micro- nutrients across 67 common garden samples of 12 Moringa taxa, including 23 samples of M. oleifera. Moringa oleifera, M. concanensis, M. stenopetala, an M. concanensis X oleifera hybrid, and M. longituba were highest in protein, with M. ruspoliana having the highest calcium levels. A protein-dry leaf mass tradeoff may preclude certain breeding possibilities, e.g. maximally high protein with large leaflets. These findings identify clear priorities and limitations for improved moringa varieties with traits such as high protein, calcium, or ease of preparation. PMID:27459315

Leaf Protein and Mineral Concentrations across the "Miracle Tree" Genus Moringa.

PubMed

Olson, Mark E; Sankaran, Renuka P; Fahey, Jed W; Grusak, Michael A; Odee, David; Nouman, Wasif

2016-01-01

The moringa tree Moringa oleifera is a fast-growing, drought-resistant tree cultivated across the lowland dry tropics worldwide for its nutritious leaves. Despite its nutritious reputation, there has been no systematic survey of the variation in leaf nutritional quality across M. oleifera grown worldwide, or of the other species of the genus. To guide informed use of moringa, we surveyed protein, macro-, and micro- nutrients across 67 common garden samples of 12 Moringa taxa, including 23 samples of M. oleifera. Moringa oleifera, M. concanensis, M. stenopetala, an M. concanensis X oleifera hybrid, and M. longituba were highest in protein, with M. ruspoliana having the highest calcium levels. A protein-dry leaf mass tradeoff may preclude certain breeding possibilities, e.g. maximally high protein with large leaflets. These findings identify clear priorities and limitations for improved moringa varieties with traits such as high protein, calcium, or ease of preparation.

Centrifugal sedimentation immunoassays for multiplexed detection of enteric bacteria in ground water

PubMed Central

Litvinov, Julia; Moen, Scott T.; Koh, Chung-Yan; Singh, Anup K.

2016-01-01

Waterborne pathogens pose significant threat to the global population and early detection plays an important role both in making drinking water safe, as well as in diagnostics and treatment of water-borne diseases. We present an innovative centrifugal sedimentation immunoassay platform for detection of bacterial pathogens in water. Our approach is based on binding of pathogens to antibody-functionalized capture particles followed by sedimentation of the particles through a density-media in a microfluidic disk. Beads at the distal end of the disk are imaged to quantify the fluorescence and determine the bacterial concentration. Our platform is fast (20 min), can detect as few as ∼10 bacteria with minimal sample preparation, and can detect multiple pathogens simultaneously. The platform was used to detect a panel of enteric bacteria (Escherichia coli, Salmonella typhimurium, Shigella, Listeria, and Campylobacter) spiked in tap and ground water samples. PMID:26858815

Determination of traces of cobalt in soils: A field method

USGS Publications Warehouse

Almond, H.

1953-01-01

The growing use of geochemical prospecting methods in the search for ore deposits has led to the development of a field method for the determination of cobalt in soils. The determination is based on the fact that cobalt reacts with 2-nitroso-1-naphthol to yield a pink compound that is soluble in carbon tetrachloride. The carbon tetrachloride extract is shaken with dilute cyanide to complex interfering elements and to remove excess reagent. The cobalt content is estimated by comparing the pink color in the carbon tetrachloride with a standard series prepared from standard solutions. The cobalt 2-nitroso-1-naphtholate system in carbon tetrachloride follows Beer's law. As little as 1 p.p.m. can be determined in a 0.1-gram sample. The method is simple and fast and requires only simple equipment. More than 40 samples can be analyzed per man-day with an accuracy within 30% or better.

Gearing up for Fast Grading and Reporting

ERIC Educational Resources Information Center

O'Connor, Ken; Jung, Lee Ann; Reeves, Douglas

2018-01-01

The authors posit that the traditional grading system involving points and percentages is not the best way to prepare students to be the self-directed, independent learners they need to be. A better system would produce grades that are FAST (fair, accurate, specific, timely). To bring about these changes, school leaders need not create full…

Is "Teach for All" Knocking on Your Door?

ERIC Educational Resources Information Center

Price, Anne; McConney, Andrew

2013-01-01

Over the past few decades there has been a rapid expansion in alternative "fast track" routes for teacher preparation. Among the most aggressive of these are Teach for All (TFA) schemes characterized not only by their ultra fast entry to teaching (6-7 week course) but also by their underlying philosophy that the so called…

A Hunger Strike on Campus

ERIC Educational Resources Information Center

Dawson, John B.

1970-01-01

This article describes a recent student fast" that occurred on the Stony Brook campus as a peaceful means of protest against Department of Defense research. The purpose of this report is to generate discussion and to stimulate preparation for dealing with similar fasts", since they are likely to occur on other campuses in the foreseeable future.…

Development and quality evaluation of quick cooking dhal-A convenience product.

PubMed

Sethi, Shruti; Samuel, D V K; Khan, Islam

2014-03-01

Owing to rapid urbanization and more women joining the workforce, use of ready-to-eat and ready-to-use convenience foods is gaining increasing popularity. Women require dhal that cooks fast and increases in volume when cooked. In an attempt to prepare quick cooking dhal from pigeon pea, variety UPAS 120 was milled, pre-treated with sodium chloride solution (1%), flaked and dried. The quick cooking dhal was packed in three packaging materials, namely, high molecular weight high density polyethylene (HMHDPE), high density polyethylene (HDPE) and laminated pouches. The quality evaluation of the prepared flakes with respect to the cooking quality attributes, changes in proximate composition, free fatty acid (FFA) and peroxide value (PV) were carried out during storage at ambient temperature (8-36°C) at regular intervals for a period of 10 months. During storage, quick cooking dhal packed in laminated pouches performed better than samples stored in other pouches with respect to the changes in the overall quality and acceptability of the product.

Detection and quantitation of Kaposi's sarcoma-associated herpesvirus (KSHV) by a single competitive-quantitative polymerase chain reaction.

PubMed

Curreli, Francesca; Robles, Monica A; Friedman-Kien, Alvin E; Flore, Ornella

2003-02-01

Kaposi's sarcoma-associated herpesvirus is a novel herpesvirus linked to AIDS-related neoplasms. Currently it is difficult to evaluate the number of virions in viral preparation or in samples obtained from patients with Kaposi's sarcoma (KS), since no protocol for determining the plaque forming units of KSHV exists. We constructed a fragment of a different size than the target viral DNA to carry out a competitive-quantitative PCR. Both fragment and viral DNA were added to a single PCR reaction to compete for the same set of primers. By knowing the amount of the competitor added to the reaction, we could determine the number of viral DNA molecules. We used this assay successfully to detect and quantify KSHV genomes from KS skin biopsies and pleural effusion lymphoma, and from different viral preparations. To date, this is the most convenient and economic method that allows an accurate and fast viral detection/quantitation with a single PCR.

Ultrasonic analysis to discriminate bread dough of different types of flour

NASA Astrophysics Data System (ADS)

García-Álvarez, J.; Rosell, C. M.; García-Hernández, M. J.; Chávez, J. A.; Turó, A.; Salazar, J.

2012-12-01

Many varieties of bread are prepared using flour coming from wheat. However, there are other types of flours milled from rice, legumes and some fruits and vegetables that are also suitable for baking purposes, used alone or in combination with wheat flour. The type of flour employed strongly influences the dough consistency, which is a relevant property for determining the dough potential for breadmaking purposes. Traditional methods for dough testing are relatively expensive, time-consuming, off-line and often require skilled operators. In this work, ultrasonic analysis are performed in order to obtain acoustic properties of bread dough samples prepared using two different types of flour, wheat flour and rice flour. The dough acoustic properties can be related to its viscoelastic characteristics, which in turn determine the dough feasibility for baking. The main advantages of the ultrasonic dough testing can be, among others, its low cost, fast, hygienic and on-line performance. The obtained results point out the potential of the ultrasonic analysis to discriminate doughs of different types of flour.

Quality control of plant food supplements.

PubMed

Sanzini, Elisabetta; Badea, Mihaela; Santos, Ariana Dos; Restani, Patrizia; Sievers, Hartwig

2011-12-01

It is essential to guarantee the safety of unprocessed plants and food supplements if consumers' health is to be protected. Although botanicals and their preparations are regulated at EU level, at least in part, there is still considerable discretion at national level, and Member States may choose to classify a product either as a food supplement or as a drug. Accurate data concerning the finished products and the plant used as the starting point are of major importance if risks and safety are to be properly assessed, but in addition standardized criteria for herbal preparation must be laid down and respected by researchers and manufacturers. Physiologically active as well as potentially toxic constituents need to be identified, and suitable analytical methods for their measurement specified, particularly in view of the increasing incidence of economically motivated adulteration of herbal raw materials and extracts. It remains the duty of food operators to keep up with the scientific literature and to provide sufficient information to enable the adaptation of specifications, sampling schemes and analytical methods to a fast-changing environment.

Defect engineering of two-dimensional WO3 nanosheets for enhanced electrochromism and photoeletrochemical performance

NASA Astrophysics Data System (ADS)

Zhou, Xiaofang; Zheng, Xiaoli; Yan, Bo; Xu, Tao; Xu, Qun

2017-04-01

The capability of introduction of oxygen vacancies in a controlled way has emerged as the heart of modern transition metal oxide semiconductor chemistry. As chemical defects, the oxygen vacancies have been proposed as electron donors, which are prone to increase carrier density and promote charge carrier separation. Herein, we have successfully prepared 2D WO3 ultrathin nanosheets with abundant surface oxygen vacancies by a combination of facile solvothermal reaction and hydrogenation method. The resultant hydrogenated WO3 ultrathin nanosheets exhibit remarkable electrochromism and photocatalytic performances compared with the non-hydrogenated samples, mainly due to their increased oxygen vacancies, narrowed band gap coupled with fast charge transfer and enhanced adsorption of visible light.

[Various methods for the determination of preservatives in food. II. Gaschromatography, high performance liquid chromatography, TAS-method (author's transl)].

PubMed

Hild, J; Gertz, C

1980-02-01

For the quantitative determination of preservatives in food, analyses were carried out by means of GLC, HPLC, and TLC according to the TAS-method. Using the alkaline extract (sample preparation see part I) the preservatives can be analysed as free acid or appropriate ester out the same GLC-column without any interference from coextractives. A fast and accurate HPLC determination can be achieved by direct injection of the alkaline extract. All preservatives were well separated and detected at a wavelength of 225 resp. 232 nm. As a quick test for the qualitative estimation the TLC (TAS) method is suggested and a suitable solvent system is proposed.

Application of blood cadmium determination to industry using a punched disc technique.

PubMed Central

Cernik, A A; Sayers, M P

1975-01-01

A paper disc flameless atomic absorption spectroscopy (AAS) method is described for the determination of cadmium (Cd) in blood, enabling difficulties in sample preparation to be minimized. By control of the ashing step the matrix can be removed without loss of cadmium. Problems with the fast signal response during atomization can be met by spectral band width and temperature control. At the 106 pg level (471 nmol Cd/1 blood; 5-3 mug/100 ml) the relative standard deviation (RSD) was 0-06. Results in four industrial situations are reported. This description of the method should facilitate further investigation of its application to industry using capillary or venous blood. PMID:1131342

Characterization of anti-theft devices directly from the surface of banknotes via easy ambient sonic spray ionization mass spectrometry.

PubMed

Schmidt, Eduardo Morgado; Franco, Marcos Fernando; Cuelbas, Claudio José; Zacca, Jorge Jardim; de Carvalho Rocha, Werickson Fortunato; Borges, Rodrigo; de Souza, Wanderley; Sawaya, Alexandra Christine Helena Frankland; Eberlin, Marcos Nogueira; Correa, Deleon Nascimento

2015-09-01

Using Brazilian banknotes as a test case, forensic examination and identification of Rhodamine B dye anti-theft device (ATD) staining on banknotes were performed. Easy ambient sonic spray ionization mass spectrometry (EASI-MS) was used since it allows fast and simple analysis with no sample preparation providing molecular screening of the surface with direct desorption and ionization of the security dye. For a more accurate molecular characterization of the ATD dye, Q Exactive Orbitrap™ Fourier transform (tandem) mass spectrometry using eletrospray ionization (ESI-HRMS/MS) was also applied. Copyright © 2015 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

Preparation of inulin-type fructooligosaccharides using fast protein liquid chromatography coupled with refractive index detection.

PubMed

Li, J; Cheong, K L; Zhao, J; Hu, D J; Chen, X Q; Qiao, C F; Zhang, Q W; Chen, Y W; Li, S P

2013-09-20

A fast protein liquid chromatography coupled with refractive index detection (FPLC-RID) method was firstly developed for preparation and purification of fructooligosaccharides with different degree of polymerization from burdock, Arctium lappa. After extraction with 60% ethanol and decolorization with MCI gel CHP20P, total fructooligosaccharides were purified on Bio-Gel P-2 column eluted with water at the flow rate of 0.3 ml/min, which was the optimized conditions. The obtained fructooligosaccharides with degree of polymerization of 3-9 were identified based on their methylation analysis, MS and NMR data. This method has the advantages of high automation, good recovery and easy performance, which could be used for preparation of FOS from other sources, as well as other targeted compounds without UV absorbance. Copyright © 2013 Elsevier B.V. All rights reserved.

Food safety concerns of fast food consumers in urban Ghana.

PubMed

Omari, Rose; Frempong, Godfred

2016-03-01

In Ghana, out-of-home ready-to-eat foods including fast food generally have been associated with food safety problems. Notwithstanding, fast food production and consumption are increasing in Ghana and therefore this study sought to determine the food safety issues of importance to consumers and the extent to which they worry about them. First, through three focus group discussions on consumers' personal opinions about food safety issues, some emergent themes were obtained, which were used to construct an open-ended questionnaire administered face-to-face to 425 respondents systematically sampled from 20 fast food restaurants in Accra. Findings showed that most fast food consumers were concerned about food hazards such as pesticide residue in vegetables, excessive use of artificial flavour enhancers and colouring substances, bacterial contamination, migrated harmful substances from plastic packages, and general unhygienic conditions under which food is prepared and sold. Consumers also raised concerns about foodborne diseases such as cholera, typhoid, food poisoning, diarrhoea, bird flu and swine flu. The logistic regression model showed that being male increased the likelihood of worrying about general food safety issues and excessive use of flavour enhancers than in females while being youthful increased the likelihood of being worried about typhoid fever than in older consumers. These findings imply that consumers in urban Ghana are aware and concerned about current trends of food safety and foodborne disease challenges in the country. Therefore, efforts targeted at improving food safety and reducing incidences of foodborne diseases should not only focus on public awareness creation but should also design more comprehensive programmes to ensure the making of food safety rules and guidelines and enforcing compliance to facilitate availability and consumers' choice of safe foods. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fast generations of tree-type three-dimensional entanglement via Lewis-Riesenfeld invariants and transitionless quantum driving

PubMed Central

Wu, Jin-Lei; Ji, Xin; Zhang, Shou

2016-01-01

Recently, a novel three-dimensional entangled state called tree-type entanglement, which is likely to have applications for improving quantum communication security, was prepared via adiabatic passage by Song et al. Here we propose two schemes for fast generating tree-type three-dimensional entanglement among three spatially separated atoms via shortcuts to adiabatic passage. With the help of quantum Zeno dynamics, two kinds of different but equivalent methods, Lewis-Riesenfeld invariants and transitionless quantum driving, are applied to construct shortcuts to adiabatic passage. The comparisons between the two methods are discussed. The strict numerical simulations show that the tree-type three-dimensional entangled states can be fast prepared with quite high fidelities and the two schemes are both robust against the variations in the parameters, atomic spontaneous emissions and the cavity-fiber photon leakages. PMID:27667583

Pulse combustion reactor as a fast and scalable synthetic method for preparation of Li-ion cathode materials

NASA Astrophysics Data System (ADS)

Križan, Gregor; Križan, Janez; Dominko, Robert; Gaberšček, Miran

2017-09-01

In this work a novel pulse combustion reactor method for preparation of Li-ion cathode materials is introduced. Its advantages and potential challenges are demonstrated on two widely studied cathode materials, LiFePO4/C and Li-rich NMC. By exploiting the nature of efficiency of pulse combustion we have successfully established a slightly reductive or oxidative environment necessary for synthesis. As a whole, the proposed method is fast, environmentally friendly and easy to scale. An important advantage of the proposed method is that it preferentially yields small-sized powders (in the nanometric range) at a fast production rate of 2 s. A potential disadvantage is the relatively high degree of disorder of synthesized active material which however can be removed using a post-annealing step. This additional step allows a further tuning of materials morphology as shown and commented in some detail.

The suitability of the simplified method of the analysis of coffee infusions on the content of Ca, Cu, Fe, Mg, Mn and Zn and the study of the effect of preparation conditions on the leachability of elements into the coffee brew.

PubMed

Stelmach, Ewelina; Pohl, Pawel; Szymczycha-Madeja, Anna

2013-12-01

A fast and straightforward method of the analysis of coffee infusions was developed for measurements of total concentrations of Ca, Cu, Fe, Mg, Mn and Zn by flame atomic absorption spectrometry. Its validity was proved by the analysis of spiked samples; recoveries of added metals were found to be within 98-104% while the precision was better than 4%. The method devised was used for the analysis of re-distilled water infusions of six popular ground coffees available in the Polish market. Using the mud coffee preparation it was established that percentages of metals leached in these conditions varied a lot among analysed coffees, especially for Ca (14-42%), Mg (6-25%) and Zn (1-24%). For remaining metals, the highest extractabilities were assessed for Mn (30-52%) while the lowest for Fe (4-16%) and Cu (2-12%). In addition, it was found that the water type and the coffee brewing preparation method influence the concentration of studied metals in coffee infusions the most. Copyright © 2013 Elsevier Ltd. All rights reserved.

The impact of different DNA extraction kits and laboratories upon the assessment of human gut microbiota composition by 16S rRNA gene sequencing.

PubMed

Kennedy, Nicholas A; Walker, Alan W; Berry, Susan H; Duncan, Sylvia H; Farquarson, Freda M; Louis, Petra; Thomson, John M; Satsangi, Jack; Flint, Harry J; Parkhill, Julian; Lees, Charlie W; Hold, Georgina L

2014-01-01

Determining bacterial community structure in fecal samples through DNA sequencing is an important facet of intestinal health research. The impact of different commercially available DNA extraction kits upon bacterial community structures has received relatively little attention. The aim of this study was to analyze bacterial communities in volunteer and inflammatory bowel disease (IBD) patient fecal samples extracted using widely used DNA extraction kits in established gastrointestinal research laboratories. Fecal samples from two healthy volunteers (H3 and H4) and two relapsing IBD patients (I1 and I2) were investigated. DNA extraction was undertaken using MoBio Powersoil and MP Biomedicals FastDNA SPIN Kit for Soil DNA extraction kits. PCR amplification for pyrosequencing of bacterial 16S rRNA genes was performed in both laboratories on all samples. Hierarchical clustering of sequencing data was done using the Yue and Clayton similarity coefficient. DNA extracted using the FastDNA kit and the MoBio kit gave median DNA concentrations of 475 (interquartile range 228-561) and 22 (IQR 9-36) ng/µL respectively (p<0.0001). Hierarchical clustering of sequence data by Yue and Clayton coefficient revealed four clusters. Samples from individuals H3 and I2 clustered by patient; however, samples from patient I1 extracted with the MoBio kit clustered with samples from patient H4 rather than the other I1 samples. Linear modelling on relative abundance of common bacterial families revealed significant differences between kits; samples extracted with MoBio Powersoil showed significantly increased Bacteroidaceae, Ruminococcaceae and Porphyromonadaceae, and lower Enterobacteriaceae, Lachnospiraceae, Clostridiaceae, and Erysipelotrichaceae (p<0.05). This study demonstrates significant differences in DNA yield and bacterial DNA composition when comparing DNA extracted from the same fecal sample with different extraction kits. This highlights the importance of ensuring that samples in a study are prepared with the same method, and the need for caution when cross-comparing studies that use different methods.

Basal measures of insulin sensitivity and insulin secretion and simplified glucose tolerance tests in dogs.

PubMed

Verkest, K R; Fleeman, L M; Rand, J S; Morton, J M

2010-10-01

There is need for simple, inexpensive measures of glucose tolerance, insulin sensitivity, and insulin secretion in dogs. The aim of this study was to estimate the closeness of correlation between fasting and dynamic measures of insulin sensitivity and insulin secretion, the precision of fasting measures, and the agreement between results of standard and simplified glucose tolerance tests in dogs. A retrospective descriptive study using 6 naturally occurring obese and 6 lean dogs was conducted. Data from frequently sampled intravenous glucose tolerance tests (FSIGTTs) in 6 obese and 6 lean client-owned dogs were used to calculate HOMA, QUICKI, fasting glucose and insulin concentrations. Fasting measures of insulin sensitivity and secretion were compared with MINMOD analysis of FSIGTTs using Pearson correlation coefficients, and they were evaluated for precision by the discriminant ratio. Simplified sampling protocols were compared with standard FSIGTTs using Lin's concordance correlation coefficients, limits of agreement, and Pearson correlation coefficients. All fasting measures except fasting plasma glucose concentration were moderately correlated with MINMOD-estimated insulin sensitivity (|r| = 0.62-0.80; P < 0.03), and those that combined fasting insulin and glucose were moderately closely correlated with MINMOD-estimated insulin secretion (r = 0.60-0.79; P < 0.04). HOMA calculated using the nonlinear formulae had the closest estimated correlation (r = 0.77 and 0.74) and the best discrimination for insulin sensitivity and insulin secretion (discriminant ratio 4.4 and 3.4, respectively). Simplified sampling protocols with half as many samples collected over 3 h had close agreement with the full sampling protocol. Fasting measures and simplified intravenous glucose tolerance tests reflect insulin sensitivity and insulin secretion derived from frequently sampled glucose tolerance tests with MINMOD analysis in dogs. Copyright 2010 Elsevier Inc. All rights reserved.

Electrospinning of calcium phosphate-poly (d,l-lactic acid) nanofibers for sustained release of water-soluble drug and fast mineralization

PubMed Central

Fu, Qi-Wei; Zi, Yun-Peng; Xu, Wei; Zhou, Rong; Cai, Zhu-Yun; Zheng, Wei-Jie; Chen, Feng; Qian, Qi-Rong

2016-01-01

Calcium phosphate-based biomaterials have been well studied in biomedical fields due to their outstanding chemical and biological properties which are similar to the inorganic constituents in bone tissue. In this study, amorphous calcium phosphate (ACP) nanoparticles were prepared by a precipitation method, and used for preparation of ACP-poly(d,l-lactic acid) (ACP-PLA) nanofibers and water-soluble drug-containing ACP-PLA nanofibers by electrospinning. Promoting the encapsulation efficiency of water-soluble drugs in electrospun hydrophobic polymer nanofibers is a common problem due to the incompatibility between the water-soluble drug molecules and hydrophobic polymers solution. Herein, we used a native biomolecule of lecithin as a biocompatible surfactant to overcome this problem, and successfully prepared water-soluble drug-containing ACP-PLA nanofibers. The lecithin and ACP nanoparticles played important roles in stabilizing water-soluble drug in the electrospinning composite solution. The electrospun drug-containing ACP-PLA nanofibers exhibited fast mineralization in simulated body fluid. The ACP nanoparticles played the key role of seeds in the process of mineralization. Furthermore, the drug-containing ACP-PLA nanofibers exhibited sustained drug release which simultaneously occurred with the in situ mineralization in simulated body fluid. The osteoblast-like (MG63) cells with spreading filopodia were well observed on the as-prepared nanofibrous mats after culturing for 24 hours, indicating a high cytocompatibility. Due to the high biocompatibility, sustained drug release, and fast mineralization, the as-prepared composite nanofibers may have potential applications in water-soluble drug loading and release for tissue engineering. PMID:27785016

Fast disintegrating films containing anastrozole as a dosage form for dysphagia patients.

PubMed

Satyanarayana, Dixit Anil; Keshavarao, Kulkarni Parthasarathi

2012-12-01

The objective of the present research was to ensure safety during oral administration of medications to dysphagia patients, by preparing fast disintegrating films (FDF) containing anastrozole (ANS) which disintegrate rapidly when placed on the tongue. Films were prepared by solvent-casting method using various polymers such as hydroxyl propyl methyl cellulose (HPMC E5 LV), hydroxy propyl cellulose (HPC), poly vinyl alcohol (PVA) and sodium alginate (Na Alginate). Among the formulations examined, film prepared using HPMC E5 LV (F1) exhibited shorter disintegration time (15 sec) with satisfactory mechanical properties. Fourier transformer infrared (FTIR) & differential scanning calorimetry (DSC) analysis revealed no chemical incompatibility between drug and excipients used in the formulation. Surface morphology revealed even distribution of ANS in the film. Dissolution of drug from F1 formulation was rapid with more than 90% drug release in 240 sec. Pharmacokinetic parameters showed no statistical difference between F1 (test) and drug solution (control) indicating comparable plasma level-time profiles. The film showed an excellent stability for 24 weeks when stored at refrigerated temperature (2-8°C). These findings suggest that the fast disintegrating film as a promising candidate for delivery of ANS in dysphagic patients.

