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Sample records for pretreatment quantitative determinations

  1. Are risks quantitatively determinable

    International Nuclear Information System (INIS)

    Buetzer, P.

    1985-01-01

    ''Chemical risks'' can only be determined with accurate figures in a few extraordinary cases. The difficulties lie, as has been shown by the example of the Flixborough catastrophe, mostly in the determination of the probabilities of occurrence. With a rough semiquantitative estimate of the potential hazards and the corresponding probabilities we can predict the risks with astonishing accuracy. Statistical data from incidents in the chemical industry are very useful, and they also show that ''chemical catastrophes'' are only to a very small extent initiated by uncontrolled chemical reactions. (orig.) [de

  2. A Novel Pretreatment-Free Duplex Chamber Digital PCR Detection System for the Absolute Quantitation of GMO Samples.

    Science.gov (United States)

    Zhu, Pengyu; Wang, Chenguang; Huang, Kunlun; Luo, Yunbo; Xu, Wentao

    2016-03-18

    Digital polymerase chain reaction (PCR) has developed rapidly since it was first reported in the 1990s. However, pretreatments are often required during preparation for digital PCR, which can increase operation error. The single-plex amplification of both the target and reference genes may cause uncertainties due to the different reaction volumes and the matrix effect. In the current study, a quantitative detection system based on the pretreatment-free duplex chamber digital PCR was developed. The dynamic range, limit of quantitation (LOQ), sensitivity and specificity were evaluated taking the GA21 event as the experimental object. Moreover, to determine the factors that may influence the stability of the duplex system, we evaluated whether the pretreatments, the primary and secondary structures of the probes and the SNP effect influence the detection. The results showed that the LOQ was 0.5% and the sensitivity was 0.1%. We also found that genome digestion and single nucleotide polymorphism (SNP) sites affect the detection results, whereas the unspecific hybridization within different probes had little side effect. This indicated that the detection system was suited for both chamber-based and droplet-based digital PCR. In conclusion, we have provided a simple and flexible way of achieving absolute quantitation for genetically modified organism (GMO) genome samples using commercial digital PCR detection systems.

  3. A Novel Pretreatment-Free Duplex Chamber Digital PCR Detection System for the Absolute Quantitation of GMO Samples

    Directory of Open Access Journals (Sweden)

    Pengyu Zhu

    2016-03-01

    Full Text Available Digital polymerase chain reaction (PCR has developed rapidly since it was first reported in the 1990s. However, pretreatments are often required during preparation for digital PCR, which can increase operation error. The single-plex amplification of both the target and reference genes may cause uncertainties due to the different reaction volumes and the matrix effect. In the current study, a quantitative detection system based on the pretreatment-free duplex chamber digital PCR was developed. The dynamic range, limit of quantitation (LOQ, sensitivity and specificity were evaluated taking the GA21 event as the experimental object. Moreover, to determine the factors that may influence the stability of the duplex system, we evaluated whether the pretreatments, the primary and secondary structures of the probes and the SNP effect influence the detection. The results showed that the LOQ was 0.5% and the sensitivity was 0.1%. We also found that genome digestion and single nucleotide polymorphism (SNP sites affect the detection results, whereas the unspecific hybridization within different probes had little side effect. This indicated that the detection system was suited for both chamber-based and droplet-based digital PCR. In conclusion, we have provided a simple and flexible way of achieving absolute quantitation for genetically modified organism (GMO genome samples using commercial digital PCR detection systems.

  4. Evaluation of ultrasound-assisted extraction as sample pre-treatment for quantitative determination of rare earth elements in marine biological tissues by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Costas, M.; Lavilla, I.; Gil, S.; Pena, F.; Calle, I.; Cabaleiro, N. de la; Bendicho, C.

    2010-01-01

    In this work, the determination of rare earth elements (REEs), i.e. Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in marine biological tissues by inductively coupled-mass spectrometry (ICP-MS) after a sample preparation method based on ultrasound-assisted extraction (UAE) is described. The suitability of the extracts for ICP-MS measurements was evaluated. For that, studies were focused on the following issues: (i) use of clean up of extracts with a C18 cartridge for non-polar solid phase extraction; (ii) use of different internal standards; (iii) signal drift caused by changes in the nebulization efficiency and salt deposition on the cones during the analysis. The signal drift produced by direct introduction of biological extracts in the instrument was evaluated using a calibration verification standard for bracketing (standard-sample bracketing, SSB) and cumulative sum (CUSUM) control charts. Parameters influencing extraction such as extractant composition, mass-to-volume ratio, particle size, sonication time and sonication amplitude were optimized. Diluted single acids (HNO 3 and HCl) and mixtures (HNO 3 + HCl) were evaluated for improving the extraction efficiency. Quantitative recoveries for REEs were achieved using 5 mL of 3% (v/v) HNO 3 + 2% (v/v) HCl, particle size <200 μm, 3 min of sonication time and 50% of sonication amplitude. Precision, expressed as relative standard deviation from three independent extractions, ranged from 0.1 to 8%. In general, LODs were improved by a factor of 5 in comparison with those obtained after microwave-assisted digestion (MAD). The accuracy of the method was evaluated using the CRM BCR-668 (mussel tissue). Different seafood samples of common consumption were analyzed by ICP-MS after UAE and MAD.

  5. Characterization of ionic liquid pretreated aspen wood using semi-quantitative methods for ethanol production.

    Science.gov (United States)

    Goshadrou, Amir; Karimi, Keikhosro; Lefsrud, Mark

    2013-07-25

    Aspen wood (Populus tremula) was pretreated with ionic liquid 1-ethyl-3-methylimidazolium acetate ([EMIM]OAc) and dilute sulfuric acid for improvement of ethanol production. The ionic liquid pretreatment included wood dissolution at 120°C and 5% solid loading for 1, 3, and 5h followed by regeneration using water as an anti-solvent. More than 95% enzymatic digestibility was achieved for the ionic liquid treated wood, while the yield from the untreated wood was only 5.3%. Furthermore, over 81% of the maximum theoretical ethanol yield was attained after 24h fermentation of the ionic liquid treated wood, whereas the yields were only 5.3% and 42.1% for the untreated and dilute acid treated materials, respectively. A side-by-side comparative analysis of the pretreated materials using semi-quantitative techniques (e.g., Simons' staining and enzyme adsorption) revealed that the ionic liquid treatment was much more successful in increasing the cellulose accessibility to cellulases and decreasing the lignin content. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Quantitative determination of formaldehyde by spectrophotometry ...

    African Journals Online (AJOL)

    Formaldehyde is a vastly used material in industry. Nowadays, it is proven that formaldehyde is toxic and carcinogenic. Thus providing a reliable method for its quantitative determination is very important. This study proposes a UV-Vis spectrophotometric based method for determination of formaldehyde. The method is ...

  7. Quantitative spectrographic determination of zirconium minerals

    International Nuclear Information System (INIS)

    Rocal Adell, M.; Alvarez Gonzalez, F.; Fernandez Cellini, R.

    1958-01-01

    The method described in the following report permits the quantitative determination of zirconium in minerals and rocks in a 0,02-100% of ZrO 2 concentration rate. The excitation is carried out by a 10 ampere continuous current arc among carbon electrodes, and placing the sample in a crater of 2 mm depth. For low concentrations a dilution of the sample with the same weight as its own in carbon powder and with 1/25 of its weight of Co 3 O 4 (internal patron) is carried out. Line Zr 2571,4, Co 2585,3 and Co 2587,2 are used. (Author) 6 refs

  8. Quantitative determination of the enhanced magnetoelectric

    Science.gov (United States)

    Oh, Yoon Seok; Kim, Kee Hoon; Crane, Steven P.; Ramesh, R.; Lee, Seongsu; Cheong, S.-W.

    2009-03-01

    With growing interest worldwide toward applications of multiferroic materials for novel memory and magnetic sensor devices, there have been numerous efforts to synthesize multiferroic thin films with large magnetoelectric coupling. Yet, quantitative information on the magnetoelectric susceptibility (MES) of the film is still lacking because it is difficult to measure a reduced magnetoelectric signal due to a tiny thickness. In the present work, we have determined quantitative MES for a 300 nm BiFeO3-CoFe2O4 nanostructure, 250 nm BiFeO3 film, and BiFeO3 single crystal with our highly sensitive magnetoelectric susceptometer operating in cryogenic (down to 2 K) and high magnetic field, H, (up to 9 T) environments. We find that the MES of the BiFeO3-CoFe2O4 nanostructure shows a typical anti-symmetric shape with DC magnetic field up to 340 K, as expected in the magnetoelectric coupling mediated by strain between piezoelectric and magnetostrictive materials. At room temperature, the transverse MES of the nanostructure shows a maximum of 2 x10-10 s/m at low H = 6 kOe. Our results also demonstrate that the MES value of the nanopillar structured film is enhanced by approximately one order of magnitude than that of pure 250 nm BiFeO3 film and BiFeO3 single crystal.

  9. [Quantitative analysis of diffusion-weighted magnetic resonance images during chemoradiation therapy for cancer of the cervix uteri: Prognostic role of pretreatment diffusion coefficient values].

    Science.gov (United States)

    Kharuzhyk, S A

    2015-01-01

    to carry out a quantitative analysis of diffusion-weighted magnetic resonance images (DWI) in cancer of the cervix uteri (CCU) and to estimate the possibility of using pretreatment measured diffusion coefficient (MDC) to predict chemoradiation therapy (CRT). The investigation prospectively enrolled 46 women with morphologically verified Stages IB-IVB CCU. All the women underwent diffusion-weighted magnetic resonance imaging of pelvic organs before and after treatment. A semiautomatic method was used to determine tumor signal intensity (SI) on DWI at b 1000 s/mm2 (SI b1000) and tumor MDC. The reproducibility of MDC measurements was assessed in 16 randomly selected women. The investigators compared the pretreatment quantitative DWI measures in complete and incomplete regression (CR and IR) groups and the presence and absence of tumor progression during a follow-up. An association of MDC with progression-free and overall survivals (PFS and OS) was determined in the patients. A semiautomatic tumor segmentation framework could determine the pretreatment quantitative DMI measures with minimal time spent and high reproducibility. The mean tumor MDC was 0.82 +/- 0.14 x 10(-3) mm2/s. CR and IR were established in 28 and 18 women, respectively. The MDC < or = 0.83 x 10(-3) mm2/s predicted CR with a sensitivity of 64.3% and a specificity of 77.8% (p=0.007). The median follow-up was 47 months (range, 3-82 months). With the MDC < or = 0.86 x 10(-3) mm2/s, 5-year PFS was 74.1% versus 42.1% with a higher MDC (p=0.023) and 5-year OS was 70.4 and 40.6%, respectively (p=0.021). The survival difference was insignificant in relation to the degree of tumor regression. The pretreatment IS at b1000 was of no prognostic value. The pretreatment tumor MDC may serve as a biomarker for predicting the efficiency of CRT for CCU.

  10. Pretreated high lipid serum method and its significance before determine INS C-P by RIA

    International Nuclear Information System (INIS)

    Wan Guangxia; Zhu Liqiang; Wu Yufang

    2004-01-01

    The method of predigest high lipid serum before determine INS and C-P for elimination of the high lipid in serum was studied. The specimen was divided into two groups, one was directly tested, the other was pretreated, then determined(including INS and QC of serum, normal and high lipid serum, pretreating serum). The results were compared by examine and analysed correlatively. Results show that INS and C-P of the specimens pretreated by PEG, were no statistic difference in relation to direct tested (P>0.05) and those were close correlatively (P<0.001) in normal. The results of high lipid serum after the specimens were predigest by PEG were marked by decrease in relation to direct tested (P<0.001). High lipid and INS antibody were eliminated by PEG so that was increased the results nicety. (authors)

  11. short communication quantitative determination of formaldehyde

    African Journals Online (AJOL)

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    ALS). Data processing by this chemometrics technique enhanced the reliability of the UV-Vis spectrophotometry for quantitative analysis of formaldehyde in real samples. KEY WORDS: Formaldehyde, Fluoral P, UV-Visible, Multivariate curve resolution alternating least squares;. Quantitative analysis. INTRODUCTION.

  12. Effect of sample pre-treatment on the determination of steroid esters in hair of bovine calves

    NARCIS (Netherlands)

    Aqai, P.; Stolker, A.A.M.; Lasaroms, J.J.P.

    2009-01-01

    The effect of three sample pre-treatment steps, washing, cutting and grinding on the determination of steroid esters in hair is studied. The study is performed by using hair samples obtained after pour-on application of steroid esters to bovine calves. After sample pre-treatment the hair is treated

  13. Determination of alkylphenols and alkylphenol ethoxylates in sewage sludge: effect of sample pre-treatment.

    Science.gov (United States)

    Fernández-Sanjuan, María; Rigol, Anna; Sahuquillo, Angels; Rodríguez-Cruz, Sonia; Lacorte, Silvia

    2009-07-01

    A complete characterization of sewage sludge collected from five biological waste water treatment plants was done to determine physico-chemical parameters, heavy metals and alkylphenols, making special emphasis on sampling, homogenization, and sample pre-treatment. Ultrasonic extraction followed by gas chromatrography coupled with mass spectrometry was used to evaluate the effect of sample pre-treatment (untreated sample, freeze-drying, drying at 40 degrees C or drying at 100 degrees C) on the concentration of octylphenol (OP), nonylphenol (NP) and nonylphenol ethoxylates (NP1EO, NP2EO). Untreated samples and samples dried at 100 degrees C gave concentration levels up to 62% and 89% lower, respectively, than freeze-dried samples. In 50% of cases, freeze-dried samples led to significantly higher concentrations than those obtained by drying at 40 degrees C. Thus, freeze-drying is the recommended sample pre-treatment to prevent possible losses of OP, NP, and NP1EO. Using this methodology, concentrations detected were from 3.2 to 199 mg kg(-1) being NP followed by NP1EO found in highest concentration. The total concentration of NP and NP1EO exceeded the limit of 50 mg kg(-1) proposed by the draft European directive on sewage sludge in three out of five samples studied. Contrarily, heavy metals were below the legislated values.

  14. Determination of alkylphenols and alkylphenol ethoxylates in sewage sludge: effect of sample pre-treatment

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Sanjuan, Maria; Rigol, Anna; Sahuquillo, Angels [University of Barcelona, Department of Analytical Chemistry, Barcelona (Spain); Rodriguez-Cruz, Sonia [University of Barcelona, Department of Analytical Chemistry, Barcelona (Spain); IRNASA-CSIC, Department of Environmental Chemistry and Geochemistry, Salamanca (Spain); Lacorte, Silvia [IDAEA-CSIC, Department of Environmental Chemistry, Barcelona (Spain)

    2009-07-15

    A complete characterization of sewage sludge collected from five biological waste water treatment plants was done to determine physico-chemical parameters, heavy metals and alkylphenols, making special emphasis on sampling, homogenization, and sample pre-treatment. Ultrasonic extraction followed by gas chromatrography coupled with mass spectrometry was used to evaluate the effect of sample pre-treatment (untreated sample, freeze-drying, drying at 40 C or drying at 100 C) on the concentration of octylphenol (OP), nonylphenol (NP) and nonylphenol ethoxylates (NP{sub 1}EO, NP{sub 2}EO). Untreated samples and samples dried at 100 C gave concentration levels up to 62% and 89% lower, respectively, than freeze-dried samples. In 50% of cases, freeze-dried samples led to significantly higher concentrations than those obtained by drying at 40 C. Thus, freeze-drying is the recommended sample pre-treatment to prevent possible losses of OP, NP, and NP{sub 1}EO. Using this methodology, concentrations detected were from 3.2 to 199 mg kg{sup -1} being NP followed by NP{sub 1}EO found in highest concentration. The total concentration of NP and NP{sub 1}EO exceeded the limit of 50 mg kg{sup -1} proposed by the draft European directive on sewage sludge in three out of five samples studied. Contrarily, heavy metals were below the legislated values. (orig.)

  15. Impact of pretreated Switchgrass and biomass carbohydrates on Clostridium thermocellum ATCC 27405 cellulosome composition: a quantitative proteomic analysis.

    Directory of Open Access Journals (Sweden)

    Babu Raman

    Full Text Available BACKGROUND: Economic feasibility and sustainability of lignocellulosic ethanol production requires the development of robust microorganisms that can efficiently degrade and convert plant biomass to ethanol. The anaerobic thermophilic bacterium Clostridium thermocellum is a candidate microorganism as it is capable of hydrolyzing cellulose and fermenting the hydrolysis products to ethanol and other metabolites. C. thermocellum achieves efficient cellulose hydrolysis using multiprotein extracellular enzymatic complexes, termed cellulosomes. METHODOLOGY/PRINCIPAL FINDINGS: In this study, we used quantitative proteomics (multidimensional LC-MS/MS and (15N-metabolic labeling to measure relative changes in levels of cellulosomal subunit proteins (per CipA scaffoldin basis when C. thermocellum ATCC 27405 was grown on a variety of carbon sources [dilute-acid pretreated switchgrass, cellobiose, amorphous cellulose, crystalline cellulose (Avicel and combinations of crystalline cellulose with pectin or xylan or both]. Cellulosome samples isolated from cultures grown on these carbon sources were compared to (15N labeled cellulosome samples isolated from crystalline cellulose-grown cultures. In total from all samples, proteomic analysis identified 59 dockerin- and 8 cohesin-module containing components, including 16 previously undetected cellulosomal subunits. Many cellulosomal components showed differential protein abundance in the presence of non-cellulose substrates in the growth medium. Cellulosome samples from amorphous cellulose, cellobiose and pretreated switchgrass-grown cultures displayed the most distinct differences in composition as compared to cellulosome samples from crystalline cellulose-grown cultures. While Glycoside Hydrolase Family 9 enzymes showed increased levels in the presence of crystalline cellulose, and pretreated switchgrass, in particular, GH5 enzymes showed increased levels in response to the presence of cellulose in general

  16. Quantitative Phase Determination by Using a Michelson Interferometer

    Science.gov (United States)

    Pomarico, Juan A.; Molina, Pablo F.; D'Angelo, Cristian

    2007-01-01

    The Michelson interferometer is one of the best established tools for quantitative interferometric measurements. It has been, and is still successfully used, not only for scientific purposes, but it is also introduced in undergraduate courses for qualitative demonstrations as well as for quantitative determination of several properties such as…

  17. [Comparison of pretreatment methods for the simultaneous determination of diclazuril and toltrazuril residues in chicken tissues].

    Science.gov (United States)

    Shi, Zuhao; Ge, Qinglian; Lu, Junxian; Liu, Xuexian; Gong, Jiansen; Zhu, Liangqiang; Qi, Kezong; Chen, Dingding; Peng, Kaisong

    2009-05-01

    The effects of four pretreatment methods (acetonitrile extraction-evaporation concentration, acetonitrile extraction-solid phase extraction (SPE), matrix solid-phase dispersion (MSPD) extraction and MSPD-SPE) for the simultaneous analysis of diclazuril and toltrazuril residues in chicken tissues were compared. The average recovery of 70% for the former three methods as achieved. In comparison with other methods, the MSPD method saved more than 60% in time and solvent. So, MSPD as the sample pretreatment method, an MSPD-high performance liquid chromatography with ultraviolet detection (MSPD-HPLC/UV) method was established for the analysis. Under the optimal chromatographic conditions, the linear range was between 50 and 1,000 microg/kg. At the added levels of 50, 500, 1,000 ng/g, the recoveries of diclazuril and toltrazuril in chicken tissues ranged from 71.13% - 84.02% with the relative standard deviations (RSD) in the range of 3.76% - 12.11%, and the RSDs of intra- and interday analyses ranged from 3.70% - 6.77%. The detection limits of diclazuril and toltrazuril were less than 10 microg/kg. The quantitative limits of diclazuril and toltrazuril were less than 20 microg/kg. The method meet the requirements of the residue analysis on accuracy and precision.

  18. Sugarcane starch: quantitative determination and characterization

    Directory of Open Access Journals (Sweden)

    Joelise de Alencar Figueira

    2011-09-01

    Full Text Available Starch is found in sugarcane as a storage polysaccharide. Starch concentrations vary widely depending on the country, variety, developmental stage, and growth conditions. The purpose of this study was to determine the starch content in different varieties of sugarcane, between May and November 2007, and some characteristics of sugarcane starch such as structure and granules size; gelatinization temperature; starch solution filterability; and susceptibility to glucoamylase, pullulanase, and commercial bacterial and fungal α-amylase enzymes. Susceptibility to debranching amylolytic isoamylase enzyme from Flavobacterium sp. was also tested. Sugarcane starch had spherical shape with a diameter of 1-3 µm. Sugarcane starch formed complexes with iodine, which showed greater absorption in the range of 540 to 620 nm. Sugarcane starch showed higher susceptibility to glucoamylase compared to that of waxy maize, cassava, and potato starch. Sugarcane starch also showed susceptibility to debranching amylolytic pullulanases similar to that of waxy rice starch. It also showed susceptibility to α-amylase from Bacillus subtilis, Bacillus licheniformis, and Aspergillus oryzae similar to that of the other tested starches producing glucose, maltose, maltotriose, maltotetraose, maltopentose and limit α- dextrin.

  19. [Erroneous vision determination and quantitative effects].

    Science.gov (United States)

    Petersen, J

    1993-10-01

    The experimentally determined psychometric function for Landolt rings (8 orientations, 183 eyes) is used to calculate the statistics of visual acuity results according to DIN 58,220 and their bias due to deviations from DIN 58,220. Test procedure fulfilling DIN 58,220, criterion 3/5: With a second test the first result is reproduced in 33.7%. In 47% the difference is 1 step, in 16.2% 2 steps, and in 2.8% 3 steps. Selecting the highest acuity value out of several tests yields a bias of +0.44 steps (2 tests), +0.66 steps (3), +0.81 steps (4 tests). Deviations from DIN 58,220, criterion 3/5: Linearly instead of log-scaled optotypes: above acuity 0.2 the effect is minimal (test despite fulfilled break condition: bias +0.3 steps; Weakened criterion of 2/5: bias +0.89 steps. Visual acuity values can contain considerable errors. There is a need for more effective algorithms and an unbiased investigator. The solution is programmed automatic testing on a computer screen.

  20. Porosity determination on pyrocarbon using automatic quantitative image analysis

    International Nuclear Information System (INIS)

    Koizlik, K.; Uhlenbruck, U.; Delle, W.; Nickel, H.

    Methods of porosity determination are reviewed and applied to the measurement of the porosity of pyrocarbon. Specifically, the mathematical basis of stereology and the procedures involved in quantitative image analysis are detailed

  1. Determination of saccharides and ethanol from biomass conversion using Raman spectroscopy: Effects of pretreatment and enzyme composition

    Energy Technology Data Exchange (ETDEWEB)

    Shih, Chien-Ju [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    This dissertation focuses on the development of facile and rapid quantitative Raman spectroscopy measurements for the determination of conversion products in producing bioethanol from corn stover. Raman spectroscopy was chosen to determine glucose, xylose and ethanol in complex hydrolysis and fermentation matrices. Chapter 1 describes the motives and main goals of this work, and includes an introduction to biomass, commonly used pretreatment methods, hydrolysis and fermentation reactions. The principles of Raman spectroscopy, its advantages and applications related to biomass analysis are also illustrated. Chapter 2 and 3 comprise two published or submitted manuscripts, and the thesis concludes with an appendix. In Chapter 2, a Raman spectroscopic protocol is described to study the efficiency of enzymatic hydrolysis of cellulose by measuring the main product in hydrolysate, glucose. Two commonly utilized pretreatment methods were investigated in order to understand their effect on glucose measurements by Raman spectroscopy. Second, a similar method was set up to determine the concentration of ethanol in fermentation broth. Both of these measurements are challenged by the presence of complex matrices. In Chapter 3, a quantitative comparison of pretreatment protocols and the effect of enzyme composition are studied using systematic methods. A multipeak fitting algorithm was developed to analyze spectra of hydrolysate containing two analytes: glucose and xylose. Chapter 4 concludes with a future perspective of this research area. An appendix describes a convenient, rapid spectrophotometric method developed to measure cadmium in water. This method requires relatively low cost instrumentation and can be used in microgravity, such as space shuttles or the International Space Station. This work was performed under the supervision of Professor Marc Porter while at Iowa State University. Research related to producing biofuel from bio-renewable resources, especially

  2. Adsorptive Stripping Voltammetric Determination of Hydroquinone using an Electrochemically Pretreated Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Abdul Niaz1,

    2008-12-01

    Full Text Available A simple and efficient adsorptive stripping voltammetric (AdSV method was developed for the determination of hydroquinone at an electrochemically pretreated glassy carbon (GC electrode in waste water. Various parameters such as solvent system, accumulation potential, accumulation time and scan rate were optimized. The electrochemically pretreated GC electrode showed good response towards hydroquinone determination by using AdSV. Under the optimized conditions the peak current showed good linear relationship with the hydroquinone concentration in the range of 0.5-4.0mg L-1 and 5-30mg L-1. The 60/40 methanol/water composition was found to be the best solvent system and 0.05mol L-1 H2SO4 was found as useful supporting electrolyte concentration. The accumulation time was 60 s and the detection limit was 50µg L-1. The developed method was successfully applied for the determination of hydroquinone in polymeric industrial discharge samples waste photographic developer solution and cream sample without any significant effect of surface fouling.

  3. Sample pretreatment for the determination of metal impurities in silicon wafer

    International Nuclear Information System (INIS)

    Chung, H. Y.; Kim, Y. H.; Yoo, H. D.; Lee, S. H.

    1999-01-01

    The analytical results obtained by microwave digestion and acid digestion methods for sample pretreatment to determine metal impurities in silicon wafer by inductively coupled plasma--mass spectrometry(ICP-MS) were compared. In order to decompose the silicon wafer, a mixed solution of HNO 3 and HF was added to the sample and the metal elements were determined after removing the silicon matrix by evaporating silicon in the form of Si-F. The recovery percentages of Ni, Cr and Fe were found to be 95∼106% for both microwave digestion and acid digestion methods. The recovery percentage of Cu obtained by the acid digestion method was higher than that obtained by the microwave digestion method. For Zn, however, the microwave digestion method gave better result than the acid digestion method. Fe was added to a silicon wafer using a spin coater. The concentration of Fe in this sample was determined by ICP-MS, and the same results were obtained in the two pretreatment methods

  4. Chemical dispersants and pre-treatments to determine clay in soils with different mineralogy

    Directory of Open Access Journals (Sweden)

    Cristiane Rodrigues

    2011-10-01

    Full Text Available Knowledge of the soil physical properties, including the clay content, is of utmost importance for agriculture. The behavior of apparently similar soils can differ in intrinsic characteristics determined by different formation processes and nature of the parent material. The purpose of this study was to assess the efficacy of separate or combined pre-treatments, dispersion methods and chemical dispersant agents to determine clay in some soil classes, selected according to their mineralogy. Two Brazilian Oxisols, two Alfisols and one Mollisol with contrasting mineralogy were selected. Different treatments were applied: chemical substances as dispersants (lithium hydroxide, sodium hydroxide, and hexametaphosphate; pre-treatment with dithionite, ammonium oxalate, and hydrogen peroxide to eliminate organic matter; and coarse sand as abrasive and ultrasound, to test their mechanical action. The conclusion was drawn that different treatments must be applied to determine clay, in view of the soil mineralogy. Lithium hydroxide was not efficient to disperse low-CEC electropositive soils and very efficient in dispersing high-CEC electronegative soils. The use of coarse sand as an abrasive increased the clay content of all soils and in all treatments in which dispersion occurred, with or without the use of chemical dispersants. The efficiency of coarse sand is not the same for all soil classes.

  5. Biogas production from ensiled meadow grass; effect of mechanical pretreatments and rapid determination of substrate biodegradability via physicochemical methods.

    Science.gov (United States)

    Tsapekos, P; Kougias, P G; Angelidaki, I

    2015-04-01

    As the biogas sector is rapidly expanding, there is an increasing need in finding new alternative feedstock to biogas plants. Meadow grass can be a suitable co-substrate and if ensiled it can be supplied to biogas plants continuously throughout the year. Nevertheless, this substrate is quite recalcitrant and therefore efficient pretreatment is needed to permit easy access of microbes to the degradable components. In this study, different mechanical pretreatment methods were applied on ensiled meadow grass to investigate their effect on biomass biodegradability. All the tested pretreatments increased the methane productivity and the increase ranged from 8% to 25%. The best mechanical pretreatment was the usage of two coarse mesh grating plates. Additionally, simple analytical methods were conducted to investigate the possibility of rapidly determining the methane yield of meadow grass. Among the methods, electrical conductivity test showed the most promising calibration statistics (R(2)=0.68). Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Quantitative predictions of bioconversion of aspen by dilute acid and SPORL pretreatments using a unified combined hydrolysis factor (CHF)

    Science.gov (United States)

    W. Zhu; Carl J. Houtman; J.Y. Zhu; Roland Gleisner; K.F. Chen

    2012-01-01

    A combined hydrolysis factor (CHF) was developed to predict xylan hydrolysis during pretreatments of native aspen (Populus tremuloides) wood chips. A natural extension of previously developed kinetic models allowed us to account for the effect of catalysts by dilute acid and two sulfite pretreatments at different pH values....

  7. Quantitative Determination of Aluminum in Deodorant Brands: A Guided Inquiry Learning Experience in Quantitative Analysis Laboratory

    Science.gov (United States)

    Sedwick, Victoria; Leal, Anne; Turner, Dea; Kanu, A. Bakarr

    2018-01-01

    The monitoring of metals in commercial products is essential for protecting public health against the hazards of metal toxicity. This article presents a guided inquiry (GI) experimental lab approach in a quantitative analysis lab class that enabled students' to determine the levels of aluminum in deodorant brands. The utility of a GI experimental…

  8. Escin in pharmaceutical oral dosage forms: quantitative densitometric HPTLC determination.

    Science.gov (United States)

    Costantini, A

    1999-01-01

    A practical and reliable method for the quantitative determination of escin in pharmaceuticals was developed. The TLC-densitometric determination was performed without using spray or dipping reagents in order to provide a more rapid and simple analytical procedure. Chromatographic separations were obtained on analytical HPTLC silica gel plates and the elution was made with 3.5:4.5:2 PropOH-ethyl acetate-water (v/v/v). Densitometric analysis was performed directly at 212 nm, corresponding to lambda max of escin obtained by in situ-scanning. A second degree polynomial regression relationship was found between the peak areas and the amounts of the escin standard deposited in the range 1.15-6.90 micrograms. The method is specific, accurate and reliable and was applied successfully to the quantitative determination of escin in commercial samples.

  9. Moessbauer methods and spectrometers specialized in qualitative and quantitative determinations

    International Nuclear Information System (INIS)

    Bibicu, I.

    1981-01-01

    A portable, field analyser devoted to fast qualitative and quantitative determination of cassiterite, which is the only tin compound of economic use in industry was made. This analyser differs from other similar ones described in the literature through the fact that pulses are cumulated only as long as the vibrator speed ensures a complete cancelation of the resonance condition. A NIM analyser was also manufactured which allows a qualitative determination of 2-3 iron compounds in a given sample, as well as of the total iron content. Working in geometry transmission and constant velocity regime, this analyser joins the inconstancy of a laboratory Moessbauer spectrometer with the swiftness and simplity of a specialized Moessbauer spectrometer. Analysis of the main factor that affects the qualitative and quantitative cassiterite determinations: sample structural composition, spectrometer calibrating, a.s.o. Determination accuracy is similar to those reported in the literature. Sample structural composition must be smaller than 0.1 mm for the qualitative and quantitative determinations of iron or total iron compounds. Data accuracy is similar to those reported before, but obtained by means of area measurements. As a consequence of the previous results, we have looked for the existence of some new phases in industrial Fe-C and Fe-Si steels or some new compounds appearance in the samples subjected to coroding. (author)

  10. Quantitative phase determination by using a Michelson interferometer

    International Nuclear Information System (INIS)

    Pomarico, Juan A; Molina, Pablo F; Angelo, Cristian D'

    2007-01-01

    The Michelson interferometer is one of the best established tools for quantitative interferometric measurements. It has been, and is still successfully used, not only for scientific purposes, but it is also introduced in undergraduate courses for qualitative demonstrations as well as for quantitative determination of several properties such as refractive index, wavelength, optical thickness, etc. Generally speaking, most of the measurements are carried out by determining phase distortions through the changes in the location and/or shape of the interference fringes. However, the extreme sensitivity of this tool, for which minimum deviations of the conditions of its branches can cause very large modifications in the fringe pattern, makes phase changes difficult to follow and measure. The purpose of this communication is to show that, under certain conditions, the sensitivity of the Michelson interferometer can be 'turned down' allowing the quantitative measurement of phase changes with relative ease. As an example we present how the angle (or, optionally, the refractive index) of a transparent standard optical wedge can be determined. Experimental results are shown and compared with the data provided by the manufacturer showing very good agreement

  11. Quantitative determination of tritium in metals and oxides

    International Nuclear Information System (INIS)

    Vance, D.E.; Smith, M.E.; Waterbury, G.R.

    1979-04-01

    Metallic samples are analyzed for tritium by heating the sample at 1225 K in a moist oxygen stream. The volatile products are trapped and the tritium is quantitatively determined by scintillation spectroscopy. The method is used to determine less than 1 ppb of tritium in 100-mg samples of lithium, iron, nickel, cerium, plutonium, and plutonium dioxide. Analysis of 18 cuts of a tritium-zirconium, copper foil standard over a 3-yr period showed a tritium content of 45 ppM and a standard deviation of 6 ppM

  12. [Semi-quantitative determination of methadone by TLC].

    Science.gov (United States)

    Ciobanu, Anne Marie; Baconi, Daniela; Bârcă, Maria; Guţu, Claudia; Bălălău, D

    2011-01-01

    Methadone is the main therapeutic option in heroin addiction treatment, but also an abuse substance. Given the analytical focus on the diagnosis of drug abuse and the usefulness of toxicological analysis methods in both overdose and monitoring substitution therapy, this study was aimed at the semi-quantitative determination of methadone by using Thin Layer Chromatography (TLC). By having the advantage of simplicity and rapidity, TLC finds its rightful place among the analysis methods when other relatively costly methods that involve instrumental performance are not available. TLC plates (silicagel GF 254 Merck), developing system methanol: strong ammonia 100: 1,5, photometric quantification at 254 nm, using TLC Scanner 3 (Camag). The results show that methadone can be determined semi-quantitatively in the chromatographic conditions mentioned in the two domains tested (5 - 40 microg and 10 - 80 microg), with the best results obtained in the 5 - 40 microg domain. Semi-quantitative TLC evaluation proposed by us has as main advantages the rapidity, simplicity and relatively low cost compared to other useful methods.

  13. PROJECT W-551 DETERMINATION DATA FOR EARLY LAW INTERIM PRETREATMENT SYSTEM SELECTION

    Energy Technology Data Exchange (ETDEWEB)

    TEDESCHI AR

    2008-08-11

    This report provides the detailed assessment forms and data for selection of the solids separation and cesium separation technology for project W-551, Interim Pretreatment System. This project will provide early pretreated low activity waste feed to the Waste Treatment Plant to allow Waste Treatment Plan Low Activity Waste facility operation prior to construction completion of the Pretreatment and High Level Waste facilities. The candidate solids separations technologies are rotary microfiltration and crossflow filtration, and the candidate cesium separation technologies are fractional crystallization, caustic-side solvent extraction, and ion-exchange using spherical resorcinol-formaldehyde resin. This data was used to prepare a cross-cutting technology summary, reported in RPP-RPT-37740.

  14. Determinants of disinfectant pretreatment efficacy for nitrosamine control in chloraminated drinking water.

    Science.gov (United States)

    McCurry, Daniel L; Krasner, Stuart W; von Gunten, Urs; Mitch, William A

    2015-11-01

    Utilities using chloramines need strategies to mitigate nitrosamine formation to meet potential future nitrosamine regulations. The ability to reduce NDMA formation under typical post-chloramination conditions of pretreatment with ultraviolet light from a low pressure mercury lamp (LPUV), free chlorine (HOCl), ozone (O3), and UV light from a medium pressure mercury lamp (MPUV) were compared at exposures relevant to drinking water treatment. The order of efficacy after application to waters impacted by upstream wastewater discharges was O3 > HOCl ≈ MPUV > LPUV. NDMA precursor abatement generally did not correlate well between oxidants, and waters exhibited different behaviors with respect to pH and temperature, suggesting a variety of source-dependent NDMA precursors. For wastewater-impacted waters, the observed pH dependence for precursor abatement suggested the important role of secondary or tertiary amine precursors. Although hydroxyl radicals did not appear to be important for NDMA precursor abatement during O3 or MPUV pretreatment, the efficacy of MPUV correlated strongly with dissolved organic carbon concentration (p = 0.01), suggesting alternative indirect photochemical pathways. The temperature dependences during pre- and post-disinfection indicated that NDMA formation is likely to increase during warm seasons for O3 pretreatment, decrease for HOCl pretreatment, and remain unchanged for MPUV treatment, although seasonal changes in source water quality may counteract the temperature effects. For two waters impacted by relatively high polyDADMAC coagulant doses, pretreatment with HOCl, O3, and MPUV increased NDMA formation during post-chloramination. For O3 pretreatment, hydroxyl radicals likely led to precursor formation from the polymer in the latter tests. MPUV treatment of polymer-impacted water increased subsequent NDMA formation through an indirect photochemical process. Many factors may mitigate the importance of this increased NDMA formation

  15. Quantitative determination of testosterone levels with biolayer interferometry.

    Science.gov (United States)

    Zhang, Hao; Li, Wei; Luo, Hong; Xiong, Guangming; Yu, Yuanhua

    2017-10-01

    Natural and synthetic steroid hormones are widely spread in the environment and are considered as pollutants due to their endocrine activities, even at low concentrations, which are harmful to human health. To detect steroid hormones in the environment, a novel biosensor system was developed based on the principle of biolayer interferometry. Detection is based on changes in the interference pattern of white light reflected from the surface of an optical fiber with bound biomolecules. Monitoring interactions between molecules does not require radioactive, enzymatic, or fluorescent labels. Here, 2 double-stranded DNA fragments of operator 1 (OP1) and OP2 containing 10-bp palindromic sequences in chromosomal Comamonas testosteroni DNA (ATCC11996) were surface-immobilized to streptavidin sensors. Interference changes were detected when repressor protein RepA bound the DNA sequences. DNA-protein interactions were characterized and kinetic parameters were obtained. The dissociation constants between the OP1 and OP2 DNA sequences and RepA were 9.865 × 10 -9  M and 2.750 × 10 -8  M, respectively. The reactions showed high specifically and affinity. Because binding of the 10-bp palindromic sequence and RepA was affected by RepA-testosterone binding, the steroid could be quantitatively determined rapidly using the biosensor system. The mechanism of the binding assay was as follows. RepA could bind both OP1 and testosterone. RepA binding to testosterone changed the protein conformation, which influenced the binding between RepA and OP1. The percentage of the signal detected negative correlation with the testosterone concentration. A standard curve was obtained, and the correlation coefficient value was approximately 0.97. We could quantitatively determine testosterone levels between 2.13 and 136.63 ng/ml. Each sample could be quantitatively detected in 17 min. These results suggested that the specific interaction between double-stranded OP1 DNA and the RepA protein

  16. An electronic nose for quantitative determination of gas concentrations

    Science.gov (United States)

    Jasinski, Grzegorz; Kalinowski, Paweł; Woźniak, Łukasz

    2016-11-01

    The practical application of human nose for fragrance recognition is severely limited by the fact that our sense of smell is subjective and gets tired easily. Consequently, there is considerable need for an instrument that can be a substitution of the human sense of smell. Electronic nose devices from the mid 1980s are used in growing number of applications. They comprise an array of several electrochemical gas sensors with partial specificity and a pattern recognition algorithms. Most of such systems, however, is only used for qualitative measurements. In this article usage of such system in quantitative determination of gas concentration is demonstrated. Electronic nose consist of a sensor array with eight commercially available Taguchi type gas sensor. Performance of three different pattern recognition algorithms is compared, namely artificial neural network, partial least squares regression and support vector machine regression. The electronic nose is used for ammonia and nitrogen dioxide concentration determination.