Curing kinetics and thermomechanical properties of latent epoxy/carbon fiber composites

NASA Astrophysics Data System (ADS)

Dalle Vacche, S.; Michaud, V.; Demierre, M.; Bourban, P.-E.; Månson, J.-A. E.

2016-07-01

In this work, resins based on diglycidyl ether of bisphenol A (DGEBA) epoxy and a latent hardener, dicyandiamide (DICY), as well as carbon fiber (CF) composites based on them, were prepared with three commercial accelerators: a methylene bis (phenyl dimethyl urea), a cycloaliphatic substituted urea, and a modified polyamine. The curing kinetics of the three DGEBA/DICY/accelerator systems were investigated by chemorheology and differential scanning calorimetry (DSC), in isothermal and over temperature change conditions. Differences in the reaction onset temperature, and in the glass transition temperature (Tg) were highlighted. For curing of thick resin samples, a slow curing cycle at the lowest possible temperature was used, followed by high temperature (160 - 180 °C) post-curing. Indeed, fast curing at higher temperatures caused the formation of hot spots and led to local burning of the samples. The obtained thermomechanical properties, assessed by ultimate tensile testing and dynamic mechanical analysis (DMA) in single cantilever configuration, were all in the expected range for epoxy resins, with tensile moduli close to 3 GPa and Tg > 140 °C. The longterm stability of these resins at room temperature was verified by DSC. Composite samples were prepared by hand lay-up by manually impregnating four layers of 5-harness satin CF textile, and curing in vacuum bag. Impregnation quality and void content were assessed by optical microscopy. The flexural properties of the post-cured composites were assessed by three-point bending test at room temperature and showed no relevant differences, all composites having bending moduli of 45 - 50 GPa. Finally, composites cured with a faster high temperature curing cycle (20 min at 140 °C) were prepared with the DGEBA/DICY/ methylene bis (phenyl dimethyl urea) system, obtaining similar properties as with the slower curing cycle, showing that the prepreg system allowed more flexibility in terms of curing cycle than the bulk resin samples.

Auto Service Career Preparation Moves to the Fast Track.

ERIC Educational Resources Information Center

Gray, Don

2000-01-01

Automotive Youth Educational Systems (AYES) is a school-to-career partnership among automotive manufacturers and dealers and selected high schools. AYES is designed to encourage students to consider careers in retail automotive service and to prepare them for entry-level positions at dealerships or colleges. (JOW)

Formulation Development and Evaluation of Fast Disintegrating Tablets of Salbutamol Sulphate for Respiratory Disorders

PubMed Central

Sharma, Deepak

2013-01-01

Recent developments in fast disintegrating tablets have brought convenience in dosing to pediatric and elderly patients who have trouble in swallowing tablets. The objective of the present study was to prepare the fast disintegrating tablet of salbutamol sulphate for respiratory disorders for pediatrics. As precision of dosing and patient's compliance become important prerequisites for a long-term treatment, there is a need to develop a formulation for this drug which overcomes problems such as difficulty in swallowing, inconvenience in administration while travelling, and patient's acceptability. Hence, the present investigation were undertaken with a view to develop a fast disintegrating tablet of salbutamol sulphate which offers a new range of products having desired characteristics and intended benefits. Superdisintegrants such as sodium starch glycolate was optimized. Different binders were optimized along with optimized superdisintegrant concentration. The tablets were prepared by direct compression technique. The tablets were evaluated for hardness, friability, weight variation, wetting time, disintegration time, and uniformity of content. Optimized formulation was evaluated by in vitro dissolution test, drug-excipient compatibility, and accelerated stability study. It was concluded that fast disintegrating tablets of salbutamol sulphate were formulated successfully with desired characteristics which disintegrated rapidly; provided rapid onset of action; and enhanced the patient convenience and compliance. PMID:23956881

Simple and rapid analytical method for detection of amino acids in blood using blood spot on filter paper, fast-GC/MS and isotope dilution technique.

PubMed

Kawana, Shuichi; Nakagawa, Katsuhiro; Hasegawa, Yuki; Yamaguchi, Seiji

2010-11-15

A simple and rapid method for quantitative analysis of amino acids, including valine (Val), leucine (Leu), isoleucine (Ile), methionine (Met) and phenylalanine (Phe), in whole blood has been developed using GC/MS. In this method, whole blood was collected using a filter paper technique, and a 1/8 in. blood spot punch was used for sample preparation. Amino acids were extracted from the sample, and the extracts were purified using cation-exchange resins. The isotope dilution method using ²H₈-Val, ²H₃-Leu, ²H₃-Met and ²H₅-Phe as internal standards was applied. Following propyl chloroformate derivatization, the derivatives were analyzed using fast-GC/MS. The extraction recoveries using these techniques ranged from 69.8% to 87.9%, and analysis time for each sample was approximately 26 min. Calibration curves at concentrations from 0.0 to 1666.7 μmol/l for Val, Leu, Ile and Phe and from 0.0 to 333.3 μmol/l for Met showed good linearity with regression coefficients=1. The method detection limits for Val, Leu, Ile, Met and Phe were 24.2, 16.7, 8.7, 1.5 and 12.9 μmol/l, respectively. This method was applied to blood spot samples obtained from patients with phenylketonuria (PKU), maple syrup urine disease (MSUD), hypermethionine and neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), and the analysis results showed that the concentrations of amino acids that characterize these diseases were increased. These results indicate that this method provides a simple and rapid procedure for precise determination of amino acids in whole blood. Copyright © 2010 Elsevier B.V. All rights reserved.

In-tube extraction and GC-MS analysis of volatile components from wild and cultivated sea buckthorn (Hippophae rhamnoides L. ssp. Carpatica) berry varieties and juice.

PubMed

Socaci, Sonia A; Socaciu, Carmen; Tofană, Maria; Raţi, Ioan V; Pintea, Adela

2013-01-01

The health benefits of sea buckthorn (Hippophae rhamnoides L.) are well documented due to its rich content in bioactive phytochemicals (pigments, phenolics and vitamins) as well as volatiles responsible for specific flavours and bacteriostatic action. The volatile compounds are good biomarkers of berry freshness, quality and authenticity. To develop a fast and efficient GC-MS method including a minimal sample preparation technique (in-tube extraction, ITEX) for the discrimination of sea buckthorn varieties based on their chromatographic volatile fingerprint. Twelve sea buckthorn varieties (wild and cultivated) were collected from forestry departments and experimental fields, respectively. The extraction of volatile compounds was performed using the ITEX technique whereas separation and identification was performed using a GC-MS QP-2010. Principal component analysis (PCA) was applied to discriminate the differences among sample composition. Using GC-MS analysis, from the headspace of sea buckthorn samples, 46 volatile compounds were separated with 43 being identified. The most abundant derivatives were ethyl esters of 2-methylbutanoic acid, 3-methylbutanoic acid, hexanoic acid, octanoic acid and butanoic acid, as well as 3-methylbutyl 3-methylbutanoate, 3-methylbutyl 2-methylbutanoate and benzoic acid ethyl ester (over 80% of all volatile compounds). Principal component analysis showed that the first two components explain 79% of data variance, demonstrating a good discrimination between samples. A reliable, fast and eco-friendly ITEX/GC-MS method was applied to fingerprint the volatile profile and to discriminate between wild and cultivated sea buckthorn berries originating from the Carpathians, with relevance to food science and technology. Copyright © 2013 John Wiley & Sons, Ltd.

Desorption atmospheric pressure photoionization high-resolution mass spectrometry: a complementary approach for the chemical analysis of atmospheric aerosols.

PubMed

Parshintsev, Jevgeni; Vaikkinen, Anu; Lipponen, Katriina; Vrkoslav, Vladimir; Cvačka, Josef; Kostiainen, Risto; Kotiaho, Tapio; Hartonen, Kari; Riekkola, Marja-Liisa; Kauppila, Tiina J

2015-07-15

On-line chemical characterization methods of atmospheric aerosols are essential to increase our understanding of physicochemical processes in the atmosphere, and to study biosphere-atmosphere interactions. Several techniques, including aerosol mass spectrometry, are nowadays available, but they all suffer from some disadvantages. In this research, desorption atmospheric pressure photoionization high-resolution (Orbitrap) mass spectrometry (DAPPI-HRMS) is introduced as a complementary technique for the fast analysis of aerosol chemical composition without the need for sample preparation. Atmospheric aerosols from city air were collected on a filter, desorbed in a DAPPI source with a hot stream of toluene and nitrogen, and ionized using a vacuum ultraviolet lamp at atmospheric pressure. To study the applicability of the technique for ambient aerosol analysis, several samples were collected onto filters and analyzed, with the focus being on selected organic acids. To compare the DAPPI-HRMS data with results obtained by an established method, each filter sample was divided into two equal parts, and the second half of the filter was extracted and analyzed by liquid chromatography/mass spectrometry (LC/MS). The DAPPI results agreed with the measured aerosol particle number. In addition to the targeted acids, the LC/MS and DAPPI-HRMS methods were found to detect different compounds, thus providing complementary information about the aerosol samples. DAPPI-HRMS showed several important oxidation products of terpenes, and numerous compounds were tentatively identified. Thanks to the soft ionization, high mass resolution, fast analysis, simplicity and on-line applicability, the proposed methodology has high potential in the field of atmospheric research. Copyright © 2015 John Wiley & Sons, Ltd.

Effects of iodinated contrast agent, xylocaine and gadolinium concentration on the signal emitted in magnetic resonance arthrography: a samples study*

PubMed Central

da Silva, Yvana Lopes Pinheiro; Costa, Rita Zanlorensi Visneck; Pinho, Kátia Elisa Prus; Ferreira, Ricardo Rabello; Schuindt, Sueliton Miyamoto

2015-01-01

Objective To investigate the effects of dilution of paramagnetic contrast agent with iodinated contrast and xylocaine on the signal intensity during magnetic resonance arthrography, and to improve the paramagnetic contrast agent concentration utilized in this imaging modality. Materials and Methods Samples specially prepared for the study with three different concentrations of paramagnetic contrast agent diluted in saline, iodinated contrast agent and xylocaine were imaged with fast spin echo T1-weighted sequences with fat saturation. The samples were placed into flasks and graphical analysis of the signal intensity was performed as a function of the paramagnetic contrast concentration. Results As compared with samples of equal concentrations diluted only with saline, the authors have observed an average signal intensity decrease of 20.67% for iodinated contrast agent, and of 28.34% for xylocaine. However, the increased gadolinium concentration in the samples caused decrease in signal intensity with all the dilutions. Conclusion Minimizing the use of iodinated contrast media and xylocaine and/or the use of a gadolinium concentration of 2.5 mmol/L diluted in saline will improve the sensitivity of magnetic resonance arthrography. PMID:25987746

A Self-Powered Fast-Sampling Profiling Float in support of a Mesoscale Ocean Observing System in the Western North Pacific

NASA Astrophysics Data System (ADS)

Valdez, T.; Chao, Y.; Davis, R. E.; Jones, J.

2012-12-01

This talk will describe a new self-powered profiling float that can perform fast sampling over the upper ocean for long durations in support of a mesoscale ocean observing system in the Western North Pacific. The current state-of-the-art profiling floats can provide several hundreds profiles for the upper ocean every ten days. To quantify the role of the upper ocean in modulating the development of Typhoons requires at least an order of magnitude reduction for the sampling interval. With today's profiling float and battery technology, a fast sampling of one day or even a few hours will reduce the typical lifetime of profiling floats from years to months. Interactions between the ocean and typhoons often involves mesoscale eddies and fronts, which require a dense array of floats to reveal the 3-dimensional structure. To measure the mesoscale ocean over a large area like the Western North Pacific therefore requires a new technology that enables fast sampling and long duration at the same time. Harvesting the ocean renewable energy associated with the vertical temperature differentials has the potential to power profiling floats with fast sampling over long durations. Results from the development and deployment of a prototype self-powered profiling float (known as SOLO-TREC) will be presented. With eight hours sampling in the upper 500 meters, the upper ocean temperature and salinity reveal pronounced high frequency variations. Plans to use the SOLO-TREC technology in support of a dense array of fast sampling profiling floats in the Western North Pacific will be discussed.

A New Fast, Reliable Technique for the Sampling of Dissolved Inorganic Carbon in Sea Ice

NASA Astrophysics Data System (ADS)

Hu, Y.; Wang, F.; Rysgaard, S.; Barber, D. G.

2015-12-01

For a long time, sea ice was considered to act as a lid over seawater preventing CO2 exchange between the atmosphere and ocean. Recent observations suggest that sea ice can be an active source or a sink for CO2, although its magnitude is not very clear. The direct measurements on CO2 flux based on the chamber method and eddy covariance often do not agree with each other. It is therefore important to measure the dissolved inorganic carbon (DIC) stock in sea ice precisely in order to better understand the CO2 flux through sea ice. The challenges in sea ice DIC sampling is how to melt the ice core without being exposed to the air gaining or losing CO2. A common practice is to seal the ice core in a self-prepared gas-tight plastic bag and suck the air out of the bag gently using a syringe (together with a needle) through a valve mounted on one side of the bag. However, this method is time consuming (takes up to several minutes to suck the air out) and very often there is large headspace found in the bag after the ice melts due to the imperfect bag-preparation, which might affect the DIC concentration in melt ice-water. We developed a new technique by using a commercially available plastic bag with a vacuum sealer to seal the ice core. In comparison to syringe-based method, this technique is fast and easy to operate; it takes less than 10 seconds to vacuum and seal the bag all in one button with no headspace left in the bag. Experimental tests with replicate ice cores sealed by those two methods showed that there is no difference in the DIC concentration measured after these two methods, suggesting that there is no loss of DIC during the course of vacuum sealing. In addition, a time series experiment on DIC in melt ice-water stored in the new bag shows that when the samples were not poisoned, the DIC concentration remains unchanged for at least 3 days in the bag; while poisoned by HgCl2, there is no change in DIC for at least 21 days, indicating that this new bag is impermeable to CO2. Therefore, this new technique offers a convenient yet reliable method for DIC sampling of sea ice.

Synthesis and characterization of core-shell magnetic molecularly imprinted polymers for solid-phase extraction and determination of Rhodamine B in food.

PubMed

Su, Xiaomeng; Li, Xiaoyan; Li, Junjie; Liu, Min; Lei, Fuhou; Tan, Xuecai; Li, Pengfei; Luo, Weiqiang

2015-03-15

Core-shell magnetic molecularly imprinted polymers (MIPs) nanoparticles (NPs), in which a Rhodamine B-imprinted layer was coated on Fe3O4 NPs. were synthesized. First, Fe3O4 NPs were prepared by a coprecipitation method. Then, amino-modified Fe3O4 NPs (Fe3O4@SiO2-NH2) was prepared. Finally, the MIPs were coated on the Fe3O4@SiO2-NH2 surface by the copolymerization with functional monomer, acrylamide, using a cross-linking agent, ethylene glycol dimethacrylate; an initiator, azobisisobutyronitrile and a template molecule, Rhodamine B. The Fe3O4@MIPs were characterized using a scanning electron microscope, Fourier transform infrared spectrometer, vibrating sample magnetometer, and re-binding experiments. The Fe3O4@MIPs showed a fast adsorption equilibrium, a highly improved imprinting capacity, and significant selectivity; they could be used as a solid-phase extraction material and detect illegal addition Rhodamine B in food. A method was developed for the selective isolation and enrichment of Rhodamine B in food samples with recoveries in the range 78.47-101.6% and the relative standard deviation was <2%. Copyright © 2014 Elsevier Ltd. All rights reserved.

Detection of Amine Impurity and Quality Assessment of the MALDI Matrix α-Cyano-4-Hydroxy-Cinnamic Acid for Peptide Analysis in the amol Range

NASA Astrophysics Data System (ADS)

Rechthaler, Justyna; Pittenauer, Ernst; Schaub, Tanner M.; Allmaier, Günter

2013-05-01

We have studied sample preparation conditions to increase the reproducibility of positive UV-MALDI-TOF mass spectrometry of peptides in the amol range. By evaluating several α-cyano-4-hydroxy-cinnamic acid (CHCA) matrix batches and preparation protocols, it became apparent that two factors have a large influence on the reproducibility and the quality of the generated peptide mass spectra: (1) the selection of the CHCA matrix, which allows the most sensitive measurements and an easier finding of the "sweet spots," and (2) the amount of the sample volume deposited onto the thin crystalline matrix layer. We have studied in detail the influence of a contaminant, coming from commercial CHCA matrix batches, on sensitivity of generated peptide mass spectra in the amol as well as fmol range of a tryptic peptide mixture. The structure of the contaminant, N, N-dimethylbutyl amine, was determined by applying MALDI-FT-ICR mass spectrometry experiments for elemental composition and MALDI high energy CID experiments utilizing a tandem mass spectrometer (TOF/RTOF). A recrystallization of heavily contaminated CHCA batches that reduces or eliminates the determined impurity is described. Furthermore, a fast and reliable method for the assessment of CHCA matrix batches prior to tryptic peptide MALDI mass spectrometric analyses is presented.

Picosecond laser micromachining prior to FIB milling for electronic microscopy sample preparation

NASA Astrophysics Data System (ADS)

Sikora, Aurélien; Fares, Lahouari; Adrian, Jérôme; Goubier, Vincent; Delobbe, Anne; Corbin, Antoine; Sentis, Marc; Sarnet, Thierry

2017-10-01

In order to check the manufacturing quality of electronic components using electron microscopy, the area of interest must be exposed. This requires the removal of a large quantity of matter without damaging the surrounding area. This step can be accomplished using ion milling but the processing can last a few hours. In order to accelerate the preparation of the samples, picosecond laser micromachining prior to Focused Ion Beam polishing is envisioned. Laser ablation allows the fast removal of matter but induces damages around the ablated area. Therefore the process has to be optimized in order to limit the size of both the heat affected zone and induced dislocation zone. For this purpose, cavities have been engraved in silicon and in electronic components, using a linearly polarized picosecond laser (∼50 ps) at three different wavelengths (343, 515 and 1030 nm). Results showed that the cross sectional shapes and the surface topologies can be tuned by the laser fluence and the number of pulses. Clear cross sections of bumps and cavity openings, exposing multilayer interfaces, are demonstrated. The silicon removal rates, tuned by the applied energy density, have been measured. Removal rates achieved at 200 kHz were typically hundred times higher than those achieved by ion milling and the best efficiency was obtained at 343 nm.

High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS).

PubMed

Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

2015-11-01

A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.

Multiresidue Method for Quantification of Sulfonamides and Trimethoprim in Tilapia Fillet by Liquid Chromatography Coupled to Quadrupole Time-of-Flight Mass Spectrometry Using QuEChERS for Sample Preparation.

PubMed

Nunes, Kátia S D; Assalin, Márcia R; Vallim, José H; Jonsson, Claudio M; Queiroz, Sonia C N; Reyes, Felix G R

2018-01-01

A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet ( Oreochromis niloticus ) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity ( r  ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g -1 and 5 ng·g -1 , respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CC α 102.6-120.0 ng·g -1 and 70 ng·g -1 for sulfonamides and trimethoprim, respectively) and detection capability (CC β 111.7-140.1 ng·g -1 and 89.9 ng·g -1 for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies.

Multiresidue Method for Quantification of Sulfonamides and Trimethoprim in Tilapia Fillet by Liquid Chromatography Coupled to Quadrupole Time-of-Flight Mass Spectrometry Using QuEChERS for Sample Preparation

PubMed Central

Nunes, Kátia S. D.; Assalin, Márcia R.; Vallim, José H.; Jonsson, Claudio M.; Queiroz, Sonia C. N.

2018-01-01

A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet (Oreochromis niloticus) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity (r ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g−1 and 5 ng·g−1, respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CCα 102.6–120.0 ng·g−1 and 70 ng·g−1 for sulfonamides and trimethoprim, respectively) and detection capability (CCβ 111.7–140.1 ng·g−1 and 89.9 ng·g−1 for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies. PMID:29686929

Zirconium(IV) functionalized magnetic nanocomposites for extraction of organophosphorus pesticides from environmental water samples.

PubMed

Jiang, Li; Huang, Tengjun; Feng, Shun; Wang, Jide

2016-07-22

The widespread use of organophosphate pesticides (OPPs) in agriculture leads to residue accumulation in the environment which is dangerous to human health and disrupts the ecological balance. In this work, one nanocomposite immobilized zirconium (Zr, IV) was prepared and used as the affinity probes to quickly and selectively extract organophosphorus pesticides (OPPs) from water samples. The Fe3O4-ethylenediamine tetraacetic acid (EDTA)@Zr(IV) nanocomposites (NPs) were prepared by simply mixing Zr(IV) ions with Fe3O4-EDTA NPs synthesized by one-pot chemical co-precipitation method. The immobilized Zr(IV) ions were further utilized to capture OPPs based on their high affinity for the phosphate moiety in OPPs. Coupled with GC-MS, four OPPs were used as models to demonstrate the feasibility of this approach. Under the optimum conditions, the limits of detection for target OPPs were in the range of 0.10-10.30ngmL(-1) with relative standard deviations (RSDs) of 0.61-4.40% (n=3), respectively. The linear ranges were over three orders of magnitudes (correlation coefficients, R(2)>0.9995). The Fe3O4-EDTA@Zr(IV) NPs were successfully applied to extract OPPs samples with recoveries of 86.95-112.60% and RSDs of 1.20-10.42% (n=3) from two spiked real water. By the proposed method, the matrix interference could be effectively eliminated. We hope our finding can provide a promising alternative for the fast extraction of OPPs from complex real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Facile and green synthesis of mesoporous Co3O4 nanocubes and their applications for supercapacitors

NASA Astrophysics Data System (ADS)

Liu, Xiangmei; Long, Qing; Jiang, Chunhui; Zhan, Beibei; Li, Chen; Liu, Shujuan; Zhao, Qiang; Huang, Wei; Dong, Xiaochen

2013-06-01

Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer.Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr00495c

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Electrochemistry coupled online to liquid chromatography-mass spectrometry for fast simulation of biotransformation reactions of the insecticide chlorpyrifos.

PubMed

Mekonnen, Tessema F; Panne, Ulrich; Koch, Matthias

2017-05-01

An automated method is presented for fast simulation of (bio)transformation products (TPs) of the organophosphate insecticide chlorpyrifos (CPF) based on electrochemistry coupled online to liquid chromatography-mass spectrometry (EC-LC-MS). Oxidative TPs were produced by a boron doped diamond (BDD) electrode, separated by reversed phase HPLC and online detected by electrospray ionization-mass spectrometry (ESI-MS). Furthermore, EC oxidative TPs were investigated by HPLC-tandem mass spectrometry (LC-MS/MS) and FT-ICR high resolution mass spectrometry (HRMS) and compared to in vitro assay metabolites (rat and human liver microsomes). Main phase I metabolites of CPF: chlorpyrifos oxon (CPF oxon), trichloropyridinol (TCP), diethylthiophosphate (DETP), diethylphosphate (DEP), desethyl chlorpyrifos (De-CPF), and desethyl chlorpyrifos oxon (De-CPF oxon), were successfully identified by the developed EC-LC-MS method. The EC-LC-MS method showed similar metabolites compared to the in vitro assay with possibilities of determining reactive species. Our results reveal that online EC-(LC)-MS brings an advantage on time of analysis by eliminating sample preparation steps and matrix complexity compared to conventional in vivo or in vitro methods.

Direct sampling of chemical weapons in water by photoionization mass spectrometry.

PubMed

Syage, Jack A; Cai, Sheng-Suan; Li, Jianwei; Evans, Matthew D

2006-05-01

The vulnerability of water supplies to toxic contamination calls for fast and effective means for screening water samples for multiple threats. We describe the use of photoionization (PI) mass spectrometry (MS) for high-speed, high-throughput screening and molecular identification of chemical weapons (CW) threats and other hazardous compounds. The screening technology can detect a wide range of compounds at subacute concentrations with no sample preparation and a sampling cycle time of approximately 45 s. The technology was tested with CW agents VX, GA, GB, GD, GF, HD, HN1, and HN3, in addition to riot agents and precursors. All are sensitively detected and give simple PI mass spectra dominated by the parent ion. The target application of the PI MS method is as a routine, real-time early warning system for CW agents and other hazardous compounds in air and in water. In this work, we also present comprehensive measurements for water analysis and report on the system detection limits, linearity, quantitation accuracy, and false positive (FP) and false negative rates for concentrations at subacute levels. The latter data are presented in the form of receiver operating characteristic curves of the form of detection probability P(D) versus FP probability P(FP). These measurements were made using the CW surrogate compounds, DMMP, DEMP, DEEP, and DIMP. Method detection limits (3sigma) obtained using a capillary injection method yielded 1, 6, 3, and 2 ng/mL, respectively. These results were obtained using 1-microL injections of water samples without any preparation, corresponding to mass detection limits of 1, 6, 3, and 2 pg, respectively. The linear range was about 3-4 decades and the dynamic range about 4-5 decades. The relative standard deviations were generally <10% at CW subacute concentrations levels.

Comparative Evaluation of Marginal Discrepancy in Tooth Colored Self Cure Acrylic Provisional Restorations With and Without Reinforcement of Glass Beads: An In-Vitro Study

PubMed Central

Yasangi, Manoj Kumar; Mannem, Dhanalakshmi; Neturi, Sirisha; Ravoori, Srinivas; Jyothi

2015-01-01

Context This invitro study was conducted to compare and evaluate marginal discrepancy in two types of tooth colored self cure provisional restorative materials {DPI&UNIFAST TRAD} before and after reinforcement of glass beads. Aim The aim of the present study was to evaluate and compare marginal discrepancy in two types of provisional restorative materials (DPI and UNI FAST TRAD) before and after reinforcement with Glass beads. Materials and Methods Tooth shaped resin copings were fabricated on custom made brass metal die. A total of 60 resin copings were fabricated in which 30 samples were prepared with DPI and 30 samples with UNIFAST material. Each group of 30 samples were divided in to two sub groups in which 15 samples were prepared with glass bead reinforcement and 15 samples without reinforcement. The marginal discrepancy was evaluated with photomicroscope {Reichet Polyvar 2 met} by placing the resin copings on custom made brass resin coping holder. Results Measurements obtained were statistically analysed by unpaired t-test to know any significance between two variables. Unreinforced DPI specimens had shown lower marginal discrepancy (442.82) than reinforced specimens (585.77). Unreinforced UNIFAST specimens have shown high values of marginal discrepancy (592.83) than reinforced specimens (436.35). p-value between reinforced and unreinforced specimens of DPI (p=0.0013) and UNIFAST (p= 0.0038) has shown statistical significance. Conclusion This in-vitro study revealed that unreinforced DPI specimens have shown lower marginal discrepancy than reinforced specimens and unreinforced UNIFAST specimens have shown higher values of marginal discrepancy than reinforced specimens. PMID:26155574

Materials for storage and release of hydrogen and methods for preparing and using same

DOEpatents

Autrey, Thomas S [West Richland, WA; Gutowska, Anna [Richland, WA; Shin, Yongsoon [Richland, WA; Li, Liyu [Richland, WA

2008-01-08

The invention relates to materials for storing and releasing hydrogen and methods for preparing and using same. The materials exhibit fast release rates at low release temperatures and are suitable as fuel and/or hydrogen sources for a variety of applications such as automobile engines.

Evaporation rate-based selection of supramolecular chirality.

PubMed

Hattori, Shingo; Vandendriessche, Stefaan; Koeckelberghs, Guy; Verbiest, Thierry; Ishii, Kazuyuki

2017-03-09

We demonstrate the evaporation rate-based selection of supramolecular chirality for the first time. P-type aggregates prepared by fast evaporation, and M-type aggregates prepared by slow evaporation are kinetic and thermodynamic products under dynamic reaction conditions, respectively. These findings provide a novel solution reaction chemistry under the dynamic reaction conditions.

Automated imaging of cellular spheroids with selective plane illumination microscopy on a chip (Conference Presentation)

NASA Astrophysics Data System (ADS)

Paiè, Petra; Bassi, Andrea; Bragheri, Francesca; Osellame, Roberto

2017-02-01

Selective plane illumination microscopy (SPIM) is an optical sectioning technique that allows imaging of biological samples at high spatio-temporal resolution. Standard SPIM devices require dedicated set-ups, complex sample preparation and accurate system alignment, thus limiting the automation of the technique, its accessibility and throughput. We present a millimeter-scaled optofluidic device that incorporates selective plane illumination and fully automatic sample delivery and scanning. To this end an integrated cylindrical lens and a three-dimensional fluidic network were fabricated by femtosecond laser micromachining into a single glass chip. This device can upgrade any standard fluorescence microscope to a SPIM system. We used SPIM on a CHIP to automatically scan biological samples under a conventional microscope, without the need of any motorized stage: tissue spheroids expressing fluorescent proteins were flowed in the microchannel at constant speed and their sections were acquired while passing through the light sheet. We demonstrate high-throughput imaging of the entire sample volume (with a rate of 30 samples/min), segmentation and quantification in thick (100-300 μm diameter) cellular spheroids. This optofluidic device gives access to SPIM analyses to non-expert end-users, opening the way to automatic and fast screening of a high number of samples at subcellular resolution.

A highly ordered mesostructured material containing regularly distributed phenols: preparation and characterization at a molecular level through ultra-fast magic angle spinning proton NMR spectroscopy.

PubMed

Roussey, Arthur; Gajan, David; Maishal, Tarun K; Mukerjee, Anhurada; Veyre, Laurent; Lesage, Anne; Emsley, Lyndon; Copéret, Christophe; Thieuleux, Chloé

2011-03-14

Highly ordered organic-inorganic mesostructured material containing regularly distributed phenols is synthesized by combining a direct synthesis of the functional material and a protection-deprotection strategy and characterized at a molecular level through ultra-fast magic angle spinning proton NMR spectroscopy.

New on-line separation workflow of microbial metabolites via hyphenation of analytical and preparative comprehensive two-dimensional liquid chromatography.

PubMed

Yan, Xia; Wang, Li-Juan; Wu, Zhen; Wu, Yun-Long; Liu, Xiu-Xiu; Chang, Fang-Rong; Fang, Mei-Juan; Qiu, Ying-Kun

2016-10-15

Microbial metabolites represent an important source of bioactive natural products, but always exhibit diverse of chemical structures or complicated chemical composition with low active ingredients content. Traditional separation methods rely mainly on off-line combination of open-column chromatography and preparative high performance liquid chromatography (HPLC). However, the multi-step and prolonged separation procedure might lead to exposure to oxygen and structural transformation of metabolites. In the present work, a new two-dimensional separation workflow for fast isolation and analysis of microbial metabolites from Chaetomium globosum SNSHI-5, a cytotoxic fungus derived from extreme environment. The advantage of this analytical comprehensive two-dimensional liquid chromatography (2D-LC) lies on its ability to analyze the composition of the metabolites, and to optimize the separation conditions for the preparative 2D-LC. Furthermore, gram scale preparative 2D-LC separation of the crude fungus extract could be performed on a medium-pressure liquid chromatograph×preparative high-performance liquid chromatography system, under the optimized condition. Interestingly, 12 cytochalasan derivatives, including two new compounds named cytoglobosin Ab (3) and isochaetoglobosin Db (8), were successfully obtained with high purity in a short period of time. The structures of the isolated metabolites were comprehensively characterized by HR ESI-MS and NMR. To be highlighted, this is the first report on the combination of analytical and preparative 2D-LC for the separation of microbial metabolites. The new workflow exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2016 Elsevier B.V. All rights reserved.

Transport Properties Of PbI2 Doped Silver Oxysalt Based Amorphous Solid Electrolytes

NASA Astrophysics Data System (ADS)

Shrisanjaykumar Jayswal, Manishkumar

Solid electrolytes are a class of materials that conduct electricity by means of motion of ions like Ag+, Na+, Li +, Cu+, H+, F-, O -2 etc. in solid phase. The host materials include crystalline, polycrystalline, glasses, polymers and composites. Ion conducting glasses are one of the most sought after solid electrolytes that are useful in various electrochemical applications like solid state batteries, gas sensors, supercapacitors, electrochromic devices, to name a few. Since the discovery of fast silver ion transport in silver oxyhalide glasses at the end of the 1960s, many glasses showing large ionic conductivity up to 10-4 10-2 S/cm at room temperature have been developed, chiefly silver and copper ion conductors. The silver ion conducting glasses owe their high ionic conductivity mainly to stabilized alpha-AgI. AgI, as we know, undergoes a structural phase transition from wurtzite (beta phase) at room temperature to body centered cubic (alpha phase) structure at temperatures higher than 146 °C. The alpha-AgI possesses approximately six order of higher ionic conductivity than beta-AgI. The high ionic conductivity of alpha-AgI is attributed to its molten sublattice type of structure, which facilitates easy Ag+ ion migration, like a liquid. And hence, several attempts have been made to stabilize it at room temperature in crystalline as well as non-crystalline hosts like oxide and non-oxide glasses. Recently, in order to stabilize AgI in glasses, instead of directly doping it, indirect routes have also been explored. Where, a metal iodide salt along with silver oxide or silver phosphate is taken and an exchange reaction permitted by Hard and Soft, Acid and Base (HSAB) principle occurs between the two and AgI and metal oxide form in the glass forming melt. Work done in the present thesis has been organized in seven chapters as follows: Chapter 1: A review and background information of different solid electrolyte materials and their development is presented. Along with that a detailed review on fast ion conducting glasses is included. At the end of the chapter, the aim of the present work has been given. Chapter 2: A discussion about various theoretical models to explain fast ion conduction mechanism in superionic conductors in general and superionic conducting glasses in particular is given. In addition to that, impedance spectroscopy and its various formalisms are discussed. Chapter 3: This chapter describes the method of preparation of the glass samples and various characterizations and techniques to study their various properties. Chapter 4: Physical properties of the prepared glass samples are studied and discussed in this chapter. The glass samples are found to be fully amorphous as exhibited by x-ray diffraction studies. The density of the prepared samples is increasing consistently with increasing PbI 2 content in the glass. For glass series (a), the molar volume also increases with PbI2 content. However, for glass series (b) and (c), molar volume is reducing with increasing PbI2 content, showing that glass is getting compacted with increasing PbI2 content. Chapter 5: Transport properties of the prepared glass samples have been investigated using impedance spectroscopy and its various formalisms. The chapter discusses DC conductivity, AC conductivity, dielectric permittivity and modulus analysis of the obtained impedance spectra. The sigma' spectra were scaled using Summerfield scaling law using sigmaDCT as the scaling factor for frequency axis and a well defined Time-Temperature Superposition (TTS) is observed as a function of temperature. The dielectric spectra show the presence of a dielectric relaxation in all glass samples. The dielectric permittivity, epsilon', spectra were scaled using the scaling law given by Sidebottom. The modulus spectra exhibit non-Debye relaxation of Ag+ ions and could be explained using KWW (Kohlrausch-Williams-Watts) decay function. Scaling analysis of the modulus spectra as a function of temperature suggest of invariance of ion relaxation process with changing temperatures. Chapter 6: Solid state battery studies: This chapter discusses about "solid state batteries" prepared by using the best conducting glass composition, from each glass Battery discharge characteristics, polarization measurements and other battery parameters like battery capacity, power density, energy, specific power etc. have been evaluated and summarized. Chapter 7: A summary of the work done and future prospects are discussed. (Abstract shortened by ProQuest.).

Open Probe fast GC-MS - combining ambient sampling ultra-fast separation and in-vacuum ionization for real-time analysis.

PubMed

Keshet, U; Alon, T; Fialkov, A B; Amirav, A

2017-07-01

An Open Probe inlet was combined with a low thermal mass ultra-fast gas chromatograph (GC), in-vacuum electron ionization ion source and a mass spectrometer (MS) of GC-MS for obtaining real-time analysis with separation. The Open Probe enables ambient sampling via sample vaporization in an oven that is open to room air, and the ultra-fast GC provides ~30-s separation, while if no separation is required, it can act as a transfer line with 2 to 3-s sample transfer time. Sample analysis is as simple as touching the sample, pushing the sample holder into the Open Probe oven and obtaining the results in 30 s. The Open Probe fast GC was mounted on a standard Agilent 7890 GC that was coupled with an Agilent 5977A MS. Open Probe fast GC-MS provides real-time analysis combined with GC separation and library identification, and it uses the low-cost MS of GC-MS. The operation of Open Probe fast GC-MS is demonstrated in the 30-s separation and 50-s full analysis cycle time of tetrahydrocannabinol and cannabinol in Cannabis flower, sub 1-min analysis of trace trinitrotoluene transferred from a finger onto a glass surface, vitamin E in canola oil, sterols in olive oil, polybrominated flame retardants in plastics, alprazolam in Xanax drug pill and free fatty acids and cholesterol in human blood. The extrapolated limit of detection for pyrene is <1 fg, but the concentration is too high and the software noise calculation is untrustworthy. The broad range of compounds amenable for analysis is demonstrated in the analysis of reserpine. The possible use with alternate standard GC-MS and Open Probe fast GC-MS is demonstrated in the analysis of heroin in its street drug powder. The use of Open Probe with the fast GC acting as a transfer line is demonstrated in <10-s analysis without separation of ibuprofen and estradiol. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Fast Scanning Calorimetry Studies of Supercooled Liquids and Glasses

NASA Astrophysics Data System (ADS)

Bhattacharya, Deepanjan

This dissertation is a compilation of research results of extensive Fast Scanning Calorimetry studies of two non-crystalline materials: Toluene and Water. Motivation for fundamental studies of non-crystalline phases, a brief overview of glassy materials and concepts and definitions related to them is provided in Chapter 1. Chapter 2 provides fundamentals and details of experimental apparata, experimental protocol and calibration procedure. Chapter 3 & 4 provides extensive studies of stable non-crystalline toluene films of micrometer and nanometer thicknesses grown by vapor deposition at distinct deposition rates and temperatures and probed by Fast Scanning Calorimetry. Fast scanning calorimetry is shown to be extremely sensitive to the structure of the vapor-deposited phase and was used to characterize simultaneously its kinetic stability and its thermodynamic properties. According to our analysis, transformation of vapor -deposited samples of toluene during heating with rates in excess 100,000 K/s follows the zero-order kinetics. The transformation rate correlates strongly with the initial enthalpy of the sample, which increases with the deposition rate according to sub-linear law. Analysis of the transformation kinetics of vapor deposited toluene films of various thicknesses reveal a sudden increase in the transformation rate for films thinner than 250 nm. The change in kinetics correlates with the surface roughness scale of the substrate, which is interpreted as evidence for kinetic anisotropy of the samples. We also show that out-of-equilibrium relaxation kinetics and possibly the enthalpy of vapor-deposited (VD) films of toluene are distinct from those of ordinary supercooled (OS) phase even when the deposition takes place at temperatures above the glass softening (Tg). The implications of these findings for the formation mechanism and structure of vapor deposited stable glasses are discussed. Chapter 5 and 6 provide detailed Fast Scanning Calorimetry studies of amorphous solid water in bulk and confining geometry (ultrathin films and nano-aggregates). Bulk-like water samples were prepared by vapor-deposition on the surface of a tungsten filament near 140 K where vapor-deposition results in low enthalpy glassy water films. The vapor deposition approach was also used to grow nano-aggregates (2- 20 nm thick) and multiple ultrathin (approximately 50 nm thick) water films alternated with benzene and methanoic films of similar dimensions. When heated from cryogenic temperatures, the ultrathin water films underwent a well manifested glass softening transition at temperatures 20 degrees below the onset of crystallization. The thermograms of nano-aggregates of ASW films show two endotherms at 40 and 10 K below the onset temperatures of crystallization. However, no such transition was observed in bulk-like water samples prior to their crystallization. These results indicate that water in confined geometry demonstrates glass softening dynamics which are dramatically distinct from those of the bulk phase. We attribute these differences to water's interfacial glass transition which occurs at temperatures tens of degrees lower than that in the bulk. Implications of these finding for past studies of glass softening dynamics in various glassy water samples are discussed in chapter 5 and 6.

Rapid determination of polycyclic aromatic hydrocarbons (PAHs) in tea using two-dimensional gas chromatography coupled with time of flight mass spectrometry.

PubMed

Drabova, Lucie; Pulkrabova, Jana; Kalachova, Kamila; Tomaniova, Monika; Kocourek, Vladimir; Hajslova, Jana

2012-10-15

A simple, fast, and cost effective sample preparation procedure has been developed and validated for the determination of 15+1 European Union Polycyclic Aromatic Hydrocarbons (15+1 EU PAHs) in dried tea leave samples. Based on a critical assessment of several sample extraction/clean-up approaches, the method based on the ethyl acetate extraction followed by the use of PAHs dedicated cartridges with molecularly imprinted polymers (MIPs) has been found as an optimal alternative in terms of time demands and obtained good extract purity. For the final identification/quantification of target PAHs, two dimensional gas chromatography coupled to a time-of-flight mass spectrometry (GC×GC-TOFMS) was used. The performance characteristics of the overall analytical method for individual PAHs determined at three spiking levels (0.5, 2.5 and 5 μg kg(-1)) were in following ranges: limits of quantitation (LOQs) 0.05-0.2 μg kg(-1), repeatabilities 2-9%, and recoveries 73-103%. The recoveries achieved by the newly developed sample preparation procedure when employed for naturally contaminated sample ("incurred" PAHs) were comparable to those obtained by other routinely used approaches employing sonication and/or pressurised liquid extraction for sample analytes isolation. The validated method was subsequently used for the determination of selected genotoxic PAHs in 36 samples of black and green tea obtained from the Czech retail market. The levels of ΣPAH4 (sum of benzo[a]anthracene (BaA), chrysene (CHR), benzo[b]fluoranthene (BbFA) and benzo[a]pyrene (BaP)) in black and green tea leaves ranged from 7.4 to 700 μg kg(-1) and from 4.5 to 102 μg kg(-1), respectively. Contamination of tested tea samples by BaP was in the range of 0.2-152 μg kg(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

Rapid determination of 226Ra in emergency urine samples

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

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

2014-02-27

A new method has been developed at the Savannah River National Laboratory (SRNL) that can be used for the rapid determination of 226Ra in emergency urine samples following a radiological incident. If a radiological dispersive device event or a nuclear accident occurs, there will be an urgent need for rapid analyses of radionuclides in urine samples to ensure the safety of the public. Large numbers of urine samples will have to be analyzed very quickly. This new SRNL method was applied to 100 mL urine aliquots, however this method can be applied to smaller or larger sample aliquots as needed.more » The method was optimized for rapid turnaround times; urine samples may be prepared for counting in <3 h. A rapid calcium phosphate precipitation method was used to pre-concentrate 226Ra from the urine sample matrix, followed by removal of calcium by cation exchange separation. A stacked elution method using DGA Resin was used to purify the 226Ra during the cation exchange elution step. This approach combines the cation resin elution step with the simultaneous purification of 226Ra with DGA Resin, saving time. 133Ba was used instead of 225Ra as tracer to allow immediate counting; however, 225Ra can still be used as an option. The rapid purification of 226Ra to remove interferences using DGA Resin was compared with a slightly longer Ln Resin approach. A final barium sulfate micro-precipitation step was used with isopropanol present to reduce solubility; producing alpha spectrometry sources with peaks typically <40 keV FWHM (full width half max). This new rapid method is fast, has very high tracer yield (>90 %), and removes interferences effectively. The sample preparation method can also be adapted to ICP-MS measurement of 226Ra, with rapid removal of isobaric interferences.« less

Closed tubes preparation of graphite for high-precision AMS radiocarbon analysis

NASA Astrophysics Data System (ADS)

Hajdas, I.; Michczynska, D.; Bonani, G.; Maurer, M.; Wacker, L.

2009-04-01

Radiocarbon dating is an established tool applied in Geochronology. Technical developments of Accelerator Mass Spectrometry AMS, which allow measurements of samples containing less than 1 mg of carbon, opened opportunities for new applications. Moreover, high resolution records of the past changes require high-resolution chronologies i.e. sampling for 14C dating. In result, the field of applications is rapidly expanding and number of radiocarbon analysis is growing rapidly. Nowadays dedicated 14C AMS machines have great capacity for analysis but in order to keep up with the demand for analysis and provide the results as fast as possible a very efficient way of sample preparation is required. Sample preparation for 14C AMS analysis consists of two steps: separation of relevant carbon from the sample material (removing contamination) and preparation of graphite for AMS analysis. The last step usually involves reaction of CO2 with H2, in the presence of metal catalyst (Fe or Co) of specific mesh size heated to 550-625°C, as originally suggested by Vogel et al. (1984). Various graphitization systems have been built in order to fulfil the requirement of sample quality needed for high-precision radiocarbon data. In the early 90ties another method has been proposed (Vogel 1992) and applied by few laboratories mainly for environmental or biomedical samples. This method uses TiH2 as a source of H2 and can be easily and flexibly applied to produce graphite. Sample of CO2 is frozen in to the tube containing pre-conditioned Zn/TiH2 and Fe catalyst. Torch sealed tubes are then placed in the stepwise heated oven at 500/550°C and left to react for several hours. The greatest problem is the lack of control of the reaction completeness and considerable fractionation. However, recently reported results (Xu et al. 2007) suggest that high precision dating using graphite produced in closed tubes might be possible. We will present results of radiocarbon dating of the set of standards and secondary IAEA standards to demonstrate to what level this method can be used for high precision radiocarbon dating. References Vogel JS. 1992. Rapid Production of Graphite without Contamination for Biomedical Ams. Radiocarbon 34: 344-350. Vogel JS, Southon JR, Nelson DE, and Brown TA. 1984. Performance of Catalytically Condensed Carbon for Use in Accelerator Mass-Spectrometry. Nuclear Instruments & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 233: 289-293. Xu X, Trumbore SE, Zheng S, Southon JR, McDuffee KE, Luttgen M, and Liu JC. 2007. Modifying a sealed tube zinc reduction method for preparation of AMS graphite targets: Reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms Accelerator Mass Spectrometry - Proceedings of the Tenth International Conference on Accelerator Mass Spectrometry 259: 320-329.

Ultrastructure and morphology of biofilms on thermoplastic orthodontic appliances in 'fast' and 'slow' plaque formers.

PubMed

Low, Bernard; Lee, Wilson; Seneviratne, C J; Samaranayake, Lakshman P; Hägg, Urban

2011-10-01

The aim of this study was to investigate the morphological features and distribution of biofilms on Invisalign orthodontic appliances, in a sample of 'slow' and 'fast' plaque formers using scanning electron microscopy (SEM). Fifty-six Chinese male/female volunteers (aged 19-39 years) were screened for their plaque-forming rate using the plaque percentage index (PPI) coupled with digital photography and computer-based image analysis, after a period of 48 hours of abstinence from oral hygiene procedures. Eleven volunteers (seven males/four females) representing the lowest and highest ends of the plaque formation spectrum were chosen as slow and fast plaque formers, respectively. The subjects wore a full-coverage splint appliance, in which four tiles of Invisalign material were embedded. These tiles were collected at intervals of 1, 3, 6, 12, 24, and 48 hours, as well as 3, 7, and 14 days, immediately fixed in 10 per cent paraformaldehyde in 0.2 M cacodylate buffer solution and prepared for SEM. The surface configuration of the Invisalign appliance was visualized, as well as the chronological pattern of biofilm formation. Significance between fast and slow plaque formers was determined using a Student's t-test. Colonization appeared to centre initially on the raised edges or textured surfaces of the appliance, and initial adhesion was quicker and more abundant in the fast plaque-forming group. In the later stages of biofilm development, both groups showed no discernible differences in biofilm accrual on the surfaces, but the fast group displayed a more complex biofilm structure. More recessed and sheltered areas of the appliance, such as the cusp tips and attachment dimples, harboured more biofilm than the flat surfaces. Hence, it seems that the novel Invisialign orthodontic appliance is a useful tool to investigate the features of biofilm formation in time-course studies.

Fast synthesis of La-substituted apatite by the dry mechanochemical method and analysis of its structure

NASA Astrophysics Data System (ADS)

Bulina, Natalia V.; Chaikina, Marina V.; Prosanov, Igor Yu.; Dudina, Dina V.; Solovyov, Leonid A.

2017-08-01

Compared to pure apatite, La-substituted apatites have improved thermal, mechanical and biological characteristics. In this article, a fast synthesis of La-substituted apatites by a dry mechanochemical method is presented. Structural studies by X-ray diffraction and Fourier transform infrared spectroscopy indicated the formation of a single-phase nanosized product after 30 min of high-energy ball milling of the reaction mixtures. The dry mechanochemical method is technologically attractive for the preparation of La-substituted apatites, as it allows reducing the processing time down to half an hour and does not require prolonged high-temperature annealing normally used in the synthesis practice of the substituted apatite. As the mechanochemically synthesized samples are nanosized, it is difficult to determine the details of their crystal structure by the Rietveld refinement method. Therefore, a series of the mechanochemically synthesized samples with different concentrations of lanthanum were annealed at 1000°C for 5 h. It was found that the annealed powders are microcrystalline La-substituted apatites Ca10-xLax(PO4)6Ox(OH)2-x, where 0 ≤ x ≤2. In their structure, the Ca2+ ions are replaced by the La3+ ions localized near the Ca2 sites, and the OH- groups are replaced by the O2- ions in the hexagonal channels.

Solid-phase extraction with the metal-organic framework MIL-101(Cr) combined with direct analysis in real time mass spectrometry for the fast analysis of triazine herbicides.

PubMed

Li, Xianjiang; Xing, Jiawei; Chang, Cuilan; Wang, Xin; Bai, Yu; Yan, Xiuping; Liu, Huwei

2014-06-01

MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) extraction time, eluent volume and salt concentration, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of surface enhanced Raman substrate and its characterization

NASA Astrophysics Data System (ADS)

Liu, Y.; Wang, J. Y.; Wang, J. Q.

2017-10-01

Surface enhanced Raman spectroscopy (SERS) is a fast, convenient and highly sensitive detection technique, and preparing the good effect and repeatable substrate is the key to realize the trace amount and quantitative detection in the field of food safety detection. In this paper, a surface enhanced Raman substrate based on submicrometer silver particles structure was prepared by chemical deposition method, and characterized its structure and optical properties.

Rapid microwave assisted synthesis of graphene nanosheets/polyethyleneimine/gold nanoparticle composite and its application to the selective electrochemical determination of dopamine.