  17. VERIFICATION HPLC METHOD OF QUANTITATIVE DETERMINATION OF AMLODIPINE IN TABLETS

    Directory of Open Access Journals (Sweden)

    Khanin V. A

    2014-10-01

    Full Text Available Introduction. Amlodipine ((±-2-[(2-aminoetoksimethyl]-4-(2-chlorophenyl-1,4-dihydro-6-methyl-3,5-pyridine dicarboxylic acid 3-ethyl 5-methyl ester as besylate and small tally belongs to the group of selective long-acting calcium channel blockers, dihydropyridine derivatives. In clinical practice, as antianginal and antihypertensive agent for the treatment of cardiovascular diseases. It is produced in powder form, substance and finished dosage forms (tablets of 2.5, 5 and 10 mg. The scientific literature describes methods of quantitative determination of the drug by spectrophotometry – by his own light absorption and by reaction product with aloksan, chromatography techniques, kinetic-spectrophotometric method in substances and preparations and methods chromatomass spectrometry and stripping voltammetry. For the quantitative determination of amlodipine besylate British Pharmacopoeia and European Pharmacopoeia recommend the use of liquid chromatography method. In connection with the establishment of the second edition of SPhU and when it is comprised of articles on the finished product, we set out to analyze the characteristics of the validation of chromatographic quantitative determination of amlodipine besylate tablets and to verify the analytical procedure. Material & methods. In conducting research using substance amlodipine besylate series number AB0401013. Analysis subject pill “Amlodipine” series number 20113 manufacturer of “Pharmaceutical company “Zdorovye”. Analytical equipment used is: 2695 chromatograph with diode array detector 2996 firms Waters Corp. USA using column Nova-Pak C18 300 x 3,9 mm with a particle size of 4 μm, weight ER-182 company AND Japan, measuring vessel class A. Preparation of the test solution. To accurately sample powder tablets equivalent to 50 mg amlodipine, add 30 ml of methanol, shake for 30 minutes, dilute the solution to 50.0 ml with methanol and filtered. 5 ml of methanol solution adjusted to

  18. Quantitative Determination of Spring Water Quality Parameters via Electronic Tongue

    Directory of Open Access Journals (Sweden)

    Noèlia Carbó

    2017-12-01

    Full Text Available The use of a voltammetric electronic tongue for the quantitative analysis of quality parameters in spring water is proposed here. The electronic voltammetric tongue consisted of a set of four noble electrodes (iridium, rhodium, platinum, and gold housed inside a stainless steel cylinder. These noble metals have a high durability and are not demanding for maintenance, features required for the development of future automated equipment. A pulse voltammetry study was conducted in 83 spring water samples to determine concentrations of nitrate (range: 6.9–115 mg/L, sulfate (32–472 mg/L, fluoride (0.08–0.26 mg/L, chloride (17–190 mg/L, and sodium (11–94 mg/L as well as pH (7.3–7.8. These parameters were also determined by routine analytical methods in spring water samples. A partial least squares (PLS analysis was run to obtain a model to predict these parameter. Orthogonal signal correction (OSC was applied in the preprocessing step. Calibration (67% and validation (33% sets were selected randomly. The electronic tongue showed good predictive power to determine the concentrations of nitrate, sulfate, chloride, and sodium as well as pH and displayed a lower R2 and slope in the validation set for fluoride. Nitrate and fluoride concentrations were estimated with errors lower than 15%, whereas chloride, sulfate, and sodium concentrations as well as pH were estimated with errors below 10%.

  19. Quantitative determination of glycyrrhizinic acid by square-wave

    Directory of Open Access Journals (Sweden)

    Aneta Dimitrovska

    2003-06-01

    Full Text Available Novel adsorptive stripping square-wave voltammetric method as well as a new high-pressure liquid chromatographic method for direct determination of glycyrrhizinic acid in dosage pharmaceutical preparation, used against virus infections, have been developed. Glycyrrhizinic acid is an electrochemically active compound, which undergoes irreversible reduction on a mercury electrode surface in an aqueous medium. Its redox properties were studied thoroughly by means of square-wave voltammetry, as one of the most advanced electroanalytical technique. The voltammetric response depends mainly on the pH of the medium, composition of the supporting electrolyte, as well as the parameters of the excitement signal. It was also observed that the voltammetric properties strongly depend on the accumulation time and potential, revealing significant adsorption of glycyrrhizinic acid onto the mercury electrode surface. Upon this feature, an adsorptive stripping voltammetric method for quantitative determination of glycyrrhizinic acid was developed. A simple, sensitive and precise reversed phase HPLC method with photodiode array UV detection has also been developed, mainly for comparison and conformation of the results obtained with the voltammetric method.

  20. Effect of mixing on enzymatic hydrolysis of steam-pretreated spruce: a quantitative analysis of conversion and power consumption

    Directory of Open Access Journals (Sweden)

    Wiman Magnus

    2011-05-01

    Full Text Available Abstract Background When scaling up lignocellulose-based ethanol production, the desire to increase the final ethanol titer after fermentation can introduce problems. A high concentration of water-insoluble solids (WIS is needed in the enzymatic hydrolysis step, resulting in increased viscosity, which can cause mass and heat transfer problems because of poor mixing of the material. In the present study, the effects of mixing on the enzymatic hydrolysis of steam-pretreated spruce were investigated using a stirred tank reactor operated with different impeller speeds and enzyme loadings. In addition, the results were related to the power input needed to operate the impeller at different speeds, taking into account the changes in rheology throughout the process. Results A marked difference in hydrolysis rate at different impeller speeds was found. For example, the conversion was twice as high after 48 hours at 500 rpm compared with 25 rpm. This difference remained throughout the 96 hours of hydrolysis. Substantial amounts of energy were required to achieve only minor increases in conversion during the later stages of the process. Conclusions Impeller speed strongly affected both the hydrolysis rate of the pretreated spruce and needed power input. Similar conversions could be obtained at different energy input by altering the mixing (that is, energy input, enzyme load and residence time, an important issue to consider when designing large-scale plants.

  1. An integrated sample pretreatment platform for quantitative N-glycoproteome analysis with combination of on-line glycopeptide enrichment, deglycosylation and dimethyl labeling

    Energy Technology Data Exchange (ETDEWEB)

    Weng, Yejing; Qu, Yanyan; Jiang, Hao; Wu, Qi [National Chromatographic Research and Analysis Center, Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); University of the Chinese Academy of Sciences, Beijing 100039 (China); Zhang, Lihua, E-mail: lihuazhang@dicp.ac.cn [National Chromatographic Research and Analysis Center, Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); Yuan, Huiming [National Chromatographic Research and Analysis Center, Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); Zhou, Yuan [National Chromatographic Research and Analysis Center, Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); University of the Chinese Academy of Sciences, Beijing 100039 (China); Zhang, Xiaodan; Zhang, Yukui [National Chromatographic Research and Analysis Center, Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China)

    2014-06-23

    Highlights: • An integrated platform for quantitative N-glycoproteome analysis was established. • On-line enrichment, deglycosylation and labeling could be achieved within 160 min. • A N{sub 2}-assisted interface was applied to improve the compatibility of the platform. • The platform exhibited improved quantification accuracy, precision and throughput. - Abstract: Relative quantification of N-glycoproteomes shows great promise for the discovery of candidate biomarkers and therapeutic targets. The traditional protocol for quantitative analysis of glycoproteomes is usually off-line performed, and suffers from long sample preparation time, and the risk of sample loss or contamination due to manual manipulation. In this study, a novel integrated sample preparation platform for quantitative N-glycoproteome analysis was established, with combination of online N-glycopeptide capture by a HILIC column, sample buffer exchange by a N{sub 2}-assisted HILIC–RPLC interface, deglycosylation by a hydrophilic PNGase F immobilized enzymatic reactor (hIMER) and solid dimethyl labeling on a C18 precolumn. To evaluate the performance of such a platform, two equal aliquots of immunoglobulin G (IgG) digests were sequentially pretreated, followed by MALDI-TOF MS analysis. The signal intensity ratio of heavy/light (H/L) labeled deglycosylated peptides with the equal aliquots was 1.00 (RSD = 6.2%, n = 3), much better than those obtained by the offline protocol, with H/L ratio as 0.76 (RSD = 11.6%, n = 3). Additionally, the total on-line sample preparation time was greatly shortened to 160 min, much faster than that of offline approach (24 h). Furthermore, such an integrated pretreatment platform was successfully applied to analyze the two kinds of hepatocarcinoma ascites syngeneic cell lines with high (Hca-F) and low (Hca-P) lymph node metastasis rates. For H/L labeled Hca-P lysates with the equal aliquots, 99.6% of log 2 ratios (H/L) of quantified glycopeptides ranged from −1

  2. Prognostic value of pretreatment volume-based quantitative {sup 18}F-FDG PET/CT parameters in patients with malignant pleural mesothelioma

    Energy Technology Data Exchange (ETDEWEB)

    Kitajima, Kazuhiro, E-mail: kitajima@med.kobe-u.ac.jp [Division of Nuclear Medicine and PET Center, Department of Radiology, Hyogo College of Medicine, Hyogo (Japan); Doi, Hiroshi, E-mail: h-doi@hyo-med.ac.jp [Department of Radiology, Hyogo College of Medicine, Hyogo (Japan); Kuribayashi, Kozo, E-mail: kuririn@hyo-med.ac.jp [Division of Respiratory Medicine, Department of Internal Medicine, Hyogo College of Medicine, Hyogo (Japan); Hashimoto, Masaki, E-mail: kogekogemasaki@gmail.com [Department of Thoracic Surgery, Hyogo College of Medicine, Hyogo (Japan); Tsuchitani, Tatsuya, E-mail: tty-823@hyo-med.ac.jp [Department of Radiological Technology, Hyogo College of Medicine College Hospital, Hyogo (Japan); Tanooka, Masao, E-mail: masao1108@gmail.com [Department of Radiological Technology, Hyogo College of Medicine College Hospital, Hyogo (Japan); Fukushima, Kazuhito, E-mail: fukuchan00106@gmail.com [Division of Nuclear Medicine and PET Center, Department of Radiology, Hyogo College of Medicine, Hyogo (Japan); Nakano, Takashi, E-mail: t-nakano@hyo-med.ac.jp [Division of Respiratory Medicine, Department of Internal Medicine, Hyogo College of Medicine, Hyogo (Japan); Hasegawa, Seiki, E-mail: hasegawa@hyo-med.ac.jp [Department of Thoracic Surgery, Hyogo College of Medicine, Hyogo (Japan); Hirota, Shozo, E-mail: hirota-s@hyo-med.ac.jp [Department of Radiology, Hyogo College of Medicine, Hyogo (Japan)

    2017-01-15

    Purpose: To investigate the relationships between pretreatment volume-based quantitative {sup 18}F-fluorodeoxyglucose (FDG) positron emission tomography/computed tomography (PET/CT) parameters and overall survival (OS) in patients with malignant pleural mesothelioma (MPM). Materials and methods: We retrospectively reviewed data from 201 MPM patients, of whom 38 underwent surgical resection, and calculated the maximum standardized uptake value (SUVmax), metabolic tumor volume (MTV), and total lesion glycolysis (TLG), including primary tumors and nodal or distant metastatic lesions, on pretreatment {sup 18}F-FDG PET/CT. Relationships between clinicopathological factors (age, sex, performance status, European Organization for Research and Treatment of Cancer [EORTC] score, histological subtype, TNM stage, and treatment strategy), volume-based quantitative PET/CT parameters, and OS were evaluated using a Cox proportional hazards model and log-rank test. Results: The median follow-up was 15 months (range, 1–96 months; median, 17 months). In a univariate analysis of all patients, older age (p < 0.05), high EORTC score (p < 0.001), non-epithelioid histological subtype (p < 0.001), high T stage (p < 0.001), positive N/M status (p < 0.05, p < 0.001), advanced TNM stage (p < 0.001), non-surgical treatment (p < 0.001), and high SUVmax (p < 0.001), MTV (p < 0.001), or TLG (p < 0.001) were associated with significantly shorter OS. A multivariate analysis confirmed non-epithelioid subtype (hazard ratio [HR]: 1.69, 95% confidence interval [CI]: 1.14–2.48; p < 0.05), non-surgical treatment (HR: 0.58, 95% CI: 0.34–0.95; p < 0.05), and high TLG (HR: 1.97, 95% CI: 1.14–3.44; p < 0.05) as independent negative predictors. Conclusions: Pretreatment volume-based quantitative {sup 18}F-FDG PET/CT parameters, especially TLG, could serve as potential surrogate markers for MPM prognosis.

  3. [Quantitative determination of PVC concentration by Raman spectrum].

    Science.gov (United States)

    Huang, Zheng-liang; Wang, Jing-dai; Jiang, Bin-bo; Yang, Yong-rong; Chen, Jie-xun; Liao, Zu-wei

    2011-03-01

    Quantitative determination of polyvinyl chloride (PVC) concentration by Raman spectrum was studied in the present work. According to partial least squares (PLS) analysis, it was found that scores of PLS factor 1 were proportional to the concentrations of the sample solutions. Meanwhile, the loadings of factor 1 could reflect the contents of PVC and cyclohexanone simultaneously. The PLS regression model for PVC concentration prediction was built. The values of r and root mean square error (RMSE) between predictive results and actual values were 0.9963 and 2.775, respectively. The Raman characteristic peaks of PVC and cyclohexanone were found, including the C-Cl bond for PVC (620 and 695 cm(-1)) and the alicyclic ketone for cyclohexanone (1709 cm(-1)). By using internal standard method, another model for PVC concentration prediction was established, and the values of r and RMSE were 0.9941 and 3.151, respectively. The results indicated that it is feasible to use Raman spectrum to detect the PVC concentration, which is of significant importance to PVC recycling.

  4. Electrochemical method for quantitative determination of trace amounts of lead.

    Science.gov (United States)

    Viyannalage, Lasantha T; Bliznakov, Stoyan; Dimitrov, Nikolay

    2008-03-15

    An ultrasensitive chronoamperometric method for quantitative determination of trace amounts of lead (down to 20 ppb) in acidic solutions is proposed in this paper. The method is based on observations that a complete underpotentially deposited (UPD) lead layer inhibits the electroreduction of nitrate on a bare Cu(111) electrode. To asses the limits of the method, both the electroreduction of nitrate and UPD of lead monolayer on copper single (111) and polycrystalline electrodes in perchloric acidic solution are studied by means of cyclic voltammetry, chronoamperometry, and rotating disk electrode (RDE) experiments. It is found that an inexpensive polycrystalline copper electrode is sensitive enough for analytical detection of lead traces in electrolytes down to 1 x 10(-8) M. Analytical results obtained by the proposed method in 2 orders of magnitude concentration range are compared to atomic absorption spectroscopy measurements to evaluate and assess the sensitivity of the employed experimental protocol. The excellent match between both analytical approaches validates the applicability of the proposed method.

  5. A Method for Quantitative Determination of Biofilm Viability

    Directory of Open Access Journals (Sweden)

    Maria Strømme

    2012-06-01

    Full Text Available In this study we present a scheme for quantitative determination of biofilm viability offering significant improvement over existing methods with metabolic assays. Existing metabolic assays for quantifying viable bacteria in biofilms usually utilize calibration curves derived from planktonic bacteria, which can introduce large errors due to significant differences in the metabolic and/or growth rates of biofilm bacteria in the assay media compared to their planktonic counterparts. In the presented method we derive the specific growth rate of Streptococcus mutans bacteria biofilm from a series of metabolic assays using the pH indicator phenol red, and show that this information could be used to more accurately quantify the relative number of viable bacteria in a biofilm. We found that the specific growth rate of S. mutans in biofilm mode of growth was 0.70 h−1, compared to 1.09 h−1 in planktonic growth. This method should be applicable to other bacteria types, as well as other metabolic assays, and, for example, to quantify the effect of antibacterial treatments or the performance of bactericidal implant surfaces.

  6. Dry-air drying at room temperature - a practical pre-treatment method of tree leaves for quantitative analyses of phenolics?

    Science.gov (United States)

    Tegelberg, Riitta; Virjamo, Virpi; Julkunen-Tiitto, Riitta

    2018-03-09

    In ecological experiments, storage of plant material is often needed between harvesting and laboratory analyses when the number of samples is too large for immediate, fresh analyses. Thus, accuracy and comparability of the results call for pre-treatment methods where the chemical composition remains unaltered and large number of samples can be treated efficiently. To study if a fast dry-air drying provides an efficient pre-treatment method for quantitative analyses of phenolics. Dry-air drying of mature leaves was done in a drying room equipped with dehumifier (10% relative humidity, room temperature) and results were compared to freeze-drying or freeze-drying after pre-freezing in liquid nitrogen. The quantities of methanol-soluble phenolics of Betula pendula Roth, Betula pubescens Ehrh., Salix myrsinifolia Salisb., Picea abies L. Karsten and Pinus sylvestris L. were analysed with HPLC and condensed tannins were analysed using the acid-butanol test. In deciduous tree leaves (Betula, Salix), the yield of most of the phenolic compounds was equal or higher in samples dried in dry-air room than the yield from freeze-dried samples. In Picea abies needles, however, dry-air drying caused severe reductions in picein, stilbenes, condensed tannin and (+)-catechin concentrations compared to freeze-drying. In Pinus sylvestris highest yields of neolignans but lowest yields of acetylated flavonoids were obtained from samples freeze-dried after pre-freezing. Results show that dry-air drying provides effective pre-treatment method for quantifying the soluble phenolics for deciduous tree leaves, but when analysing coniferous species, the different responses between structural classes of phenolics should be taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

  7. Determination of methyl methanesulfonate pretreatment effect in Drosophila melanogaster larvaes upon repair mechanisms in somatic cells

    International Nuclear Information System (INIS)

    Hernandez Paz, M.

    1992-01-01

    To make evident the existence of SOS repair mecanism in somatic cells, larvaes of drosophila melanogaster with MWH markers for females and FLR markers for males were used. This larvaes received a pretreatment with MMS at concentrations of 0.0007% and 0.0014% during 24 hours and latter a treatment with gamma rays at different dosis. SMART program was used to make stastistical evaluations. Small spots were observed which can have two origins. First could be damage in the last part of third stage in which cells are in last divisions and second could be the damage to larvaes in early stages in shich pretreatment with MMS cause lesions which prevent the reproduction of the cells. Also big spots were observed which presence is due to recombination. It was detected than the bigger the concentration of MMS and radiation dose, the bigger the induced damage. In some groups such observation was impossible may be to technical problems as relative humidity, out of phase in the growth of larvaes giving place that treatment were given in three stages. For this reasons it was impossible to discriminate if drosophila melanogaster is wheter or not capable to induce a repair mechanism (Author)

  8. Quantitative determination and monitoring of water distribution in Aespoe granite

    International Nuclear Information System (INIS)

    Zimmer, U.

    1998-01-01

    To identify possible zones of two-phase-flow and the extension of the excavation disturbed zone, geoelectric measurements are conducted in the ZEDEX- and the DEMO-tunnel. The electric resistivity of a hard rock is usually determined by its water content, its water salinity and its porosity structure. By calibration measurements of the resistivity on rocks with well known water content, a relation between resistivity and water content for Aespoe granite is determined. This relation is used to correlate the in-situ resistivity with the water content of the rock. To determine the in-situ resistivity between the ZEDEX- and the DEMO-tunnel an electrode array of nearly 300 electrodes was installed along the tunnel walls and in one borehole. With a semiautomatic recording unit which is operated by a telephone connection from the GRS-office in Braunschweig/Germany, the resistivity is monitored between and around the tunnels. To correlate the resistivity with the water content, the measured apparent resistivity has to be converted into a resistivity model of the underground. Since many thin water bearing fractures complicate this inversion process, the accuracy and resolution of the different inversion programs are checked before their application to the data. It was found that an acceptable quantitative reconstruction of the resistivity requires the integration of geometric information about the fracture zones into the inversion process. For a rough estimation of the position of possible fracture zones, a simple inversion without any geometric boundary conditions can be used. Since the maximum investigation area is limited along a single tunnel for profile measurements, tomographic measurements were also applied to estimate the resistivity distribution between the ZEDEX- and the DEMO-tunnel. These tomographic measurements have a lower resolution than the profile measurements due to the required large computer power, but result in reconstructions that give an estimate of

  9. Qualitative and quantitative determination of water in airborne particulate matter

    Directory of Open Access Journals (Sweden)

    S. Canepari

    2013-02-01

    Full Text Available This paper describes the optimization and validation of a new simple method for the quantitative determination of water in atmospheric particulate matter (PM. The analyses are performed by using a coulometric Karl-Fisher system equipped with a controlled heating device; different water contributions are separated by the application of an optimized thermal ramp (three heating steps: 50–120 °C, 120–180 °C, 180–250 °C.

    The analytical performance of the method was verified by using standard materials containing 5.55% and 1% by weight of water. The recovery was greater than 95%; the detection limit was about 20 μg. The method was then applied to NIST Reference Materials (NIST1649a, urban particulate matter and to real PM10 samples collected in different geographical areas. In all cases the repeatability was satisfactory (10–15%.

    When analyzing the Reference Material, the separation of four different types of water was obtained. In real PM10 samples the amount of water and its thermal profile differed as a function of the chemical composition of the dust. Mass percentages of 3–4% of water were obtained in most samples, but values up to about 15% were reached in areas where the chemical composition of PM is dominated by secondary inorganic ions and organic matter. High percentages of water were also observed in areas where PM is characterized by the presence of desert dust.

    A possible identification of the quality of water released from the samples was tried by applying the method to some hygroscopic compounds that are likely contained in PM (pure SiO2, Al2O3, ammonium salts, carbohydrates and dicarboxylic acids and by comparing the results with those obtained from field samples.

  10. Quantitative fuel motion determination with the CABRI fast neutron hodoscope

    International Nuclear Information System (INIS)

    Baumung, K.; Augier, G.

    1991-01-01

    The fast neutron hodoscope installed at the CABRI reactor in Cadarache, France, is employed to provide quantitative fuel motion data during experiments in which single liquid-metal fast breeder reactor test pins are subjected to simulated accident conditions. Instrument design and performance are reviewed, the methods for the quantitative evaluation are presented, and error sources are discussed. The most important findings are the axial expansion as a function of time, phenomena related to pin failure (such as time, location, pin failure mode, and fuel mass ejected after failure), and linear fuel mass distributions with a 2-cm axial resolution. In this paper the hodoscope results of the CABRI-1 program are summarized

  11. [Comparative study on five pretreatment methods for ICP-OES determination of mineral elements in Rosa rugosa].

    Science.gov (United States)

    Zhao, Ning; Yang, Bin; Duan, Yu-Cen; Lei, Ran

    2011-08-01

    Abstract Five different pretreatment methods, including dry ashing and microwave digestion with four acid systems (HNO3 + H2O2, HNO3 + H2O2 + HF, HNO3 + HClO4 and HNO3 + HClO4 + HF), were employed for digestion of the samples of Rosa rugosa. Nine major and trace elements were determined using ICP-OES method. The addition standard recovery rates indicate that, with the system of HNO3 + HClO4, better results can be obtained for most of the determined elements. With this method, except for Fe, the recovery rates are in the range of 95.4%-104.6%. For Fe, higher recovery rate (99%) was obtained with HNO3 + H2O2 + HF system.

  12. Application of quantitative and qualitative methods for determination ...

    African Journals Online (AJOL)

    This article covers the issues of integration of qualitative and quantitative methods applied when justifying management decision-making in companies implementing ... The lower level includes criteria: 1) created value, sales volume, productivity, customer satisfaction; 2) net cash flow, turnover of current assets, EBITDA; ...

  13. Study on different pre-treatment procedures for metal determination in Orujo spirit samples by ICP-AES

    International Nuclear Information System (INIS)

    Barciela, Julia; Vilar, Manuela; Garcia-Martin, Sagrario; Pena, Rosa M.; Herrero, Carlos

    2008-01-01

    In this work several pre-treatment methods were studied for metal (Na, K, Mg, Cu and Ca) determination in Orujo spirit samples using inductively coupled plasma atomic emission spectrometry (ICP-AES). Dilution, digestion, evaporation, and cryogenic desolvatation techniques were comparatively evaluated. Because of their analytical characteristics, digestion and evaporation with nitrogen current were found to be appropriate procedures for the determination of metals in alcoholic spirit samples. Yet, if simplicity and application time are to be considered, the latter-evaporation in a water bath with a nitrogen current-stands out as the optimum procedure for any further determinations in Orujo samples by ICP-AES. Low detection levels and wide linear ranges (sufficient to determine these metals in the samples studied) were achieved for each metal. The recoveries (in the 97.5-100.5% range) and the precision (R.S.D. lower than 5.6%) obtained were also satisfactory. The selected procedure was applied to determine the content of metals in 80 representative Galician Orujo spirit samples with and without a Certified Brand of Origin (CBO) which had been produced using different distillation systems. The metal concentrations ranged between 0.37 and 79.7 mg L -1 for Na, -1 for K, 0.02-4.83 mg L -1 for Mg content, -1 for Cu and 0.03-13.10 mg L -1 for Ca

  14. Absolute nondestructive quantitative determination of uranium in special nuclear materials

    International Nuclear Information System (INIS)

    Dragnev, T.; Damyanov, B.; Grozev, G.; Karamanova, J.

    1985-01-01

    An absolute nondestructive method for quantitative measurement of uranium concentration and enrichment in special nuclear materials is proposed. The method uses intrinsic calibration and portable instrumentation and the particularly suitable for IAEA safequards applications. The intrinsic calibration accumulates the positive experience of the previous measurements and the results will be continuously improving. It is possible to measure standards in laboratories and use the results for analysis at different time and places. The tests show a good agreement with known classical methods and better results in some cases

  15. Biomass pretreatment

    Science.gov (United States)

    Hennessey, Susan Marie; Friend, Julie; Elander, Richard T; Tucker, III, Melvin P

    2013-05-21

    A method is provided for producing an improved pretreated biomass product for use in saccharification followed by fermentation to produce a target chemical that includes removal of saccharification and or fermentation inhibitors from the pretreated biomass product. Specifically, the pretreated biomass product derived from using the present method has fewer inhibitors of saccharification and/or fermentation without a loss in sugar content.

  16. Electrochemically pretreated zeolite-modified carbon-paste electrodes for determination of linuron in an agricultural formulation and water

    International Nuclear Information System (INIS)

    Siara, L.R.; Lima, F. de; Cardoso, C.A.L.; Arruda, G.J.

    2015-01-01

    Highlights: • Cyclic voltammetry, square-wave voltammetry, electrochemical impedance spectroscopic, and scanning electron microscopy were employed. • Kinetic parameters (n, α, k s , and Γ) were calculated. • High sensitivity was observed in the linear concentration range. • Excellent recovery rates were achieved for tap water samples. • The method proved applicable to the determination of linuron in the presence of potential organic and inorganic interferents, none of which affected the results. - Abstract: A simple and inexpensive, yet highly sensitive electrochemical method for quantifying linuron in tap and distilled water and in agricultural formulations was developed using electrochemically pretreated zeolite-modified carbon-paste electrodes (ZMCPEs). Compared with untreated ZMCPEs, the electrochemically pretreated electrodes showed significantly enhanced peak currents for linuron oxidation. Scanning electron microscopy and energy-dispersive x-ray spectroscopy were used to examine the structure of the zeolite-modified and unmodified carbon-paste electrodes (CPEs). ZMCPEs were electrochemically characterized using cyclic voltammetry, chronocoulometry, square-wave voltammetry, and electrochemical impedance spectroscopy. A mechanism for linuron oxidation on ZMCPE surfaces was proposed. The electrochemical variables taken into account were electrode area, number of transferred electrons, electron transfer coefficient, electrode reaction standard rate constant, surface coverage, and capacitance of the electric double layer. Zeolite was found to have a strong influence on these variables. The electrochemical procedure applied to linuron was developed using electrochemically pretreated ZMCPEs under optimal conditions. Linuron oxidation currents exhibited linear concentration in the 87.36 to 625.72 nmol L −1 range, with a limit of detection of 22.57 nmol L −1 . The proposed electrochemical method was employed to quantify linuron in tap and distilled

  17. Qualitative and Quantitative Determination of Quorum Sensing Inhibition In Vitro

    DEFF Research Database (Denmark)

    Jakobsen, Tim Holm; Alhede, Maria; Hultqvist, Louise Dahl

    2018-01-01

    The formation of biofilms in conjunction with quorum sensing (QS) regulated expression of virulence by opportunistic pathogens contributes significantly to immune evasion and tolerance to a variety of antimicrobial treatments. The present protocol describes methods to determine the in vitro...

  18. Quantitative sandwich ELISA for the determination of fish in foods.

    Science.gov (United States)

    Faeste, Christiane K; Plassen, Christin

    2008-01-01

    Allergy to fish represents one of the most prevalent causes for severe food-allergic reactions. Therefore, food authorities in different countries have implemented mandatory labeling of fish in pre-packed foods. Detection of fish proteins in food has previously been based on the use of patient serum. In the present study, a novel sandwich enzyme-linked immunosorbent assay (ELISA) for the quantitation of fish in food matrixes has been developed and validated, using a polyclonal rabbit anti-cod parvalbumin antibody for capture and a biotinylated conjugate of the same antibody for detection. By employing the ubiquitous muscle protein parvalbumin as target the method succeeds to detect a variety of fish. However, the ELISA is specific for fish and does not cross-react with other species. Recoveries ranged from 68-138% in typical food matrixes, while the intra- and inter-assay precisions were parvalbumin ELISA with a limit of detection of 0.01 mg parvalbumin/kg food, about 5 mg fish/kg food, seems sufficient to detect fish protein traces in foods at levels low enough to minimize the risk for fish allergic consumers.

  19. A new trend to determine biochemical parameters by quantitative FRET assays.

    Science.gov (United States)

    Liao, Jia-yu; Song, Yang; Liu, Yan

    2015-12-01

    Förster resonance energy transfer (FRET) has been widely used in biological and biomedical research because it can determine molecule or particle interactions within a range of 1-10 nm. The sensitivity and efficiency of FRET strongly depend on the distance between the FRET donor and acceptor. Historically, FRET assays have been used to quantitatively deduce molecular distances. However, another major potential application of the FRET assay has not been fully exploited, that is, the use of FRET signals to quantitatively describe molecular interactive events. In this review, we discuss the use of quantitative FRET assays for the determination of biochemical parameters, such as the protein interaction dissociation constant (K(d)), enzymatic velocity (k(cat)) and K(m). We also describe fluorescent microscopy-based quantitative FRET assays for protein interaction affinity determination in cells as well as fluorimeter-based quantitative FRET assays for protein interaction and enzymatic parameter determination in solution.

  20. Quantitative determination of alliin in dried garlic cloves and ...

    African Journals Online (AJOL)

    Purpose: To standardize the garlic samples and its products for alliin contents. Methods: A direct high-performance thin-layer chromatographic (HPTLC) method was developed to determine alliin in Chinese (CG) and Indian garlic (IG) and two other marketed products from USA and UK, respectively. Scanning and ...

  1. Quantitative Determination of Ceramide Molecular Species in Dendritic Cells

    Directory of Open Access Journals (Sweden)

    Samar Al Makdessi

    2016-09-01

    Full Text Available Background/Aims: The activation of acid sphingomyelinase by cellular stress or receptors or the de novo synthesis lead to the formation of ceramide (N-acylsphingosine, which in turn modifies the biophysical properties of cellular membrane and greatly amplifies the intensity of the initial signal. Ceramide, which acts by re-organizing a given signalosome rather than being a second messenger, has many functions in infection biology, cancer, cardiovascular syndromes, and immune regulation. Experimental studies on the infection of human cells with different bacterial agents demonstrated the activation of the acid sphingomyelinase/ceramide system. Moreover, the release of ceramide was found to be a requisite for the uptake of the pathogen. Considering the particular importance of the cellular role of ceramide, it was necessary to develop sensitive and accurate methods for its quantification. Methods: Here, we describe a method quantifying ceramide in dendritic cells and defining the different fatty acids (FA bound to sphingosine. The main steps of the method include extraction of total lipids, separation of the ceramide by thin-layer chromatography, derivatization of ceramide-fatty acids (Cer-FA, and quantitation of these acids in their methyl form by gas chromatography on polar capillary columns. The identification of FA was achieved by means of known standards and confirmed by mass spectrometry. Results: FA ranging between C10 and C24 could be detected and quantified. The concentration of the sum of Cer-FA amounted to 14.88 ± 8.98 nmol/106 cells (n=10. Oleic acid, which accounted for approximately half of Cer-FA (7.73 ± 6.52 nmol/106 cells was the predominant fatty acid followed by palmitic acid (3.47 ± 1.54 nmol/106 cells. Conclusion: This highly sensitive method allows the quantification of different molecular species of ceramides.

  2. Study on different pre-treatment procedures for metal determination in Orujo spirit samples by ICP-AES

    Energy Technology Data Exchange (ETDEWEB)

    Barciela, Julia; Vilar, Manuela; Garcia-Martin, Sagrario [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena, Rosa M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)], E-mail: qarosa@lugo.usc.es; Herrero, Carlos [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)], E-mail: cherrero@lugo.usc.es

    2008-10-17

    In this work several pre-treatment methods were studied for metal (Na, K, Mg, Cu and Ca) determination in Orujo spirit samples using inductively coupled plasma atomic emission spectrometry (ICP-AES). Dilution, digestion, evaporation, and cryogenic desolvatation techniques were comparatively evaluated. Because of their analytical characteristics, digestion and evaporation with nitrogen current were found to be appropriate procedures for the determination of metals in alcoholic spirit samples. Yet, if simplicity and application time are to be considered, the latter-evaporation in a water bath with a nitrogen current-stands out as the optimum procedure for any further determinations in Orujo samples by ICP-AES. Low detection levels and wide linear ranges (sufficient to determine these metals in the samples studied) were achieved for each metal. The recoveries (in the 97.5-100.5% range) and the precision (R.S.D. lower than 5.6%) obtained were also satisfactory. The selected procedure was applied to determine the content of metals in 80 representative Galician Orujo spirit samples with and without a Certified Brand of Origin (CBO) which had been produced using different distillation systems. The metal concentrations ranged between 0.37 and 79.7 mg L{sup -1} for Na,

  3. Determination of propylthiouracil in pharmaceuticals by differential pulse voltammetry using a cathodically pretreated boron-doped diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Sartori, Elen Romao [Universidade Estadual de Londrina, PR (Brazil). Dept. de Quimica; Trench, Aline Barrios; Rocha-Filho, Romeu C.; Fatibello-Filho, Orlando, E-mail: bello@ufscar.br [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica

    2013-09-15

    A simple procedure is described for the determination of propylthiouracil (PTU) by differential pulse voltammetry (DPV) using a cathodically pretreated boron-doped diamond (BDD) electrode. Cyclic voltammetry studies indicate that the oxidation of PTU is irreversible at a peak potential of 1.42 V (vs. Ag/AgCl (3.0 mol L{sup -1} KCl)) in a Britton-Robinson (BR) buffer solution (pH 2.0). Under optimized conditions, the obtained analytical curve was linear (r = 0.9985) for the PTU concentration range of 1.0 to 29.1 {mu}mol L{sup -1} in a BR buffer solution (pH 2.0), with a detection limit of 0.90 {mu}mol L{sup -1}. The proposed method was successfully applied in the determination of PTU in pharmaceutical samples, with results in agreement at a 95% confidence level with those obtained using an official titration method. (author)

  4. A quantitative method for determining spatial discriminative capacity

    Directory of Open Access Journals (Sweden)

    Dennis Robert G

    2008-03-01

    Full Text Available Abstract Background The traditional two-point discrimination (TPD test, a widely used tactile spatial acuity measure, has been criticized as being imprecise because it is based on subjective criteria and involves a number of non-spatial cues. The results of a recent study showed that as two stimuli were delivered simultaneously, vibrotactile amplitude discrimination became worse when the two stimuli were positioned relatively close together and was significantly degraded when the probes were within a subject's two-point limen. The impairment of amplitude discrimination with decreasing inter-probe distance suggested that the metric of amplitude discrimination could possibly provide a means of objective and quantitative measurement of spatial discrimination capacity. Methods A two alternative forced-choice (2AFC tracking procedure was used to assess a subject's ability to discriminate the amplitude difference between two stimuli positioned at near-adjacent skin sites. Two 25 Hz flutter stimuli, identical except for a constant difference in amplitude, were delivered simultaneously to the hand dorsum. The stimuli were initially spaced 30 mm apart, and the inter-stimulus distance was modified on a trial-by-trial basis based on the subject's performance of discriminating the stimulus with higher intensity. The experiment was repeated via sequential, rather than simultaneous, delivery of the same vibrotactile stimuli. Results Results obtained from this study showed that the performance of the amplitude discrimination task was significantly degraded when the stimuli were delivered simultaneously and were near a subject's two-point limen. In contrast, subjects were able to correctly discriminate between the amplitudes of the two stimuli when they were sequentially delivered at all inter-probe distances (including those within the two-point limen, and improved when an adapting stimulus was delivered prior to simultaneously delivered stimuli. Conclusion

  5. Biogas production from ensiled meadow grass; effect of mechanical pretreatments and rapid determination of substrate biodegradability via physicochemical methods

    DEFF Research Database (Denmark)

    Tsapekos, Panagiotis; Kougias, Panagiotis; Angelidaki, Irini

    2015-01-01

    As the biogas sector is rapidly expanding, there is an increasing need in finding new alternative feedstock to biogas plants. Meadow grass can be a suitable co-substrate and if ensiled it can be supplied to biogas plants continuously throughout the year. Nevertheless, this substrate is quite...... recalcitrant and therefore efficient pretreatment is needed to permit easy access of microbes to the degradable components. In this study, different mechanical pretreatment methods were applied on ensiled meadow grass to investigate their effect on biomass biodegradability. All the tested pretreatments...

  6. Qualitative and quantitative determination of quorum sensing inhibition in vitro

    DEFF Research Database (Denmark)

    Jakobsen, Tim Holm; van Gennip, Maria; Christensen, Louise Dahl

    2011-01-01

    The formation of biofilms in conjunction with quorum sensing (QS)-regulated expression of virulence by opportunistic pathogens contributes significantly to immune evasion and tolerance to a variety of antimicrobial treatments. The present protocol describes methods to determine the in vitro...... efficacy of potential quorum sensing inhibitors (QSIs). Work on Pseudomonas aeruginosa has shown that chemical blockage of QS is a promising new antimicrobial strategy. Several live bacterial reporter systems been developed to screen extracts and pure compounds for QSI activity. Here we describe the usage...

  7. Quantitative interpretation of tracks for determination of body mass.

    Science.gov (United States)

    Schanz, Tom; Lins, Yvonne; Viefhaus, Hanna; Barciaga, Thomas; Läbe, Sashima; Preuschoft, Holger; Witzel, Ulrich; Sander, P Martin

    2013-01-01

    To better understand the biology of extinct animals, experimentation with extant animals and innovative numerical approaches have grown in recent years. This research project uses principles of soil mechanics and a neoichnological field experiment with an African elephant to derive a novel concept for calculating the mass (i.e., the weight) of an animal from its footprints. We used the elephant's footprint geometry (i.e., vertical displacements, diameter) in combination with soil mechanical analyses (i.e., soil classification, soil parameter determination in the laboratory, Finite Element Analysis (FEA) and gait analysis) for the back analysis of the elephant's weight from a single footprint. In doing so we validated the first component of a methodology for calculating the weight of extinct dinosaurs. The field experiment was conducted under known boundary conditions at the Zoological Gardens Wuppertal with a female African elephant. The weight of the elephant was measured and the walking area was prepared with sediment in advance. Then the elephant was walked across the test area, leaving a trackway behind. Footprint geometry was obtained by laser scanning. To estimate the dynamic component involved in footprint formation, the velocity the foot reaches when touching the subsoil was determined by the Digital Image Correlation (DIC) technique. Soil parameters were identified by performing experiments on the soil in the laboratory. FEA was then used for the backcalculation of the elephant's weight. With this study, we demonstrate the adaptability of using footprint geometry in combination with theoretical considerations of loading of the subsoil during a walk and soil mechanical methods for prediction of trackmakers weight.

  8. Quantitative interpretation of tracks for determination of body mass.

    Directory of Open Access Journals (Sweden)

    Tom Schanz

    Full Text Available To better understand the biology of extinct animals, experimentation with extant animals and innovative numerical approaches have grown in recent years. This research project uses principles of soil mechanics and a neoichnological field experiment with an African elephant to derive a novel concept for calculating the mass (i.e., the weight of an animal from its footprints. We used the elephant's footprint geometry (i.e., vertical displacements, diameter in combination with soil mechanical analyses (i.e., soil classification, soil parameter determination in the laboratory, Finite Element Analysis (FEA and gait analysis for the back analysis of the elephant's weight from a single footprint. In doing so we validated the first component of a methodology for calculating the weight of extinct dinosaurs. The field experiment was conducted under known boundary conditions at the Zoological Gardens Wuppertal with a female African elephant. The weight of the elephant was measured and the walking area was prepared with sediment in advance. Then the elephant was walked across the test area, leaving a trackway behind. Footprint geometry was obtained by laser scanning. To estimate the dynamic component involved in footprint formation, the velocity the foot reaches when touching the subsoil was determined by the Digital Image Correlation (DIC technique. Soil parameters were identified by performing experiments on the soil in the laboratory. FEA was then used for the backcalculation of the elephant's weight. With this study, we demonstrate the adaptability of using footprint geometry in combination with theoretical considerations of loading of the subsoil during a walk and soil mechanical methods for prediction of trackmakers weight.