PubMed

Ponnusamy, Vinoth Kumar; Mani, Veerappan; Chen, Shen-Ming; Huang, Wan-Tran; Jen, Jen-Fon

2014-03-01

In this study, a simple and fast microwave assisted chemical reduction method for the preparation of graphene nanosheet/polyethyleneimine/gold nanoparticle (GNS/PEI/AuNP) composite was developed. PEI, a cationic polymer, was used both as a non-covalent functionalizing agent for the graphene oxide nanosheets (GONSs) through electrostatic interactions in the aqueous medium and also as a stabilizing agent for the formation of AuNPs on PEI wrapped GNSs. This preparation method involves a simple mixing step followed by a simultaneous microwave assisted chemical reduction of the GONSs and gold ions. The prepared composite exhibits the dispersion of high density AuNPs which were densely decorated on the large surface area of the PEI wrapped GNS. X-ray photoelectron spectroscopy, powder X-ray diffraction, high-resolution transmission electron microscopy, field-emission scanning electron microscopy with energy dispersive X-ray spectroscopy, and thermo-gravimetric analysis, were used to characterize the properties of the resultant composite. The prepared GNS/PEI/AuNP composite film exhibited excellent electrocatalytical activity towards the selective determination of dopamine in the presence of ascorbic acid, which showed potential application in electrochemical sensors. The applicability of the presented sensor was also demonstrated for the determination of dopamine in human urine samples. © 2013 Elsevier B.V. All rights reserved.

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

Ma, Xi; Blue Sky Technology Corporation, Beijing 100083; Ma, Hongwen, E-mail: mahw@cugb.edu.cn

Highlights: • We use the anti-drop precipitation method for synthesis of magnesium hydroxide. • Boron mud which is solid waste from a borax factory is used as the magnesium source. • The magnesium hydroxide nanoflowers are prepared in a short time. • The as-prepared magnesium hydroxide can be used as an effective flame retardant. - Abstract: Using boron mud as the starting material, the flower-like magnesium hydroxide (MH) has been successfully prepared via anti-drop precipitation method. The effect of NH{sub 3}·H{sub 2}O concentration, aging time, and surfactant on the morphology of MH was investigated. The optimum precipitation conditions are droppingmore » MgSO{sub 4} solution in 5% NH{sub 3}·H{sub 2}O solution, with 3% polyethylene glycol as surfactant, aging for 30 min. XRD, SEM, FI-IR, and TG/DTA have been employed to characterize the as-prepared samples. XRD reveals that MH with high purity has the brucite structure. SEM images show that the flower-like MH exists in the form of mono-disperse well uniform spherical aggregation with diameter of 3–5 μm. TG/DTA shows a total percentage of weight loss 33.6% with a well-defined endothermic peak near 381.3 °C corresponding to the decomposition of MH. Furthermore, it reports that the extremely fast primary nucleation is of significance for crystal growth of MH.« less

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

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

Melo, B. M. G.; Graça, M. P. F., E-mail: mpfg@ua.pt; Prezas, P. R.

2016-08-07

In this work, phosphate-borate based glasses with molar composition 20.7P{sub 2}O{sub 5}–17.2Nb{sub 2}O{sub 5}–13.8WO{sub 3}–34.5A{sub 2}O–13.8B{sub 2}O{sub 3}, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric,more » and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σ{sub ac} and σ{sub dc}, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz–1 MHz.« less

Magnetic sulfur-doped porous carbon for preconcentration of trace mercury in environmental water prior to ICP-MS detection.

PubMed

Peng, Chuyu; He, Man; Chen, Beibei; Huang, Lijin; Hu, Bin

2017-11-20

A novel magnetic sulfur-doped porous carbon (MSPC) was fabricated via a simple one-step carbonization of a mixture of sucrose, basic magnesium sulfate whiskers and Fe 3 O 4 @SiO 2 nanoparticles. Due to the high S content, the prepared MSPC possessed high adsorption capacity for Hg 2+ (343 mg g -1 ) with good selectivity. Based on this, a method coupling magnetic solid phase extraction (MSPE) with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Hg 2+ in environmental water samples. Various parameters such as pH, desorption solvent and its concentration, desorption volume and time, sample volume, and adsorption time that affect the determination have been optimized. Under the optimal conditions, a high enrichment factor of 100-fold was obtained, the limit of detection (LOD) was found to be 0.52 pg mL -1 with a relative standard deviation (c = 10 pg mL -1 , n = 7) of 7.1%, and a good linearity was obtained within the concentration range of 2-5000 pg mL -1 for Hg 2+ . Besides, the proposed method has very fast adsorption/desorption kinetics, target Hg 2+ could be rapidly adsorbed on the prepared MSPC in 2 min and desorbed from the MSPC in 2 min with the assistance of a permanent magnet. Therefore, the proposed method of MSPE-ICP-MS exhibits good application potential in the determination of trace Hg 2+ in environmental water samples.

Single hair analysis of small molecules using MALDI-triple quadrupole MS imaging and LC-MS/MS: investigations on opportunities and pitfalls.

PubMed

Poetzsch, Michael; Steuer, Andrea E; Roemmelt, Andreas T; Baumgartner, Markus R; Kraemer, Thomas

2014-12-02

Single hair analysis normally requires extensive sample preparation microscale protocols including time-consuming steps like segmentation and extraction. Matrix assisted laser desorption and ionization mass spectrometric imaging (MALDI-MSI) was shown to be an alternative tool in single hair analysis, but still, questions remain. Therefore, an investigation of MALDI-MSI in single hair analysis concerning the extraction process, usage of internal standard (IS), and influences on the ionization processes were systematically investigated to enable the reliable application to hair analysis. Furthermore, single dose detection, quantitative correlation to a single hair, and hair strand LC-MS/MS results were performed, and the performance was compared to LC-MS/MS single hair monitoring. The MALDI process was shown to be independent from natural hair color and not influenced by the presence of melanin. Ionization was shown to be reproducible along and in between different hair samples. MALDI image intensities in single hair and hair snippets showed good semiquantitative correlation to zolpidem hair concentrations obtained from validated routine LC-MS/MS methods. MALDI-MSI is superior to LC-MS/MS analysis when a fast, easy, and cheap sample preparation is necessary, whereas LC-MS/MS showed higher sensitivity with the ability of single dose detection for zolpidem. MALDI-MSI and LC-MS/MS segmental single hair analysis showed good correlation, and both are suitable for consumption monitoring of drugs of abuse with a high time resolution.

Magnetic nanoparticles coated with polyaniline to stabilize immobilized trypsin

NASA Astrophysics Data System (ADS)

Maciel, J. C.; D. Mercês, A. A.; Cabrera, M.; Shigeyosi, W. T.; de Souza, S. D.; Olzon-Dionysio, M.; Fabris, J. D.; Cardoso, C. A.; Neri, D. F. M.; C. Silva, M. P.; Carvalho, L. B.

2016-12-01

It is reported the synthesis of magnetic nanoparticles via the chemical co-precipitation of Fe 3+ ions and their preparation by coating them with polyaniline. The electronic micrograph analysis showed that the mean diameter for the nanoparticles is ˜15 nm. FTIR, powder X-ray diffraction and Mössbauer spectroscopy were used to understand the chemical, crystallographic and 57Fe hyperfine structures for the two samples. The nanoparticles, which exhibited magnetic behavior with relatively high spontaneous magnetization at room temperature, were identified as being mainly formed by maghemite ( γFe2O3). The coated magnetic nanoparticles (sample labeled "mPANI") presented a real ability to bind biological molecules such as trypsin, forming the magnetic enzyme derivative (sample "mPANIG-Trypsin"). The amount of protein and specific activity of the immobilized trypsin were found to be 13±5 μg of protein/mg of mPANI (49.3 % of immobilized protein) and 24.1±0.7 U/mg of immobilized protein, respectively. After 48 days of storage at 4 ∘C, the activity of the immobilized trypsin was found to be 89 % of its initial activity. This simple, fast and low-cost procedure was revealed to be a promising way to prepare mPANI nanoparticles if technological applications addressed to covalently link biomolecules are envisaged. This route yields chemically stable derivatives, which can be easily recovered from the reaction mixture with a magnetic field and recyclable reused.

Development of coatings for automated 96-blade solid phase microextraction-liquid chromatography-tandem mass spectrometry system, capable of extracting a wide polarity range of analytes from biological fluids.

PubMed

Mirnaghi, Fatemeh S; Pawliszyn, Janusz

2012-10-26

This work presents the development and evaluation of biocompatible polyacrylonitrile-polystyrene-divinylbenzene (PAN-PS-DVB) and polyacrylonitrile-phenylboronic acid (PAN-PBA) coatings for automated 96-blades (thin-film) solid phase microextraction (SPME) system, using high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS). The SPME condition was optimized for 60 min equilibrium extraction and 40 min desorption for PAN-PS-DVB, and 120 min equilibrium extraction and 60 min desorption for PAN-PBA for parallel sample preparation of up to 96 samples. The thin film geometry of the SPME blades provided good extraction efficiency due to the larger surface area of the coating, and simultaneous sample preparation provided fast and accurate analysis. The PAN-PS-DVB and PAN-PBA 96-blade SPME coatings were evaluated for extraction of analytes in a wide range of polarity (log P=2.8 to -3.7), and they demonstrated efficient extraction recovery (3.5-98.9% for PAN-PS-DVB and 4.0-74.1% for PAN-PBA) for both polar and non-polar groups of compounds. Reusability, reproducibility, and reliability of the system were evaluated. The results demonstrated that both coatings presented chemical and mechanical stability and long-lasting extraction efficiency for more than 100 usages in phosphate-buffered saline (PBS) and human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

UHPLC determination of catechins for the quality control of green tea.

PubMed

Naldi, Marina; Fiori, Jessica; Gotti, Roberto; Périat, Aurélie; Veuthey, Jean-Luc; Guillarme, Davy; Andrisano, Vincenza

2014-01-01

An ultra-high performance liquid chromatography (UHPLC) with UV detection method was developed for the fast quantitation of the most represented and biologically important green tea catechins and caffeine. UHPLC system was equipped with C18 analytical column (50mm×2.1mm, 1.8μm), utilizing a mobile phase composed of pH 2.5 triethanolamine phosphate buffer (0.1M) and acetonitrile in a gradient elution mode; under these conditions six major catechins and caffeine were separated in a 3min run. The method was fully validated in terms of precision, detection and quantification limits, linearity, accuracy, and it was applied to the identification and quantification of catechins and caffeine present in green tea infusions. In particular, commercially available green tea leaves samples of different geographical origin (Sencha, Ceylon Green and Lung Ching) were used for infusion preparations (water at 85°C for 15min). The selectivity of the developed UHPLC method was confirmed by comparison with UHPLC-MS/MS analysis. The recovery of the main six catechins and caffeine on the three analyzed commercial tea samples ranged from 94 to 108% (n=3). Limits of detection (LOD) were comprised in the range 0.1-0.4μgmL(-1). An orthogonal micellar electrokinetic (MEKC) method was applied for comparative purposes on selectivity and quantitative data. The combined use of the results obtained by the two techniques allowed for a fast confirmation on quantitative characterization of commercial samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Spinel type CoFe oxide porous nanosheets as magnetic adsorbents with fast removal ability and facile separation.

PubMed

Ge, X; Gu, C D; Wang, X L; Tu, J P

2015-09-15

Adsorption is often time consuming due to slow diffusion kinetic. Sizing he adsorbent down might help to accelerate adsorption. For CoFe spinel oxide, a magnetically separable adsorbent, the preparation of nanosheets faces many challenges including phase separation, grain growth and difficulty in preparing two-dimensional materials. In this work, we prepared porous CoFe oxide nanosheet with chemical formula of Co2.698Fe0.302O4 through topochemical transformation of a CoFe precursor, which has a layered double hydroxide (LDH) analogue structure and a large interlayer spacing. The LDH precursor was synthesized from a cheap deep eutectic solvent (DES) system. The calcined Co2.698Fe0.302O4 has small grain size (10-20nm), nanosheet morphology, and porous structure, which contribute to a large specific surface area of 79.5m(2)g(-1). The Co2.698Fe0.302O4 nanosheets show fast removal ability and good adsorption capacity for both organic waste (305mgg(-1) in 5min for Congo red) and toxic heavy metal ion (5.27mgg(-1) in 30min for Cr (VI)). Furthermore, the Co2.698Fe0.302O4 can be separated magnetically. Considering the precursor can be prepared through a fast, simple, surfactant-free and high-yield synthetic strategy, this work should have practical significance in fabricating adsorbents. Copyright © 2015 Elsevier Inc. All rights reserved.

Small bowel preparations for capsule endoscopy with mannitol and simethicone: a prospective, randomized, clinical trial.

PubMed

Chen, Hong-bin; Huang, Yue; Chen, Su-yu; Song, Hui-wen; Li, Xiao-lin; Dai, Dong-lin; Xie, Jia-tia; He, Song; Zhao, Yuan-yuan; Huang, Chun; Zhang, Sheng-jun; Yang, Lin-na

2011-04-01

There is no consensus concerning small bowel preparation before capsule endoscopy (CE). This study evaluated the effects of 4 regimens on small bowel cleansing and diagnostic yield. Patients were randomly divided into 4 groups. Group A consumed a clear liquid diet after lunch on the day before CE, followed by overnight fasting. Group B took 250 mL 20% mannitol and 1 L 0.9% saline orally at 05:00 hours on the day of the procedure. In group C, the same regimen was taken at 20:00 hours on the day before and at 05:00 hours on the day of CE. In group D, in addition to the group C regimen, 20 mL oral simethicone was taken 30 minutes before CE. Two hundred patients were prospectively enrolled, and 7 were excluded from the final analysis because of incomplete small bowel transit. No significant difference was noted among the 4 groups for small bowel transit time. Bowel preparation in group D was significantly better than for the other regimens for overall cleansing of the proximal small bowel, and showed improved overall cleansing of the distal small bowel when compared with 10-hours overnight fasting. Pathological lesions of the proximal and distal small bowel were, respectively, achieved in 82 and 74 patients, mostly distributed in group D. Small bowel preparation that involves split-dose oral mannitol plus single-dose simethicone for CE can improve mucosal visualization and subsequent diagnostic yield when compared with 10-hours overnight fasting.

Fe3O4@Polypyrrole Microspheres with High Magnetization and Superparamagnetism for Efficient and Fast Removal of Pb(II) Ions

NASA Astrophysics Data System (ADS)

Zhang, Wei; Zhu, Wanyan; Xu, Wutong; Wang, Yan; Li, Ning; Zhang, Tingting; Wang, Hui

2017-12-01

Core-shell structured Fe3O4@PPy microspheres are synthesized successfully through a facile polyol reduction method in combination with a modified Stöber method. We show that the as-prepared Fe3O4@PPy microspheres with high saturation magnetization, superparamagnetism, and good dispersibility have a high efficient adsorption capacity for high efficient removal of Pb(II) ions of up to 391.71 mg g-1 and a fast adsorption equilibrium time of 20 min. Furthermore, the lead-adsorbed Fe3O4@PPy microspheres can be rapidly separated from solution because of the excellent superparamagnetic properties. The composite Fe3O4@PPy microspheres are characterized using X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and vibrating sample magnetometer (VSM). The adsorption data from our experiments show that the adsorption process fits well with the pseudosecond- order kinetic model and the adsorption isotherm follows the Langmuir isotherm model. The thermodynamic studies show that the adsorption of Pb(II) on Fe3O4@PPy microspheres is an endothermic and spontaneous process. Comprehensive comparison among adsorbents for the removal of Pb(II) ions that literature reported, reusability, high adsorption efficiency, fast adsorption equilibrium, and rapid magnetic separation make these Fe3O4@PPy microspheres very promising application for removal of Pb(II) ions from contaminated water.

A study on rate of infestation to Sarcocystis cysts in supplied raw hamburgers.

PubMed

Nematollahia, Ahmad; Khoshkerdar, Afsaneh; Helan, Javad Ashrafi; Shahbazi, Parisa; Hassanzadeh, Parviz

2015-06-01

This study was carried on for determination of presence of Sarcocystis cysts in raw hamburgers in Tabriz North West of Iran. Ninety-six samples of industrial (70 % meat content) and traditional (30 % meat content) hamburgers (80 samples industrial and 16 samples traditional) were obtained from retail fast food stores. The samples were examined by gross examination, and microscopic examination methods consist impression smear and peptic digestion. Macroscopic cysts did not observed in any of the samples in gross examination. Microscopic study showed that from 96 samples 54 (56.25 %) samples were infected by at least one bradyzoites of Sarcocystis. From 54 infected samples, 45 industrial hamburgers and nine traditional hamburgers samples were infected. Statistical analysis showed that there was not significant differences between industrial and traditional hamburgers in infection to Sarcocystis. Infestation of hamburgers to Sarcocystis in summer was higher than other seasons but this difference was not significant. In Iran, beef meat is used for preparation of 70 % of hamburger and infestation of cattle to sarcocystosis was reported in many investigations in Iran. With regard to the high prevalence of Sarcocystis infection in meat products such as hamburgers in this study, it is strongly recommended to avoid eating raw or under-cooked hamburgers or keep them at freezing temperature for at least 3-5 days.

prepare_taxa_charts.py: A Python program to automate generation of publication ready taxonomic pie chart images from QIIME.

PubMed

Lakhujani, Vijay; Badapanda, Chandan

2017-06-01

QIIME (Quantitative Insights Into Microbial Ecology) is one of the most popular open-source bioinformatics suite for performing metagenome, 16S rRNA amplicon and Internal Transcribed Spacer (ITS) data analysis. Although, it is very comprehensive and powerful tool, it lacks a method to provide publication ready taxonomic pie charts. The script plot_taxa_summary . py bundled with QIIME generate a html file and a folder containing taxonomic pie chart and legend as separate images. The images have randomly generated alphanumeric names. Therefore, it is difficult to associate the pie chart with the legend and the corresponding sample identifier. Even if the option to have the legend within the html file is selected while executing plot_taxa_summary . py , it is very tedious to crop a complete image (having both the pie chart and the legend) due to unequal image sizes. It requires a lot of time to manually prepare the pie charts for multiple samples for publication purpose. Moreover, there are chances of error while identifying the pie chart and legend pair due to random alphanumeric names of the images. To bypass all these bottlenecks and make this process efficient, we have developed a python based program, prepare_taxa_charts . py , to automate the renaming, cropping and merging of taxonomic pie chart and corresponding legend image into a single, good quality publication ready image. This program not only augments the functionality of plot_taxa_summary . py but is also very fast in terms of CPU time and user friendly.

Structural and electrochemical properties of Gd-doped Li4Ti5O12 as anode material with improved rate capability for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Qianyu; Verde, Michael G.; Seo, Joon Kyo; Li, Xi; Meng, Y. Shirley

2015-04-01

Pristine and Gd-doped Li4Ti5O12 (LTO) in the form of Li4-x/3Ti5-2x/3GdxO12 (x = 0.05, 0.10 and 0.15) were prepared by a simple solid-state reaction in air. The structural and electrochemical properties of the as-prepared powders were characterized using X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). XRD revealed that only a small amount of the dopant can enter the lattice structure of LTO; excessive addition beyond x = 0.10 resulted in a discrete Gd2O3 impurity phase. The Gd doping did not change the spinel structure and electrochemical reaction process of LTO. The average particle size of as-prepared samples ranged between 0.5 and 1.5 μm. The Gd-doped materials showed much improved rate capability and specific capacity compared with undoped LTO. In particular, Li4-x/3Ti5-2x/3GdxO12 (x = 0.5) exhibited the best rate capability and cycling stability among all samples. Beyond this doping level, however, Gd2O3 impurity phase in the LTO led to adverse electrochemical performance. The rate capability of the anode material made from the modified powder is significantly improved when discharged at high current rates due to the reduced charge transfer resistance and fast lithium insertion/extraction kinetics.

Simple Sample Preparation Method for Direct Microbial Identification and Susceptibility Testing From Positive Blood Cultures.

PubMed

Pan, Hong-Wei; Li, Wei; Li, Rong-Guo; Li, Yong; Zhang, Yi; Sun, En-Hua

2018-01-01

Rapid identification and determination of the antibiotic susceptibility profiles of the infectious agents in patients with bloodstream infections are critical steps in choosing an effective targeted antibiotic for treatment. However, there has been minimal effort focused on developing combined methods for the simultaneous direct identification and antibiotic susceptibility determination of bacteria in positive blood cultures. In this study, we constructed a lysis-centrifugation-wash procedure to prepare a bacterial pellet from positive blood cultures, which can be used directly for identification by matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF MS) and antibiotic susceptibility testing by the Vitek 2 system. The method was evaluated using a total of 129 clinical bacteria-positive blood cultures. The whole sample preparation process could be completed in <15 min. The correct rate of direct MALDI-TOF MS identification was 96.49% for gram-negative bacteria and 97.22% for gram-positive bacteria. Vitek 2 antimicrobial susceptibility testing of gram-negative bacteria showed an agreement rate of antimicrobial categories of 96.89% with a minor error, major error, and very major error rate of 2.63, 0.24, and 0.24%, respectively. Category agreement of antimicrobials against gram-positive bacteria was 92.81%, with a minor error, major error, and very major error rate of 4.51, 1.22, and 1.46%, respectively. These results indicated that our direct antibiotic susceptibility analysis method worked well compared to the conventional culture-dependent laboratory method. Overall, this fast, easy, and accurate method can facilitate the direct identification and antibiotic susceptibility testing of bacteria in positive blood cultures.

Fast Track Teacher Education: A Review of the Research Literature on "Teach For All" Schemes

ERIC Educational Resources Information Center

McConney, Andrew; Price, Anne; Woods-McConney, Amanda

2012-01-01

This review of the research literature was commissioned by the New Zealand Post-Primary Teachers Association (PPTA) Te Wehengarua as a means of informing the decision-making of the Association and its members about the Teach For All (TFA) scheme seeking to prepare teachers for New Zealand's schools. The systematic review is about fast track…

Liquid-Spray Formulation Of Scopolamine

NASA Technical Reports Server (NTRS)

Putcha, Lakshmi; Cintron, Nitza M.

1992-01-01

Scopolamine, fast-acting anticholinergic drug, formulated into drops administered intranasally. Formulation very useful for people who need immediate relief from motion sickness, and they can administer it to themselves. Also used in other clinical situations in which fast-acting anticholinergic medication required. Modified into such other forms as gel preparation, aqueous-base ointment, or aerosol spray or mist; also dispensed in metered-dose delivery system.

Neoliberalism and the Demise of Public Education: The Corporatization of Schools of Education

ERIC Educational Resources Information Center

Baltodano, Marta

2012-01-01

Neoliberalism has brought fundamental changes to the way schools of education prepare professional educators; among them is the pressure for schools of education to produce fast-track teacher preparation programs that bypass traditional requirements. Due to the privatization of public education, a new market has emerged to train educators and…

Bulk-scaffolded hydrogen storage and releasing materials and methods for preparing and using same

DOEpatents

Autrey, S Thomas [West Richland, WA; Karkamkar, Abhijeet J [Richland, WA; Gutowska, Anna [Richland, WA; Li, Liyu [Richland, WA; Li, Xiaohong S [Richland, WA; Shin, Yongsoon [Richland, WA

2011-06-21

Compositions are disclosed for storing and releasing hydrogen and methods for preparing and using same. These hydrogen storage and releasing materials exhibit fast release rates at low release temperatures without unwanted side reactions, thus preserving desired levels of purity and enabling applications in combustion and fuel cell applications.

FAST-Future Academic Scholars in Teaching: A High-Engagement Development Program for Future STEM Faculty

ERIC Educational Resources Information Center

Vergara, Claudia E.; Urban-Lurain, Mark; Campa, Henry, III; Cheruvelil, Kendra S.; Ebert-May, Diane; Fata-Hartley, Cori; Johnston, Kevin

2014-01-01

Doctoral granting institutions prepare future faculty members for academic positions at institutions of higher education across the nation. Growing concerns about whether these institutions are adequately preparing students to meet the demands of a changing academic environment have prompted several reform efforts. We describe a professional…

Artificial receptor-functionalized nanoshell: facile preparation, fast separation and specific protein recognition

NASA Astrophysics Data System (ADS)

Ouyang, Ruizhuo; Lei, Jianping; Ju, Huangxian

2010-05-01

This work combined molecular imprinting technology with superparamagnetic nanospheres as the core to prepare artificial receptor-functionalized magnetic nanoparticles for separation of homologous proteins. Using dopamine as a functional monomer, novel surface protein-imprinted superparamagnetic polydopamine (PDA) core-shell nanoparticles were successfully prepared in physiological conditions, which could maintain the natural structure of a protein template and achieved the development of molecularly imprinted polymers (MIPs) from one dimension to zero dimension for efficient recognition towards large biomolecules. The resultant nanoparticles could be used for convenient magnetic separation of homologous proteins with high specificity. The nanoparticles possessed good monodispersibility, uniform surface morphology and high saturation magnetization value. The bound amounts of template proteins measured by both indirect and direct methods were in good agreement. The maximum number of imprinted cavities on the surface of the bovine hemoglobin (Hb)-imprinted nanoshell was 2.21 × 1018 g - 1, which well matched their maximum binding capacity toward bovine Hb. Both the simple method for preparation of MIPs and the magnetic nanospheres showed good application potential in fast separation, effective concentration and selective biosensing of large protein molecules.

Global Cell Proteome Profiling, Phospho-signaling and Quantitative 
Proteomics for Identification of New Biomarkers in Acute Myeloid 
Leukemia Patients

PubMed Central

Aasebø, Elise; Forthun, Rakel B.; Berven, Frode; Selheim, Frode; Hernandez-Valladares, Maria

2016-01-01

The identification of protein biomarkers for acute myeloid leukemia (AML) that could find applications in AML diagnosis and prognosis, treatment and the selection for bone marrow transplant requires substantial comparative analyses of the proteomes from AML patients. In the past years, several studies have suggested some biomarkers for AML diagnosis or AML classification using methods for sample preparation with low proteome coverage and low resolution mass spectrometers. However, most of the studies did not follow up, confirm or validate their candidates with more patient samples. Current proteomics methods, new high resolution and fast mass spectrometers allow the identification and quantification of several thousands of proteins obtained from few tens of μg of AML cell lysate. Enrichment methods for posttranslational modifications (PTM), such as phosphorylation, can isolate several thousands of site-specific phosphorylated peptides from AML patient samples, which subsequently can be quantified with high confidence in new mass spectrometers. While recent reports aiming to propose proteomic or phosphoproteomic biomarkers on the studied AML patient samples have taken advantage of the technological progress, the access to large cohorts of AML patients to sample from and the availability of appropriate control samples still remain challenging. PMID:26306748

Effect of gamma-irradiation on thermal decomposition kinetics, X-ray diffraction pattern and spectral properties of tris(1,2-diaminoethane)nickel(II)sulphate

NASA Astrophysics Data System (ADS)

Jayashri, T. A.; Krishnan, G.; Rema Rani, N.

2014-12-01

Tris(1,2-diaminoethane)nickel(II)sulphate was prepared, and characterised by various chemical and spectral techniques. The sample was irradiated with 60Co gamma rays for varying doses. Sulphite ion and ammonia were detected and estimated in the irradiated samples. Non-isothermal decomposition kinetics, X-ray diffraction pattern, Fourier transform infrared spectroscopy, electronic, fast atom bombardment mass spectra, and surface morphology of the complex were studied before and after irradiation. Kinetic parameters were evaluated by integral, differential, and approximation methods. Irradiation enhanced thermal decomposition, lowering thermal and kinetic parameters. The mechanism of decomposition is controlled by R3 function. From X-ray diffraction studies, change in lattice parameters and subsequent changes in unit cell volume and average crystallite size were observed. Both unirradiated and irradiated samples of the complex belong to trigonal crystal system. Decrease in the intensity of the peaks was observed in the infrared spectra of irradiated samples. Electronic spectral studies revealed that the M-L interaction is unaffected by irradiation. Mass spectral studies showed that the fragmentation patterns of the unirradiated and irradiated samples are similar. The additional fragment with m/z 256 found in the irradiated sample is attributed to S8+. Surface morphology of the complex changed upon irradiation.

Insulin Effects on Glucose Tolerance, Hypermetabolic Response, and Circadian-metabolic Protein Expression in a Rat Burn and Disuse Model

DTIC Science & Technology

2014-04-23

laboratory, body mass, GTT, and protein expression values for fasted healthy rats subjected to housing in metabolic cages, the stress of sham and GTT...in IBH rats compared with VBH and CC. Insulin was withheld for 24 h, and rats were fasted 10 h in preparation for the procedure. Glucose tolerance...timeline. Animals were fasted for 10 h prior to testing, which was performed on day 7 or 8 for cage control rats and day 14 for insulin and vehicle

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

Collister, R.; Gwinner, G.; Tandecki, M.

We present the isotope shifts of the 7s 1/2 to 7p 1/2 transition for francium isotopes ²⁰⁶⁻²¹³Fr with reference to ²²¹Fr collected from two experimental periods. The shifts are measured on a sample of atoms prepared within a magneto-optical trap by a fast sweep of radio-frequency sidebands applied to a carrier laser. King plot analysis, which includes literature values for 7s 1/2 to 7p 3/2 isotope shifts, provides a field shift constant ratio of 1.0520(10) and a difference between the specific mass shift constants of 170(100) GHz amu between the D₁ and D₂ transitions, of sufficient precision to differentiate betweenmore » ab initio calculations.« less

Effects for rapid conversion from abalone shell to hydroxyapaptite nanosheets by ionic surfactants.

PubMed

Zhong, Shengnan; Wen, Zhenliang; Chen, Jingdi; Li, Qian; Shi, Xuetao; Ding, Shinnjyh; Zhang, Qiqing

2017-08-01

Hydroxyapatite (HAP) has been widely used for repairing or substituting human hard tissues. In this paper, two typical ionic surfactants, cation hexadecyltrimethylammonium bromide (CTAB) and anion sodium dodecyl sulfate (SDS), were used for rapid conversion of HAP from abalone shell. From field emission scanning electron microscopy (FESEM), the prepared HAP is flake-like structure. From X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and thermal analysis, these samples contain a small amount of calcium carbonate whose content gradually increases by increasing the surfactants. The results showed that the HAP formed fast on the layer of abalone shell powder with the assistance of CTAB and SDS. Copyright © 2017 Elsevier B.V. All rights reserved.

Separating inverse spin Hall voltage and spin rectification voltage by inverting spin injection direction

NASA Astrophysics Data System (ADS)

Zhang, Wenxu; Peng, Bin; Han, Fangbin; Wang, Qiuru; Soh, Wee Tee; Ong, Chong Kim; Zhang, Wanli

2016-03-01

We develop a method for universally resolving the important issue of separating the inverse spin Hall effect (ISHE) from the spin rectification effect (SRE) signal. This method is based on the consideration that the two effects depend on the spin injection direction: The ISHE is an odd function of the spin injection direction while the SRE is independent on it. Thus, the inversion of the spin injection direction changes the ISHE voltage signal, while the SRE voltage remains. It applies generally to analyzing the different voltage contributions without fitting them to special line shapes. This fast and simple method can be used in a wide frequency range and has the flexibility of sample preparation.

Optical properties of Pr-doped BaY2F8

NASA Astrophysics Data System (ADS)

Andrade, Adriano B.; de Mello, Ana C. S.; Rezende, Marcos V. dos S.; Baldochi, Sonia L.; Valerio, Mário E. G.

2014-08-01

Crystalline samples of Pr-doped BaY2F8 (BaYF) were prepared by zone melting technique. The pure phase obtained was identified by X-ray diffraction measurement. Optical absorption result was evaluated and it showed that the formation of the absorption bands can be connected to color centers generated by radiation in the matrix. Radioluminescence emission measurements after excitation by X-ray showed that the material exhibited components responsible for long lasting phosphorescence. Short decay times were also evaluated, the measurements showed a fast component around 70 ns associated to the 4f15d1 → 4f2 transition of the Pr3+ ion. The Thermoluminescence (TL) results indicate the presence of two trapping centers.

New radiocarbon measurement methods in the Hertelendi Laboratory, Hungary

NASA Astrophysics Data System (ADS)

Janovics, Róbert; Major, István; Rinyu, László; Veres, Mihály; Molnár, Mihály

2013-04-01

In this paper we present two very different and novel methods for C-14 measurement from dissolved inorganic carbonate (DIC) of water samples. A new LSC sample preparation method for liquid scintillation C-14 measurements was implemented in the ATOMKI. The first method uses direct absorption into a special absorbent (Carbosorb E®) and a following liquid scintillation measurement. Typical sample size is 20-40 litre of water. The developed CO2 absorption method is fast, and simple. The C-14 activities is measured by an ultra low background LSC (TRI-CARB 3170 TR/SL, Perkin Elmer) including quenching parameter (tSIE).The corresponding limit of C-14 dating is 31200 year. Several tests were executed with old borehole CO2 gas without significant content of C-14 and also performed on samples of known C-14 activities between 29 and 7000 pMC, previously measured by GPC. The combined uncertainty of the described determination is about 2 % in the case of recent carbon. It is a very cost-effective and easy to use method based on a novel and simple static absorption process for the CO2 extracted from groundwater. The other very sensitive method is based on accelerator mass spectrometry (AMS) using gas ion source. This method does not require graphite generation and a small volume of water sample (1-20mL) is enough for the radiocarbon measurement. The procedure is very similar to pre-treatment of carbonate contained sample preparation for stable isotope measurement with gasbench technique. We applied a MICADAS type accelerator mass spectrometry (AMS) with gas ion source for C-14 analysis. The radiocarbon content of water was sat free with phosphoric acid and then the headspace gas was rinsed vials. The whole measurement needs only 20 min of each sample. The precision of measurement is better than 1% for modern samples. The preparation is vastly reduced compared to the other AMS methods and principally allows fully automated measurements of groundwater samples with an auto-sampler. The presented two new methods can be suitable for C-14 measurements and dating of hydrological, and environmental samples as well. The new AMS facility in ATOMKI (Debrecen, Hungary) using an EnvironMICADAS AMS system with gas ion source has a great potential in groundwater C-14 analyses. The research was supported by the by TÁMOP-4.2.2.A-11/1/KONV and the Hungarian NSF (OTKA MB08-A 81515)

Technique for fast and efficient hierarchical clustering

DOEpatents

Stork, Christopher

2013-10-08

A fast and efficient technique for hierarchical clustering of samples in a dataset includes compressing the dataset to reduce a number of variables within each of the samples of the dataset. A nearest neighbor matrix is generated to identify nearest neighbor pairs between the samples based on differences between the variables of the samples. The samples are arranged into a hierarchy that groups the samples based on the nearest neighbor matrix. The hierarchy is rendered to a display to graphically illustrate similarities or differences between the samples.

Optimization of sample preparation by central composite design for multi-class determination of veterinary drugs in bovine muscle, kidney and liver by ultra-high-performance liquid chromatographic-tandem mass spectrometry.

PubMed

Rizzetti, Tiele M; de Souza, Maiara P; Prestes, Osmar D; Adaime, Martha B; Zanella, Renato

2018-04-25

In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver. Copyright © 2017 Elsevier Ltd. All rights reserved.

Ion distribution in dry polyelectrolyte multilayers: a neutron reflectometry study.

PubMed

Ghoussoub, Yara E; Zerball, Maximilian; Fares, Hadi M; Ankner, John F; von Klitzing, Regine; Schlenoff, Joseph B

2018-02-28

Ultrathin films of complexed polycation poly(diallyldimethylammonium), PDADMA, and polyanion poly(styrenesulfonate), PSS, were prepared on silicon wafers using the layer-by-layer adsorption technique. When terminated with PDADMA, all films had excess PDADMA, which was balanced by counterions. Neutron reflectivity of these as-made multilayers was compared with measurements on multilayers which had been further processed to ensure 1 : 1 stoichiometry of PDADMA and PSS. The compositions of all films, including polymers and counterions, were determined experimentally rather than by fitting, reducing the number of fit parameters required to model the reflectivity. For each sample, acetate, either protiated, CH 3 COO - , or deuterated, CD 3 COO - , served as the counterion. All films were maintained dry under vacuum. Scattering length density profiles were constrained to fit reflectivity data from samples having either counterion. The best fits were obtained with uniform counterion concentrations, even for stoichiometric samples that had been exposed to PDADMA for ca. 5 minutes, showing that surprisingly fast and complete transport of excess cationic charge occurs throughout the multilayer during its construction.

Monitoring of the microbiota profile in nukadoko, a naturally fermented rice bran bed for pickling vegetables.

PubMed

Ono, Hiroshi; Nishio, Shoko; Tsurii, Jun; Kawamoto, Tetsuhiro; Sonomoto, Kenji; Nakayama, Jiro

2014-11-01

Nukadoko is a fermented rice bran mash traditionally used for pickling vegetables in Japan. To date, the production of both homemade and commercial nukadoko depends on natural fermentation without using starter cultures. Here, we monitored chemical and microbiological changes in the initial batch fermentation of nukadoko. Nukadoko samples were prepared by spontaneous fermentation of four different brands of rice bran, and microbiome dynamics were analyzed for 2 months. In the first week, non-Lactobacillales lactic acid bacteria (LAB) species, which differed among the samples, grew proportionally to pH decrease and lactate increase. Thereafter, Lactobacillus plantarum started growing and consumed residual sugars, causing further lactate increase in nukadoko. Finally, microbial communities in all tested nukadoko samples were dominated by L. plantarum. Taken together, our results suggest that the mixture of the fast-growing LAB species and slow-growing L. plantarum may be used as a suitable starter culture to promote the initial fermentation of nukadoko. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Atmospheric pressure plasma deposition of antimicrobial coatings on non-woven textiles

NASA Astrophysics Data System (ADS)

Nikiforov, Anton Yu.; Deng, Xiaolong; Onyshchenko, Iuliia; Vujosevic, Danijela; Vuksanovic, Vineta; Cvelbar, Uros; De Geyter, Nathalie; Morent, Rino; Leys, Christophe

2016-08-01

A simple method for preparation of nanoparticle incorporated non-woven fabric with high antibacterial efficiency has been proposed based on atmospheric pressure plasma process. In this work direct current plasma jet stabilized by fast nitrogen flow was used as a plasma deposition source. Three different types of the nanoparticles (silver, copper and zinc oxide nanoparticles) were employed as antimicrobial agents. X-ray photoelectron spectroscopy (XPS) measurements have shown a positive chemical shift observed for Ag 3d 5/2 (at 368.1 eV) suggests that silver nanoparticles (AgNPs) are partly oxidized during the deposition. The surface chemistry and the antibacterial activity of the samples against Staphylococcus aureus and Escherichia coli were investigated and analyzed. It is shown that the samples loaded with nanoparticles of Ag and Cu and having the barrier layer of 10 nm characterized by almost 97% of bacterial reduction whereas the samples with ZnO nanoparticles provide 86% reduction of Staphylococcus aureus. Contribution to the topical issue "6th Central European Symposium on Plasma Chemistry (CESPC-6)", edited by Nicolas Gherardi, Ester Marotta and Cristina Paradisi

Bioavailability, pharmacokinetics, and safety of riociguat given as an oral suspension or crushed tablet with and without food

PubMed Central

Frey, Reiner; Becker, Corina; Unger, Sigrun; Wensing, Georg; Mück, Wolfgang

2016-01-01

Abstract Riociguat is approved for the treatment of pulmonary arterial hypertension and chronic thromboembolic pulmonary hypertension. Some patients have difficulty swallowing tablets; therefore, 2 randomized, nonblinded, crossover studies compared the relative bioavailability of riociguat oral suspensions and immediate-release (IR) tablet and of crushed-tablet preparations versus whole IR tablet. In study 1, 30 healthy subjects received 5 single riociguat doses: 0.3 and 2.4 mg (0.15 mg/mL suspensions), 0.15 mg (0.03 mg/mL), and 1.0 mg (whole IR tablet) under fasted conditions and 2.4 mg (0.15 mg/mL) after a high-fat, high-calorie American-style breakfast. In study 2, 25 healthy men received 4 single 2.5-mg doses: whole IR tablet and crushed IR tablet suspended in applesauce and water, respectively, under fasted conditions, and whole IR tablet after a continental breakfast. In study 1, dose-normalized pharmacokinetics of riociguat oral suspensions and 1.0-mg whole IR tablet were similar in fasted conditions; 90% confidence intervals for riociguat area under the curve (AUC) to dose and mean maximum concentration (Cmax) to dose were within bioequivalence criteria. After food, dose-normalized AUC and Cmax decreased by 15% and 38%, respectively. In study 2, riociguat exposure was similar for all preparations; AUC ratios for crushed-IR-tablet preparations to whole IR tablet were within bioequivalence criteria. The Cmax increased by 17% for crushed IR tablet in water versus whole IR tablet. Food intake decreased Cmax of the whole tablet by 16%, with unaltered AUC versus fasted conditions. Riociguat bioavailability was similar between the oral suspensions and the whole IR tablet; exposure was similar between whole IR tablet and crushed-IR-tablet preparations. Minor food effects were observed. Results suggest that riociguat formulations are interchangeable. PMID:27162630

Bioavailability, pharmacokinetics, and safety of riociguat given as an oral suspension or crushed tablet with and without food.

PubMed

Saleh, Soundos; Frey, Reiner; Becker, Corina; Unger, Sigrun; Wensing, Georg; Mück, Wolfgang

2016-03-01

Riociguat is approved for the treatment of pulmonary arterial hypertension and chronic thromboembolic pulmonary hypertension. Some patients have difficulty swallowing tablets; therefore, 2 randomized, nonblinded, crossover studies compared the relative bioavailability of riociguat oral suspensions and immediate-release (IR) tablet and of crushed-tablet preparations versus whole IR tablet. In study 1, 30 healthy subjects received 5 single riociguat doses: 0.3 and 2.4 mg (0.15 mg/mL suspensions), 0.15 mg (0.03 mg/mL), and 1.0 mg (whole IR tablet) under fasted conditions and 2.4 mg (0.15 mg/mL) after a high-fat, high-calorie American-style breakfast. In study 2, 25 healthy men received 4 single 2.5-mg doses: whole IR tablet and crushed IR tablet suspended in applesauce and water, respectively, under fasted conditions, and whole IR tablet after a continental breakfast. In study 1, dose-normalized pharmacokinetics of riociguat oral suspensions and 1.0-mg whole IR tablet were similar in fasted conditions; 90% confidence intervals for riociguat area under the curve (AUC) to dose and mean maximum concentration (C max) to dose were within bioequivalence criteria. After food, dose-normalized AUC and C max decreased by 15% and 38%, respectively. In study 2, riociguat exposure was similar for all preparations; AUC ratios for crushed-IR-tablet preparations to whole IR tablet were within bioequivalence criteria. The C max increased by 17% for crushed IR tablet in water versus whole IR tablet. Food intake decreased C max of the whole tablet by 16%, with unaltered AUC versus fasted conditions. Riociguat bioavailability was similar between the oral suspensions and the whole IR tablet; exposure was similar between whole IR tablet and crushed-IR-tablet preparations. Minor food effects were observed. Results suggest that riociguat formulations are interchangeable.

Fast detection and characterization of organic and inorganic gunshot residues on the hands of suspects by CMV-GC-MS and LIBS.

PubMed

Tarifa, Anamary; Almirall, José R

2015-05-01

A rapid method for the characterization of both organic and inorganic components of gunshot residues (GSR) is proposed as an alternative tool to facilitate the identification of a suspected shooter. In this study, two fast screening methods were developed and optimized for the detection of organic compounds and inorganic components indicative of GSR presence on the hands of shooters and non-shooters. The proposed methods consist of headspace extraction of volatile organic compounds using a capillary microextraction of volatiles (CMV) device previously reported as a high-efficiency sampler followed by detection by GC-MS. This novel sampling technique has the potential to yield fast results (<2min sampling) and high sensitivity capable of detecting 3ng of diphenylamine (DPA) and 8ng of nitroglycerine (NG). Direct analysis of the headspace of over 50 swabs collected from the hands of suspected shooters (and non-shooters) provides information regarding VOCs present on their hands. In addition, a fast laser induced breakdown spectroscopy (LIBS) screening method for the detection of the inorganic components indicative of the presence of GSR (Sb, Pb and Ba) is described. The sampling method for the inorganics consists of liquid extraction of the target elements from the same cotton swabs (previously analyzed for VOCs) and an additional 30 swab samples followed by spiking 1μL of the extract solution onto a Teflon disk and then analyzed by LIBS. Advantages of LIBS include fast analysis (~12s per sample) and high selectivity and sensitivity, with expected LODs 0.1-18ng for each of the target elements after sampling. The analytical performance of the LIBS method is also compared to previously reported methods (inductively coupled plasma-optical emission spectroscopy). The combination of fast CMV sampling, unambiguous organic compound identification with GC-MS and fast LIBS analysis provides the basis for a new comprehensive screening method for GSR. Copyright © 2015 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Ultrasonic-based membrane aided sample preparation of urine proteomes.

PubMed

Jesus, Jemmyson Romário; Santos, Hugo M; López-Fernández, H; Lodeiro, Carlos; Arruda, Marco Aurélio Zezzi; Capelo, J L

2018-02-01

A new ultrafast ultrasonic-based method for shotgun proteomics as well as label-free protein quantification in urine samples is developed. The method first separates the urine proteins using nitrocellulose-based membranes and then proteins are in-membrane digested using trypsin. The enzymatic digestion process is accelerated from overnight to four minutes using a sonoreactor ultrasonic device. Overall, the sample treatment pipeline comprising protein separation, digestion and identification is done in just 3h. The process is assessed using urine of healthy volunteers. The method shows that male can be differentiated from female using the protein content of urine in a fast, easy and straightforward way. 232 and 226 proteins are identified in urine of male and female, respectively. From this, 162 are common to both genders, whilst 70 are unique to male and 64 to female. From the 162 common proteins, 13 are present at levels statistically different (p < 0.05). The method matches the analytical minimalism concept as outlined by Halls, as each stage of this analysis is evaluated to minimize the time, cost, sample requirement, reagent consumption, energy requirements and production of waste products. Copyright © 2017 Elsevier B.V. All rights reserved.

Atmospheric Solid Analysis Probe Coupled to Ion Mobility Spectrometry-Mass Spectrometry, a Fast and Simple Method for Polyalphaolefin Characterization

NASA Astrophysics Data System (ADS)

Mendes Siqueira, Anna Luiza; Beaumesnil, Mathieu; Hubert-Roux, Marie; Loutelier-Bourhis, Corinne; Afonso, Carlos; Bai, Yang; Courtiade, Marion; Racaud, Amandine

2018-05-01

Polyalphaolefins (PAOs) are polymers produced from linear alpha olefins through catalytic oligomerization processes. The PAOs are known as synthetic high-performance base stock fluids used to improve the efficiency of many other synthetic products. In this study, we report the direct characterization of PAOs using atmospheric solid analysis probe (ASAP) coupled with ion mobility spectrometry-mass spectrometry (IMS-MS). We studied different PAOs grades exhibiting low- and high-viscosity index. Specific adjustments of the ASAP source parameters permitted the monitoring of ionization processes as three mechanisms could occur for these compounds: hydride abstraction, nitrogen addition, and/or the formation of [M-2H]+• ions. Several series of fragment ions were obtained, which allowed the identification of the alpha olefin used to synthesize the PAO. The use of the ion mobility separation dimension provides information on isomeric species. In addition, the drift time versus m/z plots permitted rapid comparison between PAO samples and to evidence their complexity. These 2D plots appear as fingerprints of PAO samples. To conclude, the resort to ASAP-IMS-MS provides a rapid characterization of the PAO samples in a direct analysis approach, without any sample preparation.

Comparison of extraction induced by emulsion breaking, ultrasonic extraction and wet digestion procedures for determination of metals in edible oil samples in Turkey using ICP-OES.

PubMed

Bakircioglu, Dilek; Kurtulus, Yasemin Bakircioglu; Yurtsever, Selcuk

2013-06-01

The content of elements (Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in edible oils (sunflower, hazelnut, canola, corn and olive oils) from Turkey was determined using inductively coupled plasma optical emission spectrometry (ICP-OES) after ultrasonic extraction, wet digestion, and extraction induced by emulsion breaking procedures (EIEB). In order to evaluate the best sample preparation procedure, EIEB procedure was compared by ultrasonic extraction and wet digestion procedures. The results in the samples (minimum-maximum in mgkg(-1)) were : 0.022-0.058, Cr 0.126-7.106, Cu 0.570-4.504, Fe 8.004-12.588, Mn 0.035-0.054, Ni 0.908-2.182, Pb 0.099-0.134 and Zn 2.206-8.982. The EIEB procedure was found to be fast, reliable, simple, and excellent in comparison with the other studied procedures. The recovery test was performed by spiking the samples with known amounts of the metals in the form of organometallic standards and applying the EIEB procedure. The recoveries were in the range of 96-109%. Copyright © 2012 Elsevier Ltd. All rights reserved.

A compact LIBS system for industrial applications

NASA Astrophysics Data System (ADS)

Noharet, B.; Sterner, C.; Irebo, T.; Gurell, J.; Bengtson, A.; Vainik, R.; Karlsson, H.; Illy, E.

2015-03-01

In recent years, laser-induced breakdown spectroscopy (LIBS) has been established as a promising analytical tool for online chemical analysis. The emitted light spectrum is analyzed for instantaneous determination of the elemental composition of the sample, enabling on-line classification of materials. Two major strengths of the technique are the possibilities to perform both fast and remote chemical analysis to determine the elemental composition of the samples under test. In order to reduce the size of LIBS systems, the use of a compact Q-switched diode-pumped solid-state laser (DPSSL) in a LIBS system is evaluated for the industrial sorting of aluminium alloys. The DPSSL, which delivers 150μJ pulses of high beam quality at more than 7KHz repetition rate, provides irradiance on the target that is appropriate for LIBS measurements. The experimental results indicate that alloy classification and quantitative analysis are possible on scrap aluminium samples placed 50 cm apart from the focusing and collecting lenses, without sample preparation. Similar calibration curves and limits of detection are obtained for traditional high-energy low-frequency flashlamp-pumped and low-energy high-frequency diode-pumped lasers, showing the applicability of compact diode-pumped lasers for industrial LIBS applications.