  9. Determination of acoustic fields in acidic suspensions of peanut shell during pretreatment with high-intensity ultrasound

    Directory of Open Access Journals (Sweden)

    Tiago Carregari Polachini

    Full Text Available Abstract The benefits of high-intensity ultrasound in diverse processes have stimulated many studies based on biomass pretreatment. In order to improve processes involving ultrasound, a calorimetric method has been widely used to measure the real power absorbed by the material as well as the cavitation effects. Peanut shells, a byproduct of peanut processing, were immersed in acidified aqueous solutions and submitted to an ultrasonic field. Acoustic power absorbed, acoustic intensity and power yield were obtained through specific heat determination and experimental data were modeled in different conditions. Specific heat values ranged from 3537.0 to 4190.6 J·kg-1·K-1, with lower values encountered for more concentrated biomass suspensions. The acoustic power transmitted and acoustic intensity varied linearly with the applied power and quadratically with solids concentration, reaching maximum values at higher applied nominal power and for less concentrated suspensions. A power yield of 82.7% was reached for dilute suspensions at 320 W, while 6.4% efficiency was observed for a concentrated suspension at low input energy (80 W.

  10. Quantitative determination of 210Po in geochemical samples

    International Nuclear Information System (INIS)

    Dyck, W.; Bristow, Q.

    1984-01-01

    To test the usefulness of 210 Po in soils as a means of detecting buried U mineralization, methods for the determination of 210 Po were investigated and adapted for routine production of 210 Po data from geochemical samples. A number of conditions affecting autodeposition and detection of 210 Po were investigated. The optimum area of deposition with a 450 mm 2 solid state detector was found to be 300 mm 2 . Convenience dictated room temperature over-night deposition times, although increased temperature increased speed and efficiency of deposition. A clear inverse relationship was observed between volume of solution and deposition efficiency with stirring times of less than 2 hours. For routine analysis, soil and rock powders were dissolved by leaching 1 g samples in teflon beakers successively with conc. HNO 3 , HF, and HNO 3 -HClO 4 , evaporating the solution to dryness between leaches, and taking the residue up in 20 mL 0.5 M HCl. The 210 Po was deposited on 19 mm diameter Ni discs and counted with an alpha spectrometer system employing 450 mm 2 ruggedized surface barrier detectors. The method achieved 90 percent recovery of 210 Po from solution and a detection efficiency of 30 percent. With a counting time of 3 hours, the method is capable of detecting 0.2 pCi of 210 Po per gram of sample

  11. Quantitative Determination of Isotope Ratios from Experimental Isotopic Distributions

    Science.gov (United States)

    Kaur, Parminder; O’Connor, Peter B.

    2008-01-01

    Isotope variability due to natural processes provides important information for studying a variety of complex natural phenomena from the origins of a particular sample to the traces of biochemical reaction mechanisms. These measurements require high-precision determination of isotope ratios of a particular element involved. Isotope Ratio Mass Spectrometers (IRMS) are widely employed tools for such a high-precision analysis, which have some limitations. This work aims at overcoming the limitations inherent to IRMS by estimating the elemental isotopic abundance from the experimental isotopic distribution. In particular, a computational method has been derived which allows the calculation of 13C/12C ratios from the whole isotopic distributions, given certain caveats, and these calculations are applied to several cases to demonstrate their utility. The limitations of the method in terms of the required number of ions and S/N ratio are discussed. For high-precision estimates of the isotope ratios, this method requires very precise measurement of the experimental isotopic distribution abundances, free from any artifacts introduced by noise, sample heterogeneity, or other experimental sources. PMID:17263354

  12. Quantitative determination of deoxyribonucleic acid in rat brain

    Science.gov (United States)

    Penn, N. W.; Suwalski, R.

    1969-01-01

    1. A procedure is given for spectrophotometric analysis of rat brain DNA after its resolution into component bases. Amounts of tissue in the range 50–100mg. can be used. 2. The amount of DNA obtained by the present method is 80% greater than that reported for rat brain by a previous procedure specific for DNA thymine. Identity of the material is established by the base ratios of purines and pyrimidines. The features responsible for the higher yield are the presence of dioxan during alkaline hydrolysis of tissue, the determination of the optimum concentration of potassium hydroxide in this step and omission of organic washes of the initial acid-precipitated residues. 3. The requirement for dioxan during alkaline hydrolysis suggests a possible association of brain DNA with lipid. The concentration of potassium hydroxide that gives maximum yield is 0·1m, indicating that there may be internucleotide linkages in this DNA that are more sensitive to alkali than those of liver or thymus DNA. 4. This procedure gives low yields of DNA from liver. It is not suitable for analysis of the DNA from this tissue. PMID:5353529

  13. Spectrophotometry of Artemisia tridentata to quantitatively determine subspecies

    Science.gov (United States)

    Richardson, Bryce; Boyd, Alicia; Tobiasson, Tanner; Germino, Matthew

    2018-01-01

    Ecological restoration is predicated on our abilities to discern plant taxa. Taxonomic identification is a first step in ensuring that plants are appropriately adapted to the site. An example of the need to identify taxonomic differences comes from big sagebrush (Artemisia tridentata). This species is composed of three predominant subspecies occupying distinct environmental niches, but overlap and hybridization are common in ecotones. Restoration of A. tridentata largely occurs using wildland collected seed, but there is uncertainty in the identification of subspecies or mix of subspecies from seed collections. Laboratory techniques that can determine subspecies composition would be desirable to ensure that subspecies match the restoration site environment. In this study, we use spectrophotometry to quantify chemical differences in the water-soluble compound, coumarin. Ultraviolet (UV) absorbance of A. tridentata subsp. vaseyana showed distinct differences among A.t. tridentata and wyomingensis. No UV absorbance differences were detected between A.t. tridentata and wyomingensis. Analyses of samples from > 600 plants growing in two common gardens showed that UV absorbance was unaffected by environment. Moreover, plant tissues (leaves and seed chaff) explained only a small amount of the variance. UV fluorescence of water-eluted plant tissue has been used for many years to indicate A.t. vaseyana; however, interpretation has been subjective. Use of spectrophotometry to acquire UV absorbance provides empirical results that can be used in seed testing laboratories using the seed chaff present with the seed to certify A. tridentata subspecies composition. On the basis of our methods, UV absorbance values 3.1 would indicate either A.t. tridentata or wyomingensis. UV absorbance values between 2.7 and 3.1 would indicate a mixture of A.t. vaseyana and the other two subspecies.

  14. Qualitative and quantitative determination of ubiquinones by the method of high-efficiency liquid chromatography

    International Nuclear Information System (INIS)

    Yanotovskii, M.T.; Mogilevskaya, M.P.; Obol'nikova, E.A.; Kogan, L.M.; Samokhvalov, G.I.

    1986-01-01

    A method has been developed for the qualitative and quantitative determination of ubiquinones CoQ 6 -CoQ 10 , using high-efficiency reversed-phase liquid chromatography. Tocopherol acetate was used as the internal standard

  15. Quantitative determination of thallium binding to ferric hexacyanoferrate: Prussian blue.

    Science.gov (United States)

    Yang, Yongsheng; Faustino, Patrick J; Progar, Joseph J; Brownell, Charles R; Sadrieh, Nakissa; May, Joan C; Leutzinger, Eldon; Place, David A; Duffy, Eric P; Yu, Lawrence X; Khan, Mansoor A; Lyon, Robbe C

    2008-04-02

    Ferric hexacyanoferrate, (Fe(4)(III)[Fe(II)(CN)(6)](3)), also known as insoluble Prussian blue (PB), is the active pharmaceutical ingredient (API) of Radiogardase which is the first approved drug product (DP) for treatment of thallium and radiocesium poisoning. The aim of this study is (1) to determine the in vitro thallium binding capacity and binding rates of insoluble PB; and (2) to evaluate the effect of physiological pH conditions, PB particle size and storage conditions on the binding to PB. Experimental pH levels from 1.0 to 7.5 were used to cover the range of pH levels that PB may encounter when traveling through the gastrointestinal (GI) tract in humans. Measurements of thallium binding were made between 1 and 24h, to cover gastric and intestinal tract residence time. PB was found to have a binding capacity of approximately 1400 mg/g at pH 7.5. When the pH decreased, the binding decreased as well. The results indicated that the hydration state of PB influences the thallium binding process. It was also found that there exits a direct correlation between the moisture loss in PB and the thallium binding rate constant. The PB with 17 mol of water had a binding rate constant of 0.52, which was reduced to 0.32 when PB was dehydrated to 2.5 mol of water. Significant differences were observed in both binding capacity and binding rate constant among PB fractions with different particle size ranges. PB fraction with particle size of 220-1000 microm had a binding rate constant of 0.43, which increased to 0.64 when the particle size was reduced to 32-90 microm. Batch-to-batch variation in thallium binding was also observed among the APIs and the DPs and this was related to particle size and hydration state. These findings can be utilized to evaluate and predict drug product quality under certain manufacturing and dry storage conditions.

  16. [Qualitative identification and quantitative determination of naringin in rhizoma Drynariae by TLC].

    Science.gov (United States)

    Wang, Y; Li, J

    1998-11-01

    To set up the method for the qualitative identification and quantitative determination of naringin in Rhizoma Drynariae. TLC and TLC-scanning. Naringin in Drynariae fortunei was identified by TLC and its content was 0.73%. The TLC identification has been proved to be convenient, and the quantitative determination by TLC-scanning has been proved to be accurate, reliable and of good reproducibility, the recovery rate being 100.48% and RSD 1.37% (n = 5).

  17. Determination of Optimal Temperature for Biosorption of Heavy Metal Mixture from Aqueous Solution by Pretreated Biomass of Aspergillus niger

    Directory of Open Access Journals (Sweden)

    Javad Yousefi

    2012-01-01

    Full Text Available Biosorption is a novel technology that uses dead and inactive biomass for removal of heavy metals from aqueous solution. Some parameters such as temperature, contact time, solution pH, initial metal concentration, biosorbent dose and also agitating speed of solution and biosorbent mixing can affect the amount of metal sorption by biosorbent. The aim of this study was to investigate the effects of different treatments of temperatures (25, 35, 45 and 55oC on biosorption of metals mixture in order to determine optimal temperature for more metals removal from aqueous solution. This study uses dead and pretreated biomass of Aspergillus niger with 0.5N NaOH for removal of Zn(II, Co(II and Cd(II. In all temperature treatments and in the case of all of heavy metals, maximum amount of metal sorption and concentration decrease was occurred in first 5 minutes and achieved to equilibrium after 20 minute. The percent of metals sorption show growth trend with temperature increase. Between 4 experimental treatments, 55oC treatment was shown maximum sorption and 25oC was shown minimum sorption amount. The percent of Cr(II sorption was increase from 28.5% in 25oC to 44.7% in 55oC. Also, this increase was from 40% to 58% for Cd(II and from 37.7% to 65.6% for Zn(II. About 60% of increase in sorption by A. niger was due to increase in temperature. Therefore the amount of metals sorption can be increase, only with temperature increase and without any biomass addition.

  18. [Quantitative determination of anethole in the fruit of Illicium verum from various places of Guangxi province].

    Science.gov (United States)

    Zhou, Jieming; Lü, Gaorong; Zhong, Xiaoqing; Wen, Hui

    2005-02-01

    The quantitative determination of anethole in the fruit of Illicium verum from various places of Guangxi province were determined by GC. The average recovery rate and the RSD are 102.31%, 1.78% respectively. The content of anethole in the fruit of Illicium verum in various places were all more than 4.5%.

  19. Quantitative determination of peripheral arterio-venous shunts by means of radioactively labelled microspheres

    International Nuclear Information System (INIS)

    Friese, K.H.

    1981-01-01

    In the present work a nuclear method of quantitative measurement of peripheral arterio-venous shunts with a whole-body scanner is standardized. This method, developed at the beginning of the 70s at Tuebingen, stands out in contrast with earlier measuring methods by the application of the theory of quantitative scintiscanning. This means that the scintigram obtained after injection of sup(99m)technetium-labelled human albumin microspheres into an artery before the shunt is corrected for the quantitative shunt calculation by several factors using a computer, to avoid systematic mistakes. For the standardization of the method, 182 scintigrams were taken during model experiments and experiments on animals and human beings. This method, having a deviation of 10% at most, is excellently suited for the quantitative determination of peripheral arterio-venous shunts. Already for a pulmonary activity of 3% a peripheral shunt is proved with 97.5% probability. (orig./MG) [de

  20. Development of Method for Quantitative Determination of Water Arsenic by Field Test Kit

    Directory of Open Access Journals (Sweden)

    Makoto SEKINE

    2018-04-01

    Full Text Available Drinking of arsenic (As contaminated ground water is threatening the health of millions of peoples of Bangladesh. The screening of tube wells (TWs water for As in Bangladesh and elsewhere in the world is done by As testing kits. The results of water-As by these kits are semi-quantitative and personal error is high. An attempt has been undertaken for quantitative determination of water-As by MITech arsenic test kit by applying quantitative image analysis method from the digital picture of the colored test paper of the kit. In the quantitative image analysis method, the color of the test paper is numerically determined by color difference between the test water samples with the standard color chart which is calculated from Lab (lightness (L, color opponent green-red (a, and color opponent blue-yellow (b values. TWs water-As concentrations in Bashailbogh village, Munshiganj, Bangladesh were determined by using MITech arsenic field test kit by conventional method, quantitative image analysis method and inductively coupled plasma mass spectrometer (ICP-MS method. The water-As by the quantitative image method gave quite close results (R2 = 0.998 to those obtained with ICP-MS method at concentration up to 50 µg As L-1. The water-As concentration more than 50 µg As L-1 by this method was underestimated. Hence, the developed method may be used for quantitative analysis of water-As in the range of 0–50 µg As L-1 for water-As screening program. [Fundam Appl Agric 2018; 3(1.000: 340-346

  1. Determining the Probability of Achieving a Successful Quantitative Analysis for Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Pinkerton, David K; Reaser, Brooke C; Berrier, Kelsey L; Synovec, Robert E

    2017-09-19

    A new approach is presented to determine the probability of achieving a successful quantitative analysis for gas chromatography coupled with mass spectrometry (GC-MS). The proposed theory is based upon a probabilistic description of peak overlap in GC-MS separations to determine the probability of obtaining a successful quantitative analysis, which has its lower limit of chromatographic resolution R s at some minimum chemometric resolution, R s *; that is to say, successful quantitative analysis can be achieved when R s ≥ R s *. The value of R s * must be experimentally determined and is dependent on the chemometric method to be applied. The approach presented makes use of the assumption that analyte peaks are independent and randomly distributed across the separation space or are at least locally random, namely, that each analyte represents an independent Bernoulli random variable, which is then used to predict the binomial probability of successful quantitative analysis. The theoretical framework is based on the chromatographic-saturation factor and chemometric-enhanced peak capacity. For a given separation, the probability of quantitative success can be improved via two pathways, a chromatographic-efficiency pathway that reduces the saturation of the sample and a chemometric pathway that reduces R s * and improves the chemometric-enhanced peak capacity. This theory is demonstrated through a simulation-based study to approximate the resolution limit, R s *, of multivariate curve resolution-alternating least-squares (MCR-ALS). For this study, R s * was determined to be ∼0.3, and depending on the analytical expectations for the quantitative bias and the obtained mass-spectral match value, a lower value of R s * ∼ 0.2 may be achievable.

  2. Gas-chromatographic quantitative determination of argon in air samples, by elimination of oxigen

    International Nuclear Information System (INIS)

    Sofronie, E.

    1982-08-01

    A method of gas-chromatographic quantitative determination of argon in air samples, by elimination of oxygen, is presented. Experiments were carried out in a static system. Conditions for the application of the method in dynamic systems are specified. Sensibility of the method: 5 10 -4 cm 3 Ar per cm 3 of air. (author)

  3. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Jat, J.R.; Nayak, A.K.; Balaji Rao, Y.; Ravindra, H.R.

    2013-01-01

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  4. Quantitative on-chip determination of taurine in energy and sports drinks

    NARCIS (Netherlands)

    Götz, S.; Revermann, T.; Karst, U.

    2007-01-01

    A new method for the quantitative determination of taurine in beverages by microchip electrophoresis was developed. A rapid and simple sample preparation procedure, only including two dilution steps and the addition of the fluorogenic labeling reagent NBD-Cl (4-chloro-7-nitrobenzofurazan), is

  5. Quantitative radioimmunological method for the determination of rubredoxin in crude extracts of Acinetobacter calcoaceticus

    International Nuclear Information System (INIS)

    Claus, R.; Haedge, D.; Asperger, O.; Fiebig, H.; Kleber, H.P.

    1980-01-01

    For the quantitative determination of rubredoxin content in bacterial crude extracts the immunogenicity of the antigen was increased by cross-linking with glutaric aldehyde. The detection limit is near 0.02 nmol rubredoxin/ml. The rubredoxin content in crude extracts of Acinetobacter calcoaceticus amounts to 4x10 -11 mol/mg bacterial protein after growth on n-alkanes

  6. [Quantitative determination of ursolic acid in Herba cynomorii by ultraviolet spectrophotometry].

    Science.gov (United States)

    Ding, H; Wang, Y; Wang, S; You, W

    1998-02-01

    Ursolic acid was isolated form Herba Cynomorii by thin layer chromatography and was quantitatively determined by ultraviolet spectrophotometry. The results indicate that the content of ursolic acid is 0.78%. The average recovery rate of ursolic acid is 97.4%, RSD = 0.45% (n = 4).

  7. Standard addition strip for quantitative electrostatic spray ionization mass spectrometry analysis: determination of caffeine in drinks.

    Science.gov (United States)

    Tobolkina, Elena; Qiao, Liang; Roussel, Christophe; Girault, Hubert H

    2014-12-01

    Standard addition strips were prepared for the quantitative determination of caffeine in different beverages by electrostatic spray ionization mass spectrometry (ESTASI-MS). The gist of this approach is to dry spots of caffeine solutions with different concentrations on a polymer strip, then to deposit a drop of sample mixed with an internal standard, here theobromine on each spot and to measure the mass spectrometry signals of caffeine and theobromine by ESTASI-MS. This strip approach is very convenient and provides quantitative analyses as accurate as the classical standard addition method by MS or liquid chromatography. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Pre-treatment microbial Prevotella-to-Bacteroides ratio, determines body fat loss success during a 6-month randomized controlled diet intervention

    DEFF Research Database (Denmark)

    Hjorth, M F; Roager, Henrik Munch; Larsen, T. M.

    2017-01-01

    Based on the abundance of specific bacterial genera, the human gut microbiota can be divided into two relatively stable groups that might play a role in personalized nutrition. We studied these simplified enterotypes as prognostic markers for successful body fat loss on two different diets. A total....... divided by Bacteroides spp. (P/B ratio) obtained by quantitative PCR analysis. Modifications of dietary effects of pre-treatment P/B group were examined by linear mixed models. Among individuals with high P/B the NND resulted in a 3.15 kg (95%CI 1.55;4.76, Pfat loss compared to ADD...... to lose body fat on diets high in fiber and wholegrain than subjects with a low P/B-ratio....

  9. Pre-treatment microbial Prevotella-to-Bacteroides ratio, determines body fat loss success during a 6-month randomized controlled diet intervention

    DEFF Research Database (Denmark)

    Hjorth, M F; Roager, Henrik Munch; Larsen, T. M.

    2017-01-01

    Based on the abundance of specific bacterial genera, the human gut microbiota can be divided into two relatively stable groups that might play a role in personalized nutrition. We studied these simplified enterotypes as prognostic markers for successful body fat loss on two different diets. A total...... of 62 participants with increased waist circumference were randomly assigned to receive an ad libitum New Nordic Diet (NND) high in fiber/wholegrain or an Average Danish Diet (ADD) for 26 weeks. Participants were grouped into two discrete enterotypes by their relative abundance of Prevotella spp....... divided by Bacteroides spp. (P/B ratio) obtained by quantitative PCR analysis. Modifications of dietary effects of pre-treatment P/B group were examined by linear mixed models. Among individuals with high P/B the NND resulted in a 3.15 kg (95%CI 1.55;4.76, Ploss compared to ADD...

  10. Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon)

    Science.gov (United States)

    Ledesma-Escobar, Carlos A.; Priego-Capote, Feliciano; Luque de Castro, María D.

    2016-01-01

    Background Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far. Objective Evaluate the effect of both the sample pretreatment and the extraction method on the profile of flavonoids isolated from lemon. Results Extracts from fresh, lyophilized and air-dried samples obtained by shaking extraction (SE), ultrasound-assisted extraction (USAE), microwave-assisted extraction (MAE) and superheated liquid extraction (SHLE) were analyzed by LC–QTOF MS/MS, and 32 flavonoids were tentatively identified using MS/MS information. ANOVA applied to the data from fresh and dehydrated samples and from extraction by the different methods revealed that 26 and 32 flavonoids, respectively, were significant (p≤0.01). The pairwise comparison (Tukey HSD; p≤0.01) showed that lyophilized samples are more different from fresh samples than from air-dried samples; also, principal component analysis (PCA) showed a clear discrimination among sample pretreatment strategies and suggested that such differences are mainly created by the abundance of major flavonoids. On the other hand, pairwise comparison of extraction methods revealed that USAE and MAE provided quite similar extracts, being SHLE extracts different from the other two. In this case, PCA showed a clear discrimination among extraction methods, and their position in the scores plot suggests a lower abundance of flavonoids in the extracts from SHLE. In the two PCA the loadings plots revealed a trend to forming groups according to flavonoid aglycones. Conclusions The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied

  11. Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon.

    Directory of Open Access Journals (Sweden)

    Carlos A Ledesma-Escobar

    Full Text Available Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far.Evaluate the effect of both the sample pretreatment and the extraction method on the profile of flavonoids isolated from lemon.Extracts from fresh, lyophilized and air-dried samples obtained by shaking extraction (SE, ultrasound-assisted extraction (USAE, microwave-assisted extraction (MAE and superheated liquid extraction (SHLE were analyzed by LC-QTOF MS/MS, and 32 flavonoids were tentatively identified using MS/MS information. ANOVA applied to the data from fresh and dehydrated samples and from extraction by the different methods revealed that 26 and 32 flavonoids, respectively, were significant (p≤0.01. The pairwise comparison (Tukey HSD; p≤0.01 showed that lyophilized samples are more different from fresh samples than from air-dried samples; also, principal component analysis (PCA showed a clear discrimination among sample pretreatment strategies and suggested that such differences are mainly created by the abundance of major flavonoids. On the other hand, pairwise comparison of extraction methods revealed that USAE and MAE provided quite similar extracts, being SHLE extracts different from the other two. In this case, PCA showed a clear discrimination among extraction methods, and their position in the scores plot suggests a lower abundance of flavonoids in the extracts from SHLE. In the two PCA the loadings plots revealed a trend to forming groups according to flavonoid aglycones.The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied conditions, liophilization provides

  12. Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon).

    Science.gov (United States)

    Ledesma-Escobar, Carlos A; Priego-Capote, Feliciano; Luque de Castro, María D

    2016-01-01

    Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far. Evaluate the effect of both the sample pretreatment and the extraction method on the profile of flavonoids isolated from lemon. Extracts from fresh, lyophilized and air-dried samples obtained by shaking extraction (SE), ultrasound-assisted extraction (USAE), microwave-assisted extraction (MAE) and superheated liquid extraction (SHLE) were analyzed by LC-QTOF MS/MS, and 32 flavonoids were tentatively identified using MS/MS information. ANOVA applied to the data from fresh and dehydrated samples and from extraction by the different methods revealed that 26 and 32 flavonoids, respectively, were significant (p≤0.01). The pairwise comparison (Tukey HSD; p≤0.01) showed that lyophilized samples are more different from fresh samples than from air-dried samples; also, principal component analysis (PCA) showed a clear discrimination among sample pretreatment strategies and suggested that such differences are mainly created by the abundance of major flavonoids. On the other hand, pairwise comparison of extraction methods revealed that USAE and MAE provided quite similar extracts, being SHLE extracts different from the other two. In this case, PCA showed a clear discrimination among extraction methods, and their position in the scores plot suggests a lower abundance of flavonoids in the extracts from SHLE. In the two PCA the loadings plots revealed a trend to forming groups according to flavonoid aglycones. The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied conditions, liophilization provides extracts

  13. Quantitative determination of elastic and inelastic attenuation coefficients by off-axis electron holography

    Energy Technology Data Exchange (ETDEWEB)

    Kern, F.; Wolf, D.; Pschera, P.; Lubk, A.

    2016-12-15

    Off-axis electron holography is a well-established transmission electron microscopy technique, typically employed to investigate electric and magnetic fields in and around nanoscale materials, which modify the phase of the reconstructed electron wave function. Here, we elaborate on a detailed analysis of the two characteristic intensity terms that are completing the electron hologram, the conventional image intensity and the interference fringe intensity. We show how both are related to elastic and inelastic scattering absorption at the sample and how they may be separated to analyze the chemical composition of the sample. Since scattering absorption is aperture dependent, a quantitative determination of the corresponding attenuation coefficients (reciprocal mean free path lengths) requires the use of holographic image modi with well-defined objective aperture stops in the back-focal plane of the objective lens. The proposed method extends quantitative electron holography to a correlated three-in-one characterization of electric and magnetic fields, Z-contrast and dielectric losses in materials. - Highlights: • Quantitative determination of attenuation coefficients by electron holography. • Separation of elastic and inelastic attenuation coefficients (mean free path length). • Quantitative determination of the objective aperture semi-angle influence. • Compilation of elastic and inelastic attenuation from different materials.

  14. Quantitative kinetics of proteolytic enzymes determined by a surface concentration-based assay using peptide arrays.

    Science.gov (United States)

    Jung, Se-Hui; Kong, Deok-Hoon; Park, Seoung-Woo; Kim, Young-Myeong; Ha, Kwon-Soo

    2012-08-21

    Peptide arrays have emerged as a key technology for drug discovery, diagnosis, and cell biology. Despite the promise of these arrays, applications of peptide arrays to quantitative analysis of enzyme kinetics have been limited due to the difficulty in obtaining quantitative information of enzymatic reaction products. In this study, we developed a new approach for the quantitative kinetics analysis of proteases using fluorescence-conjugated peptide arrays, a surface concentration-based assay with solid-phase peptide standards using dry-off measurements, and compared it with an applied concentration-based assay. For fabrication of the peptide arrays, substrate peptides of cMMP-3, caspase-3, caspase-9, and calpain-1 were functionalized with TAMRA and cysteine, and were immobilized onto amine-functionalized arrays using a heterobifunctional linker, N-[γ-maleimidobutyloxy]succinimide ester. The proteolytic activities of the four enzymes were quantitatively analyzed by calculating changes induced by enzymatic reactions in the concentrations of peptides bound to array surfaces. In addition, this assay was successfully applied for calculating the Michaelis constant (K(m,surf)) for the four enzymes. Thus, this new assay has a strong potential for use in the quantitative evaluation of proteases, and for drug discovery through kinetics studies including the determination of K(m) and V(max).

  15. Pre-treatment prediction of chemoresistance in second-line chemotherapy of ovarian carcinoma: value of serological tumor marker determination (tetranectin, YKL-40, CASA, CA 125)

    DEFF Research Database (Denmark)

    Grønlund, B; Høgdall, E V S; Christensen, Ib Jarle

    2006-01-01

    OBJECTIVE: To examine if the determination of the levels of serological tumor markers at time of relapse had any predictive value for chemoresistance in the second-line treatment of ovarian cancer patients. METHODS: From a registry of consecutive single-institution patients with epithelial ovarian...... carcinoma pretreated with paclitaxel plus platinum, we selected 82 patients with (a) solid tumor recurrence, and (b) second-line chemotherapy consisting of topotecan (platinum-resistant disease) or paclitaxel plus carboplatin (platinum-sensitive disease). Stored serum samples were analyzed...... of CASA or YKL-40, are associated with increased risk of second-line chemoresistance in patients with ovarian cancer....

  16. Simultaneous determination of the protein conversion process in porcine stratum corneum after pretreatment with skin enhancers by a combined microscopic FT-IR/DSC system

    Science.gov (United States)

    Lin, Shan-Yang; Duan, Kwo-Jen; Lin, Tsung-Chien

    1996-11-01

    A newly developed microscopic Fourier transform infrared (FT-IR) spectrometry combined with differential scanning calorimetry (DSC) has been used to investigate simultaneously the thermal response and IR spectral changes in protein structure in porcine stratum corneum (SC) after pretreatment with skin penetration enhancers (propylene glycol (PG), azone/PG, oleic acid (OA)/PG, vitamin C, and vitamin C+ OA/PG). The amide I and II bands of the protein were used as probes to determine its structural transformation with temperature. A reheating process was also performed. The dual effects of enhancer and temperature on the protein conformational changes of porcine SC were studied. The results indicate that the newly developed FT-IR/DSC system can continuously determine the thermoresponsive conversion process from α-helix to β-sheet in the keratin structure of porcine SC pretreated with different enhancers. The temperature-induced keratin conversion in the protein structure of porcine SC was irreversible, with or without pretreatment with skin penetration enhancers. The conformational transition in the protein during heating was found to be partially from the α-helix to a random coil structure, and partially from the α-helix to the β-sheet structure. The kinetics of this conversion for the first and second heating processes were significantly different; the conversion process for all the first-heated SC samples during the second heating process was slower than that of the samples during the first heating process. Moreover, it was found that the skin penetration enhancers were able to alter synergistically and promote keratin conversion in the protein structure of porcine SC when accompanying the heating process. PG, OA/PG and azone/PG were found to be the most effective.

  17. Activation autoradiography: imaging and quantitative determination of endogenous and exogenous oxygen in the rat brain

    International Nuclear Information System (INIS)

    Kawashima, K.; Iwata, R.; Kogure, K.; Ohtomo, H.; Orihara, H.; Ido, T.

    1987-01-01

    Endogenous and exogenous oxygen in the rat brain were quantitatively determined using an autoradiographic technique. The oxygen images of frozen and dried rat brain sections were obtained as 18 F images by using the 16 O ( 3 He,p) 18 F reaction for endogenous 16 O images and the 18 O(p,n) 18 F reaction for endogenous and exogenous 18 O images. These autoradiograms demonstrated the different distribution of oxygen between gray and white matter. These images also allowed differentiation of the individual structures of hippocampal formation, owing to the differing water content of the various structures. Local oxygen contents were quantitatively determined from autoradiograms of brain sections and standard sections with known oxygen contents. The estimated values were 75.6 +/- 4.6 wt% in gray matter and 72.2 +/- 4.0 wt% in white matter. The systematic error in the present method was estimated to be 4.9%

  18. Combined first pass and equilibrium radionuclide cardiographic determination of stroke volume for quantitation of valvular regurgitation

    DEFF Research Database (Denmark)

    Kelbaek, H; Aldershvile, J; Svendsen, Jesper Hastrup

    1988-01-01

    A new noninvasive procedure for quantitation of cardiac valve regurgitation was evaluated using a combination of first pass and gated equilibrium radionuclide cardiography in 38 subjects with and without cardiac valve disease. Left-sided cardiac catheterization was performed to determine the seve......A new noninvasive procedure for quantitation of cardiac valve regurgitation was evaluated using a combination of first pass and gated equilibrium radionuclide cardiography in 38 subjects with and without cardiac valve disease. Left-sided cardiac catheterization was performed to determine...... with mild mitral incompetence and 2+ aortic regurgitation, 37% in patients with moderate mitral incompetence and 3+ aortic regurgitation and 57% in patients with severe mitral incompetence and 4+ aortic regurgitation. These findings suggest that combined first pass and gated equilibrium radionuclide...

  19. Quantitative Determination of Organic Semiconductor Microstructure from the Molecular to Device Scale

    KAUST Repository

    Rivnay, Jonathan

    2012-10-10

    A study was conducted to demonstrate quantitative determination of organic semiconductor microstructure from the molecular to device scale. The quantitative determination of organic semiconductor microstructure from the molecular to device scale was key to obtaining precise description of the molecular structure and microstructure of the materials of interest. This information combined with electrical characterization and modeling allowed for the establishment of general design rules to guide future rational design of materials and devices. Investigations revealed that a number and variety of defects were the largest contributors to the existence of disorder within a lattice, as organic semiconductor crystals were dominated by weak van der Waals bonding. Crystallite size, texture, and variations in structure due to spatial confinement and interfaces were also found to be relevant for transport of free charge carriers and bound excitonic species over distances that were important for device operation.

  20. NIST-Traceable NMR Method to Determine Quantitative Weight Percentage Purity of Mustard (HD) Feedstock Samples

    Science.gov (United States)

    2018-01-01

    analysis of this sample can be done periodically as part of the instrument QC validation. Detailed QC specifications are not included in this method ... method is measured in milligrams, and the Z level is arbitrarily based on detection limits of the current instrument . The data from a P&A test is...ECBC-TR-1506 NIST-TRACEABLE NMR METHOD TO DETERMINE QUANTITATIVE WEIGHT PERCENTAGE PURITY OF MUSTARD (HD) FEEDSTOCK SAMPLES David J

  1. Quantitative determination of alpha-quartz in airborne dust samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz In airborne respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube Is employed. NiO is used as Internal standard In order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (Author) 17 refs

  2. Quantitative determination of alpha-quartz in airbone dust samples by X-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz in airbone respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube is employec. NiO is used as internal standard in order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (auth.) [es

  3. Species Determination and Quantitation in Mixtures Using MRM Mass Spectrometry of Peptides Applied to Meat Authentication.

    Science.gov (United States)

    Gunning, Yvonne; Watson, Andrew D; Rigby, Neil M; Philo, Mark; Peazer, Joshua K; Kemsley, E Kate

    2016-09-20

    We describe a simple protocol for identifying and quantifying the two components in binary mixtures of species possessing one or more similar proteins. Central to the method is the identification of 'corresponding proteins' in the species of interest, in other words proteins that are nominally the same but possess species-specific sequence differences. When subject to proteolysis, corresponding proteins will give rise to some peptides which are likewise similar but with species-specific variants. These are 'corresponding peptides'. Species-specific peptides can be used as markers for species determination, while pairs of corresponding peptides permit relative quantitation of two species in a mixture. The peptides are detected using multiple reaction monitoring (MRM) mass spectrometry, a highly specific technique that enables peptide-based species determination even in complex systems. In addition, the ratio of MRM peak areas deriving from corresponding peptides supports relative quantitation. Since corresponding proteins and peptides will, in the main, behave similarly in both processing and in experimental extraction and sample preparation, the relative quantitation should remain comparatively robust. In addition, this approach does not need the standards and calibrations required by absolute quantitation methods. The protocol is described in the context of red meats, which have convenient corresponding proteins in the form of their respective myoglobins. This application is relevant to food fraud detection: the method can detect 1% weight for weight of horse meat in beef. The corresponding protein, corresponding peptide (CPCP) relative quantitation using MRM peak area ratios gives good estimates of the weight for weight composition of a horse plus beef mixture.

  4. Quantitative Determination of Germinability of Puccinia striiformis f. sp. tritici Urediospores Using Near Infrared Spectroscopy Technology

    Directory of Open Access Journals (Sweden)

    Yaqiong Zhao

    2015-01-01

    Full Text Available Stripe rust caused by Puccinia striiformis f. sp. tritici (Pst is an important disease on wheat. In this study, quantitative determination of germinability of Pst urediospores was investigated by using near infrared reflectance spectroscopy (NIRS combined with quantitative partial least squares (QPLS and support vector regression (SVR. The near infrared spectra of the urediospore samples were acquired using FT-NIR MPA spectrometer and the germination rate of each sample was measured using traditional spore germination method. The best QPLS model was obtained with vector correction as the preprocessing method of the original spectra and 4000–12000 cm−1 as the modeling spectral region while the modeling ratio of the training set to the testing set was 4 : 1. The best SVR model was built when vector normalization was used as the preprocessing method, the modeling ratio was 5 : 1 and the modeling spectral region was 8000–11000 cm−1. The results showed that the effect of the best model built using QPLS or SVR was satisfactory. This indicated that quantitative determination of germinability of Pst urediospores using near infrared spectroscopy technology is feasible. A new method based on NIRS was provided for rapid, automatic, and nondestructive determination of germinability of Pst urediospores.

  5. Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry.

    Science.gov (United States)

    Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

    2008-06-01

    A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO(3) medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k = 2), which is equal to that expected of a talented analyst. The operation time required was the same as that for a skilled operator.

  6. Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

    2008-01-01

    A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO 3 medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k=2), which is equal to that expected of a talented analysis. The operation time required was the same as that for a skilled operator. (author)

  7. Quantitative Determination of Fusarium proliferatum Concentration in Intact Garlic Cloves Using Near-Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    Elena Tamburini

    2016-07-01

    Full Text Available Fusarium proliferatum is considered to be a pathogen of many economically important plants, including garlic. The objective of this research was to apply near-infrared spectroscopy (NIRS to rapidly determine fungal concentration in intact garlic cloves, avoiding the laborious and time-consuming procedures of traditional assays. Preventive detection of infection before seeding is of great interest for farmers, because it could avoid serious losses of yield during harvesting and storage. Spectra were collected on 95 garlic cloves, divided in five classes of infection (from 1-healthy to 5-very highly infected in the range of fungal concentration 0.34–7231.15 ppb. Calibration and cross validation models were developed with partial least squares regression (PLSR on pretreated spectra (standard normal variate, SNV, and derivatives, providing good accuracy in prediction, with a coefficient of determination (R2 of 0.829 and 0.774, respectively, a standard error of calibration (SEC of 615.17 ppb, and a standard error of cross validation (SECV of 717.41 ppb. The calibration model was then used to predict fungal concentration in unknown samples, peeled and unpeeled. The results showed that NIRS could be used as a reliable tool to directly detect and quantify F. proliferatum infection in peeled intact garlic cloves, but the presence of the external peel strongly affected the prediction reliability.

  8. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  9. Quantitative determination of phases of X-ray reflections from three-beam diffractions. Pt. 2

    International Nuclear Information System (INIS)

    Tang Mautsu; Chang Shihlin

    1988-01-01

    The method proposed by Chang and Tang of quantitative determination of X-ray reflection phases from multiple diffraction profiles is applied to nearly perfect crystals of gallium arsenide. The detailed intensity-profile-analysis procedures are given. Multiple diffraction profiles obtained with a conventional X-ray source and synchrotron radiation are subjected to this analysis. It is found that, for this particular diffraction example, errors as small as 15 0 in phase determination are achieved. Errors due to the theoretical approximation, peak position measurement and scaling factor are also discussed. (orig.)

  10. Localization and quantitative determination of catechins and proanthocyanidins in the phloem of elm and cherry.

    Science.gov (United States)

    Feucht, W; Treutter, D; Christ, E

    1992-03-01

    The localization of catechins and proanthocyanidins in the phloem of elm (Ulmus minor Mill.) and cherry (Prunus avium L.) was determined histochemically by use of 4-dimethylaminocinnamaldehyde (DMACA) reagent. The two tree species showed a characteristic distribution of these phenols, which were most abundant in the phloem rays of cherry, but were largely confined to upright parenchyma cells of elm. Quantitative determination and qualitative separation of catechins and proanthocyanidins were performed using HPLC-CRD (chemical reaction detection), with 4-dimethylaminocinnamaldehyde as the staining reagent. Up to 14 different catechins and proanthocyanidins were found in both species.

  11. Qualitative and quantitative determination of sediments phases in Chillon River by x-ray diffraction

    International Nuclear Information System (INIS)

    Miramira Tipula, Biviano; Zeballos Velasquez, Elvira; Chui Betancur, Heber; Valencia Salazar, Edilberto; Huaypar Vasquez, Yesena; Olivera de Lescano, Paula

    2008-01-01

    With this paper, we pretend to contribute with the recovery of Chillon River from a characterization of sediments. The objectives are the identification of pollution places along the bed of the Chillon River, from the Canta Province to Lima Province (Comas) and the determination of the preponderant factors of pollution. The qualitative and semi-quantitative determination of the sediments components have been carried out using the x-ray diffraction and x-ray fluorescence techniques, both of them will allow us to identify the pollute elements, for example the lead level in the Chillon River. (author)

  12. Quantitative 3D electromagnetic field determination of 1D nanostructures from single projection

    Energy Technology Data Exchange (ETDEWEB)

    Phatak, C., E-mail: cd@anl.gov [Materials Science Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Knoop, L. de; Houdellier, F.; Gatel, C. [CEMES-CNRS, 29 rue Jeanne Marvig, F-31055 Toulouse (France); Université Paul Sabatier, F-31000 Toulouse (France); Hÿtch, M.J.; Masseboeuf, A. [CEMES-CNRS, 29 rue Jeanne Marvig, F-31055 Toulouse (France)

    2016-05-15

    One-dimensional (1D) nanostructures have been regarded as the most promising building blocks for nanoelectronics and nanocomposite material systems as well as for alternative energy applications. Although they result in confinement of a material, their properties and interactions with other nanostructures are still very much three-dimensional (3D) in nature. In this work, we present a novel method for quantitative determination of the 3D electromagnetic fields in and around 1D nanostructures using a single electron wave phase image, thereby eliminating the cumbersome acquisition of tomographic data. Using symmetry arguments, we have reconstructed the 3D magnetic field of a nickel nanowire as well as the 3D electric field around a carbon nanotube field emitter, from one single projection. The accuracy of quantitative values determined here is shown to be a better fit to the physics at play than the value obtained by conventional analysis. Moreover the 3D reconstructions can then directly be visualized and used in the design of functional 3D architectures built using 1D nanostructures. - Highlights: • Novel method for tomography of 3D electromagnetic fields from a single image is presented. • The method relies upon using cylindrical symmetry and is applied to 1D nanostructures. • The 3D magnetic field of a Nickel nanowire is reconstructed. • The 3D electric field from a biased carbon cone nanotip is reconstructed. • Our method improves the quantitative measurement of the 3D electromagnetic fields.

  13. Quantitative surface topography determination by Nomarski reflection microscopy. 2: Microscope modification, calibration, and planar sample experiments

    International Nuclear Information System (INIS)

    Hartman, J.S.; Gordon, R.L.; Lessor, D.L.

    1980-01-01

    The application of reflective Nomarski differential interference contrast microscopy for the determination of quantitative sample topography data is presented. The discussion includes a review of key theoretical results presented previously plus the experimental implementation of the concepts using a commercial Momarski microscope. The experimental work included the modification and characterization of a commercial microscope to allow its use for obtaining quantitative sample topography data. System usage for the measurement of slopes on flat planar samples is also discussed. The discussion has been designed to provide the theoretical basis, a physical insight, and a cookbook procedure for implementation to allow these results to be of value to both those interested in the microscope theory and its practical usage in the metallography laboratory

  14. Quantitative determination of Auramine O by terahertz spectroscopy with 2DCOS-PLSR model

    Science.gov (United States)

    Zhang, Huo; Li, Zhi; Chen, Tao; Qin, Binyi

    2017-09-01

    Residues of harmful dyes such as Auramine O (AO) in herb and food products threaten the health of people. So, fast and sensitive detection techniques of the residues are needed. As a powerful tool for substance detection, terahertz (THz) spectroscopy was used for the quantitative determination of AO by combining with an improved partial least-squares regression (PLSR) model in this paper. Absorbance of herbal samples with different concentrations was obtained by THz-TDS in the band between 0.2THz and 1.6THz. We applied two-dimensional correlation spectroscopy (2DCOS) to improve the PLSR model. This method highlighted the spectral differences of different concentrations, provided a clear criterion of the input interval selection, and improved the accuracy of detection result. The experimental result indicated that the combination of the THz spectroscopy and 2DCOS-PLSR is an excellent quantitative analysis method.

  15. Rapid quantitative determination of C-reactive protein at chair side in dental emergency patients.

    Science.gov (United States)

    Ren, Yan-Fang; Malmstrom, Hans S

    2007-07-01

    The objective of this study was to quantitatively determine, at chair side, the serum C-reactive protein (CRP) levels in dental emergency patients. Quantitative CRP test was performed at chair side in 40 patients with acute alveolar abscess (AAA), acute periodontal abscess (APA), and alveolar osteitis (AO) at the time of dental emergency treatment and 1 week after. CRP levels were compared between groups and before and after treatments using ANOVA and Fisher's Exact tests. Serum CRP levels were greater than 5 mg/L in 30 (75%) of the 40 patients. At 1-week follow-up, the decline in CRP levels was evident in the AAA group (P .05). Serum CRP levels are often elevated in patients with odontogenic infections and postoperative complications. Rapid reduction in serum CRP levels was likely to occur following successful treatment of AAA, but less likely to occur in APA and AO.

  16. Quantitative determination of heparin levels in serum with microtiter plate-format optode

    International Nuclear Information System (INIS)

    Kim, Sung Bae; Kang, Tae Young; Cha, Geun Sig; Nam, Hakhyun

    2006-01-01

    A new assay method has been developed for the quantitative determination of heparin in serum using a microtiter plate-format optode (MPO). Heparin and proton in physiological sample are favorably co-extracted into the solvent polymeric optode membrane containing both cationic lipophilic additive, tridodecylmethyl ammonium chloride (TDMAC), and proton-selective ionophore, 3-hydroxy-4-(4-nitrophenylazo)-phenyloctadecanoate (ETH 2412), resulting in the absorbance change of the membrane to varying heparin levels. The optimized MPO composition contains low polymer-to-plasticizer ratio compared to those of conventional ion-selective optodes or electrodes, i.e., poly(vinyl chloride) (20.0)/dioctylsebacate (76.3)/ETH 2412 (1.7)/TDMAC (1.0) (wt.%): it resulted in a quantitative response to heparin from 0 to 15 unit/mL in serum with high sensitivity. The heparin-protamine titration on the MPO could provide rapid and precise determination of heparin. It was shown that the heparin levels in serum sample could be determined from the rate of absorbance change over time (ΔA/Δt); this method was more effective than the direct absorbance measurement in minimizing the interferences from color and turbidity of serum samples. MPO has been developed as a high throughput and convenient disposable sensing device, and may find a wide application in the determination of polyions and charged macromolecules

  17. Determination of scutellarin in breviscapine preparations using quantitative proton nuclear magnetic resonance spectroscopy

    Directory of Open Access Journals (Sweden)

    Zhenzuo Jiang

    2016-04-01

    Full Text Available The objective of the present study was to develop the selection criteria of proton signals for the determination of scutellarin using quantitative nuclear magnetic resonance (qNMR, which is the main bioactive compound in breviscapine preparations for the treatment of cerebrovascular disease. The methyl singlet signal of 3-(trimethylsilylpropionic-2,2,3,3-d4 acid sodium salt was selected as the internal standard for quantification. The molar concentration of scutellarin was determined by employing different proton signals. To obtain optimum proton signals for the quantification, different combinations of proton signals were investigated according to two selection criteria: the recovery rate of qNMR method and quantitative results compared with those obtained with ultra-performance liquid chromatography. As a result, the chemical shift of H-2′ and H-6′ at δ 7.88 was demonstrated as the most suitable signal with excellent linearity range, precision, and recovery for determining scutellarin in breviscapine preparations from different manufacturers, batch numbers, and dosage forms. Hierarchical cluster analysis was employed to evaluate the determination results. The results demonstrated that the selection criteria of proton signals established in this work were reliable for the qNMR study of scutellarin in breviscapine preparations.

  18. Quantitation and molecular species determination of diacylglycerols, phosphatidylcholines, ceramides, and sphingomyelins with gas chromatography.

    Science.gov (United States)

    Tserng, Kou-Yi; Griffin, Ronda

    2003-12-01

    In addition to the role of building block for biological membranes, phospholipids and their metabolites have been implicated in other important cellular functions, such as proliferation and apoptosis. Ceramides and their precursor, sphingomyelin, are thought to play a role in cellular apoptosis. In contrast, the metabolism of diacylglycerols and one of their precursors, phosphatidylcholine, is thought to be partly responsible for the opposite effect, cellular proliferation. Quantitative determination of these lipids in biological samples is important in investigating the complicated interactions between these molecules. In this report, we describe a capillary gas chromatographic procedure for the quantitative determination of molecular species of diacylglycerols, ceramides, phosphatidylcholines, and sphingomyelins. Lipid extracts are separated into these classes with a silica gel column. Diacylglycerols and ceramides are analyzed as trimethylsilyl derivatives. Phosphatidylcholines and sphingomyelins are converted to their diacylglycerol and ceramide components with sphingomyelinase hydrolysis. Internal standards for each analyzed fraction are used in the procedure. This method is used to determine the lipids in liver homogenate and subcellular fractions, including mitochondria, light mitochondria, and microsomes from young and old Fischer 344 rats. Our data show that the ceramide and sphingomyelin content is higher in the mitochondria of old rats. This relationship is consistent with the potential role of ceramide in mitochondria-induced apoptosis. More study is needed to substantiate this relationship.

  19. Determination of Mycotoxin Production of Fusarium Species in Genetically Modified Maize Varieties by Quantitative Flow Immunocytometry.

    Science.gov (United States)

    Bánáti, Hajnalka; Darvas, Béla; Fehér-Tóth, Szilvia; Czéh, Árpád; Székács, András

    2017-02-22

    Levels of mycotoxins produced by Fusarium species in genetically modified (GM) and near-isogenic maize, were determined using multi-analyte, microbead-based flow immunocytometry with fluorescence detection, for the parallel quantitative determination of fumonisin B1, deoxynivalenol, zearalenone, T-2, ochratoxin A, and aflatoxin B1. Maize varieties included the genetic events MON 810 and DAS-59122-7 , and their isogenic counterparts. Cobs were artificially infested by F. verticillioides and F. proliferatum conidia, and contained F. graminearum and F. sporotrichoides natural infestation. The production of fumonisin B1 and deoxynivalenol was substantially affected in GM maize lines: F. verticillioides , with the addition of F. graminearum and F. sporotrichoides , produced significantly lower levels of fumonisin B1 (~300 mg·kg -1 ) in DAS-59122-7 than in its isogenic line (~580 mg·kg -1 ), while F. proliferatum , in addition to F. graminearum and F. sporotrichoides , produced significantly higher levels of deoxynivalenol (~18 mg·kg -1 ) in MON 810 than in its isogenic line (~5 mg·kg -1 ). Fusarium verticillioides , with F. graminearum and F. sporotrichoides , produced lower amounts of deoxynivalenol and zearalenone than F. proliferatum , with F. graminearum and F. sporotrichoides . T-2 toxin production remained unchanged when considering the maize variety. The results demonstrate the utility of the Fungi-Plex™ quantitative flow immunocytometry method, applied for the high throughput parallel determination of the target mycotoxins.

  20. Quantitative head ultrasound measurements to determine thresholds for preterm neonates requiring interventional therapies following intraventricular hemorrhage

    Science.gov (United States)

    Kishimoto, Jessica; Fenster, Aaron; Salehi, Fateme; Romano, Walter; Lee, David S. C.; de Ribaupierre, Sandrine

    2016-04-01

    Dilation of the cerebral ventricles is a common condition in preterm neonates with intraventricular hemorrhage (IVH). This post hemorrhagic ventricle dilation (PHVD) can lead to lifelong neurological impairment through ischemic injury due to increased intracranial pressure and without treatment, can lead to death. Clinically, 2D ultrasound (US) through the fontanelles ('soft spots') of the patients are serially acquired to monitor the progression of the ventricle dilation. These images are used to determine when interventional therapies such as needle aspiration of the built up cerebrospinal fluid (CSF) ('ventricle tap', VT) might be indicated for a patient; however, quantitative measurements of the growth of the ventricles are often not performed. There is no consensus on when a neonate with PHVD should have an intervention and often interventions are performed after the potential for brain damage is quite high. Previously we have developed and validated a 3D US system to monitor the progression of ventricle volumes (VV) in IVH patients. We will describe the potential utility of quantitative 2D and 3D US to monitor and manage PHVD in neonates. Specifically, we will look to determine image-based measurement thresholds for patients who will require VT in comparison to patients with PHVD who resolve without intervention. Additionally, since many patients who have an initial VT will require subsequent interventions, we look at the potential for US to determine which PHVD patients will require additional VT after the initial one has been performed.

  1. Universally applicable model for the quantitative determination of lake sediment composition using fourier transform infrared spectroscopy.

    Science.gov (United States)

    Rosén, Peter; Vogel, Hendrik; Cunningham, Laura; Hahn, Annette; Hausmann, Sonja; Pienitz, Reinhard; Zolitschka, Bernd; Wagner, Bernd; Persson, Per

    2011-10-15

    Fourier transform infrared spectroscopy (FTIRS) can provide detailed information on organic and minerogenic constituents of sediment records. Based on a large number of sediment samples of varying age (0-340,000 yrs) and from very diverse lake settings in Antarctica, Argentina, Canada, Macedonia/Albania, Siberia, and Sweden, we have developed universally applicable calibration models for the quantitative determination of biogenic silica (BSi; n = 816), total inorganic carbon (TIC; n = 879), and total organic carbon (TOC; n = 3164) using FTIRS. These models are based on the differential absorbance of infrared radiation at specific wavelengths with varying concentrations of individual parameters, due to molecular vibrations associated with each parameter. The calibration models have low prediction errors and the predicted values are highly correlated with conventionally measured values (R = 0.94-0.99). Robustness tests indicate the accuracy of the newly developed FTIRS calibration models is similar to that of conventional geochemical analyses. Consequently FTIRS offers a useful and rapid alternative to conventional analyses for the quantitative determination of BSi, TIC, and TOC. The rapidity, cost-effectiveness, and small sample size required enables FTIRS determination of geochemical properties to be undertaken at higher resolutions than would otherwise be possible with the same resource allocation, thus providing crucial sedimentological information for climatic and environmental reconstructions.

  2. Quantitative determination of sibutramine in adulterated herbal slimming formulations by TLC-image analysis method.

    Science.gov (United States)

    Phattanawasin, Panadda; Sotanaphun, Uthai; Sukwattanasinit, Tasamaporn; Akkarawaranthorn, Jariya; Kitchaiya, Sarunyaporn

    2012-06-10

    A simple thin layer chromatographic (TLC)-image analysis method was developed for rapid determination and quantitation of sibutramine hydrochloride (SH) adulterated in herbal slimming products. Chromatographic separation of SH was achieved on a silica gel 60 F(254) TLC plate, using toluene-n-hexane-diethylamine (9:1:0.3, v/v/v) as the mobile phase and Dragendorff reagent as spot detection. Image analysis of the scanned TLC plate was performed to quantify the amount of SH. The polynomial regression data for the calibration plots showed good linear relationship in the concentration range of 1-6 μg/spot. The limits of detection and quantitation were 190 and 634 ng/spot, respectively. The method gave satisfactory specificity, precision, accuracy, robustness and was applied for determination of SH in herbal formulations. The contents of SH in adulterated samples determined by the TLC-image analysis and TLC-densitometry were also compared. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  3. [Quantitative determination of strychnine in blood and urine by gas chromatography with mass-selective detector].

    Science.gov (United States)

    Kataev, S S; Krylova, E A

    2010-01-01

    A method for the quantitative determination of strychnine in biological fluids by gas chromatography--mass spectrometry is proposed. The preparation of samples for the analysis included extraction of strychnine from blood and urine with the use of AccuBond(II) EVIDEX cartridges for solid-phase extraction and SPEC MP3 disks respectively. The efficiency of extraction was estimated at 0.05 mg/l for blood and 0.02 mg/l for urine. The detection limit was 0.10 mg/l in blood and 0.05 mg/l in urine.

  4. Comparison of two automated quantitative immunoassays for the determination of C reactive protein concentrations.

    Science.gov (United States)

    Barclay, E A; Coia, J E; Kale, P C; Masterton, R G

    1994-01-01

    Two quantitative, automated methods for the determination of C reactive protein (CRP) were compared: turbidimetry (Cobas Fara II, Roche, Welwyn Garden City, UK) and fluorescence polarisation TDx, Abbott, Wokingham, UK). One hundred and twenty routine serum samples submitted for measurement of CRP were tested using both procedures. The results were compared using regression line analysis and showed a high degree of correlation (r2 = 0.99, X coefficient = 1.01, constant = 0.11). C reactive protein can be accurately measured using the automated turbidimetric method which can be recommended as an alternative to fluorescence polarisation. Images PMID:7876389

  5. Porosity determination on pyrocarbon by means of automatic quantitative image analysis

    Energy Technology Data Exchange (ETDEWEB)

    Koizlik, K.; Uhlenbruck, U.; Delle, W.; Hoven, H.; Nickel, H.

    1976-05-01

    For a long time, the quantitative image analysis is well known as a method for quantifying the results of material investigation basing on ceramography. The development of the automatic image analyzers has made it a fast and elegant procedure for evaluation. Since 1975, it is used in IRW to determine easily and routinely the macroporosity and by this the density of the pyrocarbon coatings of nuclear fuel particles. This report describes the definition of measuring parameters, the measuring procedure, the mathematical calculations, and first experimental and mathematical results.

  6. Qualitative and quantitative determination of protopine in Fumaria spp. by TLC-densitometry method

    Directory of Open Access Journals (Sweden)

    ATANAS PAVLOV

    2012-01-01

    Full Text Available A rapid and accurate TLC-densitometry method for qualitative and quantitative determination of protopine has been developed. The best separation was achieved using a mobile phase chloroform – ethyl acetate – methanol – ammonium hydroxide (80:80:40:0.05, v/v/v/v. The results obtained by this method (CV% 3.4 corresponded well with those obtained by using a HPLC method. The reliability of the proposed method was proved through reproducibility test with alkaloid extracts from Fumaria spp.

  7. In situ quantitative determination of transuranic elements in areas of high-level gamma radiation

    International Nuclear Information System (INIS)

    Brodzinski, R.L.; Wogman, N.A.

    1978-01-01

    A technique is described for passive neutron monitoring of transuranic elements. The method provides quantitative determinations of transuranic element concentrations in a variety of field situations where no other measurement method is possible. The technique can measure concentrations of transuranic oxides as low as 8 nCi/cm 3 and is capable of operating in gamma radiation fields up to megarads per hour. Information on chemical and isotopic composition can also be obtained from the data. Several successful applications of the technique are discussed

  8. Quantitative determination of bone mineral content (QCT) - intercomparison of computer tomographs of the same construction

    International Nuclear Information System (INIS)

    Andresen, R.; Banzer, D.; Felsenberg, D.; Wolf, K.J.

    1994-01-01

    An intercomparison of 4 CT scanners of the same manufacturer was performed. The bone mineral content of 11 lumbar vertebral columns removed directly post mortem was determined in a specially constructed lucite-water phantom. Even devices of the same construction were shown to yield a variation in the quantitative evaluation markedly exceeding the annual physiological mineral loss. As long as scanner adjustment by physical calibration phantoms has not yet been established, a course assessment and therapy control of bone mineral content should always be carried out on the same QCT scanner. (orig.) [de

  9. Quantitative Determination of Caffeine in Beverages Using a Combined SPME-GC/MS Method

    Science.gov (United States)

    Pawliszyn, Janusz; Yang, Min J.; Orton, Maureen L.

    1997-09-01

    Solid-phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MS) has been applied to the analysis of various caffeinated beverages. Unlike the current methods, this technique is solvent free and requires no pH adjustments. The simplicity of the SPME-GC/MS method lends itself to a good undergraduate laboratory practice. This publication describes the analytical conditions and presents the data for determination of caffeine in coffee, tea, and coke. Quantitation by isotopic dilution is also illustrated.

  10. Development of a rapid method for the quantitative determination of deoxynivalenol using Quenchbody

    Energy Technology Data Exchange (ETDEWEB)

    Yoshinari, Tomoya [Division of Microbiology, National Institute of Health Sciences, 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501 (Japan); Ohashi, Hiroyuki; Abe, Ryoji; Kaigome, Rena [Biomedical Division, Ushio Inc., 1-12 Minamiwatarida-cho, Kawasaki-ku, Kawasaki 210-0855 (Japan); Ohkawa, Hideo [Research Center for Environmental Genomics, Kobe University, 1-1 Rokkodai, Nada, Kobe 657-8501 (Japan); Sugita-Konishi, Yoshiko, E-mail: y-konishi@azabu-u.ac.jp [Department of Food and Life Science, Azabu University, 1-17-71 Fuchinobe, Chuo-ku, Sagamihara, Kanagawa 252-5201 (Japan)

    2015-08-12

    Quenchbody (Q-body) is a novel fluorescent biosensor based on the antigen-dependent removal of a quenching effect on a fluorophore attached to antibody domains. In order to develop a method using Q-body for the quantitative determination of deoxynivalenol (DON), a trichothecene mycotoxin produced by some Fusarium species, anti-DON Q-body was synthesized from the sequence information of a monoclonal antibody specific to DON. When the purified anti-DON Q-body was mixed with DON, a dose-dependent increase in the fluorescence intensity was observed and the detection range was between 0.0003 and 3 mg L{sup −1}. The coefficients of variation were 7.9% at 0.003 mg L{sup −1}, 5.0% at 0.03 mg L{sup −1} and 13.7% at 0.3 mg L{sup −1}, respectively. The limit of detection was 0.006 mg L{sup −1} for DON in wheat. The Q-body showed an antigen-dependent fluorescence enhancement even in the presence of wheat extracts. To validate the analytical method using Q-body, a spike-and-recovery experiment was performed using four spiked wheat samples. The recoveries were in the range of 94.9–100.2%. The concentrations of DON in twenty-one naturally contaminated wheat samples were quantitated by the Q-body method, LC-MS/MS and an immunochromatographic assay kit. The LC-MS/MS analysis showed that the levels of DON contamination in the samples were between 0.001 and 2.68 mg kg{sup −1}. The concentrations of DON quantitated by LC-MS/MS were more strongly correlated with those using the Q-body method (R{sup 2} = 0.9760) than the immunochromatographic assay kit (R{sup 2} = 0.8824). These data indicate that the Q-body system for the determination of DON in wheat samples was successfully developed and Q-body is expected to have a range of applications in the field of food safety. - Highlights: • A rapid method for quantitation of DON using Q-body has been developed. • A recovery test using the anti-DON Q-body was performed. • The concentrations of DON in wheat

  11. Quantitative determination of the crystalline phases of the ceramic materials utilizing the Rietveld method

    International Nuclear Information System (INIS)

    Kniess, C.T.; Prates, P.B.; Lima, J.C. de; Kuhnen, N.C.; Riella, H.G.; Maliska, A.M.

    2009-01-01

    Ceramic materials have properties defined by their chemical and micro-structural composition. The quantification of the crystalline phases is a fundamental stage in the determination of the structure, properties and applications of a ceramic material. Within this context, this study aims is the quantitative determination of the crystalline phases of the ceramic materials developed with addition of mineral coal bottom ash, utilizing the X ray diffraction technique, through the method proposed by Rietveld. For the formulation of the ceramic mixtures a {3,3} simplex-lattice design was used, giving ten formulations of three components (two different types of clays and coal bottom ash). The crystalline phases identified in the ceramic materials after sintering at 1150 deg C during two hours are: quartz, tridimite, mullite and hematite. The proposed methodology utilizing the Rietveld method for the quantification relating to crystalline phases of the materials was shown to be adequate and efficient. (author)

  12. Quantitative on-chip determination of taurine in energy and sports drinks.

    Science.gov (United States)

    Götz, Sebastian; Revermann, Tobias; Karst, Uwe

    2007-01-01

    A new method for the quantitative determination of taurine in beverages by microchip electrophoresis was developed. A rapid and simple sample preparation procedure, only including two dilution steps and the addition of the fluorogenic labeling reagent NBD-Cl (4-chloro-7-nitrobenzofurazan), is applied. Using a home-built wavelength-resolved fluorescence detector, the separation and determination of the taurine derivative could be achieved in only 12 s, while the additional spectral information was utilized to ensure peak purity. Spanning from 0.1 to 50 mmol L(-1), the linear dynamic range of the applied method was adapted to the apparent contents in common taurine containing beverages. The smallest detectable amount of the taurine derivative actually injected into the separation channel was as low as 60 amol. The method was successfully validated by an independent liquid chromatographic method.

  13. [A quantitative approach to sports training-adapted social determinants concerning sport].

    Science.gov (United States)

    Alvis-Gómez, Martina K; Neira-Tolosa, Nury A

    2013-01-01

    Identifying and quantitatively analysing social determinants affecting disabled teenagers' inclusion/exclusion in high-performance sports. This was a descriptive cross-sectional study involving 19 12- to 19-year-old athletes suffering physical and sensory disability and 17 staff from the District Institute of Recreation and Sport. Likert-type rating scales were used, based on four analysis categories, i.e. social structure, socio-economic, educational and living condition determinants. Social inequity pervades the national paralympic sports' system. This is because 74 % of individuals only become recognised as sportspeople when they have obtained meritorious results in set competition without appropriate conditions having been previously provided by such paralympic sports institution to enable them to overcome structural and intermediate barriers. The social structure imposed on district-based paralympic sport stigmatises individuals regarding their individual abilities, affects their empowerment and freedom due to the discrimination experienced by disabled teenagers regarding their competitive achievements.

  14. Quantitative determination of total pigments in red meats using hyperspectral imaging and multivariate analysis.

    Science.gov (United States)

    Xiong, Zhenjie; Sun, Da-Wen; Xie, Anguo; Pu, Hongbin; Han, Zhong; Luo, Man

    2015-07-01

    This study investigated the potential of hyperspectral imaging (HSI) for quantitative determination of total pigments in red meats, including beef, goose, and duck. Partial least squares regression (PLSR) was applied to correlate the spectral data with the reference values of total pigments measured by a traditional method. In order to simplify the PLSR model based on the full spectra, eleven optimal wavelengths were selected using successive projections algorithm (SPA). The new SPA-PLSR model yielded good results with the coefficient of determination (R(2)p) of 0.953, root mean square error (RMSEP) of 9.896, and ratio of prediction to deviation (RPD) of 4.628. Finally, distribution maps of total pigments in red meats were developed using an image processing algorithm. The overall results from this study indicated HSI had the capability for predicting total pigments in red meats. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Quantitative Respirator Fit, Face Sizes, and Determinants of Fit in South African Diagnostic Laboratory Respirator Users.

    Science.gov (United States)

    Manganyi, Jeanneth; Wilson, Kerry S; Rees, David

    2017-11-10

    Respirators are widely used in health care settings but there is scant information on adequacy of fit and its determinants, particularly in resource-constrained settings. The aim of the study is to describe the proportion of South African diagnostic laboratory respirator users with adequate quantitative respirator fit while wearing their currently selected respirators which were generally supplied without regard to face size, and to identify determinants of fit test pass and fail. This was a cross-sectional study with 562 participants. Quantitative respirator fit testing was conducted using a PortaCount fit testing machine. Four facial dimensions were taken using callipers and a tape measure. STATA 14 was used to perform descriptive and inferential statistics. The effect of the independent variables including face dimensions, race, smoking, respirator make and size, and age group was explored using multiple logistic regression stratified by sex. Ninety one percent of the respirators supplied were medium-sized. Seventy eight percent of respirator users failed fit testing and were thus probably not protected by their currently supplied respirator. Multiple logistic regression analysis showed that face length in mm (odds ratio [OR] = 1.04, 95% confidence interval [CI] = 1.00-1.09), nasal root breadth in mm (OR = 1.16, 95% CI = 1.06-1.28), and respirator shape (OR = 0.56, 95% CI = 0.39-0.78) were significant predictors of overall fit for all subjects and for women alone, but these factors explained only a small percentage of fit test outcomes. A large proportion of diagnostic laboratory employees were using poorly fitting respirators. This creates a false impression of protection. Fit testing of respirators is therefore important and recommended. The determinants evaluated described only a small portion of the variability in fit; important determinants were absent from the models. © The Author 2017. Published by Oxford University Press on behalf of the British

  16. New chromatographic Methods for Separation of Lansoprazole from its Degradation Components and The Quantitative Determination in its Pharmaceutical Products

    International Nuclear Information System (INIS)

    Touma, M.; Rajab, A.

    2009-01-01

    New chromatographic method was found for Quantitative Determination of Lansoprazole in its pharmaceutical products. Lansoprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ)). (author)

  17. New chromatographic method for separating Omeprazole from its degradation components and the quantitatively determining it in its pharmaceutical products

    International Nuclear Information System (INIS)

    Touma, M.; Rajab, A.; Seuleiman, M.

    2007-01-01

    New chromatographic method for Quantitative Determination of Omeprazole in its Pharmaceutical Products was produced. Omeprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ) ).(author)

  18. High-throughput double quantitative competitive polymerase chain reaction for determination of genetically modified organisms.

    Science.gov (United States)

    Mavropoulou, Anastasia K; Koraki, Theodora; Ioannou, Penelope C; Christopoulos, Theodore K

    2005-08-01

    Quantitative competitive polymerase chain reaction (PCR), especially the double competitive PCR methods (DC-PCR), have evolved as reliable approaches to quantification of genetically modified organisms (GMO) in food. However, DC-PCR is a low-throughput method because it requires titration of each sample with various amounts of a competitive internal standard, a protocol that involves several PCRs per sample followed by electrophoresis and densitometry. To address this drawback, we have developed a new method for GMO quantification, namely, a high-throughput double quantitative competitive PCR (HT-DCPCR). In HT-DCPCR, electrophoresis and densitometry are replaced by a rapid, microtiter well-based bioluminometric hybridization assay and there is no need for titration of each sample. The determination of GM soya was chosen as a model. We have constructed internal standards (DNA competitors) both for the 35S promoter sequence and for a plant-specific reference gene (lectin). The competitors have identical size and share the same primer binding sites with the target sequences but differ in a 24-bp internal segment. Each target sequence (35S and lectin) is coamplified with a constant amount (1000 copies) of the respective competitor. The four amplified fragments are hybridized with specific probes and captured on a universal solid phase to achieve simplicity and high throughput. The hybrids are determined by using streptavidin conjugated to the photoprotein aequorin. The ratio of the luminescence values obtained for the target and the competitor is linearly related to the starting amount of target DNA. The limit of quantification for the 35S promoter is 24 copies. The proposed method was evaluated by determining the GMO content of soybean powder certified reference materials. Also HT-DCPCR was compared to real-time PCR in a variety of real samples.

  19. Quantitative determination of optical trapping strength and viscoelastic moduli inside living cells

    International Nuclear Information System (INIS)

    Mas, Josep; Berg-Sørensen, Kirstine; Richardson, Andrew C; Reihani, S Nader S; Oddershede, Lene B

    2013-01-01

    With the success of in vitro single-molecule force measurements obtained in recent years, the next step is to perform quantitative force measurements inside a living cell. Optical traps have proven excellent tools for manipulation, also in vivo, where they can be essentially non-invasive under correct wavelength and exposure conditions. It is a pre-requisite for in vivo quantitative force measurements that a precise and reliable force calibration of the tweezers is performed. There are well-established calibration protocols in purely viscous environments; however, as the cellular cytoplasm is viscoelastic, it would be incorrect to use a calibration procedure relying on a viscous environment. Here we demonstrate a method to perform a correct force calibration inside a living cell. This method (theoretically proposed in Fischer and Berg-Sørensen (2007 J. Opt. A: Pure Appl. Opt. 9 S239)) takes into account the viscoelastic properties of the cytoplasm and relies on a combination of active and passive recordings of the motion of the cytoplasmic object of interest. The calibration procedure allows us to extract absolute values for the viscoelastic moduli of the living cell cytoplasm as well as the force constant describing the optical trap, thus paving the way for quantitative force measurements inside the living cell. Here, we determine both the spring constant of the optical trap and the elastic contribution from the cytoplasm, influencing the motion of naturally occurring tracer particles. The viscoelastic moduli that we find are of the same order of magnitude as moduli found in other cell types by alternative methods. (paper)

  20. A simple, quantitative method using alginate gel to determine rat colonic tumor volume in vivo.

    Science.gov (United States)

    Irving, Amy A; Young, Lindsay B; Pleiman, Jennifer K; Konrath, Michael J; Marzella, Blake; Nonte, Michael; Cacciatore, Justin; Ford, Madeline R; Clipson, Linda; Amos-Landgraf, James M; Dove, William F

    2014-04-01

    Many studies of the response of colonic tumors to therapeutics use tumor multiplicity as the endpoint to determine the effectiveness of the agent. These studies can be greatly enhanced by accurate measurements of tumor volume. Here we present a quantitative method to easily and accurately determine colonic tumor volume. This approach uses a biocompatible alginate to create a negative mold of a tumor-bearing colon; this mold is then used to make positive casts of dental stone that replicate the shape of each original tumor. The weight of the dental stone cast correlates highly with the weight of the dissected tumors. After refinement of the technique, overall error in tumor volume was 16.9% ± 7.9% and includes error from both the alginate and dental stone procedures. Because this technique is limited to molding of tumors in the colon, we utilized the Apc(Pirc/+) rat, which has a propensity for developing colonic tumors that reflect the location of the majority of human intestinal tumors. We have successfully used the described method to determine tumor volumes ranging from 4 to 196 mm³. Alginate molding combined with dental stone casting is a facile method for determining tumor volume in vivo without costly equipment or knowledge of analytic software. This broadly accessible method creates the opportunity to objectively study colonic tumors over time in living animals in conjunction with other experiments and without transferring animals from the facility where they are maintained.

  1. Quantitative determination of minerals in Nevada Test Site samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1983-07-01

    The external standard intensity ratio technique has been developed into a routine procedure for quantitatively determining mineralogic compositions of Nevada Test Site (NTS) samples by x-ray diffraction. This technique used ratios of x-ray intensity peaks from the same run which eliminates many possible errors. Constants have been determined for each of thirteen minerals commonly found in NTS samples - quartz, montmorillonite, illite, clinoptilolite, cristobalite, feldspars, calcite, dolomite, hornblende, kaolinite, muscovite, biotite, and amorphous glass. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of quartz are used to calculate sample composition. The technique has been tested on samples with three to eleven components representative of geologic environments at NTS, and is accurate to 7.0 wt % of the total sample. The minimum amount of each of these minerals detectable by x-ray diffraction has also been determined. QUANTS is a computer code that calculates mineral contents and produces a report sheet. Constants for minerals in NTS samples other than those listed above can easily be determined, and added to QUANTS at any time

  2. Quantitative HPLC Analysis of an Analgesic/Caffeine Formulation: Determination of Caffeine

    Science.gov (United States)

    Ferguson, Glenda K.

    1998-04-01

    A modern high performance liquid chromatography (HPLC) laboratory experiment which entails the separation of acetaminophen, aspirin, and caffeine and the quantitative assay of caffeine in commercial mixtures of these compounds has been developed. Our HPLC protocol resolves these compounds in only three minutes with a straightforward chromatographic apparatus which consists of a C-18 column, an isocratic mobile phase, UV detection at 254 nm, and an integrator; an expensive, sophisticated system is not required. The separation is both repeatable and rapid. Moreover, the experiment can be completed in a single three-hour period. The experiment is appropriate for any chemistry student who has completed a minimum of one year of general chemistry and is ideal for an analytical or instrumental analysis course. The experiment detailed herein involves the determination of caffeine in Goody's Extra Strength Headache Powders, a commercially available medication which contains acetaminophen, aspirin, and caffeine as active ingredients. However, the separation scheme is not limited to this brand of medication nor is it limited to caffeine as the analyte. With only minor procedural modifications, students can simultaneously quantitate all of these compounds in a commercial mixture. In our procedure, students prepare a series of four caffeine standard solutions as well as a solution from a pharmaceutical analgesic/caffeine mixture, chromatographically analyze each solution in quadruplicate, and plot relative average caffeine standard peak area versus concentration. From the mathematical relationship that results, the concentration of caffeine in the commercial formulation is obtained. Finally, the absolute standard deviation of the mean concentration is calculated.

  3. Detection of Colorectal Cancer by a Quantitative Fluorescence Determination of DNA Amplification in Stool

    Directory of Open Access Journals (Sweden)

    Daniele Calistri

    2004-09-01

    Full Text Available DNA amplification of exfoliated cells in stool repre sents an inexpensive and rapid test, but has only 50% to 60% sensitivity. A new quantitative method, calle( fluorescence long DNA, was developed and validate( in our laboratory on stool obtained from 86 patient., with primary colorectal cancer and from 62 health individuals. It consists of the amplification of stoo DNA with fluorescence primers and the quantification of the amplification using a standard curve. Results are arbitrarily expressed in nanograms. The potential of thi new method compared to the conventional approact was analyzed in a subgroup of 94 individuals (51 patients and 38 healthy volunteers. In the presen series, DNA amplification analysis showed a specific ity of 97% and a sensitivity of only 50%. Conversely fluorescence DNA evaluation, using the best cutoff o 25 ng, showed a sensitivity of about 76% and a spec ificity of 93%. Similar sensitivity was observed regard less of Dukes stage, tumor location, and size, thu., also permitting the detection of early-stage tumors The present study seems to indicate that quantitative fluorescence DNA determination in stool successfully identifies colorectal cancer patients with a sensitivity comparable, if not superior, to that of multiple gene analysis but at a lower cost and in a shorter time.

  4. Quantitation of RHD by real-time polymerase chain reaction for determination of RHD zygosity and RHD mosaicism/chimerism

    DEFF Research Database (Denmark)

    Krog, Grethe Risum; Clausen, Frederik Banch; Dziegiel, Morten Hanefeld

    2007-01-01

    Determination of RHD zygosity of the spouse is crucial in preconception counseling of families with history of hemolytic disease of the fetus and newborn caused by anti-D. RHD zygosity can be determined by quantitative real-time polymerase chain reaction (PCR) basically by determining RHD dosage...

  5. Quantitative spectrographic determination of zirconium minerals; Determinacion espectrografica cuantitative de circonio en minerales

    Energy Technology Data Exchange (ETDEWEB)

    Rocal Adell, M.; Alvarez Gonzalez, F.; Fernandez Cellini, R.

    1958-07-01

    The method described in the following report permits the quantitative determination of zirconium in minerals and rocks in a 0,02-100% of ZrO{sub 2} concentration rate. The excitation is carried out by a 10 ampere continuous current arc among carbon electrodes, and placing the sample in a crater of 2 mm depth. For low concentrations a dilution of the sample with the same weight as its own in carbon powder and with 1/25 of its weight of Co{sub 3}O{sub 4} (internal patron) is carried out. Line Zr 2571,4, Co 2585,3 and Co 2587,2 are used. (Author) 6 refs.

  6. ANSI/ASHRAE/IES Standard 90.1-2013 Determination of Energy Savings: Quantitative Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Halverson, Mark A.; Athalye, Rahul A.; Rosenberg, Michael I.; Xie, YuLong; Wang, Weimin; Hart, Philip R.; Zhang, Jian; Goel, Supriya; Mendon, Vrushali V.

    2014-09-04

    This report provides a final quantitative analysis to assess whether buildings constructed according to the requirements of ANSI/ASHRAE/IES Standard 90.1-2013 would result in improved energy efficiency in commercial buildings. The final analysis considered each of the 110 addenda to Standard 90.1-2010 that were included in Standard 90.1-2013. PNNL reviewed all addenda included by ASHRAE in creating Standard 90.1-2013 from Standard 90.1-2010, and considered their combined impact on a suite of prototype building models across all U.S. climate zones. Most addenda were deemed to have little quantifiable impact on building efficiency for the purpose of DOE’s final determination. However, out of the 110 total addenda, 30 were identified as having a measureable and quantifiable impact.

  7. Quantitative determination of uranium distribution homogeneity in material test reactor (MTR) fuel type plates

    International Nuclear Information System (INIS)

    Ferrufino, F.B.J.; Durazzo, M.

    2010-01-01

    IPEN-CNEN/SP produces the fuel to supply its nuclear research reactor IEA-R1. The fuel is assembled from fuel plates containing a core of U 3 Si 2 -Al composite. A good homogeneity in the distribution of uranium in the core of the fuel plate is important from the standpoint of performance under irradiation. Considering the low power reactor IEA-R1, currently the distribution of uranium in the fuel plate is evaluated only by visual inspection of radiographs. However, in view of the possibility of IPEN manufacture the fuel for the new Brazilian Multipurpose Reactor, which has high power, it became urgent to develop a methodology to determine quantitatively the distribution of uranium into the fuel. This paper presents a methodology based on X-ray attenuation, quantifying the distribution of the uranium concentration in the core of the fuel plate by using optical densities of radiographs and comparison with standards. (author)

  8. The renal quantitative scintillation camera study for determination of renal function

    International Nuclear Information System (INIS)

    Thompson, I.M. Jr.; Boineau, F.G.; Evans, B.B.; Schlegel, J.U.