Spherical Nanoindentation Stress-Strain Measurements of BOR-60 14YWT-NFA1 Irradiated Tubes

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

Weaver, Jordan; Carvajal Nunez, Ursula; Krumwiede, David

Spherical nanoindentation stress-strain protocols were applied to characterize unirradiated and fast neutron irradiated nanostructured ferritic alloy (NFA) 14YWT and compared against Berkovich nanohardness and available tensile data. The predicted uniaxial yield strength from spherical, 100 and 5 micron radii, indentation yield strength measurements was 1100-1400 MPa which compares well with the predictions from Berkovich nanohardness, 1200 MPa, and available tensile data, ~1100 MPa. However, spherical indentation measurements predict an increase in the uniaxial yield strength of ~1 GPa while Berkovich nanohardness measurements predict an increase of only ~250 MPa. No tensile data exists on the irradiated condition. It is believedmore » the difference in the predicted uniaxial yield strength between spherical and Berkovich nanoindentation are due to a low number of tests on the irradiated sample combined with the significant heterogeneity in the microstructure, the differences in sensitivity to sample preparation on the irradiated sample between the two indentation protocols , and/or in how strain localizes under the indenter with the possibility of dislocation channeling under Berkovich hardness indents leading to strain softening. Nanoindentation capabilities to test neutron irradiated samples in a radiological area were realized.« less

Development of molecularly imprinted column-on line-two dimensional liquid chromatography for rapidly and selectively monitoring estradiol in cosmetics.

PubMed

Guo, Pengqi; Xu, Xinya; Xian, Liang; Ge, Yanhui; Luo, Zhimin; Du, Wei; Jing, Wanghui; Zeng, Aiguo; Chang, Chun; Fu, Qiang

2016-12-01

Nowadays, the illegal use of estradiol in cosmetics has caused a series of events which endangering public health seriously. Therefore, it is imperative to establish a simple, fast and specific method for monitoring the illegal use of estradiol in cosmetics. In current study, we developed a molecular imprinted monolithic column two dimensional liquid chromatography method (MIMC-2D-LC) for rapid and selective determination of estradiol in various cosmetic samples. The best polymerization, morphology, structure property, surface groups, and the adsorption performance of the prepared material were investigated. The MIMC-2D-LC was validated and successfully used for detecting estradiol in cosmetic samples with good selectivity, sensitivity, efficiency and reproducibility. The linear range of the MIMC-2D-LC for estradiol was 0.5-50μgg -1 with the limit of detection of 0.08μgg -1 . Finally, six batches of cosmetic samples obtained from local markets were tested by the proposed method. The test results showed that the illegal use of estradiol still existed in the commercially available samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Future Assets, Student Talent (FAST)

NASA Technical Reports Server (NTRS)

1992-01-01

Future Assets, Student Talent (FAST) motivates and prepares talented students with disabilities to further their education and achieve High Tech and professional employment. The FAST program is managed by local professionals, business, and industry leaders; it is modeled after High School High Tech project TAKE CHARGE started in Los Angeles in 1983. Through cooperative efforts of Alabama Department of Education, Vocational Rehabilitation, Adult and Children Services, and the President's Committee on Employment of People with Disabilities, north central Alabama was chosen as the second site for a High School High Tech project. In 1986 local business, industry, education, government agencies, and rehabilitation representatives started FAST. The program objectives and goals, results and accomplishments, and survey results are included.

Research on identification and determination of mixed pesticides in apples using surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Zhai, Chen; Li, Yongyu; Peng, Yankun; Xu, Tianfeng; Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei

2015-05-01

Residual pesticides in fruits and vegetables have become one of the major food safety concerns around the world. At present, routine analytical methods used for the determination of pesticide residue on the surface of fruits and vegetables are destructive, complex, time-consuming, high cost and not environmentally friendly. In this study, a novel Surface Enhanced Raman Spectroscopy (SERS) method with silver colloid was developed for fast and sensitive nondestructive detection of residual pesticides in fruits and vegetables by using a self-developed Raman system. SERS technology is a combination of Raman spectroscopy and nanotechnology. SERS can greatly enhance the Raman signal intensity, achieve single-molecule detection, and has a simple sample pre-treatment characteristic of high sensitivity and no damage; in recent years it has begun to be used in food safety testing research. In this study a rapid and sensitive method was developed to identify and analyze mixed pesticides of chlorpyrifos, deltamethrin and acetamiprid in apple samples by SERS. Silver colloid was used for SERS measurement by hydroxylamine hydrochloride reduced. The advantages of this method are seen in its fast preparation at room temperature, good reproducibility and immediate applicability. Raman spectrum is highly interfered by noise signals and fluorescence background, which make it too complex to get good result. In this study the noise signals and fluorescence background were removed by Savitzky-Golay filter and min-max signal adaptive zooming method. Under optimal conditions, pesticide residues in apple samples can be detected by SERS at 0.005 μg/cm2 and 0.002 μg/cm2 for individual acetamiprid and thiram, respectively. When mixing the two pesticides at low concentrations, their characteristic peaks can still be identified from the SERS spectrum of the mixture. Based on the synthesized material and its application in SERS operation, the method represents an ultrasensitive SERS performance in apple samples detection without sample pre-treatment, which indicates that it could be served as a useful means in monitoring pesticide residues.

Nanomechanical sensor applied to blood culture pellets: a fast approach to determine the antibiotic susceptibility against agents of bloodstream infections.

PubMed

Stupar, P; Opota, O; Longo, G; Prod'hom, G; Dietler, G; Greub, G; Kasas, S

2017-06-01

The management of bloodstream infection, a life-threatening disease, largely relies on early detection of infecting microorganisms and accurate determination of their antibiotic susceptibility to reduce both mortality and morbidity. Recently we developed a new technique based on atomic force microscopy capable of detecting movements of biologic samples at the nanoscale. Such sensor is able to monitor the response of bacteria to antibiotic's pressure, allowing a fast and versatile susceptibility test. Furthermore, rapid preparation of a bacterial pellet from a positive blood culture can improve downstream characterization of the recovered pathogen as a result of the increased bacterial concentration obtained. Using artificially inoculated blood cultures, we combined these two innovative procedures and validated them in double-blind experiments to determine the susceptibility and resistance of Escherichia coli strains (ATCC 25933 as susceptible and a characterized clinical isolate as resistant strain) towards a selection of antibiotics commonly used in clinical settings. On the basis of the variance of the sensor movements, we were able to positively discriminate the resistant from the susceptible E. coli strains in 16 of 17 blindly investigated cases. Furthermore, we defined a variance change threshold of 60% that discriminates susceptible from resistant strains. By combining the nanomotion sensor with the rapid preparation method of blood culture pellets, we obtained an innovative, rapid and relatively accurate method for antibiotic susceptibility test directly from positive blood culture bottles, without the need for bacterial subculture. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Is scratch-cooking a cost-effective way to prepare healthy school meals with US Department of Agriculture foods?

PubMed

Woodward-Lopez, Gail; Kao, Janice; Kiesel, Kristin; Lewis Miller, Markell; Boyle, Maria; Drago-Ferguson, Soledad; Braff-Guajardo, Ellen; Crawford, Patricia

2014-09-01

Despite the resurgence of interest in scratch-cooking as a way to increase the quality and appeal of school meals, many school districts are concerned about the cost implications of switching to scratch-cooking. US Department of Agriculture (USDA) Foods are the single largest source of ingredients for school meals, and about half of USDA Foods are diverted for processing before being sent to the school district. We aimed to determine whether school lunch entrées made in a district from basic or raw USDA Foods ingredients can be healthier and less expensive to prepare than those sent to external processors. This cross-sectional study examined the relationship between the extent of scratch-cooking and the nutritional content and cost to prepare entrées. Information was gathered by interview with school foodservice personnel and from school foodservice records from a convenience sample of 10 school districts in California that employed varying degrees of scratch-cooking and is diverse in terms of geographic location and the sociodemographics of the student body. The sample included all elementary school lunch entrées that contain USDA Foods offered during October 2010 for a total sample of 146 entrées. Ordinary least squares regressions were used to test for statistically significant differences in cost and nutrient content of entrées according to the level of scratch-cooking. There was no significant relationship between total costs and level of scratch-cooking. Entrées with the highest scratch-cooking scores had significantly lower food costs, higher labor costs, and not significantly different total costs compared with entrées with no scratch-cooking. Nutrient content was not consistently associated with scratch-cooking, but scratch-cooked entrées did include a larger variety of non-fast-food-type entrées. The findings suggest that scratch-cooking can be a cost-effective way to expand the variety of healthy school lunches prepared with USDA Foods. Copyright © 2014 Academy of Nutrition and Dietetics. Published by Elsevier Inc. All rights reserved.

Language Teacher Education in a Fast-Changing World. Anthology Series 29. Selected Papers from a Seminar on Language Teacher Education in a Fast-Changing World (April 1992).

ERIC Educational Resources Information Center

Sadtono, Eugenius, Ed.

Selected papers from a 1992 seminar on innovations in language teacher education include: "Collaboration in Assessment: Empowering the Individual Course Member" (Leslie Dickinson); "An Approach to the Evaluation of ELT Preparation Programs" (Stephen J. Gaies); "Human Resources Development in the Management of English Language Programs: An…

Effect of preparation methods and doping on the structural and tunable emissions of CdS

NASA Astrophysics Data System (ADS)

Mohamed, Mohamed Bakr; Abdel-Kader, M. H.; Alhazime, Ali A.; Almarashi, Jamal Q. M.

2018-03-01

Fe, Mn and Mg doped CdS samples were prepared by thermolysis method in air and under flow of nitrogen. Structural, compositional and optical properties of the prepared samples were investigated using x-ray powder diffraction (XRD), scanning electron microscope (SEM/EDS mapping), Fourier transform infrared red (FTIR), UV-vis absorption and photoluminescence (PL) spectroscopes. Rietveld refinement of x-ray data showed that all the undoped and doped CdS samples prepared in air and under flow of nitrogen have both cubic and hexagonal structures. The percentages of hexagonal and cubic phases for all prepared samples were determined. The crystallite size increased for CdS prepared under flow of N2 compared with the sample prepared in air. The energy gap of all the samples was calculated using UV data. The intensity of PL emission changed according to the method of preparation and the kind of doping elements. PL emission revealed a blue shift for CdS prepared in air compared with CdS prepared under flow of nitrogen; also all doped samples showed a red shift of PL spectra compared with undoped samples. Undoped and doped CdS with Fe and Mg samples emitted violet and blue sub-spectra. Mn doped CdS prepared in air revealed violet, blue and yellow sub-spectra, while the sample prepared under flow of N2 emitted violet, blue and green sub-spectra.

An ion-imprinted silica-supported organic-inorganic hybrid sorbent prepared by a surface imprinting technique combined with a polysaccharide incorporated sol-gel process for selective separation of cadmium(II) from aqueous solution.

PubMed

Li, Feng; Jiang, Hongquan; Zhang, Shusheng

2007-03-15

Ion-imprinting concept and polysaccharide incorporated sol-gel process were applied to the preparation of a new silica-supported organic-inorganic hybrid sorbent for selective separation of Cd(II) from aqueous solution. In the prepared shell/core composite sorbent, covalently surface coating on the supporting silica gel was achieved by using a Cd(II)-imprinting sol-gel process starting from an inorganic precursor, gamma-glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS). The sorbent was prepared through self-hydrolysis of GPTMS, self-condensation and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, in combination with in situ covalent cross-linking of CS with partial amine shielded by Cd(II) complexation. Extraction of the imprinting molecules left a predetermined arrangement of ligands and tailored binding pockets for Cd(II). The prepared sorbent was characterized by using X-ray energy dispersion spectroscopy (EDX), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Batch experiments were conducted to study the sorption performance by removal of Cd(II) when present singly or in binary system, an aqueous Cd(II) and Zn(II) mixture. The ion-imprinted composite sorbent offered a fast kinetics for the sorption of Cd(II) and the maximum capacity was 1.14mmolg(-1). The uptake capacity of the imprinted sorbent and the selectivity coefficient were much higher than that of the non-imprinted sorbent. The imprinted sorbent exhibited high reusability. The prepared functional sorbent was shown to be promising for the preconcentration of cadmium in environmental and biological samples.

In vitro investigation of the cleaning efficacy, shaping ability, preparation time and file deformation of continuous rotary, reciprocating rotary and manual instrumentations in primary molars.

PubMed

Ramazani, Nahid; Mohammadi, Abbas; Amirabadi, Foroogh; Ramazani, Mohsen; Ehsani, Farzane

2016-01-01

Background. Efficient canal preparation is the key to successful root canal treatment. This study aimed to assess the cleaning and shaping ability, preparation time and file deformation of rotary, reciprocating and manual instrumentation in canal preparation of primary molars. Methods. The mesiobuccal canals of 64 extracted primary mandibular second molars were injected with India ink. The samples were randomly divided into one control and three experimental groups. Experimental groups were instrumented with K-file, Mtwo in continuous rotation and Reciproc in reciprocating motion, respectively. The control group received no treatment. The files were discarded after four applications. Shaping ability was evaluated using CBCT. After clearing, ink removal was scored. Preparation time and file fracture or deformation was also recorded. Data were analyzed with SPSS 19 using chi-squared, Fisher's exact test, Kruskal-Wallis and post hoc tests at a significance level of 0.05. Results. Considering cleanliness, at coronal third Reciproc was better than K-file (P < 0.001), but not more effective than Mtwo (P = 0.080). Furthermore, Mtwo leaved the canal cleaner than K-file (P = 0.001). In the middle third, only Reciproc exhibited better cleaning efficacy than K-file (P = 0.005). In the apical third, no difference was detected between the groups (P = 0.794). Regarding shaping ability, no differences were found between Reciproc and Mtwo (P = 1.00). Meanwhile, both displayed better shaping efficacy than K-file (P < 0.05). Between each two groups, there were differences in preparation time (P < 0.05), with Reciproc being the fastest. No file failure occurred. Conclusion. Fast and sufficient cleaning and shaping could be achieved with Mtwo and especially with Reciproc.

Chromium(III)-imprinted silica gel for speciation analysis of chromium in environmental water samples with ICP-MS detection.

PubMed

Zhang, Nan; Suleiman, Jibrin Sabo; He, Man; Hu, Bin

2008-04-15

A new chromium(III)-imprinted 3-(2-aminoethylamino) propyltrimethoxysilane (AAPTS)-functionalized silica gel sorbent was synthesized by a surface imprinting technique and was employed as a selective solid-phase extraction material for speciation analysis of chromium in environmental water samples prior to its determination by inductively coupled plasma mass spectrometry (ICP-MS). The prepared Cr(III)-imprinted silica gel shows the selectivity coefficient of more than 700 for Cr(III) in the presence of Mn(II). The static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cr(III) were 30.5 mg g(-1) and 13.4 mg g(-1). It was also found that Cr(VI) could be adsorbed at low pH by the prepared imprinted silica gel, and this finding makes it feasible to enrich and determine Cr(VI) at low pH without adding reducing reagents. The imprinted silica gel sorbent offered a fast kinetics for the adsorption and desorption of both chromium species. Under the optimized conditions, the detection limits of 4.43 pg mL(-1) and 8.30 pg mL(-1) with the relative standard deviations (R.S.D.s) of 4.44% and 4.41% (C=0.5 ng mL(-1), n=7) for Cr(III) and Cr(VI) were obtained, respectively. The proposed method was successfully applied to the speciation of trace chromium in environmental water samples. To validate the proposed method, two certified reference materials were analyzed and the determined values were in a good agreement with the certified values. The developed method is rapid, selective, sensitive and applicable for the speciation of trace chromium in environmental water samples.

Effects of fasting on intestinal transfer of sugars and amino acids in vitro

PubMed Central

Newey, H.; Sanford, P. A.; Smyth, D. H.

1970-01-01

1. Transfer of sugars, amino acids and fluid and metabolism of glucose were studied with everted sacs of small intestine prepared from fed and 3-day fasted rats. 2. In the absence of glucose there was some evidence for increased intestinal transfer of sugars and amino acids in fasted animals. In the presence of glucose there was in general decrease in transfer of amino acids and fluid. 3. In fasted animals glucose transfer was reduced except in the lower ileum, and there was a general reduction in glucose metabolism. 4. Because of the large reduction in gut weight in fasted animals, expressing transfer on a weight basis is considered not to be a valid procedure in studying the effects of fasting on intestinal transfer. 5. The results have been discussed in relation to effects of fasting on energy availability, efficiency of transfer mechanisms, permeability of the intestine and the value of in vitro methods in the study of physiological absorption. PMID:5499792

Magnetic molecularly imprinted polymer for the selective extraction of quercetagetin from Calendula officinalis extract.

PubMed

Ma, Run-Tian; Shi, Yan-Ping

2015-03-01

A new magnetic molecularly imprinted polymers (MMIPs) for quercetagetin was prepared by surface molecular imprinting method using super paramagnetic core-shell nanoparticle as the supporter. Acrylamide as the functional monomer, ethyleneglycol dimethacrylate as the crosslinker and acetonitrile as the porogen were applied in the preparation process. Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Vibrating sample magnetometer (VSM) were applied to characterize the MMIPs, and High performance liquid chromatography (HPLC) was utilized to analyze the target analytes. The selectivity of quercetagetin MMIPs was evaluated according to their recognition to template and its analogues. Excellent binding for quercetagetin was observed in MMIPs adsorption experiment, and the adsorption isotherm models analysis showed that the homogeneous binding sites were distributed on the surface of the MMIPs. The MMIPs were employed as adsorbents in solid phase extraction for the determination of quercetagetin in Calendula officinalis extracts. Furthermore, this method is fast, simple and could fulfill the determination and extraction of quercetagetin from herbal extract. Copyright © 2014 Elsevier B.V. All rights reserved.

New materials for solid-phase extraction and multiclass high-performance liquid chromatographic analysis of pesticides in grapes.

PubMed

Melo, Lucio F C; Collins, Carol H; Jardim, Isabel C S F

2004-04-02

Sample preparation procedures which included the use of new aminopropyl (NH2) and octadecyl (C18) solid-phase extraction (SPE) sorbents are proposed for the simultaneous multiclass determination of the fungicide benomyl and of the herbicides tebuthiuron, diuron, simazine, atrazine, and ametryn in grapes, using single wavelength high-performance liquid chromatography. Sorbent preparation uses a fast, easy, and effective procedure to obtain silica-based materials, made by depositing polysiloxanes on a silica support followed by thermal immobilization. Recovery results of the compounds, after elution from the SPE cartridges, indicate that the most efficient system employed silica loaded with 40% of an aminofunctional polydimethylsiloxane as sorbent, using dichloromethane:methanol (95:5, v/v) as eluent. Method validation, carried out in agreement with International Conference on Harmonization directives, was performed at three fortification levels (100, 200, and 1000 microg kg(-1)). Limits of detection and quantification show that the method developed can be used to detect the pesticides at concentrations below the maximum residue levels established by Codex Alimentarius, the US Environmental Protection Agency, the European Union, and Brazilian legislation.

BrAD-seq: Breath Adapter Directional sequencing: a streamlined, ultra-simple and fast library preparation protocol for strand specific mRNA library construction.

PubMed

Townsley, Brad T; Covington, Michael F; Ichihashi, Yasunori; Zumstein, Kristina; Sinha, Neelima R

2015-01-01

Next Generation Sequencing (NGS) is driving rapid advancement in biological understanding and RNA-sequencing (RNA-seq) has become an indispensable tool for biology and medicine. There is a growing need for access to these technologies although preparation of NGS libraries remains a bottleneck to wider adoption. Here we report a novel method for the production of strand specific RNA-seq libraries utilizing the terminal breathing of double-stranded cDNA to capture and incorporate a sequencing adapter. Breath Adapter Directional sequencing (BrAD-seq) reduces sample handling and requires far fewer enzymatic steps than most available methods to produce high quality strand-specific RNA-seq libraries. The method we present is optimized for 3-prime Digital Gene Expression (DGE) libraries and can easily extend to full transcript coverage shotgun (SHO) type strand-specific libraries and is modularized to accommodate a diversity of RNA and DNA input materials. BrAD-seq offers a highly streamlined and inexpensive option for RNA-seq libraries.

Evaluation of phases in Pu-C-O and (U, Pu)-C-O systems by X-ray diffractometry and chemical analysis

NASA Astrophysics Data System (ADS)

Jain, G. C.; Ganguly, C.

1993-12-01

Preparation and characterisation of the carbides of uranium, plutonium and mixed uranium and plutonium form a part of advanced fuel development programs for fast breeder reactors. In the present study, the compositions of the phases of Pu-C-O and (U.Pu)-C-O systems have been determined by chemical analysis and lattice parameter measurement. The carbide samples have been prepared by vacuum carbothermic synthesis of tabletted oxide-graphite powder mixture. Dependence of stoichiometry of Pu 2C 3 phase on the oxygen content of Pu(C,O) phase in Pu(C,O) + Pu 2C 3 phase mixture has been evaluated. Stoichiometry and oxygen solubility of (U 0.3Pu 0.7)(C,O) phase in multiple phase mixture have been determined. Segregation of plutonium in (U,Pu) 2C 3 phase of (U,Pu)(C,O) + (U,Pu) 2C 3 phase mixture and its dependence on the oxygen content of (U,Pu)(C,O) phase have also been determined from the measurement of the lattice parameter of (U,Pu) 2C 3 phase.

Fast Filtration of Bacterial or Mammalian Suspension Cell Cultures for Optimal Metabolomics Results

PubMed Central

Bordag, Natalie; Janakiraman, Vijay; Nachtigall, Jonny; González Maldonado, Sandra; Bethan, Bianca; Laine, Jean-Philippe; Fux, Elie

2016-01-01

The metabolome offers real time detection of the adaptive, multi-parametric response of the organisms to environmental changes, pathophysiological stimuli or genetic modifications and thus rationalizes the optimization of cell cultures in bioprocessing. In bioprocessing the measurement of physiological intracellular metabolite levels is imperative for successful applications. However, a sampling method applicable to all cell types with little to no validation effort which simultaneously offers high recovery rates, high metabolite coverage and sufficient removal of extracellular contaminations is still missing. Here, quenching, centrifugation and fast filtration were compared and fast filtration in combination with a stabilizing washing solution was identified as the most promising sampling method. Different influencing factors such as filter type, vacuum pressure, washing solutions were comprehensively tested. The improved fast filtration method (MxP® FastQuench) followed by routine lipid/polar extraction delivers a broad metabolite coverage and recovery reflecting well physiological intracellular metabolite levels for different cell types, such as bacteria (Escherichia coli) as well as mammalian cells chinese hamster ovary (CHO) and mouse myeloma cells (NS0).The proposed MxP® FastQuench allows sampling, i.e. separation of cells from medium with washing and quenching, in less than 30 seconds and is robustly designed to be applicable to all cell types. The washing solution contains the carbon source respectively the 13C-labeled carbon source to avoid nutritional stress during sampling. This method is also compatible with automation which would further reduce sampling times and the variability of metabolite profiling data. PMID:27438065

Characterization of the Particle Size and Polydispersity of Dicumarol Using Solid-State NMR Spectroscopy.

PubMed

Dempah, Kassibla Elodie; Lubach, Joseph W; Munson, Eric J

2017-03-06

A variety of particle sizes of a model compound, dicumarol, were prepared and characterized in order to investigate the correlation between particle size and solid-state NMR (SSNMR) proton spin-lattice relaxation ( 1 H T 1 ) times. Conventional laser diffraction and scanning electron microscopy were used as particle size measurement techniques and showed crystalline dicumarol samples with sizes ranging from tens of micrometers to a few micrometers. Dicumarol samples were prepared using both bottom-up and top-down particle size control approaches, via antisolvent microprecipitation and cryogrinding. It was observed that smaller particles of dicumarol generally had shorter 1 H T 1 times than larger ones. Additionally, cryomilled particles had the shortest 1 H T 1 times encountered (8 s). SSNMR 1 H T 1 times of all the samples were measured and showed as-received dicumarol to have a T 1 of 1500 s, whereas the 1 H T 1 times of the precipitated samples ranged from 20 to 80 s, with no apparent change in the physical form of dicumarol. Physical mixtures of different sized particles were also analyzed to determine the effect of sample inhomogeneity on 1 H T 1 values. Mixtures of cryoground and as-received dicumarol were clearly inhomogeneous as they did not fit well to a one-component relaxation model, but could be fit much better to a two-component model with both fast-and slow-relaxing regimes. Results indicate that samples of crystalline dicumarol containing two significantly different particle size populations could be deconvoluted solely based on their differences in 1 H T 1 times. Relative populations of each particle size regime could also be approximated using two-component fitting models. Using NMR theory on spin diffusion as a reference, and taking into account the presence of crystal defects, a model for the correlation between the particle size of dicumarol and its 1 H T 1 time was proposed.

Sample stacking of fast-moving anions in capillary zone electrophoresis with pH-suppressed electroosmotic flow.

PubMed

Quirino, J P; Terabe, S

1999-07-30

On-line sample concentration of fast moving inorganic anions by large volume sample stacking (LVSS) and field enhanced sample injection (FESI) with a water plug under acidic conditions is presented. Detection sensitivity enhancements were around 100 and 1000-fold for LVSS and FESI, respectively. However, reproducibility and linearity of response in the LVSS approach is superior compared to the FESI approach.