    1983-01-01

    The renal quantitative scintillation camera study assesses glomerular filtration rate and effective renal plasma flow based upon renal uptake of 99mtechnetium-iron ascorbate and 131iodine-hippuran, respectively. The method was compared to inulin, para-aminohippuric acid and creatinine clearance studies in 7 normal subjects and 9 patients with various degrees of reduced renal function. The reproducibility of the technique was determined in 15 randomly selected pediatric patients. The values of glomerular filtration rate and effective renal plasma flow were not significantly different from those of inulin and para-aminohippuric acid studies. The reproducibility of the technique was comparable to that of inulin and para-aminohippuric acid studies. Patient acceptance of the technique is excellent and the cost is minimal. Renal morphology and excretory dynamics also are demonstrated. The technique is advocated as a clinical measure of renal function

  9. Quantitative determination of alveolar bone density using digital image analysis of microradiographs

    International Nuclear Information System (INIS)

    Jaeger, A.; Radlanski, R.J.; Taufall, D.; Klein, C.; Steinhoefel, N.; Doeler, W.

    1990-01-01

    Horizontal 100 μm ground sections of 20 alveolar bone specimens from adult human mandibles obtained from autopsies were prepared for microradiography. Quantitative analysis of bone density of the alveolar cortex was performed using a semiautomatic digital image analysis system (KONTRON). The results demonstrated that bone density was higher in the lingual than in the labial alveolar cortex (p < 0.05). In addition, the coronal portion of alveolar cortical bone was significantly more porous than the medial and apical ones (p < 0.05). These variances were primarily due to increased canal size rather than to an increased number of canals. No significant age dependent changes in bone density could be determined. (author)

  10. Quantitative 3D determination of self-assembled structures on nanoparticles using small angle neutron scattering.

    Science.gov (United States)

    Luo, Zhi; Marson, Domenico; Ong, Quy K; Loiudice, Anna; Kohlbrecher, Joachim; Radulescu, Aurel; Krause-Heuer, Anwen; Darwish, Tamim; Balog, Sandor; Buonsanti, Raffaella; Svergun, Dmitri I; Posocco, Paola; Stellacci, Francesco

    2018-04-09

    The ligand shell (LS) determines a number of nanoparticles' properties. Nanoparticles' cores can be accurately characterized; yet the structure of the LS, when composed of mixture of molecules, can be described only qualitatively (e.g., patchy, Janus, and random). Here we show that quantitative description of the LS' morphology of monodisperse nanoparticles can be obtained using small-angle neutron scattering (SANS), measured at multiple contrasts, achieved by either ligand or solvent deuteration. Three-dimensional models of the nanoparticles' core and LS are generated using an ab initio reconstruction method. Characteristic length scales extracted from the models are compared with simulations. We also characterize the evolution of the LS upon thermal annealing, and investigate the LS morphology of mixed-ligand copper and silver nanoparticles as well as gold nanoparticles coated with ternary mixtures. Our results suggest that SANS combined with multiphase modeling is a versatile approach for the characterization of nanoparticles' LS.

  11. Atomic structure of large angle grain boundaries determined by quantitative X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Fitzsimmons, M.R.; Sass, S.L.

    1988-01-01

    Quantitative X-ray diffraction techniques have been used to determine the atomic structure of the Σ = 5 and 13 [001] twist boundaries in Au with a resolution of 0.09 Angstrom or better. The reciprocal lattices of these boundaries were mapped out using synchrotron radiation. The atomic structures were obtained by testing model structures against the intensity observations with a chi square analysis. The boundary structure were modeled using polyhedra, including octahedra, special configurations of tetrahedra and Archimedian anti-prisms, interwoven together by the boundary symmetry. The results of this work point to the possibility of obtaining general rules for grain boundary structure based on X-ray diffraction observations that give the atomic positions with high resolution

  12. Identification and quantitative determination of atorvastatin calcium polymorph in tablets using FT-Raman spectroscopy.

    Science.gov (United States)

    Skorda, Dimitra; Kontoyannis, Christos G

    2008-01-15

    Atorvastatin calcium (ATC) is the active pharmaceutical ingredient (API) of the best selling lipid-lowering formulation Lipitor. Twelve ATC crystal forms are known and several pharmaceutical companies are developing or have developed generic drug formulations based on different ATC polymorphs. The strong overlap of the X-ray diffraction patterns (XRD) of the polymorphs with the respective patterns of the excipients, the presence of small API quantities in the tablet and the similarity of the crystal phase VIII XRD pattern used in the tablet examined in this work to that of phases IV and IX made identification difficult. Quantitative determination of ATC was attempted using Raman spectroscopy (RS), IR spectroscopy and X-ray powder diffraction. It was found that RS exhibited lower detection limit and a calibration model was constructed. Its application on commercial ATC tablets with 40mg strength yielded an error of 1.25%.

  13. Spectroscopic characterization and quantitative determination of atorvastatin calcium impurities by novel HPLC method

    Science.gov (United States)

    Gupta, Lokesh Kumar

    2012-11-01

    Seven process related impurities were identified by LC-MS in the atorvastatin calcium drug substance. These impurities were identified by LC-MS. The structure of impurities was confirmed by modern spectroscopic techniques like 1H NMR and IR and physicochemical studies conducted by using synthesized authentic reference compounds. The synthesized reference samples of the impurity compounds were used for the quantitative HPLC determination. These impurities were detected by newly developed gradient, reverse phase high performance liquid chromatographic (HPLC) method. The system suitability of HPLC analysis established the validity of the separation. The analytical method was validated according to International Conference of Harmonization (ICH) with respect to specificity, precision, accuracy, linearity, robustness and stability of analytical solutions to demonstrate the power of newly developed HPLC method.

  14. Determination of a Quantitative Job Severity Score Value for Health Hazards in Industry

    Directory of Open Access Journals (Sweden)

    A. Nayebzadeh

    2007-09-01

    Full Text Available Background and aims   There are numerous types of health hazards in every workplace which threaten the health and well-being of employees. Therefore, various types of engineering and  administrative control approaches have been developed in industry. Control of hazardous agents can be difficult in most conditions due to economical and technical limitations. However, certain types of administrative control methods can be implemented in these cases instead of engineering or process controls. Since creating a safe environment with zero chance of occupational exposures to hazardous agents is practically impossible, it can be expected that every employee may have a certain level of exposure to one or more of hazardous agents. The probability and extent of these  exposures will depend on job's demands or work environment's conditions. Under this condition,  a "job severity score" as a quantitative value can be determined in order to choose and employ the  best possible control methodology and also to create a long-term occupational health plan.   Methods   In this study, the main goal is to develop a questionnaire as a model for assessment of job severity and tasks harmfulness. This questionnaire has five sections in which there are numbers  of questions each with a specified quantitative score.  These scores have been identified according to the brainstorming among the some experienced  experts in the fields safety, occupational health, and industrial psychology. When the final  questionnaire was completed, two well-known industrial sectors were selected as pilot plants for final verification of questionnaire in order to obtain valid questions.    Results & Conclusion   The result of this study was providing a questionnaire which might be used in similar studies for determination of job severity level at any industrial plants.

  15. Quantitative determination of moisture in lubricants by Fourier transform infrared spectroscopy.

    Science.gov (United States)

    van de Voort, F R; Sedman, J; Yaylayan, V; Saint Laurent, C; Mucciardi, C

    2004-02-01

    This paper describes the development of a practical Fourier transform infrared (FT-IR) method for the determination of moisture in lubricants through the combined use of signal transduction and differential spectroscopy to circumvent matrix effects. The acid-catalyzed stoichiometric reaction of 2,2-dimethoxypropane (DMP) with moisture to produce acetone was used to provide IR signals proportional to the amount of moisture present in oils. Calibration standards were prepared by spiking polyalphaolefin (PAO) gravimetrically with water using dioxane as a carrier. For FT-IR analysis, standards and samples were diluted with acidified isooctane and then split, with one aliquot treated with DMP and the other with a blank reagent. The spectra of the two aliquots were collected, and a differential spectrum was obtained so as to ratio out the invariant spectral contributions from the sample. Quantitation for moisture was based on measurement of the peak height of the nu(C=O) absorption of acetone at 1717 cm(-1), yielding a standard error of calibration of approximately 40 ppm H2O. The method was validated by standard addition of water in dioxane to PAO containing added base as well as to new and used oils. In all cases the method responded quantitatively to standard addition, the average standard error of prediction being approximately 80 ppm, with the results showing only a minor dependence on the oil formulation. From an analytical perspective, the FT-IR method is both more reproducible and more accurate than Karl Fischer methods and has advantages in terms of environmental considerations, sample size, and speed of analysis as well as the variety of oil types that can be handled. Signal transduction/differential spectroscopy may have broader utility as an alternative means for the determination of low levels of moisture in complex matrices.

  16. Hepatotoxic potential of asarones: In vitro evaluation of hepatotoxicity and quantitative determination in herbal products

    Directory of Open Access Journals (Sweden)

    Dhavalkumar Narendrabha Patel

    2015-02-01

    Full Text Available α and β asarones are natural constituents of some aromatic plants, especially species of the genus Acorus. In addition to beneficial properties of asarones, genotoxicity and carcinogenicity are also reported. Due to potential toxic effects of β-asarone, a limit of exposure from herbal products of approximately 2 μg/kg body weight/day has been set temporarily until a full benefit/risk assessment has been carried out by the European Medicines Agency. Therefore, it is important to monitor levels of β-asarone in herbal products. In this study, we developed a simple, rapid and validated GC-MS method for quantitative determination of asarones and applied it in 20 pediatric herbal products after detecting high concentrations of β-asarone in a product suspected to be implicated in hepatotoxicity in a 3 month old infant. Furthermore, targeted toxicological effects were further investigated in human hepatocytes (THLE-2 cells by employing various in vitro assays, with the goal of elucidating possible mechanisms for the observed toxicity. Results showed that some of the products contained as much as 4 to 25 times greater amounts of β-asarone than the recommended levels. In 4 of 10 samples found to contain asarones, the presence of asarones could not be linked to the labeled ingredients, possibly due to poor quality control. Cell-based investigations in THLE2 cells confirmed the cytotoxicity of -asarone (IC50 = 40.0 ± 2.0 µg/mL which was associated with significant lipid peroxidation and glutathione depletion. This observed cytotoxicity effect is likely due to induction of oxidative stress by asarones. Overall, the results of this study ascertained the usability of this GC-MS method for the quantitative determination of asarones from herbal products, and shed light on the importance of controlling the concentration of potentially toxic asarones in herbal products to safeguard consumer safety. Further investigations of the toxicity of asarones are

  17. Monte Carlo simulation in quantitative determination of 137Cs in sand and water samples

    International Nuclear Information System (INIS)

    Ahuja, B.L.; Sharma, M.; Joshi, K.B.

    2002-01-01

    To understand the distribution of radionuclides in the high background area, one mainly needs to analyse sand, soil, water and other food stuff samples by gamma-spectroscopy. Due to interaction of photons emitted by these radionuclides within the sample, the underestimation of quantity of radionuclides in the sample cannot be ruled out. To overcome this situation, the Monte Carlo method to determine the effect of multiple scattering in Compton profiles has been extended to take better account of interaction of radiation with environmental samples. In this paper, we present the feasibility of Monte Carlo simulation in determining the absorption and multiple scattering of gamma-rays from 137 Cs radionuclides in the sand and water samples. It is seen that only 67 % and 90 % photons escaped from the sand and water respectively, can be detected by nuclear spectroscopy techniques. The high percentage of photoelectric absorption and Compton scattering of photons in these samples warrant the underestimation of quantitative determination of 137 Cs in these samples. (author)

  18. Validation of the methodology for quantitative determination of arsenic in drinking water by hydride generation

    International Nuclear Information System (INIS)

    Silva Trejos, Paulina

    2008-01-01

    The analytical methodology was validated to quantitatively determine the arsenic in drinking water. The atomic absorption method for hydride generation was used. The percentage of recovery for the digestion of the samples was determined in a microwave oven with lots of HNO 3 , the results concluded that the optimal amount to 5,00 mL of sample was 0,50 mL with a recovery rate of 90,5 ±0, 5. The field of optimal linearity was 0-30 ppb with a correlation coefficient of 0,9994. The limits of detection and quantification limits according to Miller and Miller were 1,20 ± 0,02 and 4,01±0,02, respectively. The precision was evaluated by determining the repeatability and reproducibility, the results obtained were 0,34 and 0,30, respectively. The evaluation of the accuracy can report a -1,1 bias. The drinking water sample taken from the laboratory pipe showed As concentrations below the limits of quantification reported in this investigation. (author) [es

  19. Digital Image Quantitative Evaluations for Low Cost Film Digitizers Height Determination

    International Nuclear Information System (INIS)

    Khairul Anuar Mohd Salleh; Arshad Yassin; Ahmad Nasir Yusof; Noorhazleena Azaman

    2016-01-01

    Non Destructive Testing (NDT) technology contributes significant improvement to the quality of industrial products, and the integrity of equipment and plants. Introduction of powerful computers and reliable imaging technology has had significant impact on the traditional nuclear based NDT technology. Demand for faster, reliable, low cost, and flexible technology is rapidly increased. With the growing demand for more efficient digital archiving, digital image analysis, and reporting results with a low cost technology, one cannot deny the importance of having another cheaper solution. This project will apply fundamental principle of image digitization to be used in building up a low cost film digitization solution. The height of the film digitization was carefully determined by examining each digital images produced. Three (3) repetitive quantitative evaluations (Modulation Transfer Function [MTF], Characteristic Transfer Curve [CTC], and Contrast to Noise Ratio [CNR]) were performed at different condition to assist with the determination of the low cost film digitizers height. All 3 evaluations were successfully applied and the most appropriate height was successfully determined. (author)

  20. Quantitative determination of fibrinogen of patients with coronary heart diseases through piezoelectric agglutination sensor.

    Science.gov (United States)

    Chen, Qinghai; Hua, Xing; Fu, Weiling; Liu, Dongbo; Chen, Ming; Cai, Guoru

    2010-01-01

    Fibrinogen can transform fibrin through an agglutination reaction, finally forming fibrin polymer with grid structure. The density and viscosity of the reaction system changes drastically during the course of agglutination. In this research, we apply an independently-developed piezoelectric agglutination sensor to detect the fibrinogen agglutination reaction in patients with coronary heart diseases. The terminal judgment method of determining plasma agglutination reaction through piezoelectric agglutination sensor was established. In addition, the standard curve between plasma agglutination time and fibrinogen concentration was established to determinate fibrinogen content quantitatively. The results indicate the close correlation between the STAGO paramagnetic particle method and the method of piezoelectric agglutination sensor for the detection of Fibrinogen. The correlation coefficient was 0.91 (γ = 0.91). The determination can be completed within 10 minutes. The fibrinogen concentration in the coronary heart disease group was significantly higher than that of the healthy control group (P diseases. Compared with other traditional methods, the method of piezoelectric agglutination sensor has some merits such as operation convenience, small size, low cost, quick detecting, good precision and the common reacting agents with paramagnetic particle method.

  1. Quantitative Determination of Fibrinogen of Patients with Coronary Heart Diseases through Piezoelectric Agglutination Sensor

    Directory of Open Access Journals (Sweden)

    Ming Chen

    2010-03-01

    Full Text Available Fibrinogen can transform fibrin through an agglutination reaction, finally forming fibrin polymer with grid structure. The density and viscosity of the reaction system changes drastically during the course of agglutination. In this research, we apply an independently-developed piezoelectric agglutination sensor to detect the fibrinogen agglutination reaction in patients with coronary heart diseases. The terminal judgment method of determining plasma agglutination reaction through piezoelectric agglutination sensor was established. In addition, the standard curve between plasma agglutination time and fibrinogen concentration was established to determinate fibrinogen content quantitatively. The results indicate the close correlation between the STAGO paramagnetic particle method and the method of piezoelectric agglutination sensor for the detection of Fibrinogen. The correlation coefficient was 0.91 (γ = 0.91. The determination can be completed within 10 minutes. The fibrinogen concentration in the coronary heart disease group was significantly higher than that of the healthy control group (P < 0.05. The results reveal that high fibrinogen concentration is closely correlated to the incurrence, development and prognosis of coronary heart diseases. Compared with other traditional methods, the method of piezoelectric agglutination sensor has some merits such as operation convenience, small size, low cost, quick detecting, good precision and the common reacting agents with paramagnetic particle method.

  2. Simultaneous quantitative determination of paracetamol and tramadol in tablet formulation using UV spectrophotometry and chemometric methods

    Science.gov (United States)

    Glavanović, Siniša; Glavanović, Marija; Tomišić, Vladislav

    2016-03-01

    The UV spectrophotometric methods for simultaneous quantitative determination of paracetamol and tramadol in paracetamol-tramadol tablets were developed. The spectrophotometric data obtained were processed by means of partial least squares (PLS) and genetic algorithm coupled with PLS (GA-PLS) methods in order to determine the content of active substances in the tablets. The results gained by chemometric processing of the spectroscopic data were statistically compared with those obtained by means of validated ultra-high performance liquid chromatographic (UHPLC) method. The accuracy and precision of data obtained by the developed chemometric models were verified by analysing the synthetic mixture of drugs, and by calculating recovery as well as relative standard error (RSE). A statistically good agreement was found between the amounts of paracetamol determined using PLS and GA-PLS algorithms, and that obtained by UHPLC analysis, whereas for tramadol GA-PLS results were proven to be more reliable compared to those of PLS. The simplest and the most accurate and precise models were constructed by using the PLS method for paracetamol (mean recovery 99.5%, RSE 0.89%) and the GA-PLS method for tramadol (mean recovery 99.4%, RSE 1.69%).

  3. [Optimization of sample pretreatment method for the determination of typical artificial sweeteners in soil by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Feng, Biting; Gan, Zhiwei; Hu, Hongwei; Sun, Hongwen

    2014-09-01

    The sample pretreatment method for the determination of four typical artificial sweeteners (ASs) including sucralose, saccharin, cyclamate, and acesulfame in soil by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was optimized. Different conditions of extraction, including four extractants (methanol, acetonitrile, acetone, deionized water), three kinds of ionic strength of sodium acetate solution (0.001, 0.01, 0.1 mol/L), four pH values (3, 4, 5 and 6) of 0.01 mol/L acetate-sodium acetate solution, four set durations of extraction (20, 40, 60, 120 min) and number of extraction times (1, 2, 3, 4 times) were compared. The optimal sample pretreatment method was finally set up. The sam- ples were extracted twice with 25 mL 0.01 mol/L sodium acetate solution (pH 4) for 20 min per cycle. The extracts were combined and then purified and concentrated by CNW Poly-Sery PWAX cartridges with methanol containing 1 mmol/L tris (hydroxymethyl) amino methane (Tris) and 5% (v/v) ammonia hydroxide as eluent. The analytes were determined by HPLC-MS/MS. The recoveries were obtained by spiked soil with the four artificial sweeteners at 1, 10, 100 μg/kg (dry weight), separately. The average recoveries of the analytes ranged from 86.5% to 105%. The intra-day and inter-day precisions expressed as relative standard deviations (RSDs) were in the range of 2.56%-5.94% and 3.99%-6.53%, respectively. Good linearities (r2 > 0.995) were observed between 1-100 μg/kg (dry weight) for all the compounds. The limits of detection were 0.01-0.21 kg/kg and the limits of quantification were 0.03-0.70 μg/kg for the analytes. The four artificial sweeteners were determined in soil samples from farmland contaminated by wastewater in Tianjin. This method is rapid, reliable, and suitable for the investigation of artificial sweeteners in soil.

  4. ANSI/ASHRAE/IESNA Standard 90.1-2010 Preliminary Determination Quantitative Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Halverson, Mark A.; Liu, Bing; Rosenberg, Michael I.

    2010-11-01

    The United States (U.S.) Department of Energy (DOE) conducted a preliminary quantitative analysis to assess whether buildings constructed according to the requirements of the American National Standards Institute (ANSI)/American Society of Heating, Refrigerating and Air-Conditioning Engineers (ASHRAE)/Illuminating Engineering Society of North America (IESNA) Standard 90.1-2010 (ASHRAE Standard 90.1-2010, Standard 90.1-2010, or 2010 edition) would result in energy savings compared with buildings constructed to ANSI/ASHRAE/IESNA Standard 90.1-2007(ASHRAE Standard 90.1-2007, Standard 90.1-2007, or 2007 edition). The preliminary analysis considered each of the 109 addenda to ASHRAE Standard 90.1-2007 that were included in ASHRAE Standard 90.1-2010. All 109 addenda processed by ASHRAE in the creation of Standard 90.1-2010 from Standard 90.1-2007 were reviewed by DOE, and their combined impact on a suite of 16 building prototype models in 15 ASHRAE climate zones was considered. Most addenda were deemed to have little quantifiable impact on building efficiency for the purpose of DOE’s preliminary determination. However, out of the 109 addenda, 34 were preliminarily determined to have measureable and quantifiable impact.

  5. ANSI/ASHRAE/IESNA Standard 90.1-2007 Final Determination Quantitative Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Halverson, Mark A.; Liu, Bing; Richman, Eric E.; Winiarski, David W.

    2011-05-01

    The United States (U.S.) Department of Energy (DOE) conducted a final quantitative analysis to assess whether buildings constructed according to the requirements of the American National Standards Institute (ANSI)/American Society of Heating, Refrigerating and Air-Conditioning Engineers (ASHRAE)/Illuminating Engineering Society of North America (IESNA) Standard 90.1-2007 would result in energy savings compared with buildings constructed to ANSI/ASHRAE/IESNA Standard 90.1-2004. The final analysis considered each of the 44 addenda to ANSI/ASHRAE/IESNA Standard 90.1-2004 that were included in ANSI/ASHRAE/IESNA Standard 90.1-2007. All 44 addenda processed by ASHRAE in the creation of Standard 90.1-2007 from Standard 90.1-2004 were reviewed by DOE, and their combined impact on a suite of 15 building prototype models in 15 ASHRAE climate zones was considered. Most addenda were deemed to have little quantifiable impact on building efficiency for the purpose of DOE’s final determination. However, out of the 44 addenda, 9 were preliminarily determined to have measureable and quantifiable impact.

  6. A miniaturized technique for assessing protein thermodynamics and function using fast determination of quantitative cysteine reactivity.

    Science.gov (United States)

    Isom, Daniel G; Marguet, Philippe R; Oas, Terrence G; Hellinga, Homme W

    2011-04-01

    Protein thermodynamic stability is a fundamental physical characteristic that determines biological function. Furthermore, alteration of thermodynamic stability by macromolecular interactions or biochemical modifications is a powerful tool for assessing the relationship between protein structure, stability, and biological function. High-throughput approaches for quantifying protein stability are beginning to emerge that enable thermodynamic measurements on small amounts of material, in short periods of time, and using readily accessible instrumentation. Here we present such a method, fast quantitative cysteine reactivity, which exploits the linkage between protein stability, sidechain protection by protein structure, and structural dynamics to characterize the thermodynamic and kinetic properties of proteins. In this approach, the reaction of a protected cysteine and thiol-reactive fluorogenic indicator is monitored over a gradient of temperatures after a short incubation time. These labeling data can be used to determine the midpoint of thermal unfolding, measure the temperature dependence of protein stability, quantify ligand-binding affinity, and, under certain conditions, estimate folding rate constants. Here, we demonstrate the fQCR method by characterizing these thermodynamic and kinetic properties for variants of Staphylococcal nuclease and E. coli ribose-binding protein engineered to contain single, protected cysteines. These straightforward, information-rich experiments are likely to find applications in protein engineering and functional genomics. Copyright © 2010 Wiley-Liss, Inc.

  7. Quantitative structure determination of nanostructured materials using the atomic pair distribution function analysis

    Science.gov (United States)

    Masadeh, Ahmad Salah

    The employed experimental method in this Ph.D. dissertation research is the atomic pair distribution function (PDF) technique specializing in high real space resolution local structure determination. The PDF is obtained via Fourier transform from powder total scattering data including the important local structural information in the diffuse scattering intensities underneath, and in-between, the Bragg peaks. Having long been used to study liquids and amorphous materials, the PDF technique has been recently successfully applied to highly crystalline materials owing to the advances in modern X-ray and neutron sources and computing power. The conventional XRD experiments probe for the presence of periodic structure which are reflected in the Bragg peaks. Local structural deviations or disorder mainly affect the diffuse scattering background. In order to have information about both long-range order and local structure disorder, a technique that takes both Bragg and diffuse scattering need to be used, such as the atomic pair distribution function (PDF) technique. This Ph.D. work introduces a PDF based methodology to quantitatively study nanostructure materials in general. The introduced methodology have been applied to a size-dependent structural study on CdSe nanoparticles (NPs). Quantitative structural information about structure, crystallinity level, core size, NP size, and inhomogeneous internal strain in the studied NPs have been obtained. This method is generally applicable to the characterization of the nano-scale solid, many of which may exhibit complex disorder and strain. The introduced methodology have been also applied on technologically important system, ultra-small CdSe NPs.

  8. Quantitative determination of micronization-induced changes in the solid state of lactose.

    Science.gov (United States)

    Della Bella, A; Müller, M; Soldati, L; Elviri, L; Bettini, R

    2016-05-30

    Lactose, in particular α-lactose monohydrate, is the most used carrier for inhalation. Its surface and solid-state properties play a key role in determining Dry Powder Inhalers (DPIs) performance. Techniques such as X-Ray Powder Diffraction (XRPD) and Differential Scanning Calorimetry (DSC), which are commonly used for the characterization of lactose, are not always capable of explaining the solid-state changes induced by processing, such as micronization. In the present work, the evaluation of the effect of the micronization process on the solid-state properties of lactose was carried out by XRPD and DSC and a satisfactory, although not unequivocal, interpretation of the thermal behaviour of lactose was obtained. Thus, a new gravimetric method correlating in a quantitative manner the weight change in specific sections of the Dynamic Vapour Sorption (DVS) profile and the amount of different forms of α-lactose (hygroscopic anhydrous, stable anhydrous and amorphous) simultaneously present in a given sample was developed and validated. The method is very simple and provides acceptable accuracy in phase quantitation (LOD=1.6, 2.4 and 2.7%, LOQ=5.4, 8.0 and 8.9% for hygroscopic anhydrous, stable anhydrous and amorphous α-lactose, respectively). The application of this method to a sample of micronized lactose led to results in agreement with those obtained by DSC and evidenced that hygroscopic anhydrous α-lactose, rather than amorphous lactose, can be generated in the micronization process. The proposed method may find a more general application for the quantification of polymorphs of compounds different than lactose, provided that the various solid phases afford different weight variations in specific regions of the DVS profile. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Development and application of novelty pretreatment method for the concurrent quantitation of eleven water-soluble B vitamins in ultrafiltrates after renal replacement therapy.

    Science.gov (United States)

    Wirkus, Dorota; Jakubus, Aleksandra; Owczuk, Radosław; Stepnowski, Piotr; Paszkiewicz, Monika

    2017-02-01

    Continous renal replacement therapy (CRRT) is particularly recommended for septic shock patients in intensive care units. The CRRT technique used most frequently is high volume continuous veno-venous haemofiltration. It provides a high rate of clearance of uremic toxins and inflammatory cytokines. However, it should also be taken into account that substances important for homeostasis may be concurrently unintentionally removed. Accordingly, water-soluble vitamins can be removed during continuous renal replacement therapy, and the estimate of the loss is critical to ensure appropriate supplementation. The aim of this work was to develop a simple methodology for a purification step prior to the LC-MS/MS determination of water-soluble vitamins in ultrafiltrate samples. For this purpose, two types of resin and a mix of resins were used as sorbents for the purification step. Moreover, parameters such as the amount of resin and the extraction time were optimized. The LC-MS/MS method was developed and validated for final determination of 11 vitamins. The results demonstrated the high purification capability of DEAE Sephadex resin with recoveries between 65 and 101% for water-soluble vitamins from ultrafiltrate samples. An optimized method was applied to assess the loss of B-group vitamins in patients after 24h of renal replacement therapy. The loss of vitamins B2, B6 pyridoxamine, B6 pyridoxal, B7, B1, and B5 in ultrafiltrates was similar in all patients. In the native ultrafiltrates, vitamins B6 pyridoxine, B9 and B12 were not detected. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. UV SPECTROPHOTOMETRY APPLICATION FOR QUANTITATIVE DETERMINATION OF VINPOCETINE IN DRUG FORMULATIONS

    Directory of Open Access Journals (Sweden)

    J. V. Monaykina

    2014-12-01

    Full Text Available Introduction. In this paper simple, rapid and sensitive assay methods for quantitative determination of vinpocetine in two new drug formulations (suppositories and nasal cream are proposed. Analysis has been performed directly by using zero-order UV spectrophotometry. It is known from the special literature that the chromatographic techniques used for vinpocetine assay require expensive equipment and are rather time consuming. Therefore UV spectrophotometry is preferable due to its accuracy and simplicity. The object of this study was to develop new, simple, rapid, precise and accurate UV spectrophotometric procedure for the quantitative determination of vinpocetine in suppositories and nasal cream and evaluation of some validation characteristics of the methods. Materials and methods. The objects of the study were the new drug formulations of vinpocetine, namely 0,01 suppositories and 0,5% nasal cream developed by the scientists of The Chair of Technology of Drugs of Zaporizhzhia State Medical University. Distilled water and 0.05M HCl were used as the solvents, working standard sample of vinpocetine was used as a reference standard. Analytical equipment: spectrophotometer Specord 200, electronic balance ABT-120-5DM, measuring glassware of class A. Assay procedure: An accurately weighed sample of cream (1,200 – 2,000 g or one suppository was dissolved in 0.05M HCl and filtered into a 50,00 ml volumetric flask. Then the solution was brought to the mark with the same solvent and stirred. 3,00 ml or 4,00 ml of the resulting solutions (for suppositories or cream respectively were transferred into a 25,00 ml volumetric flask and brought to the mark with distilled water. Absorbance was measured at a wavelength of 272 nm on the blank of distilled water. The parallel measurement with 1,00 ml of 0,064% vinpocetine standard solution was carried out. The content of active substance was calculated according to standard formulas. Results. The suggested

  11. APPLICATION OF UV-SPECTROPHOTOMETRY FOR THE QUANTITATIVE DETERMINATION OF CAPTOPRIL IN DRUG

    Directory of Open Access Journals (Sweden)

    Yu. V. Monaykina

    2015-04-01

    Full Text Available Introduction. In this paper the simple, rapid and sensitive assay method for the quantitative determination of captopril in two new pharmaceutical formulations (suppositories and nasal gel is proposed. Analysis was performed directly by using zero-order UV spectrophotometry. It is known from the special literature that the chromatographic techniques used for captopril assay require the expensive equipment and are rather time consuming. Therefore UV spectrophotometry is preferable due to its accuracy, sensitivity and simplicity. The aim of this study was to develop and validate a new, simple, rapid, precise and accurate UV spectrophotometric method for the quantitative determination of captopril in suppositories and nasal gel. Materials and methods. The objects of the study were the new drug formulations of captopril, namely 0,05 suppositories and 2,5% nasal gel developed by the scientists of The Chair of Technology of Drugs ofZaporozhye State Medical University. Distilled water was used as the solvent, working standard sample of captopril was used as a reference standard. Analytical equipment: spectrophotometer Specord 200, electronic balance ABT-120-5DM, measuring glassware of class A. Assay procedure: An accurately weighed sample of gel (0,4000 –0,8000 g or one suppository was dissolved in distilled water and filtered into a volumetric flask (50,00 ml for gel and 250,0 ml for suppository . Then the solution was brought to the mark with the same solvent and stirred. 1,00 ml of the resulting solution was transferred into a 25,00 ml volumetric flask and brought to the mark with distilled water. Absorbance was measured at a wavelength of 203 nm on the blank of a solvent. The parallel measurement with 1,00 ml of 0,03% captopril standard solution was carried out. The content of active substance was calculated according to standard formulas. Results. The suggested procedure was successfully applied for the analysis of two new pharmaceutical

  12. Quantitative determination of volatile organic compounds in indoor dust using gas chromatography-UV spectrometry.

    Science.gov (United States)

    Nilsson, Anders; Lagesson, Verner; Bornehag, Carl-Gustaf; Sundell, Jan; Tagesson, Christer

    2005-10-01

    A novel technique, gas chromatography-UV spectrometry (GC-UV), was used to quantify volatile organic compounds (VOCs) in settled dust from 389 residences in Sweden. The dust samples were thermally desorbed in an inert atmosphere and evaporated compounds were concentrated by solid phase micro extraction and separated by capillary GC. Eluting compounds were then detected, identified, and quantified using a diode array UV spectrophotometer. Altogether, 28 compounds were quantified in each sample; 24 of these were found in more than 50% of the samples. The compounds found in highest concentrations were saturated aldehydes (C5-C10), furfuryl alcohol, 2,6-di-tert-butyl-4-methylphenol (BHT), 2-furaldehyde, and benzaldehyde. Alkenals were also found, notably 2-butenal (crotonaldehyde), 2-methyl-propenal (methacrolein), hexenal, heptenal, octenal, and nonenal. The concentrations of each of the 28 compounds ranged between two to three orders of magnitude, or even more. These results demonstrate the presence of a number of VOCs in indoor dust, and provide, for the first time, a quantitative determination of these compounds in a larger number of dust samples from residents. The findings also illustrate the potential use of GC-UV for analysing volatile compounds in indoor dust, some of which are potential irritants (to the skin, eyes or respiratory system) if present at higher concentrations. The potential use of GC-UV for improving survey and control of the human exposure to particle-bound irritants and other chemicals is inferred.

  13. Sensitive time-resolved fluoroimmunoassay for quantitative determination of clothianidin in agricultural samples.

    Science.gov (United States)

    Li, Ming; Sheng, Enze; Yuan, Yulong; Liu, Xiaofeng; Hua, Xiude; Wang, Minghua

    2014-05-01

    Europium (Eu(3+))-labeled antibody was used as a fluorescent label to develop a highly sensitive time-resolved fluoroimmunoassay (TRFIA) for determination of clothianidin residues in agricultural samples. Toward this goal, the Eu(3+)-labeled polyclonal antibody and goat anti-rabbit antibody were prepared for developing and evaluating direct competitive TRFIA (dc-TRFIA) and indirect competitive TRFIA (ic-TRFIA). Under optimal conditions, the half-maximal inhibition concentration (IC50) and the limit of detection (LOD, IC10) of clothianidin were 9.20 and 0.0909 μg/L for the dc-TRFIA and 2.07 and 0.0220 μg/L for the ic-TRFIA, respectively. The ic-TRFIA has no obvious cross-reactivity with the analogues of clothianidin except for dinotefuran. The average recoveries of clothianidin from spiked water, soil, cabbage, and rice samples were estimated to range from 74.1 to 115.9 %, with relative standard deviations of 3.3 to 11.7 %. The results of TRFIA for the blind samples were largely consistent with gas chromatography (R (2) = 0.9902). The optimized ic-TRFIA might become a sensitive and satisfactory analytical method for the quantitative monitoring of clothianidin residues in agricultural samples.

  14. Quantitative Determination of Catechin as Chemical Marker in Pediatric Polyherbal Syrup by HPLC/DAD.

    Science.gov (United States)

    Sheikh, Zeeshan A; Siddiqui, Zafar A; Naveed, Safila; Usmanghani, Khan

    2016-09-01

    Vivabon syrup is a balanced composition of dietary ingredients of phytopharmaceutical nature for maintaining the physique, vigor, vitality and balanced growth of children. The herbal ingredients of pediatric syrup are rich in bioflavonoid, proteins, vitamins, glycosides and trace elements. Vivabon is formulated with herbal drugs such as Phoenix sylvestris, Emblica officinalis, Withania somnifera, Centella asiatica, Amomum subulatum, Zingiber officinalis, Trigonella foenum-graecum, Centaurea behen and Piper longum Catechins are flavan-3-ols that are found widely in the medicinal herbs and are utilized for anti-inflammatory, cardio protective, hepato-protective, neural protection and other biological activities. In general, the dietary intake of flavonoids has been regarded traditionally as beneficial for body growth. Standardization of Vivabon syrup dosage form using HPLC/DAD has been developed for quantitative estimation of Catechin as a chemical marker. The method was validated as per ICH guidelines. Validation studies demonstrated that the developed HPLC method is quite distinct, reproducible as well as quick and fast. The relatively high recovery and low comparable standard deviation confirm the suitability of the developed method for the determination of Catechin in syrup. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yen, Nguyen; Thu, Nguyen; Zhao, Bing Tian; Woo, Mi Hee; Min, Byung Sun [Catholic Univ. of Daegu, Gyeongsan (Korea, Republic of); Lee, Jae Hyun [Dongguk Univ., Yongin (Korea, Republic of); Kim, Jeong Ah [Kyungpook National Univ., Daegu (Korea, Republic of); Son, Jong Keun [Yeungnam Univ., Gyeongsan (Korea, Republic of); Choi, Jae Sui [Pukyung National Univ., Busan (Korea, Republic of); Woo, Eun Rhan [Chosun Univ., Gwangju (Korea, Republic of)

    2014-07-15

    To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside, 3-caffeoylquinic acid and calceolarioside B. Particular attention was focused on the main compound, 3-caffeoylquinic acid, which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-β-D-glucopyranoside was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb.

  16. A set of enhanced green fluorescent protein concatemers for quantitative determination of nuclear localization signal strength.

    Science.gov (United States)

    Böhm, Jennifer; Thavaraja, Ramya; Giehler, Susanne; Nalaskowski, Marcus M

    2017-09-15

    Regulated transport of proteins between nucleus and cytoplasm is an important process in the eukaryotic cell. In most cases, active nucleo-cytoplasmic protein transport is mediated by nuclear localization signal (NLS) and/or nuclear export signal (NES) motifs. In this study, we developed a set of vectors expressing enhanced GFP (EGFP) concatemers ranging from 2 to 12 subunits (2xEGFP to 12xEGFP) for analysis of NLS strength. As shown by in gel GFP fluorescence analysis and αGFP Western blotting, EGFP concatemers are expressed as fluorescent full-length proteins in eukaryotic cells. As expected, nuclear localization of concatemeric EGFPs decreases with increasing molecular weight. By oligonucleotide ligation this set of EGFP concatemers can be easily fused to NLS motifs. After determination of intracellular localization of EGFP concatemers alone and fused to different NLS motifs we calculated the size of a hypothetic EGFP concatemer showing a defined distribution of EGFP fluorescence between nucleus and cytoplasm (n/c ratio = 2). Clear differences of the size of the hypothetic EGFP concatemer depending on the fused NLS motif were observed. Therefore, we propose to use the size of this hypothetic concatemer as quantitative indicator for comparing strength of different NLS motifs. Copyright © 2017 Elsevier Inc. All rights reserved.

  17. Quantitative Determination of Ivermectin in Raw Milk Using Positive ESI LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Meenakshi Dahiya

    2010-01-01

    Full Text Available Ivermectin, a veterinary drug, is commonly used endectocide for animal husbandry. The drug is available in the form of subcutaneous or topical formulations. Its application may cause accumulation of its residues into the animal tissues, which ultimately find their way into the food products, such as milk and meat products. In order to determine the residues of ivermectin in milk, a comparatively simple, sensitive and rapid method was developed and validated using LC-MS/MS. The MRM transitions corresponding to m/z 892.71>569.6, 892.71>551.5 and 892.71>307.3 were used for the purpose of quantification and evaluation of other parameters of the method. The limit of detection of the method was found to be 0.1 μg/kg and the limit of quantitation was calculated as 0.2 μg/kg. The method was found to be linear in the range of 1.0 ng/mL to 100.0 ng/mL with correlation coefficient of 0.9992 for pure calibration curve and 0.9990 for the matrix- matched calibration curve. The recoveries of ivermectin from the spiked samples of raw milk were found between 85 to 105%.

  18. Quantitative determination of uranium distribution homogeneity in MTR fuel type plates

    International Nuclear Information System (INIS)

    Ferrufino, Felipe Bonito Jaldin

    2011-01-01

    IPEN/CNEN-SP produces the fuel to supply its nuclear research reactor IEA-R1. The fuel is assembled with fuel plates containing an U 3 Si 2 -Al composite meat. A good homogeneity in the uranium distribution inside the fuel plate meat is important from the standpoint of irradiation performance. Considering the lower power of reactor IEA-R1, the uranium distribution in the fuel plate has been evaluated only by visual inspection of radiographs. However, with the possibility of IPEN to manufacture the fuel for the new Brazilian Multipurpose Reactor (RMB), with higher power, it urges to develop a methodology to determine quantitatively the uranium distribution into the fuel. This paper presents a methodology based on X-ray attenuation, in order to quantify the uranium concentration distribution in the meat of the fuel plate by using optical densities in radiographs and comparison with standards. The results demonstrated the inapplicability of the method, considering the current specification for the fuel plates due to the high intrinsic error to the method. However, the study of the errors involved in the methodology, seeking to increase their accuracy and precision, can enable the application of the method to qualify the final product. (author)

  19. Development and validation of HPLC analytical method for quantitative determination of metronidazole in human plasma

    International Nuclear Information System (INIS)

    Safdar, K.A.; Shyum, S.B.; Usman, S.