Determination of ractopamine in pork using a magnetic molecularly imprinted polymer as adsorbent followed by HPLC.

PubMed

Tang, Yiwei; Gao, Jingwen; Liu, Xiuying; Lan, Jianxing; Gao, Xue; Ma, Yong; Li, Min; Li, Jianrong

2016-06-15

A new magnetic molecularly imprinted polymers (MMIPs) for separation and concentration of ractopamine (RAC) were prepared using surface molecular imprinting technique with methacryloyl chloride as functional monomer and RAC as template. The MMIPs were characterized using transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and vibrating sample magnetometer. The results of re-binding experiments indicated that the MMIPs had fast adsorption kinetics and could reach binding equilibrium within 20 min, and the adsorption capacity of the MMIPs was 2.87-fold higher than that of the corresponding non-imprinted polymer. The selectivity of the MMIPs was evaluated according to its recognition to RAC and its analogues. The synthesized MMIPs were successfully applied to extraction, followed by high performance liquid chromatography to determine RAC in real food samples. Spiked recoveries ranged from 73.60% to 94.5%, with relative standard deviations of <11.17%. Copyright © 2016 Elsevier Ltd. All rights reserved.

EASI-IMS an expedite and secure technique to screen for 25I-NBOH in blotter papers.

PubMed

de Morais, Damila Rodrigues; Barbosa, Ingrid Lopes; Cunha, Kelly Francisco; Tripodi, Guilherme Lucas; Angolini, Célio Fernando Figueiredo; Franco, Marcos Fernando; de Aquino, Elvis Medeiros; Eberlin, Marcos Nogueira; Costa, Jose Luiz

2017-10-01

The increasing number of new psychoactive substances (NPS) and their quick worldwide spreading, often only slightly modified in the form of new derivatives and analogues, have brought the need for fast, wide-ranging, and unequivocal identification methods in clinical and forensic investigations. Because it usually provides secure results, gas chromatography coupled to mass spectrometry (GC-MS) has been routinely employed as the standard technique for the detection of NPS in blotter papers. For 25I-NBOH (N-(2-hydroxybenzyl)-2-(4-iodo-2,5-dimethoxyphenyl)ethan-1-aminium), however, GC-MS analysis of an blotter paper extract leads to incorrect results. In this work, we investigated whether easy ambient sonic-spray mass spectrometry imaging (EASI-IMS), and ambient ionization MS method can be applied directly to the surface of the sample requiring therefore no extraction or sample preparations, would serve as an efficient, sensitive, and secure alternative for 25I-NBOH screening. Copyright © 2017 John Wiley & Sons, Ltd.

Simplified multi-element analysis of ground and instant coffees by ICP-OES and FAAS.

PubMed

Szymczycha-Madeja, Anna; Welna, Maja; Pohl, Pawel

2015-01-01

A simplified alternative to the wet digestion sample preparation procedure for roasted ground and instant coffees has been developed and validated for the determination of different elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, Zn) and flame atomic absorption spectrometry (FAAS) (Ca, Fe, K, Mg, Na). The proposed procedure, i.e. the ultrasound-assisted solubilisation in aqua regia, is quite fast and simple, requires minimal use of reagents, and demonstrated good analytical performance, i.e. accuracy from -4.7% to 1.9%, precision within 0.5-8.6% and recovery in the range 93.5-103%. Detection limits of elements were from 0.086 ng ml(-1) (Sr) to 40 ng ml(-1) (Fe). A preliminary classification of 18 samples of ground and instant coffees was successfully made based on concentrations of selected elements and using principal component analysis and hierarchic cluster analysis.

Analysis of potential migrants from plastic materials in milk by liquid chromatography-mass spectrometry with liquid-liquid extraction and low-temperature purification.

PubMed

Bodai, Zsolt; Szabó, Bálint Sámuel; Novák, Márton; Hámori, Susanne; Nyiri, Zoltán; Rikker, Tamás; Eke, Zsuzsanna

2014-10-15

A simple and fast analytical method was developed for the determination of six UV stabilizers (Cyasorb UV-1164, Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, and Tinuvin 1577) and five antioxidants (Irgafos 168, Irganox 1010, Irganox 3114, Irganox 3790, and Irganox 565) in milk. For sample preparation liquid-liquid extraction with low-temperature purification combined with centrifugation was used to remove fats, proteins, and sugars. After the cleanup step, the sample was analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). External standard and matrix calibrations were tested. External calibration proved to be acceptable for Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, Irganox 3114, and Irganox 3790. The method was successfully validated with matrix calibration for all compounds. Method detection limits were between 0.25 and 10 μg/kg. Accuracies ranged from 93 to 109%, and intraday precisions were <13%.

Effect of cooking procedures of kiymali pide, a traditional Turkish fast-food, on destruction of Escherichia coli O157:H7.

PubMed

Ilhak, Osman İrfan; Dikici, Abdullah; Can, Ozlem Pelin; Seker, Pınar; Oksüztepe, Gülsüm; Calıcıoğlu, Mehmet

2013-06-01

The objective of the present study was to obtain data about cooking time and temperature of kiymali pide in the restaurants and to investigate thermal inactivation of E. coli O157:H7 during experimental kiymali pide making. A field study was conducted in randomly selected 23 of 87 pide restaurants. Processing parameters including oven temperature, cooking period and post-cooking temperature were determined. Kiymali pide samples were prepared using ground beef filling experimentally inoculated with E. coli O157:H7 (7.6 log10 CFU/g). Pide samples were cooked at a conventional oven at 180 °C for 180, 240, 270, 300 and 330 s. Results of the current study suggest that cooking kiymali pide at 180 °C for at least 330 s (5.5 min) may provide sufficient food safety assurance (≥6 log10 CFU/g) for E. coli O157:H7. Copyright © 2013 Elsevier Ltd. All rights reserved.

Authentication of processed meat products by peptidomic analysis using rapid ambient mass spectrometry.

PubMed

Montowska, Magdalena; Alexander, Morgan R; Tucker, Gregory A; Barrett, David A

2015-11-15

We present the application of a novel ambient LESA-MS method for the authentication of processed meat products. A set of 25 species and protein-specific heat stable peptide markers has been detected in processed samples manufactured from beef, pork, horse, chicken and turkey meat. We demonstrate that several peptides derived from myofibrillar and sarcoplasmic proteins are sufficiently resistant to processing to serve as specific markers of processed products. The LESA-MS technique required minimal sample preparation without fractionation and enabled the unambiguous and simultaneous identification of skeletal muscle proteins and peptides as well as other components of animal origin, including the milk protein such as casein alpha-S1, in whole meat product digests. We have identified, for the first time, six fast type II and five slow/cardiac type I MHC peptide markers in various processed meat products. The study demonstrates that complex mixtures of processed proteins/peptides can be examined effectively using this approach. Copyright © 2015 Elsevier Ltd. All rights reserved.

Polymethacrylate-based monoliths as stationary phases for separation of biopolymers and immobilization of enzymes.

PubMed

Martinović, Tamara; Josić, Djuro

2017-11-01

The experiences in the production and application of polymethacrylate-based monolithic supports, since their development almost thirty years ago, are presented. The main driving force for the development of new chromatographic supports was the necessity for the isolation and separation of physiologically active biopolymers and their use for therapeutic purposes. For this sake, a development of a method for fast separation, preventing denaturation and preserving their biological activity was necessary. Development of polysaccharide-based supports, followed by the introduction of polymer-based chromatographic media, is shortly described. This development was followed by the advances in monolithic media that are now used for both large- and small-scale separation of biopolymers and nanoparticles. Finally, a short overview is given about the applications of monoliths for sample displacement chromatography, resulting in isolation of physiologically active biomolecules, such as proteins, protein complexes, and nucleic acid, as well as high-throughput sample preparation for proteomic investigations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of heavy metal ions in water using near-infrared spectroscopy with preconcentration by nano-hydroxyapatite.

PubMed

Ning, Yu; Li, Jihui; Cai, Wensheng; Shao, Xueguang

2012-10-01

A method for simultaneous determination of metal ions in river water was developed by using preconcentration and near-infrared diffuse reflectance spectroscopy (NIRDRS). An inorganic biomaterial, nano-hydroxyapatite (HAP) was used as a high-efficient adsorbent for gathering the ions from water samples. After adsorbing the analytes onto the adsorbent, NIRDRS was measured and partial least squares (PLS) models were established for fast and simultaneous quantitative prediction. With the samples prepared by river water, determination of Pb(2+), Zn(2+), Cu(2+), Cd(2+) and Cr(3+) was investigated. The calibration models of Cu(2+), Cr(3+) and total content were proven to be efficient enough for precise prediction. The determination coefficients (R(2)) of the independent validation were found as high as 0.9924, 0.9869 and 0.9273 for Cu(2+), Cr(3+) and total content, respectively. Therefore, the feasibility of NIRDRS for microanalysis of heavy metal ions in waste water was demonstrated. Copyright © 2012 Elsevier B.V. All rights reserved.

A new validated HPLC-FLD method for detecting ochratoxin A in dry-cured meat and in blue cheese.

PubMed

Dall'asta, C; Galaverna, G; De Dea Lindner, J; Virgili, R; Neviani, E; Dossena, A

2007-09-01

In the present study, a fast and sensitive method for the quantification of ochratoxin A in two lipidicproteic food matrices has been developed. In particular, the sample preparation procedure has been optimized for dry-cured meat products and blue cheeses and tested for several validation parameters (LOD, LOQ, recovery, repeatability and within-laboratory precision). The procedure has been then applied to several dry-cured meat products and blue cheeses from the market.Ochratoxin A has been occasionally found in dry-cured and smoked ham from the market and the contamination occurred both in the outer and in the inner part of the products. Concerning the blue cheese, the occurrence of ochratoxin A is reported for the first time: OTA was occasionally found at low levels (0.1-3 μg/kg) in commercial samples of Roquefort from France and Gorgonzola from Italy, opening a new issue for risk assessment and quality control.

A rapid Fourier-transform infrared (FTIR) spectroscopic method for direct quantification of paracetamol content in solid pharmaceutical formulations

NASA Astrophysics Data System (ADS)

Mallah, Muhammad Ali; Sherazi, Syed Tufail Hussain; Bhanger, Muhammad Iqbal; Mahesar, Sarfaraz Ahmed; Bajeer, Muhammad Ashraf

2015-04-01

A transmission FTIR spectroscopic method was developed for direct, inexpensive and fast quantification of paracetamol content in solid pharmaceutical formulations. In this method paracetamol content is directly analyzed without solvent extraction. KBr pellets were formulated for the acquisition of FTIR spectra in transmission mode. Two chemometric models: simple Beer's law and partial least squares employed over the spectral region of 1800-1000 cm-1 for quantification of paracetamol content had a regression coefficient of (R2) of 0.999. The limits of detection and quantification using FTIR spectroscopy were 0.005 mg g-1 and 0.018 mg g-1, respectively. Study for interference was also done to check effect of the excipients. There was no significant interference from the sample matrix. The results obviously showed the sensitivity of transmission FTIR spectroscopic method for pharmaceutical analysis. This method is green in the sense that it does not require large volumes of hazardous solvents or long run times and avoids prior sample preparation.

Separation of polychlorinated biphenyls by fast gas chromatography.

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

Alvarado, J. S.; Silzer, J.; Lemley, F.

1997-12-01

The separation of commercially available polychlorinated biphenyls (PCBs) by fast gas chromatography (fast GC) has been studied. Aroclor 1254 was separated by using two column types: DB-1 and SPB-608. The fast GC used a split-splitless injector to introduce the sample, followed by a cold trap at -90 C to focus the sample. Rapid heating was used to introduce the sample into the short chromatographic column to decrease band broadening. Hydrogen was the carrier gas at velocities of 100 to 125 cm s-1. Analyses were performed by using an electron capture detector (ECD). Separation was achieved with both columns in lessmore » than 6 min. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost.« less

Direct analysis of deodorants for determination of metals by inductively coupled plasma optical emission spectrometry.

PubMed

da Costa, Wiviane Kássia Oliveira Correia; da Silva, Caroline Santos; Figueiredo, José Fernando Dagnone; Nóbrega, Joaquim Araujo; Paim, Ana Paula Silveira

2018-06-05

A fast and simple dilute-and-shoot procedure for determination of Al, As, Ba, Cd, Cu, Fe, Mg, Mn, Ni, Pb, Sc, Ti, V, Zn and Zr in deodorants by inductively coupled plasma optical emission spectrometry (ICP OES) was developed. Sample preparation was carried out by diluting 1 mL of deodorant sample in 1% (v v -1 ) HNO 3 . The accuracy of the analytical procedure was evaluated using addition and recovery experiments, and recoveries ranged from 80 to 119%. The limits of detection varied from 0.001 to 0.76 mg kg -1 . Nine deodorants samples of different brands were analyzed. The maximum concentrations found (mg kg -1 ) were: Fe (1.0), Mn (0.1), Ti (1.02), V (0.33), Zn (255.2) and Zr (0.5); for Al and Mg, determined concentrations varied from 0.01 to 7.0% and from 0.005 to 1.44 mg kg -1 , respectively, showing wide variation depending on the sample type. The developed procedure was adequate for determining these analytes in routine analysis presenting high sample throughput and demonstrated the feasibility of direct analysis measurements after simple dilution step. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation of dummy template imprinted polymers at surface of silica microparticles for the selective extraction of trace bisphenol A from water samples.

PubMed

Zhao, Wenhui; Sheng, Na; Zhu, Rong; Wei, Fangdi; Cai, Zheng; Zhai, Meijuan; Du, Shuhu; Hu, Qin

2010-07-15

Molecularly imprinted polymers for bisphenol A (BPA) were prepared by using surface molecular imprinting technique. Analogues of BPA, namely 4,4'-dihydroxybiphenyl and 3,3',5,5'-tetrabromobisphenol A, were used as the dummy templates instead of BPA, to avoid the leakage of a trace amount of the target analyte (BPA). The resulting dummy molecularly imprinted polymers (DMIPs) showed the large sorption capacity, high recognition ability and fast binding kinetics for BPA. The maximal sorption capacity was up to 958 micromol g(-1), and it only took 40 min for DMIPs to achieve the sorption equilibrium. The DMIPs were successfully applied to the solid-phase extraction coupled with HPLC/UV for the determination of BPA in water samples. The calibration graph of the analytical method was linear with a correlation coefficient more than 0.999 in the concentration range of 0.0760-0.912 ng mL(-1) of BPA. The limit of detection was 15.2 pg mL(-1) (S/N=3). Recoveries were in the range of 92.9-102% with relative standard deviation (RSD) less than 11%. The trace amounts of BPA in tap water, drinking water, rain and leachate of one-off tableware were determined by the method built, and the satisfactory results were obtained. 2010 Elsevier B.V. All rights reserved.

Omnidirectional anti-reflection properties of vertically align SiO2 nanorod films prepared by electron beam evaporation with glancing angle deposition

NASA Astrophysics Data System (ADS)

Prachachet, R.; Samransuksamer, B.; Horprathum, M.; Eiamchai, P.; Limwichean, S.; Chananonnawathorn, C.; Lertvanithphol, T.; Muthitamongkol, P.; Boonruang, S.; Buranasiri, P.

2018-03-01

Omnidirectional anti-reflection coating nanostructure film have attracted enormous attention for the developments of the optical coating, lenses, light emitting diode, display and photovoltaic. However, fabricated of the omnidirectional antireflection nanostructure film on glass substrate in large area was a challenge topic. In the past two decades, the invention of glancing angle deposition technique as a growth of well-controlled two and three-dimensional morphologies has gained significant attention because of it is simple, fast, cost-effective and high mass production capability. In this present work, the omnidirectional anti-reflection nanostructure coating namely silicon dioxide (SiO2) nanorods has been investigated for optimized high transparent layer at all light incident angle. The SiO2 nanorod films of an optimally low refractive index have been fabricated by electron beam evaporation with the glancing angle deposition technique. The morphological of the prepared sampled were characterized by field-emission scanning electron microscope (FE-SEM) and high-resolution transmission electron microscope (HRTEM). The optical transmission and omnidirectional property of the SiO2 nanorod films were investigated by UV-Vis-NIR spectrophotometer. The measurement were performed at normal incident angle and a full spectral range of 200 - 2000 nm. The angle dependent transmission measure were investigated by rotating the specimen, with incidence angle defined relative to the surface normal of the prepared samples. The morphological characterization results showed that when the glancing angle deposition technique was applied, the vertically align SiO2 nanorods with partially isolated columnar structure can be constructed due to the enhanced shadowing and limited addtom diffusion effect. The average transmission of the vertically align SiO2 nanorods were higher than the glass substrate reference sample over the visible wavelength range at all incident angle due to the transition in the refractive index profile from air to the nanostructure layer that improved the anti-reflection characteristics.

Magnetic covalent triazine framework for rapid extraction of phthalate esters in plastic packaging materials followed by gas chromatography-flame ionization detection.

PubMed

Yan, Zijun; He, Man; Chen, Beibei; Gui, Bo; Wang, Cheng; Hu, Bin

2017-11-24

Covalent triazine frameworks (CTFs), featuring with high surface area, good thermal, chemical and mechanical stability, are good adsorbents in sample pretreatment. Herein, magnetic CTFs/Ni composite was prepared by in situ reduction of nickel ions on CTFs matrix with a solvothermal method. The prepared CTFs/Ni composite exhibited good preparation reproducibility, high chemical stability, and high extraction efficiency for targeted phthalate esters (PAEs) due to π-π interaction and hydrophobic effect. The porous structure of CTFs/Ni composite benefited the fast transfer of target PAEs from aqueous solution to the adsorbents, and the integrated magnetism contributed to the rapid separation of adsorbents from sample and elution solution. Based on it, a novel method of magnetic solid phase extraction (MSPE) combined with gas chromatography-flame ionization detector (GC-FID) was developed for the analysis of PAEs including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexl phthalate (DEHP), and di-n-octyl phthalate (DNOP) in plastic packaging materials. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) for six PAEs were found to be in the range of 0.024-0.085mg/kg. The linear range was 0.32-16mg/kg for DMP, DEP, 0.08-80mg/kg for DBP, 0.16-32mg/kg for BBP, DEHP, and 0.32-32mg/kg for DNOP, respectively. The enrichment factors ranged from 59 to 88-fold (theoretical enrichment factor was 133-fold). The proposed method was successfully applied to the analysis of PAEs in various plastic packaging materials with recoveries in the range of 70.6-119% for the spiked samples. This method is characterized with short operation time, high sensitivity, low consumption of harmful organic solvents and can be extended to the analysis of other trace aromatic compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Media exposure and parental mediation on fast-food consumption among children in metropolitan and suburban Indonesian.

PubMed

Lwin, May O; Malik, Shelly; Ridwan, Hardinsyah; Au, Cyndy Sook Sum

2017-01-01

Fast-food companies have been reproached for rising obesity levels due to aggressive marketing tactics targeted at children. They have countered that parents should be held responsible considering their critical role as nutritional gatekeepers. This study examined the comparative effects of media exposure and parental mediation on Indonesian children's fast food consumption and how the effects compare in the metropolitan versus suburban areas. The sample consisted of 394 child-mother pairs comprising grade three and four children and their mothers from two schools each in Jakarta and Bogor representing 40.9% metropolitan sample and 59.1% suburban sample, respectively. The children completed a guided inclass survey, while the mothers completed a paper-and-pen survey at home. Measures comprised children's weekly media exposure to broadcast media, computer and mobile games, print media, and online and social media, active and restrictive parental mediation strategies, children's fast food consumption and nutrition knowledge. The relationship of media exposure and parental mediation with children's fast food consumption was analyzed using Structural Equation Modelling. Fast food consumption was positively influenced by exposure to broadcast media among metropolitan children, and by exposure to online and social media among suburban children. Active parental mediation was related to lower fast food consumption, but only for suburban children. Active parental mediation is critical in preventing fast food consumption. The media play a key role in influencing fast food consumption, and hence, literacy education is important to alleviate the adverse effects of exposure to junk food marketing.

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 2 2012-01-01 2012-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

Calibrations and Comparisons of Aerosol Spectrometers linking Ground and Airborne Measurements

NASA Astrophysics Data System (ADS)

Williamson, C.; Brock, C. A.; Erdesz, F.

2015-12-01

The nucleation-mode aerosol size spectrometer (NMASS), a fast-time response instrument measuring aerosol size distributions between 5 and 60nm, is to sample in the boundary layer and free troposphere on NASA's Atmospheric Tomography mission (ATom), providing contiguous data with global coverage in all four seasons. In preparation for this the NMASS is calibrated for the expected flight conditions and compatibility studies are made with ground-based instrumentation. The NMASS is comprised of 5 parallel condensation particle counters (CPCs) using perfluoro-tributylamine as a working fluid. Understanding the variation of CPC counting efficiencies with respect to the chemical composition of the sample is important for accurate data analysis and can be used to give indirect information about sample chemical composition. This variation is strongly dependent on the working fluid. The absolute responses and associated variations of the NMASS to ammonium sulfate and limonene ozonolysis products, compounds pertinent to the composition of particles nucleated in the free troposphere and boundary later, are compared to those of butanol, diethylene-glycol and water based CPCs, which are more commonly used in ground-based measurements. While fast time-response is key to measuring aerosol size distributions on flights, high size-resolution is often prioritized for ground-based measurements, and so a scanning mobility particle sizer (SMPS) is commonly used. Inter-comparison between NMASS and SMPS data is non-trivial because of the different working principles and resolutions of the instruments and yet it is vital, for example, for understanding the sources of particles observed during flights and the global relevance of phenomena observed from field stations and in chambers. We report compatibility studies on inversions of data from the SMPS and NMASS, evaluating temporal and spatial resolution and sources of uncertainty.

Resole resin products derived from fractionated organic and aqueous condensates made by fast-pyrolysis of biomass materials

DOEpatents

Chum, Helena L.; Black, Stuart K.; Diebold, James P.; Kreibich, Roland E.

1993-01-01

A process for preparing phenol-formaldehyde resole resins by fractionating organic and aqueous condensates made by fast-pyrolysis of biomass materials while using a carrier gas to move feed into a reactor to produce phenolic-containing/neutrals in which portions of the phenol normally contained in said resins are replaced by a phenolic/neutral fractions extract obtained by fractionation.

Resole resin products derived from fractionated organic and aqueous condensates made by fast-pyrolysis of biomass materials

DOEpatents

Chum, H.L.; Black, S.K.; Diebold, J.P.; Kreibich, R.E.

1993-08-10

A process for preparing phenol-formaldehyde resole resins by fractionating organic and aqueous condensates made by fast-pyrolysis of biomass materials while using a carrier gas to move feed into a reactor to produce phenolic-containing/neutrals in which portions of the phenol normally contained in said resins are replaced by a phenolic/neutral fractions extract obtained by fractionation.

Successful lyophilization by adopting a fast ramp rate during primary drying in protein formulations.

PubMed

Ohori, Ryo; Akita, Tomomi; Yamashita, Chikamasa

2018-06-15

In the lyophilization process for injections, the shelf temperature (T s ) and chamber pressure (P c ) have mainly been investigated to optimize the primary drying process. The objective of this study was to show that lyophilization of protein formulations can be achieved by adopting a fast ramp rate of T s in the beginning of the primary drying process. Bovine serum albumin was used as the model protein, and seven different lyophilized formulations obtained were stored at elevated temperature. We found that although acceptable cake appearance was confirmed by the fast ramp cycle, all formulations of lyophilized cakes obtained by the slow ramp cycle severely collapsed (macrocollapse). It is thought that the collapse in the slow ramp cycle occurred during the shelf ramp in the beginning of primary drying and that insufficient removal of water from the dried matrix caused viscous flow (product collapse). Regarding storage stability, moisture-induced degradation was confirmed in some of the formulations prepared by the slow ramp cycle, whereas all lyophilized BSA formulations prepared by the fast ramp cycle were stable. Thus, the results indicate that the ramp rate appears to be one of the critical operational parameters required to establish a successful lyophilization cycle. Copyright © 2018. Published by Elsevier B.V.

Quality Control of Gamma Irradiated Dwarf Mallow (Malva neglecta Wallr.) Based on Color, Organic Acids, Total Phenolics and Antioxidant Parameters.

PubMed

Pinela, José; Barros, Lillian; Antonio, Amilcar L; Carvalho, Ana Maria; Oliveira, M Beatriz P P; Ferreira, Isabel C F R

2016-04-08

This study addresses the effects of gamma irradiation (1, 5 and 8 kGy) on color, organic acids, total phenolics, total flavonoids, and antioxidant activity of dwarf mallow (Malva neglecta Wallr.). Organic acids were analyzed by ultra fast liquid chromatography (UFLC) coupled to a photodiode array (PDA) detector. Total phenolics and flavonoids were measured by the Folin-Ciocalteu and aluminium chloride colorimetric methods, respectively. The antioxidant activity was evaluated based on the DPPH(•) scavenging activity, reducing power, β-carotene bleaching inhibition and thiobarbituric acid reactive substances (TBARS) formation inhibition. Analyses were performed in the non-irradiated and irradiated plant material, as well as in decoctions obtained from the same samples. The total amounts of organic acids and phenolics recorded in decocted extracts were always higher than those found in the plant material or hydromethanolic extracts, respectively. The DPPH(•) scavenging activity and reducing power were also higher in decocted extracts. The assayed irradiation doses affected differently the organic acids profile. The levels of total phenolics and flavonoids were lower in the hydromethanolic extracts prepared from samples irradiated at 1 kGy (dose that induced color changes) and in decocted extracts prepared from those irradiated at 8 kGy. The last samples also showed a lower antioxidant activity. In turn, irradiation at 5 kGy favored the amounts of total phenolics and flavonoids. Overall, this study contributes to the understanding of the effects of irradiation in indicators of dwarf mallow quality, and highlighted the decoctions for its antioxidant properties.

Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods.

PubMed

Han, Lijun; Matarrita, Jessie; Sapozhnikova, Yelena; Lehotay, Steven J

2016-06-03

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography - tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid ("enhanced matrix removal of lipids") and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500mg for 2.5mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83-98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC-MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70-120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76-85 of the 117 analytes achieved satisfactory results (recoveries of 70-120% and RSD≤20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5-10ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods. Published by Elsevier B.V.

Rapid screening of abused drugs by direct analysis in real time (DART) coupled to time-of-flight mass spectrometry (TOF-MS) combined with ion mobility spectrometry (IMS).

PubMed

Lian, Ru; Wu, Zhongping; Lv, Xiaobao; Rao, Yulan; Li, Haiyang; Li, Jinghua; Wang, Rong; Ni, Chunfang; Zhang, Yurong

2017-10-01

Increasing in cases involving drugs of abuse leads to heavy burden for law enforcement agencies, exacerbating demand for rapid screening technique. In this study, atmospheric pressure ionization technologies including direct analysis in real time (DART) ion source coupled to a time-of-flight mass spectrometer (DART-TOF-MS)as well asdopant-assisted positive photoionization ion mobility spectrometry (DAPP-IMS) without radioactivity were utilized together as the powerful analytical tool for the rapid screening and identification of 53 abused drugs.The limits of detection (LOD) were 0.05-2μg/mL when using DART-TOF-MS and 0.02-2μg when using DAPP-IMS which could satisfy the actual requirement in forensic science laboratory. The advantages of this method included fast response, high-throughput potential, high specificity, and minimal sample preparation. A screening library of reduced mobility (K 0 ), accurate mass of informative precursor ion ([M+H] + ) and fragment ions was established respectively by employing a bench-top DAPP-IMS and TOF-MS in-source collision induced dissociation (CID) mode. Then the standardized screening procedure was developed with criteria for the confirmation of positive result. A total of 50 seized drug samples provided by local forensic laboratory we reanalyzed to testify the utility of the method. This study suggests that a method combing DART-TOF-MS and DAPP-IMS is promising for the rapid screening and identification of abused drugs with minimal sample preparation and absence of chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

Recent progress in preparation and application of microfluidic chip electrophoresis

NASA Astrophysics Data System (ADS)

Cong, Hailin; Xu, Xiaodan; Yu, Bing; Yuan, Hua; Peng, Qiaohong; Tian, Chao

2015-05-01

Since its discovery in 1990, microfluidic chip electrophoresis (MCE) has allowed the development of applications with small size, fast analysis, low cost, high integration density and automatic level, which are easy to carry and have made commercialization efficient. MCE has been widely used in the areas of environmental protection, biochemistry, medicine and health, clinical testing, judicial expertise, food sanitation, pharmaceutical checking, drug testing, agrochemistry, biomedical engineering and life science. As one of the foremost fields in the research of capillary electrophoresis, MCE is the ultimate frontier to develop the miniaturized, integrated, automated all-in-one instruments needed in modern analytical chemistry. By adopting the advanced technologies of micro-machining, lasers and microelectronics, and the latest research achievements in analytical chemistry and biochemistry, the sampling, separation and detection systems of commonly used capillary electrophoresis are integrated with high densities onto glass, quartz, silicon or polymer wafers to form the MCE, which can finish the analysis of multi-step operations such as injection, enrichment, reaction, derivatization, separation, and collection of samples in a portable, efficient and super high speed manner. With reference to the different technological achievements in this area, the latest developments in MCE are reviewed in this article. The preparation mechanisms, surface modifications, and properties of different materials in MCE are compared, and the different sampling, separation and detection systems in MCE are summarized. The performance of MCE in analysis of fluorescent substance, metallic ion, sugar, medicine, nucleic acid, DNA, amino acid, polypeptide and protein is discussed, and the future direction of development is forecast.

DNA migration mechanism analyses for applications in capillary and microchip electrophoresis

PubMed Central

Forster, Ryan E.; Hert, Daniel G.; Chiesl, Thomas N.; Fredlake, Christopher P.; Barron, Annelise E.

2009-01-01

In 2009, electrophoretically driven DNA separations in slab gels and capillaries have the sepia tones of an old-fashioned technology in the eyes of many, even while they remain ubiquitously used, fill a unique niche, and arguably have yet to reach their full potential. For comic relief, what is old becomes new again: agarose slab gel separations are used to prepare DNA samples for “next-gen” sequencing platforms (e.g., the Illumina and 454 machines)—dsDNA molecules within a certain size range are “cut out” of a gel and recovered for subsequent “massively parallel” pyrosequencing. In this review, we give a Barron lab perspective on how our comprehension of DNA migration mechanisms in electrophoresis has evolved, since the first reports of DNA separations by CE (∼1989) until now, 20 years later. Fused silica capillaries, and borosilicate glass and plastic microchips, quietly offer increasing capacities for fast (and even “ultra-fast”), efficient DNA separations. While the channel-by-channel scaling of both old and new electrophoresis platforms provides key flexibility, it requires each unique DNA sample to be prepared in its own micro- or nanovolume. This Achille's heel of electrophoresis technologies left an opening through which pooled-sample, next-gen DNA sequencing technologies rushed. We shall see, over time, whether sharpening understanding of transitions in DNA migration modes in crosslinked gels, nanogel solutions, and uncrosslinked polymer solutions will allow electrophoretic DNA analysis technologies to flower again. Microchannel electrophoresis, after a quiet period of metamorphosis, may emerge sleeker and more powerful, to claim its own important niche applications. PMID:19582705

Fast Food Jobs. National Study of Fast Food Employment.

ERIC Educational Resources Information Center

Charner, Ivan; Fraser, Bryna Shore

A study examined employment in the fast-food industry. The national survey collected data from employees at 279 fast-food restaurants from seven companies. Female employees outnumbered males by two to one. The ages of those fast-food employees in the survey sample ranged from 14 to 71, with fully 70 percent being in the 16- to 20-year-old age…

Plasma phenylalanine and tyrosine responses to different nutritional conditions (fasting/postprandial) in patients with phenylketonuria: effect of sample timing.

PubMed

van Spronsen, F J; van Rijn, M; van Dijk, T; Smit, G P; Reijngoud, D J; Berger, R; Heymans, H S

1993-10-01

To evaluate the adequacy of dietary treatment in patients with phenylketonuria, the monitoring of plasma phenylalanine and tyrosine concentrations is of great importance. The preferable time of blood sampling in relation to the nutritional condition during the day, however, is not known. It was the aim of this study to define guidelines for the timing of blood sampling with a minimal burden for the patient. Plasma concentrations of phenylalanine and tyrosine were measured in nine patients with phenylketonuria who had no clinical evidence of tyrosine deficiency. These values were measured during the day both after a prolonged overnight fast, and before and after breakfast. Phenylalanine showed a small rise during prolonged fasting, while tyrosine decreased slightly. After an individually tailored breakfast, phenylalanine remained stable, while tyrosine showed large fluctuations. It is concluded that the patient's nutritional condition (fasting/postprandial) is not important in the evaluation of the phenylalanine intake. To detect a possible tyrosine deficiency, however, a single blood sample is not sufficient and a combination of a preprandial and postprandial blood sample on the same day is advocated.

Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC).

PubMed

de Jager, L S; Andrews, A R

2000-11-01

A novel, fast screening method for organochlorine pesticides (OCPs) in water samples has been developed. Total analysis time was less than 9 min, allowing 11 samples to be screened per hour. The relatively new technique of solvent microextraction (SME) was used to extract and preconcentrate the pesticides into a single drop of hexane. The use of a conventional carbon dioxide cryotrap was investigated for introduction of the extract onto a micro-bore (0.1 mm) capillary column for fast GC analysis. A pulsed-discharge electron capture detector was used which yielded selective and sensitive measurement of the pesticide peaks. Fast GC conditions were optimised and tested with the previously developed SME procedure. Calibration curves yielded good linearity and concentrations down to 0.25 ng mL-1 were detectable with RSD values ranging from 12.0 to 28% and LOD for most OCPs at 0.25 ng mL-1. Spiked river water samples were tested and using the developed screen we were able to differentiate between spiked samples and samples containing no OCPs.

Sublingual fast dissolving niosomal films for enhanced bioavailability and prolonged effect of metoprolol tartrate.

PubMed

Allam, Ayat; Fetih, Gihan

2016-01-01

The aim of the present work was to prepare and evaluate sublingual fast dissolving films containing metoprolol tartrate-loaded niosomes. Niosomes were utilized to allow for prolonged release of the drug, whereas the films were used to increase the drug's bioavailability via the sublingual route. Niosomes were prepared using span 60 and cholesterol at different drug to surfactant ratios. The niosomes were characterized for size, zeta-potential, and entrapment efficiency. The selected niosomal formulation was incorporated into polymeric films using hydroxypropyl methyl cellulose E15 and methyl cellulose as film-forming polymers and Avicel as superdisintegrant. The physical characteristics (appearance, texture, pH, uniformity of weight and thickness, disintegration time, and palatability) of the prepared films were studied, in addition to evaluating the in vitro drug release, stability, and in vivo pharmacokinetics in rabbits. The release of the drug from the medicated film was fast (99.9% of the drug was released within 30 minutes), while the drug loaded into the niosomes, either incorporated into the film or not, showed only 22.85% drug release within the same time. The selected sublingual film showed significantly higher rate of drug absorption and higher drug plasma levels compared with that of commercial oral tablet. The plasma levels remained detectable for 24 hours following sublingual administration, compared with only 12 hours after administration of the oral tablet. In addition, the absolute bioavailability of the drug (ie, relative to intravenous administration) following sublingual administration was found to be significantly higher (91.06%±13.28%), as compared with that after oral tablet administration (39.37%±11.4%). These results indicate that the fast dissolving niosomal film could be a promising delivery system to enhance the bioavailability and prolong the therapeutic effect of metoprolol tartrate.

Sublingual fast dissolving niosomal films for enhanced bioavailability and prolonged effect of metoprolol tartrate

PubMed Central

Allam, Ayat; Fetih, Gihan

2016-01-01

The aim of the present work was to prepare and evaluate sublingual fast dissolving films containing metoprolol tartrate-loaded niosomes. Niosomes were utilized to allow for prolonged release of the drug, whereas the films were used to increase the drug’s bioavailability via the sublingual route. Niosomes were prepared using span 60 and cholesterol at different drug to surfactant ratios. The niosomes were characterized for size, zeta-potential, and entrapment efficiency. The selected niosomal formulation was incorporated into polymeric films using hydroxypropyl methyl cellulose E15 and methyl cellulose as film-forming polymers and Avicel as superdisintegrant. The physical characteristics (appearance, texture, pH, uniformity of weight and thickness, disintegration time, and palatability) of the prepared films were studied, in addition to evaluating the in vitro drug release, stability, and in vivo pharmacokinetics in rabbits. The release of the drug from the medicated film was fast (99.9% of the drug was released within 30 minutes), while the drug loaded into the niosomes, either incorporated into the film or not, showed only 22.85% drug release within the same time. The selected sublingual film showed significantly higher rate of drug absorption and higher drug plasma levels compared with that of commercial oral tablet. The plasma levels remained detectable for 24 hours following sublingual administration, compared with only 12 hours after administration of the oral tablet. In addition, the absolute bioavailability of the drug (ie, relative to intravenous administration) following sublingual administration was found to be significantly higher (91.06%±13.28%), as compared with that after oral tablet administration (39.37%±11.4%). These results indicate that the fast dissolving niosomal film could be a promising delivery system to enhance the bioavailability and prolong the therapeutic effect of metoprolol tartrate. PMID:27536063

Inspiring Teaching: Preparing Teachers to Succeed in Mission-Driven Schools

ERIC Educational Resources Information Center

Feiman-Nemser, Sharon, Ed.; Tamir, Eran, Ed.; Hammerness, Karen, Ed.

2014-01-01

How can we best prepare pre-service teachers to succeed in the classroom--and to stay in teaching over time? The one-size-fits-all model of traditional teacher education programs has been widely criticized, yet the most popular alternative--fast-track programs--have at best a mixed record of success. An increasing number of districts and charter…

Fast Start: Training Better Teachers Faster, with Focus, Practice and Feedback

ERIC Educational Resources Information Center

Menzes, Ana; Maier, Adam

2014-01-01

The field of teacher preparation is falling short of its most important responsibility: ensuring that the teachers we train are ready to do the job. For more than a decade,TNTP preparation programs produced teachers who were no more or less effective than teachers from any other program-- some were great, some were poor, most were about average.…

Walleye age estimation using otoliths and dorsal spines: Preparation techniques and sampling guidelines based on sex and total length

USGS Publications Warehouse

Dembkowski, Daniel J.; Isermann, Daniel A.; Koenigs, Ryan P.

2017-01-01

We used dorsal spines and otoliths from 735 Walleye Sander vitreus collected from 35 Wisconsin water bodies to evaluate whether 1) otolith and dorsal spine cross sections provided age estimates similar to simpler methods of preparation (e.g., whole otoliths and dorsal spines, cracked otoliths); and 2) between-reader precision and differences between spine and otolith ages varied in relation to total length (TL), sex, and growth rate. Ages estimated from structures prepared using simpler techniques were generally similar to ages estimated using thin sections of dorsal spines and otoliths, suggesting that, in some instances, much of the additional processing time and specialized equipment associated with thin sectioning could be avoided. Overall, between-reader precision was higher for sectioned otoliths (mean coefficient of variation [CV] = 3.28%; standard error [SE] = 0.33%) than for sectioned dorsal spines (mean CV = 9.20%; SE = 0.56%). When using sectioned otoliths for age assignment, between-reader precision did not vary between sexes or growth categories (i.e., fast, moderate, slow), but between-reader precision was higher for females than males when using sectioned dorsal spines. Dorsal spines were generally effective at replicating otolith ages for male Walleye <450 mm TL and female Walleye <600 mm TL, suggesting that dorsal spines can be used to estimate ages for male Walleye <450 mm TL and female Walleye <600 mm TL. If sex is unknown, we suggest dorsal spines be used to estimate ages for Walleye <450 mm TL, but that otoliths be used for fish >450 mm TL. Our results provide useful guidance on structure and preparation technique selection for Walleye age estimation, thereby allowing biologists to develop sampling guidelines that could be implemented using information that is always (TL) or often (sex) available at the time of fish collection.

An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions.

PubMed

Ruan, Guihua; Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui; Du, Fuyou

2016-04-22

A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of Nα-benzoyl-l-arginine ethyl ester to Nα-benzoyl-l-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. Copyright © 2016 Elsevier Inc. All rights reserved.

Comparative study of the molecularly imprinted polymers prepared by reversible addition-fragmentation chain transfer "bulk" polymerization and traditional radical "bulk" polymerization.

PubMed

Ma, Yue; Pan, Guoqing; Zhang, Ying; Guo, Xianzhi; Zhang, Huiqi

2013-05-01

Bisphenol A (BPA) and propranolol-imprinted polymers have been prepared via both reversible addition-fragmentation chain transfer "bulk" polymerization (RAFTBP) and traditional radical "bulk" polymerization (TRBP) under similar reaction conditions, and their equilibrium binding properties were compared in detail for the first time. The chemical compositions, specific surface areas, equilibrium bindings, and selectivity of the obtained molecularly imprinted polymers (MIPs) were systematically characterized. The experimental results showed that the MIPs with molecular imprinting effects and quite fast binding kinetics could be readily prepared via RAFTBP, but they did not show improved template binding properties in comparison with those prepared via TRBP, which is in sharp contrast to many previous reports. This could be attributed to the heavily interrupted equilibrium between the dormant species and active radicals in the RAFT mechanism because of the occurrence of fast gelation during RAFTBP. The findings presented here strongly demonstrates that the application of controlled radical polymerizations (CRPs) in molecular imprinting does not always benefit the binding properties of the resultant MIPs, which is of significant importance for the rational use of CRPs in generating MIPs with improved properties. Copyright © 2013 John Wiley & Sons, Ltd.

Pharmacological Fingerprints of Contextual Uncertainty

PubMed Central

Ruge, Diane; Stephan, Klaas E.

2016-01-01

Successful interaction with the environment requires flexible updating of our beliefs about the world. By estimating the likelihood of future events, it is possible to prepare appropriate actions in advance and execute fast, accurate motor responses. According to theoretical proposals, agents track the variability arising from changing environments by computing various forms of uncertainty. Several neuromodulators have been linked to uncertainty signalling, but comprehensive empirical characterisation of their relative contributions to perceptual belief updating, and to the selection of motor responses, is lacking. Here we assess the roles of noradrenaline, acetylcholine, and dopamine within a single, unified computational framework of uncertainty. Using pharmacological interventions in a sample of 128 healthy human volunteers and a hierarchical Bayesian learning model, we characterise the influences of noradrenergic, cholinergic, and dopaminergic receptor antagonism on individual computations of uncertainty during a probabilistic serial reaction time task. We propose that noradrenaline influences learning of uncertain events arising from unexpected changes in the environment. In contrast, acetylcholine balances attribution of uncertainty to chance fluctuations within an environmental context, defined by a stable set of probabilistic associations, or to gross environmental violations following a contextual switch. Dopamine supports the use of uncertainty representations to engender fast, adaptive responses. PMID:27846219

Fast determination of ethylene glycol, 1,2-propylene glycol and glycolic acid in blood serum and urine for emergency and clinical toxicology by GC-FID.

PubMed

Hložek, Tomáš; Bursová, Miroslava; Čabalaa, Radomír

2014-12-01

A simple, cost effective, and fast gas chromatography method with flame ionization detection (GC-FID) for simultaneous measurement of ethylene glycol, 1,2-propylene glycol and glycolic acid was developed and validated for clinical toxicology purposes. This new method employs a relatively less used class of derivatization agents - alkyl chloroformates, allowing the efficient and rapid derivatization of carboxylic acids within seconds while glycols are simultaneously derivatized by phenylboronic acid. The entire sample preparation procedure is completed within 10 min. To avoid possible interference from naturally occurring endogenous acids and quantitation errors 3-(4-chlorophenyl) propionic acid was chosen as an internal standard. The significant parameters of the derivatization have been found using chemometric procedures and these parameters were optimized using the face-centered central composite design. The calibration dependence of the method was proved to be quadratic in the range of 50-5000 mg mL(-1), with adequate accuracy (92.4-108.7%) and precision (9.4%). The method was successfully applied to quantify the selected compounds in serum of patients from emergency units. Copyright © 2014 Elsevier B.V. All rights reserved.

The woven fiber organic electrochemical transistors based on polypyrrole nanowires/reduced graphene oxide composites for glucose sensing.

PubMed

Wang, Yuedan; Qing, Xing; Zhou, Quan; Zhang, Yang; Liu, Qiongzhen; Liu, Ke; Wang, Wenwen; Li, Mufang; Lu, Zhentan; Chen, Yuanli; Wang, Dong

2017-09-15

Novel woven fiber organic electrochemical transistors based on polypyrrole (PPy) nanowires and reduced graphene oxide (rGO) have been prepared. SEM revealed that the introduction of rGO nanosheets could induce the growth and increase the amount of PPy nanowires. Moreover, it could enhance the electrical performance of fiber transistors. The hybrid transistors showed high on/off ratio of 10 2 , fast switch speed, and long cycling stability. The glucose sensors based on the fiber organic electrochemical transistors have also been investigated, which exhibited outstanding sensitivity, as high as 0.773 NCR/decade, with a response time as fast as 0.5s, a linear range of 1nM to 5μM, a low detection concentration as well as good repeatability. In addition, the glucose could be selectively detected in the presence of ascorbic acid and uric acid interferences. The reliability of the proposed glucose sensor was evaluated in real samples of rabbit blood. All the results indicate that the novel fiber transistors pave the way for portable and wearable electronics devices, which have a promising future for healthcare and biological applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Gliding movement of and bidirectional transport along single native microtubules from squid axoplasm: evidence for an active role of microtubules in cytoplasmic transport

PubMed Central

1985-01-01

Native microtubules prepared from extruded and dissociated axoplasm have been observed to transport organelles and vesicles unidirectionally in fresh preparations and more slowly and bidirectionally in older preparations. Both endogenous and exogenous (fluorescent polystyrene) particles in rapid Brownian motion alight on and adhere to microtubules and are transported along them. Particles can switch from one intersecting microtubule to another and move in either direction. Microtubular segments 1 to 30 microns long, produced by gentle homogenization, glide over glass surfaces for hundreds of micrometers in straight lines unless acted upon by obstacles. While gliding they transport particles either in the same (forward) direction and/or in the backward direction. Particle movement and gliding of microtubule segments require ATP and are insensitive to taxol (30 microM). It appears, therefore, that the mechanisms producing the motive force are very closely associated with the native microtubule itself or with its associated proteins. Although these movements appear irreconcilable with several current theories of fast axoplasmic transport, in this article we propose two models that might explain the observed phenomena and, by extension, the process of fast axoplasmic transport itself. The findings presented and the possible mechanisms proposed for fast axoplasmic transport have potential applications across the spectrum of microtubule-based motility processes. PMID:2580845

Development of Novel Potentiometric Sensors for Determination of Lidocaine Hydrochloride in Pharmaceutical Preparations, Serum and Urine Samples

PubMed Central

Ali, Tamer Awad; Mohamed, Gehad Genidy; Yahya, Ghada A.

2017-01-01

This article is focused on the determination of lidocaine hydrochloride as a local anaesthetic drug. A potentiometric method based on modified screen-printed and modified carbon paste ion-selective electrodes was described for the determination of lidocaine hydrochloride in different pharmaceutical preparations and biological fluids (urine and serum). It was based on potentiometric titration of lidocaine hydrochloride using modified screen-printed and carbon paste electrodes as end point indicator sensors. The influences of the paste composition, different conditioning parameters and foreign ions on the electrodes performance were investigated and response times of the electrodes were studied. The electrodes showed Nernstian response of 58.9 and 57.5 mV decade-1 in the concentration range of 1×10-7–1×10-2 and 6.2×10-7–1×10-2 mol L-1 for modified screen-printed and carbon paste electrodes, respectively. The electrodes were found to be usable within the pH range of 2.0–8.0 and 2.0-7.5, exhibited a fast response time (about 6 and 4) low detection limit (1×10-7 and 6.2×10-7 mol L-1), long lifetime (6 and 4 months) and good stability for modified screen-printed (Electrode VII) and carbon paste electrodes (Electrode III), respectively. The electrodes were successfully applied for the determination of lidocaine hydrochloride in pure solutions, pharmaceutical preparation and biological fluids (urine and serum) samples. The results obtained applying these potentiometric electrodes were comparable with British pharmacopeia. The method validation parameters were optimized and the method can be applied for routine analysis of lidocaine hydrochloride drug. PMID:28979305

Development of Novel Potentiometric Sensors for Determination of Lidocaine Hydrochloride in Pharmaceutical Preparations, Serum and Urine Samples.

PubMed

Ali, Tamer Awad; Mohamed, Gehad Genidy; Yahya, Ghada A

2017-01-01

This article is focused on the determination of lidocaine hydrochloride as a local anaesthetic drug. A potentiometric method based on modified screen-printed and modified carbon paste ion-selective electrodes was described for the determination of lidocaine hydrochloride in different pharmaceutical preparations and biological fluids (urine and serum). It was based on potentiometric titration of lidocaine hydrochloride using modified screen-printed and carbon paste electrodes as end point indicator sensors. The influences of the paste composition, different conditioning parameters and foreign ions on the electrodes performance were investigated and response times of the electrodes were studied. The electrodes showed Nernstian response of 58.9 and 57.5 mV decade -1 in the concentration range of 1×10 -7 -1×10 -2 and 6.2×10 -7 -1×10 -2 mol L -1 for modified screen-printed and carbon paste electrodes, respectively. The electrodes were found to be usable within the pH range of 2.0-8.0 and 2.0-7.5, exhibited a fast response time (about 6 and 4) low detection limit (1×10 -7 and 6.2×10 -7 mol L -1 ), long lifetime (6 and 4 months) and good stability for modified screen-printed (Electrode VII) and carbon paste electrodes (Electrode III), respectively. The electrodes were successfully applied for the determination of lidocaine hydrochloride in pure solutions, pharmaceutical preparation and biological fluids (urine and serum) samples. The results obtained applying these potentiometric electrodes were comparable with British pharmacopeia. The method validation parameters were optimized and the method can be applied for routine analysis of lidocaine hydrochloride drug.