    2016-01-01

    The objective of the present study was to develop a simple, rapid and sensitive reversed-phase high performance liquid chromatographic (RP-HPLC) analytical method with UV detection system for the quantitative determination of metronidazole in human plasma. The chromatographic separation was performed by using C18 RP column (250mm X 4.6mm, 5 meu m) as stationary phase and 0.01M potassium dihydrogen phosphate buffered at pH 3.0 and acetonitrile (83:17, v/v) as mobile phase at flow rate of 1.0 ml/min. The UV detection was carried out at 320nm. The method was validated as per the US FDA guideline for bioanalytical method validation and was found to be selective without interferences from mobile phase components, impurities and biological matrix. The method found to be linear over the concentration range of 0.2812 meu g/ml to 18.0 meu g/ml (r2 = 0.9987) with adequate level of accuracy and precision. The samples were found to be stable under various recommended laboratory and storage conditions. Therefore, the method can be used with adequate level of confidence and assurance for bioavailability, bioequivalence and other pharmacokinetic studies of metronidazole in human. (author)

  20. Comparation of fundamental analytical methods for quantitative determination of copper(IIion

    Directory of Open Access Journals (Sweden)

    Ačanski Marijana M.

    2008-01-01

    Full Text Available Copper is a ductile metal with excellent electrical conductivity, and finds extensive use as an electrical conductor, heat conductor, as a building material, and as a component of various alloys. In this work accuracy of methods for quantitative determination (gravimetric and titrimetric methods of analysis of copper(II ion was studied. Gravimetric methods do not require a calibration or standardization step (as all other analytical procedures except coulometry do because the results are calculated directly from the experimental data and molar masses. Thus, when only one or two samples are to be analyzed, a gravimetric procedure may be the method of choice because it involves less time and effort than a procedure that requires preparation of standards and calibration. In this work in gravimetric analysis the concentration of copper(II ion is established through the measurement of a mass of CuSCN and CuO. Titrimetric methods is a process in which a standard reagent is added to a solution of an analyze until the reaction between the analyze and reagent is judged to be complete. In this work in titrimetric analysis the concentration of copper(II ion is established through the measurement of a volume of different standard reagents: Km, Na2S2O3 and AgNO3. Results were discussed individually and mutually with the aspect of exactility, reproductivity and rapidity. Relative error was calculated for all methods.

  1. Quantitative determination of Sulfur and Chlorine in Crude Oils by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ayala Jimenez, R.E.

    1986-01-01

    Given the importance of sulfur and chlorine content in crude petroleum, and that the actual methods used in the country to its determination are slow and cumbersome, the present work consisted in applying a new method, based on X-ray fluorescence spectrometry, to make this analysis as fast as possible with greater sensibility and precision. Samples of crude petroleum were analyzed using two different quantitative methods: a) through calibration curves elaborated with standard aqueous solutions of inorganic salts of S and Cl and b) through standard addition method using CS 2 as standard for S and CCl 4 for Cl. The measuring system consisted of Fe-55 radioactive source (10 mCi), Si-Li semiconductor detector, spectrum amplifier, multichannel analyzer and a DIGITAL Computer. The peak areas and their deviations were obtained through AXIL software. The values of area and deviation joined to weight of sample and amount of standard added were used to calculate the concentration of the analite and its deviation. In conclusion, calibration curves enable only semiquantitative analysis. However, the standard addition method has advantages over ASTM methods D 129-64 and D 808-63 for sulfur and chlorine respectively. The main advantage is the great speed with which an analysis is made: 20 minutes, while ASTM methods need approximately 16 hours. Likewise it was obtained: sensibility 0.05%; accuracy: maximum 0.02%, minimum 10%; and precision: maximum 2%, minimum 10%. (author)

  2. Quantitative Determination on Ionic-Liquid-Gating Control of Interfacial Magnetism.

    Science.gov (United States)

    Zhao, Shishun; Zhou, Ziyao; Peng, Bin; Zhu, Mingmin; Feng, Mengmeng; Yang, Qu; Yan, Yuan; Ren, Wei; Ye, Zuo-Guang; Liu, Yaohua; Liu, Ming

    2017-05-01

    Ionic-liquid gating on a functional thin film with a low voltage has drawn a lot of attention due to rich chemical, electronic, and magnetic phenomena at the interface. Here, a key challenge in quantitative determination of voltage-controlled magnetic anisotropy (VCMA) in Au/[DEME] + [TFSI] - /Co field-effect transistor heterostructures is addressed. The magnetic anisotropy change as response to the gating voltage is precisely detected by in situ electron spin resonance measurements. A reversible change of magnetic anisotropy up to 219 Oe is achieved with a low gating voltage of 1.5 V at room temperature, corresponding to a record high VCMA coefficient of ≈146 Oe V -1 . Two gating effects, the electrostatic doping and electrochemical reaction, are distinguished at various gating voltage regions, as confirmed by X-ray photoelectron spectroscopy and atomic force microscopy experiments. This work shows a unique ionic-liquid-gating system for strong interfacial magnetoelectric coupling with many practical advantages, paving the way toward ion-liquid-gating spintronic/electronic devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Quantitative determinants of aerobic glycolysis identify flux through the enzyme GAPDH as a limiting step

    Science.gov (United States)

    Shestov, Alexander A; Liu, Xiaojing; Ser, Zheng; Cluntun, Ahmad A; Hung, Yin P; Huang, Lei; Kim, Dongsung; Le, Anne; Yellen, Gary; Albeck, John G; Locasale, Jason W

    2014-01-01

    Aerobic glycolysis or the Warburg Effect (WE) is characterized by the increased metabolism of glucose to lactate. It remains unknown what quantitative changes to the activity of metabolism are necessary and sufficient for this phenotype. We developed a computational model of glycolysis and an integrated analysis using metabolic control analysis (MCA), metabolomics data, and statistical simulations. We identified and confirmed a novel mode of regulation specific to aerobic glycolysis where flux through GAPDH, the enzyme separating lower and upper glycolysis, is the rate-limiting step in the pathway and the levels of fructose (1,6) bisphosphate (FBP), are predictive of the rate and control points in glycolysis. Strikingly, negative flux control was found and confirmed for several steps thought to be rate-limiting in glycolysis. Together, these findings enumerate the biochemical determinants of the WE and suggest strategies for identifying the contexts in which agents that target glycolysis might be most effective. DOI: http://dx.doi.org/10.7554/eLife.03342.001 PMID:25009227

  4. Development of a quantitative approach using Raman spectroscopy for carotenoids determination in processed sweet potato.

    Science.gov (United States)

    Sebben, Juliano Antônio; da Silveira Espindola, Juliana; Ranzan, Lucas; Fernandes de Moura, Neusa; Trierweiler, Luciane Ferreira; Trierweiler, Jorge Otávio

    2018-04-15

    The orange-fleshed sweet potato is a vegetable-rich in carotenoids. The thermic treatment for sweet potato processing can decrease the content of these constituents in the foods, lowering their bioactive properties. Raman spectroscopy has been growing as a fast tool to food analysis, especially for detection of low concentrations of carotenoids and to the monitoring of its degradation profile over time. Therefore, in this work were evaluated two methods of drying, hot air and microwaving with rotary drum, combined with quantitative Raman spectroscopy. The results showed carotenoids degradation around 50% for both types of drying processes studied. PCA plot proved the potential of reproducibility of analyses for microwave drying samples. For samples heated with hot air, the best linear correlation achieved was R 2  = 0.90 and by microwave was R 2  = 0.88. Also, partial least squares (PLS) regression models were constructed obtaining a satisfactory coefficient of determination. Copyright © 2017. Published by Elsevier Ltd.

  5. Quantitative determination of retained austenite in the continuous annealing production line of cold-rolled steel

    International Nuclear Information System (INIS)

    Ichikawa, Fumihiko; Kitagawa, Hajime.

    1987-01-01

    An X-ray diffraction method has been developed for quantitative determination of retained austenite in the continuous annealing production line, CAL, of cold rolled steel sheets. A new unit of diffractometer(Cr-K α source with two proportional counters) was specially designed for the CAL. Intensities of {220} austenite reflection, I γ , and background, I BG , are measured separately by the two detectors. From I γ and I BG , real-time calculation of normalized intensity of austenite, I S , is executed by the following equation ; I S = (I γ -I BG )/I BG . I S was little affected by the fluctuation of the distance between the diffractometer and travelling material. Normalized intensity is well correlated both with the tensile strength and with volume fraction of martensite, of high strength ''dual-phase'' steel sheets. From this findings, the presently developed X-ray diffractometer unit is proved to be successfully employable in the CAL as an effectual method for control of material properties in the high strength ''dual-phase'' steel sheet by monitoring the normalized intensity of austenite. (author)

  6. Quantitative determination of superoxide in plant leaves using a modified NBT staining method.

    Science.gov (United States)

    Bournonville, Carlos F Grellet; Díaz-Ricci, Juan Carlos

    2011-01-01

    In plants, the ROS (reactive oxygen species) level is tightly regulated because their accumulation produces irreversible damage leading to cell death. However, ROS accumulation plays a key role in plant signaling under biotic or abiotic stress. Although various methods were reported to evaluate ROS accumulation, they are restricted to model plants or provide only qualitative information. Develop a simple method to quantify superoxide radicals produced in plant tissues, based on the selective extraction of the formazan produced after nitroblue tetrazolium (NBT) reduction in histochemical staining. Plant leaves were stained with a standard NBT method and the formazan precipitated in tissues was selectively extracted using chloroform. The organic phase was dried and formazan residue dissolved in dimethylsulfoxide-potassium hydroxide and quantified by spectrophotometry. The method was tested in strawberry plant leaves under different stressing conditions. Formazan extracted from leaves subjected to stress conditions showed similar absorption spectra to those obtained from standard solutions using pure formazan. Calibration curves showed a linear relationship between absorbance and formazan amounts, within the range 0.5-8 µg. Outcomes suggested that formazan was retained in the solid residue of leaf tissues. This protocol allowed us to quantify superoxide radicals produced under different stress conditions. Chloroform allowed a selective formazan extraction and removal of potential endogenous, exogenous or procedural artefacts that may interfere with the quantitative determination. This protocol can be used to quantify the superoxide produced in plant tissues using any traditional qualitative NBT histochemical staining method. Copyright © 2011 John Wiley & Sons, Ltd.

  7. New copper resistance determinants in the extremophile acidithiobacillus ferrooxidans: a quantitative proteomic analysis.

    Science.gov (United States)

    Almárcegui, Rodrigo J; Navarro, Claudio A; Paradela, Alberto; Albar, Juan Pablo; von Bernath, Diego; Jerez, Carlos A

    2014-02-07

    Acidithiobacillus ferrooxidans is an extremophilic bacterium used in biomining processes to recover metals. The presence in A. ferrooxidans ATCC 23270 of canonical copper resistance determinants does not entirely explain the extremely high copper concentrations this microorganism is able to stand, suggesting the existence of other efficient copper resistance mechanisms. New possible copper resistance determinants were searched by using 2D-PAGE, real time PCR (qRT-PCR) and quantitative proteomics with isotope-coded protein labeling (ICPL). A total of 594 proteins were identified of which 120 had altered levels in cells grown in the presence of copper. Of this group of proteins, 76 were up-regulated and 44 down-regulated. The up-regulation of RND-type Cus systems and different RND-type efflux pumps was observed in response to copper, suggesting that these proteins may be involved in copper resistance. An overexpression of most of the genes involved in histidine synthesis and several of those annotated as encoding for cysteine production was observed in the presence of copper, suggesting a possible direct role for these metal-binding amino acids in detoxification. Furthermore, the up-regulation of putative periplasmic disulfide isomerases was also seen in the presence of copper, suggesting that they restore copper-damaged disulfide bonds to allow cell survival. Finally, the down-regulation of the major outer membrane porin and some ionic transporters was seen in A. ferrooxidans grown in the presence of copper, indicating a general decrease in the influx of the metal and other cations into the cell. Thus, A. ferrooxidans most likely uses additional copper resistance strategies in which cell envelope proteins are key components. This knowledge will not only help to understand the mechanism of copper resistance in this extreme acidophile but may help also to select the best fit members of the biomining community to attain more efficient industrial metal leaching

  8. Quantitative determination of the proportion of microtubule polymer present during the mitosis-interphase transition.

    Science.gov (United States)

    Zhai, Y; Borisy, G G

    1994-04-01

    We have developed a new method for determining levels of tubulin polymer, based on quantitative fluorescence detection of x-rhodamine tubulin microinjected into living cells and we have applied this method to analysis of the mitosis-interphase transition. LLC-PK cells in interphase and mitosis were microinjected, then cooled and rewarmed to drive tubulin incorporation. Total tubulin fluorescence in individual, living cells was quantified using a cooled, scientific grade CCD image sensor. Cells were then washed and lysed into a microtubule-stabilizing buffer to extract the soluble pool. Total tubulin polymer fluorescence was determined for the extracted cells in the same way as for living cells. Fluorescence images were corrected by flat-fielding and background subtraction. The ratio of extracted cell fluorescence/living cell fluorescence for individual cells, was taken as the proportion of tubulin as polymer. Cells in M-phase, G1 and random interphase were analyzed. G1 cells had almost the same proportion as random interphase cells. Mitotic cells gave a value of 90 +/- 5% of G1 cells at 37 degrees C. Within M-phase, levels of tubulin as polymer in metaphase and early anaphase were not significantly different. In contrast to the general expectation of microtubule depolymerization at anaphase onset, these results indicate that as cells exit mitosis, the overall proportion of tubulin as polymer does not change dramatically even though the mitotic spindle disassembles. We conclude that the mitosis-interphase transition is accompanied by a redistribution of tubulin at an essentially constant polymer level. Therefore, a global shift to depolymerization conditions is not the driving force for anaphase chromosome movement.

  9. Simultaneous determination of florfenicol with its metabolite based on modified quick, easy, cheap, effective, rugged, and safe sample pretreatment and evaluation of their degradation behavior in agricultural soils.

    Science.gov (United States)

    Xu, Mingfei; Qian, Mingrong; Zhang, Hu; Ma, Junwei; Wang, Jianmei; Wu, Huizhen

    2015-01-01

    A simple and simultaneous method for the determination of florfenicol and its metabolite florfenicol amine in agricultural soils using modified quick, easy, cheap, effective, rugged, and safe sample pretreatment and reversed-phase high-performance liquid chromatography with tandem mass spectrometry is presented. Florfenicol and its metabolite florfenicol amine residues in agricultural soils were extracted with alkalized acetonitrile and an aliquot was cleaned up with Si(CH2)3NH(CH2)2NH2 and C18 sorbent, which were powder materials. High-performance liquid chromatography with tandem mass spectrometry was applied to simultaneously determine the level of florfenicol and florfenicol amine in agricultural soils. Excellent linearity was achieved for florfenicol and florfenicol amine over a range of concentrations from 0.1-500 μg/L with coefficients more than 0.99. Average recoveries at four different levels (0.005, 0.05, 0.5, and 5.0 mg/kg) for florfenicol and florfenicol amine ranged from 73.6-94.9% with relative standard deviations of 2.9-12.5%. The limits of detection for florfenicol and florfenicol amine in agricultural soils were 2.0 μg/kg, and the limits of quantification were 6.0 μg/kg. Based on this method, the degradation behavior of florfenicol and its metabolite florfenicol amine in three soils (Nanchang, Hangzhou, and Changchun) under sterilized and native conditions was investigated and the transformation rate of florfenicol amine from florfenicol was evaluated. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Quantitative mineralogy of the Yukon River system: Changes with reach and season, and determining sediment provenance

    Science.gov (United States)

    Eberl, D.D.

    2004-01-01

    mineral dissolution during transport between Eagle and Pilot Station, a distance of over 2000 km. We estimate that approximately 3 wt% of the quartz, 15 wt% of the feldspar (1 wt% of the alkali and 25 wt% of the plagioclase), and 26 wt% of the carbonates (31 wt% of the calcite and 15 wt% of the dolomite) carried by the river dissolve in this reach. The mineralogies of the suspended sediments change with the season. For example, during the summer of 2002 the quartz content varied by 20 wt%, with a minimum in mid-summer. The calcite content varied by a similar amount, and had a maximum corresponding to the quartz minimum. These modes are related to the relative amount of sediment flowing from the White River system, which is relatively poor in quartz, but rich in carbonate minerals. Suspended total clay minerals varied by as much as 25 wt%, with maxima in mid July, and suspended feldspar varied up to 10 wt%. Suspended sediment data from the summers of 2001 and 2003 support the 2002 trends. A calculation technique was developed to determine theproportion of various sediment sources in a mixed sediment by unmixing its quantitative mineralogy. Results from this method indicate that at least three sediment sources can be identified quantitatively with good accuracy. With this technique, sediment mineralogies can be used to calculate the relative flux of sediment from different tributaries, thereby identifying sediment provenance.

  11. ANSI/ASHRAE/IES Standard 90.1-2010 Final Determination Quantitative Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Halverson, Mark A.; Rosenberg, Michael I.; Liu, Bing

    2011-10-31

    The U.S. Department of Energy (DOE) conducted a final quantitative analysis to assess whether buildings constructed according to the requirements of the American National Standards Institute (ANSI)/American Society of Heating, Refrigerating and Air-Conditioning Engineers (ASHRAE)/Illuminating Engineering Society of North America (IESNA) Standard 90.1-2010 (ASHRAE Standard 90.1-2010, Standard 90.1-2010, or 2010 edition) would result in energy savings compared with buildings constructed to ANSI/ASHRAE/IESNA Standard 90.1-2007(ASHRAE Standard 90.1-2007, Standard 90.1-2007, or 2007 edition). The final analysis considered each of the 109 addenda to ASHRAE Standard 90.1-2007 that were included in ASHRAE Standard 90.1-2010. All 109 addenda processed by ASHRAE in the creation of Standard 90.1-2010 from Standard 90.1-2007 were reviewed by DOE, and their combined impact on a suite of 16 building prototype models in 15 ASHRAE climate zones was considered. Most addenda were deemed to have little quantifiable impact on building efficiency for the purpose of DOE's final determination. However, out of the 109 addenda, 34 were preliminarily determined to have a measureable and quantifiable impact. A suite of 240 computer energy simulations for building prototypes complying with ASHRAE 90.1-2007 was developed. These prototypes were then modified in accordance with these 34 addenda to create a second suite of corresponding building simulations reflecting the same buildings compliant with Standard 90.1-2010. The building simulations were conducted using the DOE EnergyPlus building simulation software. The resulting energy use from the complete suite of 480 simulation runs was then converted to energy use intensity (EUI, or energy use per unit floor area) metrics (Site EUI, Primary EUI, and energy cost intensity [ECI]) results for each simulation. For each edition of the standard, these EUIs were then aggregated to a national basis for each prototype using weighting factors based

  12. Quantitative determination and classification of energy drinks using near-infrared spectroscopy.

    Science.gov (United States)

    Rácz, Anita; Héberger, Károly; Fodor, Marietta

    2016-09-01

    Almost a hundred commercially available energy drink samples from Hungary, Slovakia, and Greece were collected for the quantitative determination of their caffeine and sugar content with FT-NIR spectroscopy and high-performance liquid chromatography (HPLC). Calibration models were built with partial least-squares regression (PLSR). An HPLC-UV method was used to measure the reference values for caffeine content, while sugar contents were measured with the Schoorl method. Both the nominal sugar content (as indicated on the cans) and the measured sugar concentration were used as references. Although the Schoorl method has larger error and bias, appropriate models could be developed using both references. The validation of the models was based on sevenfold cross-validation and external validation. FT-NIR analysis is a good candidate to replace the HPLC-UV method, because it is much cheaper than any chromatographic method, while it is also more time-efficient. The combination of FT-NIR with multidimensional chemometric techniques like PLSR can be a good option for the detection of low caffeine concentrations in energy drinks. Moreover, three types of energy drinks that contain (i) taurine, (ii) arginine, and (iii) none of these two components were classified correctly using principal component analysis and linear discriminant analysis. Such classifications are important for the detection of adulterated samples and for quality control, as well. In this case, more than a hundred samples were used for the evaluation. The classification was validated with cross-validation and several randomization tests (X-scrambling). Graphical Abstract The way of energy drinks from cans to appropriate chemometric models.

  13. Quantitative Determination of Serum Proteins in Persons Occupationally Exposed to Radar

    International Nuclear Information System (INIS)

    Kasuba, V.; Garaj-Vrhovac, V.

    1998-01-01

    Radio-wave communications are used extensively in the modern society. We are all subject to radio frequency radiation (RFR) created by a radio, television, wireless telephony, emergency communications, and radar. The interest in the health effects of RFR has been motivated the rapid growth in wireless communications. Recently, many investigations are headed to the influence of nonionizing electromagnetic radiation to people. The interpretation of nonionizing radiation effects depends on apsorption characteristics of biological material and on thermoregulative system of exposed persons. This article includes serum protein analysis of 14 people who work in a radar zone. All the examinees are men aged 39 in average. The average exposure period in the radar zone was 16 years (twelve hours each second day). Human serum proteins in all samples were detected by electrophoresis on cellulose acetate membranes (Cellogel 500, Chemeton, Italy) in sodium-Veronal-Veronal-TRIS buffer pH 8.6. The duration of electrophoresis was two hours at 130-140 V at 11 cm bridge. Electroferograms were stained with 0.1 % Ponceau,s (w/v) (Chemetron, Italy) in 5% trichloracetic acid (v/v). Quantitative determination, i.e. densitometry of five serum protein fractions (albumin, α 1 - , α 2 - , β 1 - and γ -globulin) was carried out by photometry at multipolar densitometer. The results show gradual decrease of albumin 58.0 - 44.0 g/l versus control (64.05 g/l), except in three examinees where the values were almost equal to the normal value. One can also observe the changes in γ -globulin levels. All examinees except one showed increase in g -globulin levels (19.0 - 30.0 g/l vs. normal 15.0 g/l). The effect of nonionizing electromagnetic and microwave radiation on those who work in related field certainly needs much more investigation. (author)

  14. Prognostic Role of Methylation Status of the MGMT Promoter Determined Quantitatively by Pyrosequencing in Glioblastoma Patients.

    Science.gov (United States)

    Kim, Dae Cheol; Kim, Ki Uk; Kim, Young Zoon

    2016-01-01

    This study investigated whether pyrosequencing can be used to determine the methylation status of the MGMT promoter as a clinical biomarker using relatively old archival tissue samples of glioblastoma. We also examined other prognostic factors for survival of glioblastoma patients. The available study set included formalin-fixed paraffin-embedded (FFPE) tissue from 104 patients at two institutes from 1997 to 2012, all of which were diagnosed histopathologically as glioblastoma. Clinicopathologic data were collected by review of medical records. For pyrosequencing analysis, the PyroMark Q96 CpG MGMT kit (Qiagen, Hilden, Germany) was used to detect the level of methylation at exon 1 positions 17-39 of the MGMT gene, which contains 5 CpGs. Methylation of the MGMT promoter was detected in 43 (41.3%) of 104 samples. The average percentage methylation was 14.0±16.8% overall and 39.0±14.7% for methylated cases. There was no significant pattern of linear increase or decrease according to the age of the FFPE block (p=0.687). In multivariate analysis, age, performance status, extent of surgery, method of adjuvant therapy, and methylation status estimated by pyrosequencing were independently associated with overall survival. Additionally, patients with a high level of methylation survived longer than those with low methylation (p=0.016). In this study, the status and extent of methylation of the MGMT promoter analyzed by pyrosequencing were associated with overall survival in glioblastoma patients. Pyrosequencing is a quantitative method that overcomes the problems of MSP and a simple technique for accurate analysis of DNA sequences.

  15. Quantitative 3D Determination of Radiosensitization by Bismuth-Based Nanoparticles.

    Science.gov (United States)

    Alqathami, Mamdooh; Blencowe, Anton; Geso, Moshi; Ibbott, Geoffrey

    2016-03-01

    The nanoparticle-induced dose enhancement effect has been shown to improve the therapeutic efficacy of ionizing radiation in external beam radiotherapy. Whereas previous studies have focused on gold nanoparticles (AuNPs), no quantitative studies have been conducted to investigate the potential superiority of other high atomic number (Z) nanomaterials such as bismuth-based nanoparticles. The aims of this study were to experimentally validate and quantify the dose enhancement properties of commercially available bismuth-based nanoparticles (bismuth oxide (Bi2O3-NPs) and bismuth sulfide (Bi2S3-NPs)), and investigate their potential superiority over AuNPs in terms of radiation dose enhancement. Phantom cuvettes doped with and without nanoparticles where employed for measuring radiation dose enhancement produced from the interaction of radiation with metal nanoparticles. Novel 3D phantoms were employed to investigate the 3D spatial distribution of ionising radiation dose deposition. The phantoms were irradiated with kilovoltage and megavoltage X-ray beams and optical absorption changes were measured using a spectrophotometer and optical CT scanner. The radiation dose enhancement factors (DEFs) obtained for 50 nm diameter Bi2O3-NPs and AuNPs were 1.90 and 1.77, respectively, for 100 kV energy and a nanoparticle concentration of 0.5 mM. In addition, the DEFs of 5 nm diameter Bi2S3-NPs and AuNPs were determined to be 1.38 and 1.51, respectively, for 150 kV energy and a nanoparticle concentration of 0.25 mM. The results demonstrate that both bismuth-based nanoparticles can enhance the effects of radiation. For 6 MV energy the DEFs for all the investigated nanoparticles were lower (< 15%) than with kilovoltage energy.

  16. Quantitative Analysis by Isotopic Dilution Using Mass Spectroscopy: The Determination of Caffeine by GC-MS.

    Science.gov (United States)

    Hill, Devon W.; And Others

    1988-01-01

    Describes a laboratory technique for quantitative analysis of caffeine by an isotopic dilution method for coupled gas chromatography-mass spectroscopy. Discusses caffeine analysis and experimental methodology. Lists sample caffeine concentrations found in common products. (MVL)

  17. FTIR as an easy and fast analytical approach to follow up microbial growth during fungal pretreatment of poplar wood with **Phanerochaete chrysosporium**

    OpenAIRE

    Cornet, I.; Wittner, N.; Tofani, G.; Tavernier, S.

    2018-01-01

    Abstract: Since the determination of the fermentation kinetics is one of the main challenges in solid state fermentation, the quantitative measurement of biomass growth during microbial pretreatment by FTIR spectroscopy in Attenuated Total Reflectance mode was evaluated. Peaks at wave numbers of 1651 cm−1 and 1593 cm−1 showed to be affected during pretreatment of poplar wood particles by Phanerochaete chrysosporium MUCL 19343. Samples with different microbial biomass fractions were obtained f...

  18. Nucleation and initial growth of atomic layer deposited titanium oxide determined by spectroscopic ellipsometry and the effect of pretreatment by surface barrier discharge

    Energy Technology Data Exchange (ETDEWEB)

    Cameron, David C., E-mail: dccameron@mail.muni.cz [R& D Centre for Low-Cost Plasma and Nanotechnology Surface Modification, Masaryk University, Kotlářská 267/2, 611 37 Brno (Czech Republic); Krumpolec, Richard, E-mail: richard.krumpolec@fmph.uniba.sk [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Mlynská dolina, 842 4 Bratislava (Slovakia); Ivanova, Tatiana V., E-mail: tatiana.ivanova@lut.fi [ASTRaL team, Laboratory of Green Chemistry, Lappeenranta University of Technology, Sammonkatu 12, 50130 Mikkeli (Finland); Homola, Tomáš, E-mail: tomas.homola@mail.muni.cz [R& D Centre for Low-Cost Plasma and Nanotechnology Surface Modification, Masaryk University, Kotlářská 267/2, 611 37 Brno (Czech Republic); Černák, Mirko, E-mail: cernak@physics.muni.cz [R& D Centre for Low-Cost Plasma and Nanotechnology Surface Modification, Masaryk University, Kotlářská 267/2, 611 37 Brno (Czech Republic)

    2015-08-01

    Highlights: • Spectroscopic ellipsometry shows initial nucleation and growth process in atomic layer deposited titanium dioxide. • Quantum confinement effects were used to measure evolution of crystallite size. • Crystallite surface density can be extracted from ellipsometric surface roughness data and crystallite size. • Pretreatment of silicon substrates by diffuse coplanar surface barrier discharge has only minor effects on titanium dioxide film nucleation and growth. - Abstract: This paper reports on the use of spectroscopic ellipsometry to characterise the initial nucleation stage of the atomic layer deposition of the anatase phase of titanium dioxide on silicon substrates. Careful control and analysis of the ellipsometric measurements enables the determination of the evolution of crystallite diameter and surface density in the nucleation stage before a continuous film is formed. This growth behaviour is in line with atomic force microscopy measurements of the crystallite size. The crystallite diameter is a linear function of the number of ALD cycles with a slope of approximately 1.7 Å cycle{sup −1} which is equivalent to a layer growth rate of 0.85 Å cycle{sup −1} consistent with a ripening process which increases the crystallite size while reducing their density. The crystallite density decreases from ∼3 × 10{sup 17} m{sup −3} in the initial nucleation stages to ∼3 × 10{sup 15} m{sup −3} before the film becomes continuous. The effect of exposing the substrate to a diffuse coplanar surface barrier discharge in an air atmosphere before deposition was measured and only small differences were found: the plasma treated samples were slightly rougher in the initial stages and required a greater number of cycles to form a continuous film (∼80) compared to the untreated films (∼50). A thicker layer of native oxide was found after plasma treatment.

  19. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-04

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. A quantitative comparative analysis of Advancement via Independent Determination (AVID) in Texas middle schools

    Science.gov (United States)

    Reed, Krystal Astra

    The "Advancement via Individual Determination (AVID) program was designed to provide resources and strategies that enable underrepresented minority students to attend 4-year colleges" (AVID Center, 2013, p. 2). These students are characterized as the forgotten middle in that they have high test scores, average-to-low grades, minority or low socioeconomic status, and will be first-generation college students (AVID, 2011). Research indicates (Huerta, Watt, & Butcher, 2013) that strict adherence to 11 program components supports success of students enrolled in AVID, and AVID certification depends on districts following those components. Several studies (AVID Center, 2013) have investigated claims about the AVID program through qualitative analyses; however, very few have addressed this program quantitatively. This researcher sought to determine whether differences existed between student achievement and attendance rates between AVID and non-AVID middle schools. To achieve this goal, the researcher compared eighth-grade science and seventh- and eighth-grade mathematics scores from the 2007 to 2011 Texas Assessment of Knowledge and Skills (TAKS) and overall attendance rates in demographically equivalent AVID and non-AVID middle schools. Academic Excellence Indicator System (AEIS) reports from the Texas Education Agency (TEA) were used to obtain 2007 to 2011 TAKS results and attendance information for the selected schools. The results indicated a statistically significant difference between AVID demonstration students and non-AVID students in schools with similar CI. No statistically significant differences were found on any component of the TAKS for AVID economically disadvantaged students. The mean scores indicated an achievement gap between non-AVID and AVID demonstration middle schools. The findings from the other three research questions indicated no statistically significant differences between AVID and non-AVID student passing rates on the seventh- and eighth

  1. Pretreatment of the macroalgae Chaetomorpha linum for the production of bioethanol - Comparison of five pretreatment technologies

    DEFF Research Database (Denmark)

    Schultz-Jensen, Nadja; Thygesen, Anders; Thomsen, Sune Tjalfe

    2013-01-01

    -assisted pretreatment (PAP) and ball milling (BM), to determine effects of the pretreatment methods on the conversion of C. linum into ethanol by simultaneous saccharification and fermentation (SSF). WO and BM showed the highest ethanol yield of 44. g ethanol/100. g glucan, which was close to the theoretical ethanol......A qualified estimate for pretreatment of the macroalgae Chaetomorpha linum for ethanol production was given, based on the experience of pretreatment of land-based biomass. C. linum was subjected to hydrothermal pretreatment (HTT), wet oxidation (WO), steam explosion (STEX), plasma...... yield of 57. g ethanol/100. g glucan. A 64% higher ethanol yield, based on raw material, was reached after pretreatment with WO and BM compared with unpretreated C. linum, however 50% of the biomass was lost during WO. Results indicated that the right combination of pretreatment and marine macroalgae...

  2. Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

    Science.gov (United States)

    Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

    2004-01-01

    An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

  3. Quantitative determination of titin and nebulin in poultry meat by SDS-PAGE with an internal standard

    NARCIS (Netherlands)

    Tomaszewska Gras, J.; Kijowski,; Schreurs, F.J.G.

    2002-01-01

    The method of quantitative determination of titin and nebulin in chicken meat by SDS-PAGE electrophoresis technique was developed by application of β-galactosidase as the internal standard. The method was tested first on marker protein samples of known concentrations (myosin, transferrin, glutamic

  4. Hydrolysis Studies and Quantitative Determination of Aluminum Ions Using [superscript 27]Al NMR: An Undergraduate Analytical Chemistry Experiment

    Science.gov (United States)

    Curtin, Maria A.; Ingalls, Laura R.; Campbell, Andrew; James-Pederson, Magdalena

    2008-01-01

    This article describes a novel experiment focused on metal ion hydrolysis and the equilibria related to metal ions in aqueous systems. Using [superscript 27]Al NMR, the students become familiar with NMR spectroscopy as a quantitative analytical tool for the determination of aluminum by preparing a standard calibration curve using standard aluminum…

  5. The Role of Product Inhibition as a Yield-Determining Factor in Enzymatic High-Solid Hydrolysis of Pretreated Corn Stover

    DEFF Research Database (Denmark)

    Nymand Olsen, Søren; Borch, Kim; Cruys-Bagger, Nicolaj

    2014-01-01

    . The results suggest that the solid effect is mainly controlled by product inhibition under the given experimental conditions (washed pretreated corn stover as substrate). Cellobiose was found to be approximately 15 times more inhibitory than glucose on a molar scale. However, considering that glucose...

  6. Quantitative determination of pulmonary artery flow by scintiscanning in patients with mitral stenosis

    International Nuclear Information System (INIS)

    Carvalho, N.; Fujioka, T.; Dias Neto, A.; Papaleo Netto, M.

    1974-01-01

    In twenty-two patients with pure or predominant mitral stenosis, with pulmonary hypertension, the quantitative blood flow of the pulmonary artery systems through the distribution of macroaggregated radio-iodinated ( 131 I) albumin is studied, by pulmonary digital scanning. Through the relations ship between the radioactive concentration in each organ, it is possible to classify three types of images: normal, balanced and inverted. This technique is useful for quantitative analysis of pulmonary artery flow, as a test that should preced cardiac catheterization and in the follow-up of the surgical results [pt

  7. A Colorimetric Analysis Experiment Not Requiring a Spectrophotometer: Quantitative Determination of Albumin in Powdered Egg White

    Science.gov (United States)

    Charlton, Amanda K.; Sevcik, Richard S.; Tucker, Dorie A.; Schultz, Linda D.

    2007-01-01

    A general science experiment for high school chemistry students might serve as an excellent review of the concepts of solution preparation, solubility, pH, and qualitative and quantitative analysis of a common food product. The students could learn to use safe laboratory techniques, collect and analyze data using proper scientific methodology and…

  8. ANSI/ASHRAE/IES Standard 90.1-2013 Preliminary Determination: Quantitative Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Halverson, Mark A.; Rosenberg, Michael I.; Wang, Weimin; Zhang, Jian; Mendon, Vrushali V.; Athalye, Rahul A.; Xie, YuLong; Hart, Reid; Goel, Supriya

    2014-03-01

    This report provides a preliminary quantitative analysis to assess whether buildings constructed according to the requirements of ANSI/ASHRAE/IES Standard 90.1-2013 would result in energy savings compared with buildings constructed to ANSI/ASHRAE/IES Standard 90.1-2010.

  9. Rapid Quantitative Determination of Squalene in Shark Liver Oils by Raman and IR Spectroscopy.

    Science.gov (United States)

    Hall, David W; Marshall, Susan N; Gordon, Keith C; Killeen, Daniel P

    2016-01-01

    Squalene is sourced predominantly from shark liver oils and to a lesser extent from plants such as olives. It is used for the production of surfactants, dyes, sunscreen, and cosmetics. The economic value of shark liver oil is directly related to the squalene content, which in turn is highly variable and species-dependent. Presented here is a validated gas chromatography-mass spectrometry analysis method for the quantitation of squalene in shark liver oils, with an accuracy of 99.0 %, precision of 0.23 % (standard deviation), and linearity of >0.999. The method has been used to measure the squalene concentration of 16 commercial shark liver oils. These reference squalene concentrations were related to infrared (IR) and Raman spectra of the same oils using partial least squares regression. The resultant models were suitable for the rapid quantitation of squalene in shark liver oils, with cross-validation r (2) values of >0.98 and root mean square errors of validation of ≤4.3 % w/w. Independent test set validation of these models found mean absolute deviations of the 4.9 and 1.0 % w/w for the IR and Raman models, respectively. Both techniques were more accurate than results obtained by an industrial refractive index analysis method, which is used for rapid, cheap quantitation of squalene in shark liver oils. In particular, the Raman partial least squares regression was suited to quantitative squalene analysis. The intense and highly characteristic Raman bands of squalene made quantitative analysis possible irrespective of the lipid matrix.

  10. Quantitative determination of optical trapping strength and viscoelastic moduli inside living cells

    DEFF Research Database (Denmark)

    Mas, Josep; Richardson, Andrew Callum; Reihani, S. Nader S.

    2013-01-01

    is viscoelastic, it would be incorrect to use a calibration procedure relying on a viscous environment. Here we demonstrate a method to perform a correct force calibration inside a living cell. This method (theoretically proposed in Fischer and Berg-Sørensen (2007 J. Opt. A: Pure Appl. Opt. 9 S239)) takes......With the success of in vitro single-molecule force measurements obtained in recent years, the next step is to perform quantitative force measurements inside a living cell. Optical traps have proven excellent tools for manipulation, also in vivo, where they can be essentially non-invasive under...... correct wavelength and exposure conditions. It is a pre-requisite for in vivo quantitative force measurements that a precise and reliable force calibration of the tweezers is performed. There are well-established calibration protocols in purely viscous environments; however, as the cellular cytoplasm...

  11. Quantitative determination of the intensities of known components in spectra obtained from surface analytical techniques

    International Nuclear Information System (INIS)

    Nelson, G.C.

    1984-01-01

    Linear least-squares methods have been used to quantitatively decompose experimental data obtained from surface analytical techniques into its separate components. The mathematical procedure for accomplishing this is described and examples are given of the use of this method with data obtained from Auger electron spectroscopy [both N(E) and derivative], x-ray photoelectron spectroscopy, and low energy ion scattering spectroscopy. The requirements on the quality of the data are discussed

  12. Copper quantitative determination in soils and rocks by the spectrophotometric method

    International Nuclear Information System (INIS)

    Jardim, G.S.

    1982-01-01

    Soil samples were collected and processed according to recommended techniques. A copper standard solution was prepared. Qualitative and quantitative analyses of copper were carried out by paper chromatography, choosing rubeanic acid as the most adequate developer solution, and by spectrophotometry, respectively. The results showed a variation from 3.6 ppm to 22.2 ppm of copper in the soils analysed. (C.L.B.) [pt

  13. Quantitative determination of cyclobutane thymine dimers in DNA by stable isotope-dilution mass spectrometry

    International Nuclear Information System (INIS)

    Podmore, I.D.; Cooke, M.S.; Herbert, K.E.; Lunec, J.

    1996-01-01

    In order to understand the role of UV-induced DNA lesions in biological processes such as mutagenesis and carcinogenesis, it is essential to detect and quantify DNA damage in cells. In this paper we present a novel and both highly selective and sensitive assay using capillary gas chromatography (GC) combined with mass spectrometry (MS) for the detection and accurate quantitation of a major product of UV-induced DNA damage (cis-syb cyclobutadithymine). Quantitation of the cyclobutane thymine dimer was achieved by the use of an internal standard in the form of a stable 2 H-labeled analogue. Both isotopically labeled and nonlabeled dimers were prepared directly from their corresponding monomers. Each was identified as their trimethylsilyl ether derivative by GC-MS. Calibration plots were obtained for known quantities of both nonlabeled and analyte and internal standard. Quantitation of cis-syn cyclobutadithymine was demonstrated in DNA exposed to UVC radiation over a dose range of 0 3500 J m -2 . Under the conditions used, the limit of detection was found to be 20-50 fmol on column (equivalent to 0.002-0.005 nmol dimer per mg DNA). The results of the present study indicate that capillary GC-MS is an ideally suited technique for selective and sensitive quantification of cis-syn cyclobutadithymine in DNA and hence UV-induced DNA damage. (author)

  14. X-ray fluorescence-based method for the quantitative determination of uranium in the aqueous solutions

    Science.gov (United States)

    Dubrovka, S.; Chursin, S.; Verkhoturova, V.

    2017-01-01

    Currently, one of the important issues in the field of nuclear technology is providing special handling with respect to nuclear materials, due to their energy and commercial significancy, as well as their potential radiation contamination threat. There is a necessity to have information about the full qualitative and quantitative composition of the sample as a part of special handling with nuclear materials. Spectrometric methods solve this problem effectively. One of these methods is the X-ray fluorescence analysis, which is fast, nondestructive and environmentally friendly with a high accuracy and reproducibility of the results. Development of uranium quantitative determination method in aqueous solutions to solve the problems of accounting and control of nuclear materials is the subject of research in this article. The development of the uranium concentration determination method in the aqueous solutions of uranyl nitrate UO2(NO3)2 was carried out using Spectroscan MAKC-G - wavelength dispersive crystal diffraction XRF spectrometer.

  15. Quantitative performance of a quadrupole-orbitrap-MS in targeted LC-MS determinations of small molecules.

    Science.gov (United States)

    Grund, Baptiste; Marvin, Laure; Rochat, Bertrand

    2016-05-30

    High-resolution mass spectrometry (HRMS) has been associated with qualitative and research analysis and QQQ-MS with quantitative and routine analysis. This view is now challenged and for this reason, we have evaluated the quantitative LC-MS performance of a new high-resolution mass spectrometer (HRMS), a Q-orbitrap-MS, and compared the results obtained with a recent triple-quadrupole MS (QQQ-MS). High-resolution full-scan (HR-FS) and MS/MS acquisitions have been tested with real plasma extracts or pure standards. Limits of detection, dynamic range, mass accuracy and false positive or false negative detections have been determined or investigated with protease inhibitors, tyrosine kinase inhibitors, steroids and metanephrines. Our quantitative results show that today's available HRMS are reliable and sensitive quantitative instruments and comparable to QQQ-MS quantitative performance. Taking into account their versatility, user-friendliness and robustness, we believe that HRMS should be seen more and more as key instruments in quantitative LC-MS analyses. In this scenario, most targeted LC-HRMS analyses should be performed by HR-FS recording virtually "all" ions. In addition to absolute quantifications, HR-FS will allow the relative quantifications of hundreds of metabolites in plasma revealing individual's metabolome and exposome. This phenotyping of known metabolites should promote HRMS in clinical environment. A few other LC-HRMS analyses should be performed in single-ion-monitoring or MS/MS mode when increased sensitivity and/or detection selectivity will be necessary. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Quantitative determination of anisotropic magnetoelectric coupling in BiFeO$_{3}$-CoFe$_{2}$O$_{4}$ nanostructures

    OpenAIRE

    Oh, Yoon Seok; Crane, S.; Zheng, H.; Chu, Y. H.; Ramesh, R.; Kim, Kee Hoon

    2010-01-01

    The transverse and longitudinal magnetoelectric susceptibilities (MES) were quantitatively determined for (001) heteroepitaxial BiFeO$_{3}$-CoFe$_{2}$O$_{4}$ nanostructures. Both of these MES values were sharply enhanced at magnetic fields below 6 kOe and revealed asymmetric lineshapes with respect to the dc magnetic field, demonstrating the strain-induced magnetoelectric effect. The maximum transverse MES, which reached as high as $\\sim$60 mV/cm Oe, was about five times larger than the longi...

  17. Methods for pretreating biomass

    Science.gov (United States)

    Balan, Venkatesh; Dale, Bruce E; Chundawat, Shishir; Sousa, Leonardo

    2017-05-09

    A method for pretreating biomass is provided, which includes, in a reactor, allowing gaseous ammonia to condense on the biomass and react with water present in the biomass to produce pretreated biomass, wherein reactivity of polysaccharides in the biomass is increased during subsequent biological conversion as compared to the reactivity of polysaccharides in biomass which has not been pretreated. A method for pretreating biomass with a liquid ammonia and recovering the liquid ammonia is also provided. Related systems which include a biochemical or biofuel production facility are also disclosed.

  18. A quantitative method for determination of aflatoxin B in roasted corn.

    Science.gov (United States)

    Shannon, G M; Shotwell, O L

    1975-07-01

    Roasting aflatoxin-contaminated corn will reduce toxin levels. A quantitative analysis for aflatoxin in roasted corn has been developed by modifying a cleanup technique for green coffee extracts approved as official first action by the AOAC. A chloroform extract is partially purified on a Florisil column, and thin layer chromatographic (TLC) plates are developed with methylene chloride-chloroform-isoamyl alcohol-formic acid (81+15+3+1). Recoveries average 101% and the sensitivity limit is 5 ppb aflatoxin B1. A 2-dimensional TLC procedure can also be used to separate the aflatoxins from background interferences.

  19. Simultaneous, simple and rapid determination of five bioactive free anthraquinones in Radix et Rhizoma Rhei by quantitative 1H NMR

    International Nuclear Information System (INIS)

    Dong, Jian-Wei; Cai, Le; Fang, Yun-Shan; Duan, Wei-He; Li, Zhen-Jie; Ding, Zhong-Tao

    2016-01-01

    Radix et Rhizoma Rhei has been recognized for centuries in traditional medicine for its multiple pharmacological actions. The free anthraquinones including physcion, chrysophanol, emodin, rhein, and aloe-emodin are the main bioactive components in Radix et Rhizoma Rhei. In the present study, a fast quantitative 1 H nuclear magnetic resonance (q-HNMR) method for the determination and quantitation of five free anthraquinones in Radix et Rhizoma Rhei was developed. Validation of the quantitative method was performed in terms of specificity, accuracy, precision, and stability. The results showed that the solvent acetone-d 6 enabled satisfactory separation of the signals to be integrated. Five anthraquinones in Radix et Rhizoma Rhei could be quantified accurately using featured signals from 1 H NMR. This work implied that q-HNMR represents a feasible alternative to high-performance liquid chromatography (HPLC)-based methods for quantitation of anthraquinones in Radix et Rhizoma Rhei and is suitable for the quality control of Radix et Rhizoma Rhei. (author)

  20. Quantitative 1H-NMR Method for the Determination of Tadalafil in Bulk Drugs and its Tablets

    Directory of Open Access Journals (Sweden)

    Qingyun Yang

    2015-07-01

    Full Text Available A simple, rapid, accurate, and selective quantitative nuclear magnetic resonance method for the determination of tadalafil in bulk drugs and its tablets was established and evaluated. Spectra were obtained in dimethylsulfoxide-d6 using 2,4-dinitrotoluene as the internal standard. In this study, the method’s linearity, range, limit of quantification, stability, precision, and accuracy were validated. The results were consistent with those obtained from high-performance liquid chromatography analysis. Thus, the proposed method is a useful and practical tool for the determination of tadalafil in bulk drugs and its tablets.

  1. Orientation order and rotation mobility of nitroxide biradicals determined by quantitative simulation of EPR spectra.

    Science.gov (United States)

    Bogdanov, Alexey V; Vorobiev, Andrey Kh

    2016-11-16

    The problem of quantitative numerical simulation of electron paramagnetic resonance (EPR) spectra of biradical probes in both isotropic and aligned media was solved for the first time. The models suitable for the description of the spectra of the probes, both in the rigid limit and in the presence of rotational motions, were developed and successfully applied to model systems. The simulation of EPR spectra allows obtaining the following information about the molecular structure and dynamics: the values of orientation order parameters, the type of rotation mobility and its quantitative characteristics, and the sign and value of the spin exchange constant of the biradical. Model systems used in this work include solutions of nitroxide biradicals in a viscous solvent (squalane) in the range of temperatures 100-370 K and in the aligned liquid crystal n-octylcyanobiphenyl (8CB, 100-298.5 K). Unexpectedly, it was found that in 8CB the main orientation axis of the biradical molecule is perpendicular to the longest molecular axis.

  2. Quantitative determination of elemental sulfur at the arsenopyrite surface after oxidation by ferric iron: mechanistic implications

    Directory of Open Access Journals (Sweden)

    Hamers Robert J

    2001-07-01

    Full Text Available The elemental sulfur formed at the arsenopyrite surface after oxidation by ferric iron was quantitatively measured by extraction in perchloroethylene and subsequent quantitative analysis by HPLC. Reactions with ferric iron in perchloric acid solutions or in sulfuric acid solutions (both at pH = 1 and 42°C, which approximate extreme acid mine drainage conditions produced elemental sulfur in quantities greater than 50% of the total reacted sulfur. The controversy surrounding the mechanism of the oxidative dissolution of arsenopyrite is discussed in light of these measurements. Based on the observation of greater than 50% production of elemental sulfur, a mechanism by which all the sulfur from the mineral proceeds through thiosulfate can be eliminated as a possible description of the dissolution of arsenopyrite. Instead, it is likely the other constituents of the mineral lattice, Fe and As, are leached out, leaving behind a S0 lattice. Nucleation reactions will then result in the formation of stable S8 rings.

  3. Use of near-infrared spectrometry for quantitative determinations of selamectin and moisture in topical formulations.

    Science.gov (United States)

    Webster, Gregory K; Farrand, Douglas A; Johnson, Erin; Litchman, Mark A; Broad, Neville; Maris, Simon

    2003-09-15

    A rapid near-infrared spectrometric (NIR) method was qualified for use with the quantitative analysis of selamectin and moisture in topical formulations. Selamectin is currently marketed as a pet endectocide and is available in several formulations for cats and dogs. The use of NIR in this investigation replaces the in-process testing by liquid chromatography and concurrently provided moisture content that would otherwise only be available with additional Karl Fischer titration investigations. A seven-factor partial least square regression (PLS) of the second derivative spectra encompassing the wavelength region of 1450-2200 nm was used to quantify both selamectin and moisture content. A second three-factor PLS solely for water content was also applied and compared with the full model. This qualification confirms that this method may be used to quantitate selamectin and moisture as a process tool or to examine finished good samples. Each sample can be rapidly analyzed within 5 min on the current bench top system.

  4. Acceptability criteria for linear dependence in validating UV-spectrophotometric methods of quantitative determination in forensic and toxicological analysis

    Directory of Open Access Journals (Sweden)

    L. Yu. Klimenko

    2014-08-01

    Full Text Available Introduction. This article is the result of authors’ research in the field of development of the approaches to validation of quantitative determination methods for purposes of forensic and toxicological analysis and devoted to the problem of acceptability criteria formation for validation parameter «linearity/calibration model». The aim of research. The purpose of this paper is to analyse the present approaches to acceptability estimation of the calibration model chosen for method description according to the requirements of the international guidances, to form the own approaches to acceptability estimation of the linear dependence when carrying out the validation of UV-spectrophotometric methods of quantitative determination for forensic and toxicological analysis. Materials and methods. UV-spectrophotometric method of doxylamine quantitative determination in blood. Results. The approaches to acceptability estimation of calibration models when carrying out the validation of bioanalytical methods is stated in international papers, namely «Guidance for Industry: Bioanalytical method validation» (U.S. FDA, 2001, «Standard Practices for Method Validation in Forensic Toxicology» (SWGTOX, 2012, «Guidance for the Validation of Analytical Methodology and Calibration of Equipment used for Testing of Illicit Drugs in Seized Materials and Biological Specimens» (UNODC, 2009 and «Guideline on validation of bioanalytical methods» (ЕМА, 2011 have been analysed. It has been suggested to be guided by domestic developments in the field of validation of analysis methods for medicines and, particularly, by the approaches to validation methods in the variant of the calibration curve method for forming the acceptability criteria of the obtained linear dependences when carrying out the validation of UV-spectrophotometric methods of quantitative determination for forensic and toxicological analysis. The choice of the method of calibration curve is

  5. Steroidal saponins from Yucca gloriosa L. rhizomes: LC-MS profiling, isolation and quantitative determination.

    Science.gov (United States)

    Skhirtladze, Alexandre; Perrone, Angela; Montoro, Paola; Benidze, Mariam; Kemertelidze, Ether; Pizza, Cosimo; Piacente, Sonia

    2011-01-01

    The occurrence of steroidal saponins in the rhizomes of Yucca gloriosa has been detected by LC-MS. On the basis of the LC-MS analysis, five steroidal glycosides, including three spirostane, one furostane and one cholestane glycosides, along with seven known compounds have been isolated and characterized by ESI-MS and by the extensive use of 1D- and 2D-NMR experiments. Quantitative analysis of the steroidal glycosides in Y. gloriosa rhizomes was performed by an LC-MS method validated according to European Medicines Agency (EMEA) guidelines. The dried BuOH extract obtained from rhizomes contains more than 25% w/w of glycosides, thus Y. gloriosa rhizomes can be considered a rich source of steroidal glycosides. Copyright © 2010 Elsevier Ltd. All rights reserved.

  6. Establishment of a quantitative ELISA capable of determining peptide - MHC class I interaction

    DEFF Research Database (Denmark)

    Sylvester-Hvid, C; Kristensen, N; Blicher, T

    2002-01-01

    Many different assays for measuring peptide-MHC interactions have been suggested over the years. Yet, there is no generally accepted standard method available. We have recently generated preoxidized recombinant MHC class I molecules (MHC-I) which can be purified to homogeneity under denaturing...... conditions (i.e., in the absence of any contaminating peptides). Such denatured MHC-I molecules are functional equivalents of "empty molecules". When diluted into aqueous buffer containing beta-2 microglobulin (beta2m) and the appropriate peptide, they fold rapidly and efficiently in an entirely peptide...... dependent manner. Here, we exploit the availability of these molecules to generate a quantitative ELISA-based assay capable of measuring the affinity of the interaction between peptide and MHC-I. This assay is simple and sensitive, and one can easily envisage that the necessary reagents, standards...

  7. [Quantitative determination of glass content in monazite glass-ceramics by IR technique].

    Science.gov (United States)

    He, Yong; Zhang, Bao-min

    2003-04-01

    Monazite glass-ceramics consist of both monazite and metaphoshate glass phases. The absorption bands of both phases do not overlap each other, and the absorption intensities of bands 1,275 and 616 cm-1 vary with the glass contents. The correlation coefficient between logarithmic absorbance ratio of the two bands and glass contents was r = 0.9975 and its regression equation was y = 48.356 + 25.93x. The absorbance ratio of bands 952 and 616 cm-1 also varied with different ratios of Ce2O3/La2O3 in synthetic monazites, with r = 0.9917 and a regression equation y = 0.2211 exp (0.0221x). High correlation coefficients show that the IR technique could find new application in the quantitative analysis of glass content in phosphate glass-ceramics.

  8. Automatized image processing of bovine blastocysts produced in vitro for quantitative variable determination

    Science.gov (United States)

    Rocha, José Celso; Passalia, Felipe José; Matos, Felipe Delestro; Takahashi, Maria Beatriz; Maserati, Marc Peter, Jr.; Alves, Mayra Fernanda; de Almeida, Tamie Guibu; Cardoso, Bruna Lopes; Basso, Andrea Cristina; Nogueira, Marcelo Fábio Gouveia

    2017-12-01

    There is currently no objective, real-time and non-invasive method for evaluating the quality of mammalian embryos. In this study, we processed images of in vitro produced bovine blastocysts to obtain a deeper comprehension of the embryonic morphological aspects that are related to the standard evaluation of blastocysts. Information was extracted from 482 digital images of blastocysts. The resulting imaging data were individually evaluated by three experienced embryologists who graded their quality. To avoid evaluation bias, each image was related to the modal value of the evaluations. Automated image processing produced 36 quantitative variables for each image. The images, the modal and individual quality grades, and the variables extracted could potentially be used in the development of artificial intelligence techniques (e.g., evolutionary algorithms and artificial neural networks), multivariate modelling and the study of defined structures of the whole blastocyst.

  9. Simultaneous quantitative determination of cinnamaldehyde and methyl eugenol from stem bark of Cinnamomum zeylanicum Blume using RP-HPLC.

    Science.gov (United States)

    Gursale, Atish; Dighe, Vidya; Parekh, Guarang

    2010-01-01

    A simple, sensitive, and precise reversed-phase high performance liquid chromatographic (HPLC) method has been developed, validated and used for simultaneous quantitative determination of cinnamaldehyde and methyl eugenol from the methanolic extract of dried bark powder of Cinnamomum zeylanicum Blume (family Lauraceae). The ultrasonic extraction method was used for the extraction of these compounds. The reversed-phase HPLC analysis was carried out using a Intersil ODS-3V-C(18) (150 mm x 4.6 mm, 5 microm) column and a mobile phase comprising of methanol-acetonitrile-water in the volume ratio of 35:20:45, delivered at a flow rate of 1.0 cm(3)/min. The detection and quantitation of both the compounds was carried out at 221 nm.

  10. Pretreatment of microbial sludges

    Science.gov (United States)

    Rivard, Christopher J.; Nagle, Nicholas J.

    1995-01-01

    Methods are described for pretreating microbial sludges to break cells and disrupt organic matter. One method involves the use of sonication, and another method involves the use of shear forces. The pretreatment of sludge enhances bioconversion of the organic fraction. This allows for efficient dewatering of the sludge and reduces the cost for final disposal of the waste.

  11. Quantitative phase determination by X-ray diffractometry in electrofused calcium aluminate cements

    International Nuclear Information System (INIS)

    Zanetti, S.M.; Franco, M.B.; Splettstoser Junior, J.; Placido, W.F.

    1989-01-01

    The knowledge of the percentual composition of phases in calcium aluminate cements and clinkers is of great importance to foresight the behaviour of the cement and refractory concretes made thereof. There are some analytical techniques for these determinations, optical and eletronic microscopy as well as selective chemical attacks, each technique presenting its own difficulties. Using pure phases of CA, CA 2 , C 2 AS and C 12 A 7 obtained by electrofusion in a laboratory electric are furnace, calibration curves were developed for X-ray diffratometric determination of phases. The method is very efficient for determination of CA, CA 2 , C 2 AS and ∝ - A1 2 O 3 . The determination of C 12 A 7 presents some variations due to its low concentration in electrofused clinkers. The method finds practical application in quality control of calcium aluminate cements [pt

  12. Quantitative method of determining beryllium or a compound thereof in a sample

    Science.gov (United States)

    McCleskey, T. Mark; Ehler, Deborah S.; John, Kevin D.; Burrell, Anthony K.; Collis, Gavin E.; Minogue, Edel M.; Warner, Benjamin P.

    2010-08-24

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  13. Quantitative determination of uranium in organic solution by X-ray fluorescence

    International Nuclear Information System (INIS)

    Leyt, D.V. de; Colangelo, C.H.

    1987-01-01

    An X-ray fluorescent method for the determination of uranium in tributilphosphate-kerosene-nitriacid solution has been developed. Chemical properties of the matrix elements were studied in order to select a convenient procedure to determine samples and standards on the same way. The method avoids the destruction of the organic material and has proved to be very useful for the fast control of uranium concentration. (Author) [es

  14. Socioeconomic factors that determine the phenomenon of\\ud migration in current Greece: a quantitative approach

    OpenAIRE

    Karli, Chrysoula

    2016-01-01

    This doctoral thesis commences with a meticulous examination on whether financial, social and institutional determinants associate with the migration performance in Europe and accordingly in Greece. Motivated by the intensity, the magnitude and the financial recession, this thesis presents three empirical chapters on the examination of the determinants that affect the phenomenon of migration. Prior to these three empirical studies a chapter introduces and defines all the variables used as wel...

  15. Quantitative determination of americium and curium in solutions using potassium tungstophosphate

    International Nuclear Information System (INIS)

    Chistyakov, V.M.; Baranov, A.A.; Erin, E.A.; Timoaeev, G.A.

    1990-01-01

    Two methods of americium (4) and curium (4) titration-replacement and redox ones - have been considered. According to the replacement method thorium nitrate solution was used as a titrant and the final point of titration was determined spectophotometrically. Using the method developed, on the basis of experimental data, the composition of thorium (4) complex with potassium tungstophosphate was determined. In case of the redox titration sodium nitrite was used, and the final titration point was indicated either spectrophotometrically or potentiometrically

  16. Carbonic Acid Pretreatment of Biomass

    Energy Technology Data Exchange (ETDEWEB)

    G. Peter van Walsum; Kemantha Jayawardhana; Damon Yourchisin; Robert McWilliams; Vanessa Castleberry

    2003-05-31

    acid compared to water alone. 6) Determine optimal conditions for carbonic acid pretreatment of aspen wood. Optimal severities appeared to be in the mid range tested. ASPEN-Plus modeling and economic analysis of the process indicate that the process could be cost competitive with sulfuric acid if the concentration of solids in the pretreatment is maintained very high (~50%). Lower solids concentrations result in larger reactors that become expensive to construct for high pressure applications.

  17. Comparing the soil quality changes of different land uses determined by two quantitative methods.

    Science.gov (United States)

    Fu, Bo-jie; Liu, Shi-liang; Lu, Yi-he; Chen, Li-ding; Ma, Ke-ming; Liu, Guo-hua

    2003-03-01

    Soil quality is one of the most important environmental factors in sustaining the global biosphere and developing sustainable agricultural practices. A study was initiated in Wolong Nature Reserve, Sichuan Province, China to elucidate the soil quality changes of natural secondary succession, forest planting and agricultural practices after deforestation in the humid mountainous region. The soil qualities of six land use types (natural forestland, grassland, shrub land, secondary forestland, cultivated land and reforested land) were compared using two quantitative methods: the integrated soil quality index (QI) and soil deterioration index (DI). The QI values of natural forestland, grassland, shrub land, secondary forestland, cultivated land, reforested land were 0.8039, 0.3277, 0.9127, 0.6881, 0.0285 and 0.3183, respectively. The DI values were 0%, -14%, 12%, 1%, -26% and -18% respectively. Both indexes suggested that shrub land can restore soil properties. To compare the two methods more directly, a deduced index QI' based on QI value was developed. The results showed that DI and QI' had a very high linear correlation coefficient (r = 0.9775) despite the values were different. Both methods were efficient in evaluating the soil quality levels and DI was a more simple way in soil quality assessment, while QI could show more ecological meanings.

  18. Quantitative enzyme activity determination with zeptomole sensitivity by microfluidic gradient-gel zymography.

    Science.gov (United States)

    Hughes, Alex J; Herr, Amy E

    2010-05-01

    We describe a sensitive zymography technique that utilizes an automated microfluidic platform to report enzyme molecular weight, amount, and activity (including k(cat) and K(m)) from dilute protein mixtures. Calf intestinal alkaline phosphatase (CIP) is examined in detail as a model enzyme system, and the method is also demonstrated for horseradish peroxidase (HRP). The 40 min assay has a detection limit of 5 zmol ( approximately 3 000 molecules) of CIP. Two-step pore-limit electrophoresis with enzyme assay (PLENZ) is conducted in a single, straight microchannel housing a polyacrylamide (PA) pore-size gradient gel. In the first step, pore limit electrophoresis (PLE) sizes and pseudoimmobilizes resolved proteins. In the second step, electrophoresis transports both charged and neutral substrates into the PLE channel to the entrapped proteins. Arrival of substrate at the resolved enzyme band generates fluorescent product that reveals enzyme molecular weight against a fluorescent protein ladder. Additionally, the PLENZ zymography assay reports the kinetic properties of CIP in a fully quantitative manner. In contrast to covalent enzyme immobilization, physical pseudoimmobilization of CIP in the PA gel does not significantly reduce its maximum substrate turnover rate. However, an 11-fold increase in the Michaelis constant (over the free solution value) is observed, consistent with diffusional limitations on substrate access to the enzyme active site. PLENZ offers a robust platform for rapid and multiplexed functional analysis of heterogeneous protein samples in drug discovery, clinical diagnostics, and biocatalyst engineering.

  19. Determination of a quantitative parameter to evaluate swimming technique based on the maximal tethered swimming test.

    Science.gov (United States)

    Soncin, Rafael; Mezêncio, Bruno; Ferreira, Jacielle Carolina; Rodrigues, Sara Andrade; Huebner, Rudolf; Serrão, Julio Cerca; Szmuchrowski, Leszek

    2017-06-01

    The aim of this study was to propose a new force parameter, associated with swimmers' technique and performance. Twelve swimmers performed five repetitions of 25 m sprint crawl and a tethered swimming test with maximal effort. The parameters calculated were: the mean swimming velocity for crawl sprint, the mean propulsive force of the tethered swimming test as well as an oscillation parameter calculated from force fluctuation. The oscillation parameter evaluates the force variation around the mean force during the tethered test as a measure of swimming technique. Two parameters showed significant correlations with swimming velocity: the mean force during the tethered swimming (r = 0.85) and the product of the mean force square root and the oscillation (r = 0.86). However, the intercept coefficient was significantly different from zero only for the mean force, suggesting that although the correlation coefficient of the parameters was similar, part of the mean velocity magnitude that was not associated with the mean force was associated with the product of the mean force square root and the oscillation. Thus, force fluctuation during tethered swimming can be used as a quantitative index of swimmers' technique.

  20. DNA internal standard for the quantitative determination of hallucinogenic plants in plant mixtures.

    Science.gov (United States)

    Luciano, Pino; Bertea, Cinzia M; Temporale, Giovanni; Maffei, Massimo E

    2007-12-01

    Here, we show a new, simple, and rapid SYBR Green-based Real-Time PCR assay for the quantification of hallucinogenic plants in plant mixtures. As a test plant, Salvia divinorum Epling & Játiva-M., a perennial herb belonging to the Lamiaceae family able to induce hallucinations, changes in perception, or other psychologically induced changes with similar potency as LSD, was used. The method was tested on seven mixtures 100/0%, 80/20%, 60/40%, 40/60%, 20/80%, 10/90%, 0/100% (w/w) S. divinorum versus a non-hallucinogenic plant, Salvia officinalis. Total DNA was extracted from samples and quantified by Real-Time PCR. Arabidopsis thaliana genomic DNA was added, as internal standard, at the beginning of each extraction. A new formula for the interpretation of Real-Time PCR data, based on the relative quantification of DNA extracted from mixture versus a reference DNA extracted from a known amount of pure S. divinorum, was developed. The results of this work show an almost perfect correspondence between Real-Time PCR-calculated weight and the weight estimated by an analytical weighted method, proving the effectiveness of this method for the quantitative analysis of a given species in a plant mixture.

  1. Quantitative determination of urinary tetrahydroaldosterone by a radioimmunological method. Contribution to the study of its excretion

    International Nuclear Information System (INIS)

    Carayon, Alain.

    1978-06-01

    The aim here is to propose a method of urinary tetrahydroaldosterone determination based on radioimmunology, the advantages of which distinguish this technique from the many others already available. The work is divided into three parts: - the first, of more basic interest, gives an overall view of the biological and biochemical properties of tetrahydroaldosterone, the understanding of its analysis and the interpretation of the results via that of its metabolism; - part two considers aspects of the radioimmunological method, first in general then applied to tetrahydroaldosterone determination, and the elements needed for its use: reference standard, immunogen and antiserum preparation. Its value is governed by two fundamental sets of requirements those concerning the conditions of validity of any analysis technique and those relating to radioimmunology; - part three discusses in practical terms the determination of more than 470 pathological cases. Results already obtained by other authors on certain aspects of corticoadrenal pathology are examined for comparative purposes [fr

  2. Analysis and quantitative determination of group B saponins in processed soybean products.

    Science.gov (United States)

    Berhow, Mark A; Cantrell, Charles L; Duval, Sandra M; Dobbins, Thomas A; Maynes, Jonathan; Vaughn, Steven F

    2002-01-01

    Pure analytical standards for the major saponins present in processed soy products, the group B saponins (soyasaponins I, II, III and IV), were isolated in mg quantities by a combination of processing, precipitation/re-solubilisation, TLC and preparative HPLC. These standards were determined to be pure by LC-ESI/MS analysis and NMR. The standards were used to perfect a facile analytical HPLC method using spectrometric detection to determine the percent composition of the group B soyasaponins in various products from processing of soybean.

  3. Quantitative analysis of the productivity of an indeterminate and a determinate genotype of Vicia faba

    International Nuclear Information System (INIS)

    Stuetzel, H.; Aufhammer, W.

    1990-01-01

    Full text: Experiments were carried out with the indeterminate faba bean cv. 'Herz Freya' and the determinate cv. 'Ticol'. Total and reproductive dry matter were greater in 'Herz Freya' than in 'Ticol'. However, light interception tended to be higher in 'Ticol', therefore the conversion of light into dry matter was less efficient. The two cultivars differed apparently in their light utilisation efficiency. It appears that a large part of the differences between 'Ticol' and 'Herz Freya' are the result of differences in primary productivity, not necessarily related to the indeterminate or determinate growth habit. (author)

  4. A quantitative analysis of major determinants of rural-urban migration in Nigeria.

    Science.gov (United States)

    Anyanwu, S O

    1992-11-01

    "This paper discusses some major determinants of rural-urban migration in Nigeria using the logit estimation technique. It utilizes cross-sectional data generated from a national sample survey of internal migration conducted...between January and March 1988.... The empirical results revealed that the significant determinants of rural-urban migration in Nigeria are income, contact, cost, spoken English, ability to speak two Nigerian languages, distance, marital status, sex and ethnicity. The results further suggest that rural-urban migration is selective of single people and males. Proximity to urban areas where prospective migrants have relatives, friends and townspeople is an important factor." excerpt

  5. Analyses and quantitative determination of the strontium radioisotopes 89 and 90 in milk powder

    International Nuclear Information System (INIS)

    Jeanmaire, L.; Michon, G.

    1959-01-01

    The authors describe a procedure for the determination of the strontium radioisotopes 89 and 90. The concentration of strontium is made possible by the insolubility of its nitrate salt in strong nitric acid which allows the removal of greatest part of calcium. The purification is performed on a cation exchange column. The amount of radioisotope 90 is determined by means of its daughter product yttrium 90 necessary calibrations and computations are treated in special paragraphs. With regard to the reproducibility of the measurements, the fluctuations are less than 20 per cent. This seems satisfaction for such a technique which have great sensibility while being long and necessitative great carefulness. (author) [fr

  6. An Illustration of Determining Quantitatively the Rock Mass Quality Parameters of the Hoek-Brown Failure Criterion

    Science.gov (United States)

    Wu, Li; Adoko, Amoussou Coffi; Li, Bo

    2018-04-01

    In tunneling, determining quantitatively the rock mass strength parameters of the Hoek-Brown (HB) failure criterion is useful since it can improve the reliability of the design of tunnel support systems. In this study, a quantitative method is proposed to determine the rock mass quality parameters of the HB failure criterion, namely the Geological Strength Index (GSI) and the disturbance factor ( D) based on the structure of drilling core and weathering condition of rock mass combined with acoustic wave test to calculate the strength of rock mass. The Rock Mass Structure Index and the Rock Mass Weathering Index are used to quantify the GSI while the longitudinal wave velocity ( V p) is employed to derive the value of D. The DK383+338 tunnel face of Yaojia tunnel of Shanghai-Kunming passenger dedicated line served as illustration of how the methodology is implemented. The values of the GSI and D are obtained using the HB criterion and then using the proposed method. The measured in situ stress is used to evaluate their accuracy. To this end, the major and minor principal stresses are calculated based on the GSI and D given by HB criterion and the proposed method. The results indicated that both methods were close to the field observation which suggests that the proposed method can be used for determining quantitatively the rock quality parameters, as well. However, these results remain valid only for rock mass quality and rock type similar to those of the DK383+338 tunnel face of Yaojia tunnel.

  7. Towards quantitative determination of the spring constant of a scanning force microscope cantilever with a microelectromechanical nano-force actuator

    International Nuclear Information System (INIS)

    Gao, Sai; Herrmann, Konrad; Zhang, Zhikai; Wu, Yong

    2010-01-01

    The calibration of the performance of an SFM (scanning force microscope) cantilever has gained more and more interest in the past years, particularly due to increasing applications of SFMs for the determination of the mechanical properties of materials, such as biological structures and organic molecules. In this paper, a MEMS-based nano-force actuator with a force resolution up to nN (10 −9 N) is presented to quantitatively determine the stiffness of an SFM cantilever. The principle, structure design and realization of the nano-force actuator are detailed. Preliminary experiments demonstrate that the long-term self-calibration stability of the actuator is better than 3.7 × 10 −3 N m −1 (1σ) over 1 h. With careful calibration of the stiffness of the actuator, the MEMS actuator has the capability to determine the stiffness of various types of cantilevers (from 100 N m −1 down to 0.1 N m −1 ) with high accuracy. In addition, thanks to the large displacement and force range (up to 8 µm and 1 mN, respectively) of the actuator, the calibration procedure with our MEMS nano-force actuator features simple and active operation, and therefore applicability for different types of quantitative SFMs

  8. Quantitative analysis of proteins via sulfur determination by HPLC coupled to isotope dilution ICPMS with a hexapole collision cell.

    Science.gov (United States)

    Wang, Meng; Feng, Weiyue; Lu, Wenwei; Li, Bai; Wang, Bing; Zhu, Motao; Wang, Yun; Yuan, Hui; Zhao, Yuliang; Chai, Zhifang

    2007-12-01

    Quantitative analysis of proteins is an essential part and also constitutes a major challenge in modern proteomics. Quantification of proteins by inductively coupled plasma mass spectrometry (ICPMS) offers an alternative method for quantitative proteomics. In this study, we developed a method of absolute quantification of proteins via sulfur by size exclusion chromatography (SEC) coupled to ICPMS with a collision cell (ICP-CC-MS) and postcolumn isotope dilution. Bovine serum albumin (BSA), superoxide dismutase (SOD), and metallothionein-II (MT-II) served as model proteins. Enriched 34S, 65Cu, and 67Zn isotopic solutions were continuously mixed with the eluate from the SEC. Oxygen was added as a reactive gas into the collision cell where sulfur reacts with oxygen to form sulfur-oxygen ion, the ratio of 32S16O(+)/34S16O(+) thus representing 32S(+)/34S(+). The absolute quantity of proteins could be calculated by the isotopic dilution equation and the content of sulfur in the proteins. The detection limits for BSA, SOD, and MT-II are 8, 31, and 15 pmol, respectively. The relative standard deviations for the proteins are less than 3%. The ratios of S/Cu and S/Zn in the proteins were also determined. The quantitative method was validated by comparing with gravimetric results.

  9. Determination of optical properties of turbid media spanning visible and near-infrared regimes via spatially modulated quantitative spectroscopy.

    Science.gov (United States)

    Saager, Rolf B; Cuccia, David J; Durkin, Anthony J

    2010-01-01

    We present a novel, noncontact method for the determination of quantitative optical properties of turbid media from 430 to 1050 nm. Through measuring the broadband reflectance from an unknown sample as a function of the spatial frequency of the projected illumination patterns, the absolute absorption and reduced scattering coefficients can be calculated without a priori assumptions of the chromophores present. This technique, which is called spatially modulated quantitative spectroscopy (SMoQS), was validated through the quantification of optical properties of homogenous liquid phantoms with known concentrations of absorbers and scatterers. The properties of the phantoms were recovered across the range of values prepared with R(2) values of 0.985 and 0.996 for absorption and reduced scattering, respectively. A measurement was also performed on skin tissue as a demonstration of the method's performance in vivo. The resultant absorption spectrum was well described by a multichromophore fit, and the quantitative values for oxy- and deoxyhemoglobin, water, and melanin were within published ranges for skin.

  10. Use of Quantitative PCR for Determining Copy Numbers of Transgenes in Lesquerella fendleri

    Science.gov (United States)

    The first successful attempt to apply a real-time polymerase chain reaction (PCR)-based method to determine transgene copy number in Lesquerella fendleri is described. The system utilized a known one copy gene, LfKCS4/5, from L. fendleri as an endogenous calibrator and the threshold crossing point (...

  11. CLSM as quantitative method to determine the size of drug crystals in a solid dispersion

    NARCIS (Netherlands)

    de Waard, Hans; Hessels, Martin J T; Boon, Maarten; Sjollema, Klaas A; Hinrichs, Wouter L J; Eissens, Anko C; Frijlink, Henderik W

    2011-01-01

    PURPOSE: To test whether confocal laser scanning microscopy (CLSM) can be used as an analytical tool to determine the drug crystal size in a powder mixture or a crystalline solid dispersion. METHODS: Crystals of the autofluorescent drug dipyridamole were incorporated in a matrix of crystalline

  12. [Quantitative determination of ursolic acid in folium Ilicis cornutae (gouguye) gathered in different and periods].

    Science.gov (United States)

    Guo, Y; Cui, Y; Zhou, J; Yan, Y; Yuan, P

    1995-10-01

    The content of ursolic acid in Folium Ilicis Cornutae (Gouguye) gathered in different periods from Yongfeng county of Jiangxi province was determined by TLCS method. The result shows that the content appears to be low in samples gathered in April, but about the same in samples of February, June, August, October and December.

  13. Quantitative Ultrasound-Assisted Extraction for Trace-Metal Determination: An Experiment for Analytical Chemistry

    Science.gov (United States)

    Lavilla, Isela; Costas, Marta; Pena-Pereira, Francisco; Gil, Sandra; Bendicho, Carlos

    2011-01-01

    Ultrasound-assisted extraction (UAE) is introduced to upper-level analytical chemistry students as a simple strategy focused on sample preparation for trace-metal determination in biological tissues. Nickel extraction in seafood samples and quantification by electrothermal atomic absorption spectrometry (ETAAS) are carried out by a team of four…

  14. Novel electrochemical paper-based immunocapture assay for the quantitative determination of ethinylestradiol in water samples.

    Science.gov (United States)

    Scala-Benuzzi, María L; Raba, Julio; Soler-Illia, Galo J A A; Schneider, Rudolf J; Messina, Germán A

    2018-02-23

    We report a novel and innovative electrochemical paper-based immunocapture assay (EPIA) to address the need for ultrasensitive detection of emerging pollutants without regulatory status and whose effects on environment and human health are not completely yet understood. In particular, we present the application of this system towards highly sensitive detection of the emerging pollutant ethinyl estradiol (EE2). The EPIA approach is based on the use of paper microzones modified with silica nanoparticles (SNs) and anti-EE2 specific antibodies for capture and pre-concentration of EE2 from river water samples. After the pre-concentration procedure, the paper microzones are placed onto a screen-printed carbon electrode modified with electrochemically reduced graphene (RG). The bound EE2 is subsequently desorbed adding a diluted solution of sulfuric acid on the paper microzones. Finally, recovered EE2 is electrochemically detected by OSWV. The proposed novel methodology showed an appropriate LOD and linear range for the quantification of EE2 for water samples with different origins. The non-sophisticated equipment required, the adequate recovery values obtained (from 97% to 104%, with a RSD less than 4.9%), an appropriate LOD and linear range value (0.1 ng L-1 and 0.5-120 ng L-1, respectively) achieved by our immunocapture sensor present significant analytical figures of merit, particularly when the routine quantification of EE2 is considered. In addition, our system was based on electrochemical paper-based technology, which allows obtaining portable, easy-to-use, inexpensive and disposable devices. The EPIA can also serve as a general-purpose immunoassay platform applicable to quantitation of other drugs and emerging pollutants in environmental samples.

  15. Compressed sensing in quantitative determination of GAG concentration in cartilage by microscopic MRI.

    Science.gov (United States)

    Wang, Nian; Badar, Farid; Xia, Yang

    2018-06-01

    To evaluate the potentials of compressed sensing (CS) in MRI quantification of glycosaminoglycan (GAG) concentration in articular cartilage at microscopic resolution. T 1 -weighted 2D experiments of cartilage were fully sampled in k-space with five inversion times at 17.6 μm resolution. These fully sampled k-space data were re-processed, by undersampling at various 1D and 2D CS undersampling factors (UFs). The undersampled data were reconstructed individually into 2D images using nonlinear reconstruction, which were used to calculate 2D maps of T 1 and GAG concentration. The values of T 1 and GAG in cartilage were evaluated at different UFs (up to 16, which used 6.25% of the data). K-space sampling pattern and zonal variations were also investigated. Using 2D variable density sampling pattern, the T 1 images at UFs up to eight preserved major visual information and produced negligible artifacts. The GAG concentration remained accurate for different sub-tissue zones at various UFs. The variation of the mean GAG concentration through the whole tissue depth was 1.20%, compared to the fully sampled results. The maximum variation was 2.24% in the deep zone of cartilage. Using 1D variable density sampling pattern, the quantitative T 1 mapping and GAG concentration at UFs up to 4 showed negligible variations. This study demonstrates that CS could be beneficial in microscopic MRI (µMRI) studies of cartilage by acquiring less data, without losing significant accuracy in the quantification of GAG concentration. Magn Reson Med 79:3163-3171, 2018. © 2017 International Society for Magnetic Resonance in Medicine. © 2017 International Society for Magnetic Resonance in Medicine.

  16. The use of conditioned place preference to determine broiler preferences for quantitative or qualitative dietary restriction.

    Science.gov (United States)

    Buckley, L A; Sandilands, V; Hocking, P M; Tolkamp, B J; D'eath, R B

    2012-01-01

    1. Calcium propionate (CAP) may improve the welfare of feed restricted broiler breeders by improving their satiety when included within the feed ration. However, the evidence for this is mixed. 2. This study used a closed economy conditioned place preference (CPP) task and aimed to identify whether broilers (as a model for broiler breeders) preferred an environment associated with quantitative food restriction (QFR) or an environment associated with a diet quality-adjusted by the inclusion of CAP. Birds taught to associate different environments with QFR and ad libitum (AL) access to feed were used to validate the methodology. 3. The two treatment groups were (1) QFR/AL (n = 12) in which birds alternated every 2 d between QFR and ad libitum access to food, and (2) QFR/CAP (n = 12) in which birds alternated every 2 d between QFR and QFR + calcium propionate (increased from 3-9% over the study period). Birds were taught to associate one diet option with vertical stripes and the other with horizontal black and white stripes. Each bird was tested twice for a CPP (once per diet). 4. QFR/AL birds showed a significant preference for the pen associated with ad libitum access to feed, but only when tested hungry (i.e. fed QFR on day of testing). QFR/CAP birds did not show a preference under either hunger state. 5. Reasons for the failure of QFR/CAP birds to show a preference are unclear but could include a lack of preference or failure to learn the task. 6. The existence of state-dependent effects indicates that care is needed in the design of future CPP studies and that the effect of calcium propionate and level of hunger on ability to learn a CPP needs further investigation.

  17. Tracers application method for the quantitative determination of the source of oxygenic inclusions in steel

    International Nuclear Information System (INIS)

    Rewienska-Kosciukowa, B.; Dalecki, W.; Michalik, J.S.

    1976-01-01

    The sense and the possibility of radioactive and nonradioactive isotopic tracers application in investigations of the origin of oxygenic nonmetalic inclusions is presented. The discussed methods touch the investigations such as the origin of egzogenic inclusions which passed from external sources (fireproof lining, slag) to the steel or as the endogenic ones formed during the process of steel deoxidisation. The question of the tracers choice for refractory material and the further investigations concerned the determination of the origin of nonmetallic inclusions are discussed. The question of so called isotopic replacement tracers for the main steel deoxidizing agents is considered. The criterion of determination of oxygenic inclusions formed during the process of steel deoxidization is also discussed. Several results of laboratory and industrial investigations and also the examples of application of the discussed methods in the industrial scale are presented. (author)

  18. Detection and quantitative determination by PIXE of the mutagen Sn{sup 2+} in yeast cells

    Energy Technology Data Exchange (ETDEWEB)

    Viau, C.M. [Departamento de Biofisica/Centro de Biotecnologia, Universidade Federal do Rio Grande do Sul, UFRGS (Brazil); Yoneama, M.-L. [Instituto de Fisica, UFRGS, Av. Bento Goncalves 9500, CEP 91501-970, CP 15051, Porto Alegre, RS (Brazil)]. E-mail: jfdias@if.ufrgs.br; Dias, J.F. [Instituto de Fisica, UFRGS, Av. Bento Goncalves 9500, CEP 91501-970, CP 15051, Porto Alegre, RS (Brazil); Pungartnik, C. [Departamento de Ciencias Biologicas, Universidade Estadual de Santa Cruz, UESC, Ilheus, BA (Brazil); Brendel, M. [Departamento de Biofisica/Centro de Biotecnologia, Universidade Federal do Rio Grande do Sul, UFRGS (Brazil); Departamento de Ciencias Biologicas, Universidade Estadual de Santa Cruz, UESC, Ilheus, BA (Brazil); Henriques, J.A.P. [Departamento de Biofisica/Centro de Biotecnologia, Universidade Federal do Rio Grande do Sul, UFRGS (Brazil); Faculdade de Farmacia, Universidade Luterana do Brasil, ULBRA, Porto Alegre, RS (Brazil)

    2006-08-15

    The main goal of this work was to determine the concentration of Sn{sup 2+} ions in cells of the yeast Saccharomyces cerevisiae and to correlate their quantity with the genotoxicity of intracellularly accumulated metal ions. The intracellular metal content of yeast cells was determined by PIXE (particle-induced X-ray emission) after cell exposure to SnCl{sub 2}. To that end, a thick target protocol was developed for PIXE analysis. The samples were irradiated with a 2 MeV proton beam, while the induced X-rays were detected with a high-purity germanium detector. The results of the toxicity of SnCl{sub 2} and the PIXE analysis performed with two different yeast strains (haploid and diploid) suggest that the exposure of haploid and diploid yeast to Sn{sup 2+} induces DNA lesions and that the absorption depends on the genetic background of each strain.

  19. Detection and quantitative determination by PIXE of the mutagen Sn2+ in yeast cells

    International Nuclear Information System (INIS)

    Viau, C.M.; Yoneama, M.-L.; Dias, J.F.; Pungartnik, C.; Brendel, M.; Henriques, J.A.P.

    2006-01-01

    The main goal of this work was to determine the concentration of Sn 2+ ions in cells of the yeast Saccharomyces cerevisiae and to correlate their quantity with the genotoxicity of intracellularly accumulated metal ions. The intracellular metal content of yeast cells was determined by PIXE (particle-induced X-ray emission) after cell exposure to SnCl 2 . To that end, a thick target protocol was developed for PIXE analysis. The samples were irradiated with a 2 MeV proton beam, while the induced X-rays were detected with a high-purity germanium detector. The results of the toxicity of SnCl 2 and the PIXE analysis performed with two different yeast strains (haploid and diploid) suggest that the exposure of haploid and diploid yeast to Sn 2+ induces DNA lesions and that the absorption depends on the genetic background of each strain

  20. Rapid semi-quantitative determination of bismuth in minerals using ascending paper chromatography (1961)

    International Nuclear Information System (INIS)

    Agrinier, H.

    1961-01-01

    The bismuth is separated by a solvent made up of acetone, water, and hydrofluoric and hydrochloric acids. The bismuth is developed with dimercapto-2.5 thio-diazole-1.3.4 and ammonium sulphide. The use of this method for the detection of bismuth in minerals makes it possible to determine the metal at a concentration of 5 x 10 -6 . (author) [fr

  1. Quantitative LC/MS-MS determination of sulfonamides and some other antibiotics in honey.

    Science.gov (United States)

    Kaufmann, Anton; Roth, Sven; Ryser, Bianca; Widmer, Mirjam; Guggisberg, Domink

    2002-01-01

    A simple and rapid method was developed for the determination of 20 antibiotics (sulfonamides, tetacyclines, and flumequine) in honey by liquid chromatography tandem mass spectrometry. The proposed method is sensitive (limit of detection 0.5 to 10 ppb for the various antibiotics) and selective. A hydrolysis step ensures the liberation of sugar-bound sulfonamides. The approach has been used to analyze some 300 honey samples. A number of them were found to have exceeded the Swiss limit of 50 ppb.

  2. Quantitative Determination of Fibrinogen of Patients with Coronary Heart Diseases through Piezoelectric Agglutination Sensor

    OpenAIRE

    Chen; Hua; Fu; Liu; Chen; Cai

    2010-01-01

    Fibrinogen can transform fibrin through an agglutination reaction, finally forming fibrin polymer with grid structure. The density and viscosity of the reaction system changes drastically during the course of agglutination. In this research, we apply an independently-developed piezoelectric agglutination sensor to detect the fibrinogen agglutination reaction in patients with coronary heart diseases. The terminal judgment method of determining plasma agglutination reaction through piezoelectri...

  3. Quantitative determination of pefloxacin mesylate by residual-base neutralisation method

    Directory of Open Access Journals (Sweden)

    HULIKALCHANDRA SHEKAR PRAMEELA

    2004-05-01

    Full Text Available This work describes two procedures based on residual base determination for the quantification of pefloxacin mesylate (PFM in bulk drug and in pharmaceutical products. In the first method involving titrimetry, the drug solution is treated with a measured excess of sodium hydroxide followed by back titration of the residual base with hydrochloric acid using a phenol red-bromothymol blue mixed indicator. The second spectrophotometrie method involves treatment of a fixed amount of sodium hydroxide – phenol red mixture with varying amounts of the drug, and measuring the decrease in the absorbance of the dye at 560 nm. In the titrimetric method, a reaction stoichiometry of 1:1 was found in the quantification range of 4–20 mg of drug. The spectrophotometric method allows the determination of PFM in the 5–40 mg ml-1 range. The molar absorptivity is 5.91¤103 l mol-1 cm-1 and the Sandell sensitivity is 56.37 ng cm-2. The methods were applied successfully to the determination of PFM in pharmaceutical preparations.

  4. A novel method for quantitative determination of tea polysaccharide by resonance light scattering

    Science.gov (United States)

    Wei, Xinlin; Xi, Xionggang; Wu, Muxia; Wang, Yuanfeng

    2011-09-01

    A new method for the determination of tea polysaccharide (TPS) in green tea ( Camellia sinensis) leaves has been developed. The method was based on the enhancement of resonance light scattering (RLS) of TPS in the presence of cetylpyridinium chloride (CPC)-NaOH system. Under the optimum conditions, the RLS intensity of CPC was greatly enhanced by adding TPS. The maximum peak of the enhanced RLS spectra was located at 484.02 nm. The enhanced RLS intensity was proportional to the concentration of TPS in the range of 2.0-20 μg/ml. It showed that the new method and phenol-sulfuric acid method give some equivalent results by measuring the standard compounds. The recoveries of the two methods were 96.39-103.7% (novel method) and 100.15-103.65% (phenol-sulfuric acid method), respectively. However, it showed that the two methods were different to some extent. The new method offered a limit of detection (LOD) of 0.047 μg/ml, whereas the phenol-sulfuric acid method gives a LOD of 1.54 μg/ml. Interfered experiment demonstrated that the new method had highly selectivity, and was more suitable for the determination of TPS than phenol-sulfuric method. Stability test showed that new method had good stability. Moreover, the proposed method owns the advantages of easy operation, rapidity and practicability, which suggested that the proposed method could be satisfactorily applied to the determination of TPS in green tea.

  5. [Quantitative determination of melamine by fluorescence spectroscopy and radial basis function neural networks].

    Science.gov (United States)

    Chen, Guo-qing; Wei, Bai-lin; Wang, Jun; Wu, Ya-min; Gao, Shu-mei; Kong, Yan; Zhu, Tuo

    2010-01-01

    Based on the experimental study, it was found that melamine solution excited by UV light can generate a strong fluorescence. The fluorescence spectrum is within a range from 310 to 600 nm, the peak wavelength of the fluorescence is about 420 nm, and the relationship between fluorescence intensity and melamine solution concentration is nonlinear. A method for the determination of melamine solution concentration was presented, which was based on fluorescence spectroscopy and radial basis function neural networks. For each sample, 30 emission wavelength values were selected, the fluorescence intensity corresponding to the selected wavelength was used as the network data, and a radial basis function neural network was trained and constructed. The trained radial basis function neural network was employed to predict the melamine solution concentration in five kinds of samples, and the relative errors of the results were 0.93%, 0.09%, 0.31%, 1.55% and 4.61%, respectively. The results show that this method can determine the content of melamine quickly and accurately. The whole research outcomes will provide a new method for determining the content of melamine and food safety supervision.

  6. Quantitative Determination of the Breakdown Field of Air from Van de Graaff Generator Discharge

    Science.gov (United States)

    Beach, John; Chartrand, Bridget; Gallagher, Hugh

    2016-03-01

    The Van de Graaff generator (VG) is ubiquitous in electrostatic demonstrations because of the large static charge and dramatic sparks produced. We have developed a novel technique for determining the breakdown field of air using the VG. When a spark occurs, the force of attraction between the VG and a discharge sphere suspended above it is measured by a Pasco force sensor. At this time the charge is not symmetric but pulled towards the near side of the spheres by mutual attraction. In order to interpret the measured force in terms of the breakdown field, an accurate model of the charge distribution is needed. Using the method of images for a spherical conductor in an iterative fashion we can provide this model. The electric field in the vicinity of the spheres is then calculated from the charge distribution and its maximum value is the breakdown field. In preliminary work, we determined the breakdown field to be 3.1x106 N/C at 24.9 C and 18% relative humidity. We will report our most recent determination of the breakdown field using this method and discuss the validity of the results in terms of accepted values, experimental limitations and sensitivity to the charge distribution model.

  7. Exploring Determinants of Handwashing with Soap in Indonesia: A Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Mitsuaki Hirai

    2016-09-01

    Full Text Available Handwashing with soap is recognized as a cost-effective intervention to reduce morbidity and mortality associated with enteric and respiratory infections. This study analyzes rural Indonesian households’ hygiene behaviors and attitudes to examine how motivations for handwashing, locations of handwashing space in the household, and handwashing moments are associated with handwashing with soap as potential determinants of the behavior. The analysis was conducted using results from a UNICEF cross-sectional study of 1700 households in six districts across three provinces of Indonesia. A composite measure of handwashing with soap was developed that included self-reported handwashing, a handwashing demonstration, and observed handwashing materials and location of facilities in the home. Prevalence ratios were calculated to analyze associations between handwashing with soap and hypothesized determinants of the behavior. Our results showed that determinants that had a significant association with handwashing with soap included: (1 a desire to smell nice; (2 interpersonal influences; (3 the presence of handwashing places within 10 paces of the kitchen and the toilet; and (4 key handwashing moments when hands felt dirty, including after eating and after cleaning child stools. This study concludes that handwashing with soap may be more effectively promoted through the use of non-health messages.

  8. [Diagnostic significance of serum free DNA human telomerase reverse transcriptase quantitative determination on spinal cord injury].

    Science.gov (United States)

    Yang, M K; Tang, J; Xiang, Z; Zhang, X; Wang, J; Li, Z; Li, Y; Sheng, W B

    2018-02-06

    Objective: To investigate the relationship between the content of human telomerase reverse transcriptase (hTERT) and its clinical features in serum free DNA in patients with different degree of spinal cord injury. Methods: From December 2013 to December 2016, inpatients of the Central Hospital of Bazhong, Sichuan Province were enrolledand divided into the experimental group, the disease control group and the negative control group. For the experimental group: 46 patients with spinal cord injury were graded according to the criteria of the American Association of Spinal Cord Injury (ASIA), including 12 cases of grade A, 10 cases of grade B, 10 cases of grade C, 7 cases of grade D and 7 cases of grade E; for the disease control group: 15 patients with spinal fractures (without spinal cord injury) at the same period were included; and for the negative control group: 20 healthy adult volunteers aged 18-50 years were selected.Real-time fluorescence quantitative PCR and immunoblotting were performed to detect the content of hTERT in serum free DNA both in patients and healthy controls and to compare the difference between them. The results of the somatosensory evoked potential (SEP) of all patients were compared and analyzed.The receiver operating characteristic (ROC) curve was used to analyze the diagnostic value of hTERT content in serum free DNA in patients with spinal cord injury. Results: Comparison of serum free DNA hTERT content: in the experimental group, the serum free DNA hTERT content of grade A, B, C, D, E was (99.63±8.23), (76.24±4.37), (46.07±5.43), (16.30±0.95) and (15.74±1.12)μg/L, respectively.While it was (15.01±1.39)μg/L in the disease control group and (14.54±1.03)μg/L in the negative control group. The total difference was statistically significant between patients of each group and the control group ( F =857.917, P spinal cord injury has a certain guiding significance for the diagnosis of spinal cord injury and the degree of injury.

  9. A convenient method for the quantitative determination of elemental sulfur in coal by HPLC analysis of perchloroethylene extracts

    Science.gov (United States)

    Buchanan, D.H.; Coombs, K.J.; Murphy, P.M.; Chaven, C.

    1993-01-01

    A convenient method for the quantitative determination of elemental sulfur in coal is described. Elemental sulfur is extracted from the coal with hot perchloroethylene (PCE) (tetrachloroethene, C2Cl4) and quantitatively determined by HPLC analysis on a C18 reverse-phase column using UV detection. Calibration solutions were prepared from sublimed sulfur. Results of quantitative HPLC analyses agreed with those of a chemical/spectroscopic analysis. The HPLC method was found to be linear over the concentration range of 6 ?? 10-4 to 2 ?? 10-2 g/L. The lower detection limit was 4 ?? 10-4 g/L, which for a coal sample of 20 g is equivalent to 0.0006% by weight of coal. Since elemental sulfur is known to react slowly with hydrocarbons at the temperature of boiling PCE, standard solutions of sulfur in PCE were heated with coals from the Argonne Premium Coal Sample program. Pseudo-first-order uptake of sulfur by the coals was observed over several weeks of heating. For the Illinois No. 6 premium coal, the rate constant for sulfur uptake was 9.7 ?? 10-7 s-1, too small for retrograde reactions between solubilized sulfur and coal to cause a significant loss in elemental sulfur isolated during the analytical extraction. No elemental sulfur was produced when the following pure compounds were heated to reflux in PCE for up to 1 week: benzyl sulfide, octyl sulfide, thiane, thiophene, benzothiophene, dibenzothiophene, sulfuric acid, or ferrous sulfate. A sluury of mineral pyrite in PCE contained elemental sulfur which increased in concentration with heating time. ?? 1993 American Chemical Society.

  10. A Statistical-Probabilistic Pattern for Determination of Tunnel Advance Step by Quantitative Risk Analysis

    Directory of Open Access Journals (Sweden)

    sasan ghorbani

    2017-12-01

    Full Text Available One of the main challenges faced in design and construction phases of tunneling projects is the determination of maximum allowable advance step to maximize excavation rate and reduce project delivery time. Considering the complexity of determining this factor and unexpected risks associated with inappropriate determination of that, it is necessary to employ a method which is capable of accounting for interactions among uncertain geotechnical parameters and advance step. The main objective in the present research is to undertake optimization and risk management of advance step length in water diversion tunnel at Shahriar Dam based on uncertainty of geotechnical parameters following a statistic-probabilistic approach. In the present research, in order to determine optimum advance step for excavation operation, two hybrid methods were used: strength reduction method-discrete element method- Monte Carlo simulation (SRM/DEM/MCS and strength reduction method- discrete element method- point estimate method (SRM/DEM/PEM. Moreover, Taguchi analysis was used to investigate the sensitivity of advance step to changes in statistical distribution function of input parameters under three tunneling scenarios at sections of poor to good qualities (as per RMR classification system. Final results implied the optimality of the advance step defined in scenario 2 where 2 m advance per excavation round was proposed, according to shear strain criterion and SRM/DEM/MCS, with minimum failure probability and risk of 8.05% and 75281.56 $, respectively, at 95% confidence level. Moreover, in either of normal, lognormal, and gamma distributions, as the advance step increased from Scenario 1 to 2, failure probability was observed to increase at lower rate than that observed when advance step in scenario 2 was increased to that In Scenario 3. In addition, Taguchi tests were subjected to signal-to-noise analysis and the results indicated that, considering the three statistical

  11. Technique for Determination of Rational Boundaries in Combining Construction and Installation Processes Based on Quantitative Estimation of Technological Connections

    Science.gov (United States)

    Gusev, E. V.; Mukhametzyanov, Z. R.; Razyapov, R. V.

    2017-11-01

    The problems of the existing methods for the determination of combining and technologically interlinked construction processes and activities are considered under the modern construction conditions of various facilities. The necessity to identify common parameters that characterize the interaction nature of all the technology-related construction and installation processes and activities is shown. The research of the technologies of construction and installation processes for buildings and structures with the goal of determining a common parameter for evaluating the relationship between technologically interconnected processes and construction works are conducted. The result of this research was to identify the quantitative evaluation of interaction construction and installation processes and activities in a minimum technologically necessary volume of the previous process allowing one to plan and organize the execution of a subsequent technologically interconnected process. The quantitative evaluation is used as the basis for the calculation of the optimum range of the combination of processes and activities. The calculation method is based on the use of the graph theory. The authors applied a generic characterization parameter to reveal the technological links between construction and installation processes, and the proposed technique has adaptive properties which are key for wide use in organizational decisions forming. The article provides a written practical significance of the developed technique.

  12. Quantitative determination of total and individual flavonoids in stems and leaves of Buddleja davidii and Buddleja albiflora.

    Science.gov (United States)

    Ying, Cheng; Wan, Dingrong

    2012-10-01

    Buddleja davidii and B. albiflora are two different original plants of the famous crude medicine "Diaoyangchen". An ultraviolet-visible spectrophotometric method and a HPLC method were used for the determination of total and individual flavonoids (luteolin and apigenin) contents from their stems and leaves for the first time. From the comparative evaluation, remarkable differences in flavonoids contents were observed between different origins and different parts of the samples. And content of specific flavonoid did not correspond to the total flavonoids contents in Buddleja davidii and Buddleja albiflora. With a better accuracy and precision, the methods had been proved simple, rapid, and reliable for quantitative determination of the total flavonoids and luteolin and apigenin in the two phytomedicines. Furthermore, our present study will pave the way of guidelines for the differentiation and standardization and exploitation of individual parts of this herb material.

  13. [Development of quantitative analyse method for determination of alkaloid cytisin in Spartium junceum L., growing in Georgia].

    Science.gov (United States)

    Iavich, P A; Churadze, L I; Suladze, T Sh; Rukhadze, T A

    2011-12-01

    The aim of the research was to develop a method for quantitative determination of cytisine in Spartium junceum L. We used the above-ground parts of plants. In developing a method of analysis we used the method of 3-phase extraction. In this case the best results were obtained in the system: chopped raw material - water solution of ammonia - chloroform. In this case, the amount of alkaloids extracted almost entirely from the plant and goes into the chloroform phase. Evaluation of the results was carried out by the validation. The method for determination of cytisine in raw product was proposed. The method comprises the following steps-extraction of raw materials extracting chloroform phase and its evaporation, the translation of solids in methanol, the chromatographic separation cytisine and its fixation of the spectrophotometer method. The method is reproducible, has the required accuracy, is easy to analysis (less than 9 hours).

  14. Optimization and Validation of Quantitative Spectrophotometric Methods for the Determination of Alfuzosin in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    M. Vamsi Krishna

    2007-01-01

    Full Text Available Three accurate, simple and precise spectrophotometric methods for the determination of alfuzosin hydrochloride in bulk drugs and tablets are developed. The first method is based on the reaction of alfuzosin with ninhydrin reagent in N, N'-dimethylformamide medium (DMF producing a colored product which absorbs maximally at 575 nm. Beer’s law is obeyed in the concentration range 12.5-62.5 µg/mL of alfuzosin. The second method is based on the reaction of drug with ascorbic acid in DMF medium resulting in the formation of a colored product, which absorbs maximally at 530 nm. Beer’s law is obeyed in the concentration 10-50 µg/mL of alfuzosin. The third method is based on the reaction of alfuzosin with p-benzoquinone (PBQ to form a colored product with λmax at 400 nm. The products of the reaction were stable for 2 h at room temperature. The optimum experimental parameters for the reactions have been studied. The validity of the described procedures was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed methods could be used for the determination of alfuzosin in pharmaceutical formulations. The procedures were rapid, simple and suitable for quality control application.

  15. Compositional characteristics of commercial yoghurt based on quantitative determination of viable lactic acid bacteria

    Directory of Open Access Journals (Sweden)

    Niketić Gordana B.

    2009-01-01

    Full Text Available Yoghurt quality is particularly difficult to standardize because of the many forms, varieties, manufacturing methods, ingredients and consumer preferences that exist. Since these factors will always play an important role, it is unlikely that a uniform yoghurt quality concept will ever emerge, such as has been developed for other dairy products. There are a number of common denominators, however that have bearing on yoghurt quality. Since a number of producers are recognized within the broad category entitled yoghurt. This situation makes yoghurt an interesting, challenging, but also a confusing area to work in. The present investigation was undertaken to isolate from commercial yoghurt the strains involved in its manufacture and determine the characteristics of Streptococcus thermophilus and Lactobacillus delbrueckii subsp.bulgaricus. This study is concerned with the lactic acid bacteria (L.delbrueckii subsp. bulgaricus and S. thermophilus growth in yoghurt from involving different procedures and with the determination of the number of lactic acid bacteria in dependence of the temperature and acidity in the period of storage. Predominant samples of yoghurt were with 11-107/ml lactic acid lactococci (44.28%.

  16. Gravimetric quantitative determination of packaging residues in feed from former food.

    Science.gov (United States)

    Amato, Giuseppina; Desiato, Rosanna; Giovannini, Tiziana; Pinotti, Luciano; Tretola, Marco; Gili, Marilena; Marchis, Daniela

    2017-08-01

    Valorisation of former foodstuff products (FFP) in feed is part of a long-term strategy for sustainability. An approach to valorise FFP outside the waste value chain is their use as an alternative source of feed materials, with a subsequent optimisation of the environmental impact of products. In the current practice of food production, food packaging is provided to ensure the maintenance of food quality and safety during transport and storage. One of the problems of reusing FFP is how to deal with packaging materials or remains that can become residues in the feed. The aim of this study is to propose a fast and sensitive gravimetric method, fit for routine official controls, for the determination of packaging residues in feed. The developed method can briefly be summarised as: (1) visual selection of the undesired ingredients which can be identified as remnants of packaging materials; (2) weighing of the selected materials; (3) defatting; (4) dehydration; (5) final weighing; and (6) reporting of weight and percentage. Moreover, the method has been validated through the determination of some of the parameters listed in Council Regulation 2004/882/EC (i.e., specificity, limit of quantification (LOQ), recovery, repeatability, within-laboratory reproducibility and measurement uncertainty).

  17. The value of quantitative fibrin monomer determination in the early diagnosis of postoperative deep vein thrombosis.

    Science.gov (United States)

    Vogel, G; Dempfle, C E; Spannagl, M; Leskopf, W

    1996-01-15

    A new test for the determination of fibrin monomer in plasma was clinically evaluated in comparison to the plasma concentration of D-D, TAT and F1,2 for the early diagnosis of prethrombotic conditions. For this purpose 129 patients who underwent abdominal surgery were followed longitudinally. 12 patients developed DVT postoperatively, proved by phlebography. The identical specificity level 73.2% was chosen for all 4 tests. At this specificity, FM had the highest sensitivity (91.7%), followed by D-D (75.0%), TAT (41.7%) and F1,2 (33.3%). All FM-positive DVT-patients had pathological FM-values at least one day prior to the clinical manifestation of thrombosis. In a group of 255 obviously healthy persons the cut-off value for the new FM test was determined at 3.6 mg/l (95th percentile). No clinically relevant influence of gender, age, smoking habits or oral anticonception could be observed. It is concluded that FM is a valuable diagnostic tool for the early diagnosis of prethrombotic conditions.

  18. Determining concentrations of 2-bromoallyl alcohol and dibromopropene in ground water using quantitative methods

    Science.gov (United States)

    Panshin, Sandra Y.

    1997-01-01

    A method for determining levels of 2-bromoallyl alcohol and 2,3-dibromopropene from ground-water samples using liquid/liquid extraction followed by gas chromatography/mass spectrometry is described. Analytes were extracted from the water using three aliquots of dichloromethane. The aliquots were combined and reduced in volume by rotary evaporation followed by evaporation using a nitrogen stream. The extracts were analyzed by capillary-column gas chromatography/mass spectrometry in the full-scan mode. Estimated method detection limits were 30 nanograms per liter for 2-bromoallyl alcohol and 10 nanograms per liter for 2,3-dibromopropene. Recoveries were determined by spiking three matrices at two concentration levels (0.540 and 5.40 micrograms per liter for 2-bromoallyl alcohol; and 0.534 and 5.34micro-grams per liter for dibromopropene). For seven replicates of each matrix at the high concentration level, the mean percent recoveries ranged from 43.9 to 64.9 percent for 2-bromoallyl alcohol, and from 87.5 to 99.3 percent for dibromopropene. At the low concentration level, the mean percent recoveries ranged from 43.8 to 95.2 percent for 2-bromoallyl alcohol, and from 71.3 to 84.9 percent for dibromopropene.

  19. Quantitative determination of mineral coal impurities from Brazil through optical emission spectrography technique

    International Nuclear Information System (INIS)

    Clain, Almir Faria

    1982-01-01

    The aim of the present research was to develop a spectrographic technique to determine the highest possible number of the chemical elements micro-constituents of Brazilian mineral coals. The experimental technique developed corresponds to the so called total-burning procedure. Coal samples were calcined to ashes at 400°C and then totally burned in graphite electrodes by a DC arc. The spectrographic measurements were made in a Jarrell-Ash emission spectrograph, Ebert mounting type, model Mark IV. An inert atmosphere chamber (for a gaseous mixture 20% 0 2 and 80% air) and a seven step rotating sector were used as main accessories. The analytical curves for the different elements, were obtained using synthetic standards in the concentration range of 10 to 1.000 ppm, and the standards as well as the coal ashes were diluted with spectrographically pure graphite in 1:1 ratio. Seventeen coal samples from different shells and strata of Morungava and Charqueadas mines - Rio Grande do Sul State - were analyzed to test the proposed technique, being possible to determine the following elements: B, Be, Bi, Cd, Co, Cr, Cu, Ga,Pb, Ge, Mn, Mo, Ni, Sn, Sb, V, Y, Zn and Zr. The coefficient of variation was 14% in average for all the elements and the sensitivity was so that the majority of the impurities present in the coals were analyzed. (author)

  20. Ab initio structure determination and quantitative disorder analysis on nanoparticles by electron diffraction tomography.

    Science.gov (United States)

    Krysiak, Yaşar; Barton, Bastian; Marler, Bernd; Neder, Reinhard B; Kolb, Ute

    2018-03-01

    Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffraction tomography (ADT), crystal disorder modelling and electron diffraction simulations. Zeolite beta was chosen for a proof-of-principle study of the techniques, because it consists of two different intergrown polymorphs that are built from identical layer types but with different stacking sequences. Imaging of the projected inner Coulomb potential of zeolite beta crystals shows the intergrowth of the polymorphs BEA and BEB. The structures of BEA as well as BEB could be extracted from one single ADT data set using direct methods. A ratio for BEA/BEB = 48:52 was determined by comparison of the reconstructed reciprocal space based on ADT data with simulated electron diffraction data for virtual nanocrystals, built with different ratios of BEA/BEB. In this way, it is demonstrated that this smart interplay of the above-mentioned techniques allows the elaboration of the real structures of functional materials in detail - even if they possess a severely disordered structure.

  1. The use of stable isotopes in quantitative determinations of exogenous water and added ethanol in wines

    Science.gov (United States)

    Magdas, D. A.; Moldovan, Z.; Cristea, G.

    2012-02-01

    The application of oxygen isotope ratios analysis to wine water according to EU regulation no. 822/97 to determine wine's origin and also, the possible water addition to wines, gained great importance in wines authenticity control. In the natural cycle of water isotopic fractionation, during water evaporation process, the water vapors are depleted in heavy isotopes. On the other hand inside the plants take place an isotope enrichment of heavy stable isotopes of water compared with meteoric water due to photosynthesis and plants transpiration. This process makes possible the detection of exogenous water from wines 18O/16O ratios. Carbon isotopic ratios were used to estimate the supplementary addition of ethanol obtained from C4 plants (sugar cane or corn). This work presents the way in which the isotopic fingerprints (δ13C and δ18O) were used to determine the content of exogenous water from wines and the added supplementary ethanol coming from C4 plants. By using this method, the calculated values obtained for the degree of wine adulteration were in a good agreement with the real exogenous percent of water and ethanol from investigated samples.

  2. FLAVONOIDS QUANTITATIVE DETERMINATION IN THE INFLORESCENCES OF TAGETES ERECTA AND TAGETES PATULA

    Directory of Open Access Journals (Sweden)

    Е. A. Malyugina

    2013-12-01

    Full Text Available INTRODUCTION The Genus marigold (Tagetes belongs to the family Asteraceae. The native land of this genus is the Central America. The genus marigold contains about 56 species and more than 600 forms and cultivars that are widely distributed around the world. The most distributed species are T. erecta L. and T. patula L. The chemical constituents of marigolds and their biological activity are intensively studied now. These plants contain more than 100 secondary metabolites, e.g. flavonoids, carotenoids, steroids, alkaloids, phenol derivate and others. The biological active carotenoids, flavonoids, essential oil, vitamins that contained in the inflorescences and herbs of Tagetes L. has anti-oxidant, anti-inflammatory, antibacterial and other activity. Tagetes L. genus plants widely used in traditional medicine as wound healing, hepatoprotective, choleretic, and adaptogenic medicines. The essential oil of marigolds has insecticidal properties and used in national economics. Also this plants are used in ophthalmology. The main biological active compounds of Tagetes L. are flavonoids. Composition of the most perspective carotenoid-contain species and cultivars of Tagetes L., such as T. patula nana L. (Gold Kopfen, Orangeflamme and T. erecta L. remains poorly understood. They need to be studied as perspective source of the biological active flavonoids. OBJECTIVE The aim of the study was to determine flavonoids contain in the inflorescences of Tagetes erecta L. cultivars “Equinox” and “Hawaii” and Tagetes patula L. cultivars “Gold Kopfen” and “Orangeflamme”. To determine the most perspective cultivars for obtaining the medicines. MATERIALS AND METHODS Tagetes patula L. and Tagetes erecta L. was selected in the present study. Plant material (inflorescences was collected from different regions of Ukraine. About 0.1 of crushed inflorescences was extracted by ethanol about 30 minutes twice, filtered and cooled. Appropriate quantities of

  3. Determination of avermectins by the internal standard recovery correction - high performance liquid chromatography - quantitative Nuclear Magnetic Resonance method.

    Science.gov (United States)

    Zhang, Wei; Huang, Ting; Li, Hongmei; Dai, Xinhua; Quan, Can; He, Yajuan

    2017-09-01

    Quantitative Nuclear Magnetic Resonance (qNMR) is widely used to determine the purity of organic compounds. For the compounds with lower purity especially molecular weight more than 500, qNMR is at risk of error for the purity, because the impurity peaks are likely to be incompletely separated from the peak of major component. In this study, an offline ISRC-HPLC-qNMR (internal standard recovery correction - high performance liquid chromatography - qNMR) was developed to overcome this problem. It is accurate by excluding the influence of impurity; it is low-cost by using common mobile phase; and it extends the applicable scope of qNMR. In this method, a mix solution of the sample and an internal standard was separated by HPLC with common mobile phases, and only the eluents of the analyte and the internal standard were collected in the same tube. After evaporation and re-dissolution, it was determined by qNMR. A recovery correction factor was determined by comparison of the solutions before and after these procedures. After correction, the mass fraction of analyte was constant and it was accurate and precise, even though the sample loss varied during these procedures, or even in bad resolution of HPLC. Avermectin B 1 a with the purity of ~93% and the molecular weight of 873 was analyzed. Moreover, the homologues of avermectin B 1 a were determined based on the identification and quantitative analysis by tandem mass spectrometry and HPLC, and the results were consistent with the results of traditional mass balance method. The result showed that the method could be widely used for the organic compounds, and could further promote qNMR to become a primary method in the international metrological systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Comparative and quantitative determination of total hemoglobin concentration in normal and psoriatic patients

    International Nuclear Information System (INIS)

    Mahesar, S.M.; Dahot, M.U.; Khuhawar, M.Y.; Mahesar, H.U.

    2004-01-01

    The cyanmethaemoglobin technique is now recommended as the standard method by International Committee for Standardization in Hematology and British Standards Institution 1966. The hemoglobin is treated with reagent containing potassium ferricyanide, Potassium cyanide and potassium dihydrogen phosphate. The ferricyanide forms methamoglobin which is converted to cyanmethaemoglobin by the cyanide. The average values of hemoglobin, percent determined from the blood samples of normal and psoriatic (n=44) males and (n=35) females were 15.0, 12.7, 13.6 and 11.2 g/100ml. The decrease in hemoglobin concentration could be due to anemia resulting during the cell proliferation epidermis in inflammatory state and Keratolytic disorder which take place in psoriasis. (author)

  5. Quantitative determination of glycine in aqueous solution using glutamate dehydrogenase-immobilized glyoxal agarose beads.

    Science.gov (United States)

    Keskin, Semra Yilmazer; Keskin, Can Serkan

    2014-01-01

    In this study, an enzymatic procedure for the determination of glycine (Gly) was developed by using a column containing immobilized glutamate dehydrogenase (GDH) on glyoxal agarose beads. Ammonia is produced from the enzymatic reactions between Gly and GDH with NAD(+) in phosphate buffer medium. The indophenol blue method was used for ammonia detection based on the spectrophotometric measurements of blue-colored product absorbing at 640 nm. The calibration graph is linear in the range of 0.1-10 mM of Gly concentrations. The effect of pH, temperature, and time interval was studied to find column stability, and also the interference effects of other amino acids was investigated. The interaction between GDH and glyoxal agarose beads was analyzed by Fourier transform infrared (FTIR) spectroscopy. The morphology of the immobilized and non-immobilized agarose beads were characterized by atomic force microscopy (AFM).

  6. Quantitative methodology to extract regional magnetotelluric impedances and determine the dimension of the conductivity structure

    Energy Technology Data Exchange (ETDEWEB)

    Groom, R. [PetRos EiKon Incorporated, Ontario (Canada); Kurtz, R.; Jones, A.; Boerner, D. [Geological Survey of Canada, Ontario (Canada)

    1996-05-01

    This paper describes a systematic method for determining the appropriate dimensionality of magnetotelluric (MT) data from a site, and illustrates the application of this method to analyze both synthetic data and real data. Additionally, it describes the extraction of regional impedance responses from multiple sites. This method was examined extensively with synthetic data, and proven to be successful. It was demonstrated for two neighboring sites that the analysis methodology can be extremely useful in unraveling the bulk regional response when hidden by strong three-dimensional effects. Although there may still be some uncertainties remaining in the true levels for the regional responses for stations LIT000 and LITW02, the analysis has provided models which not only fit the data but are consistent for neighboring sites. It was suggested from these data that the stations are seeing significantly different structures. 12 refs.

  7. Multiplex dipstick immunoassay for semi-quantitative determination of Fusarium mycotoxins in cereals

    Energy Technology Data Exchange (ETDEWEB)

    Lattanzio, Veronica M.T., E-mail: veronica.lattanzio@ispa.cnr.it [National Research Council of Italy, Institute of Sciences of Food Production (ISPA-CNR), Via Amendola 122/O, 70126 Bari (Italy); Nivarlet, Noan [UNISENSOR S.A., Zoning industriel du Dossay, Rue du Dossay no 3, B-4020 Liege (Belgium); Lippolis, Vincenzo; Gatta, Stefania Della [National Research Council of Italy, Institute of Sciences of Food Production (ISPA-CNR), Via Amendola 122/O, 70126 Bari (Italy); Huet, Anne-Catherine; Delahaut, Philippe [Centre d' Economie Rurale (CER Groupe), Rue du Point du Jour no 8, B-6900 Marloie (Belgium); Granier, Benoit [UNISENSOR S.A., Zoning industriel du Dossay, Rue du Dossay no 3, B-4020 Liege (Belgium); Visconti, Angelo [National Research Council of Italy, Institute of Sciences of Food Production (ISPA-CNR), Via Amendola 122/O, 70126 Bari (Italy)

    2012-03-09

    Highlights: Black-Right-Pointing-Pointer We developed a rapid method based on a multiplex dipstick immunoassay. Black-Right-Pointing-Pointer The assay allowed the determination of major Fusarium toxins in wheat, oats, maize. Black-Right-Pointing-Pointer We obtained cut off levels close to EU regulatory levels. - Abstract: A multiplex dipstick immunoassay based method for the simultaneous determination of major Fusarium toxins, namely zearalenone, T-2 and HT-2 toxins, deoxynivalenol and fumonisins in wheat, oats and maize has been developed. The dipstick format was based on an indirect competitive approach. Four test lines (mycotoxin-BSA conjugates) and one control line were located on the strip membrane. Labelled antibodies were freeze-dried within the microwell. Two matrix-related sample preparation protocols have been developed for wheat/oats (not containing fumonisins) and maize (containing fumonisins) respectively. The use of a methanol/water mixture for sample preparation allowed recoveries in the range 73-109% for all mycotoxins in all tested cereals, with relative standard deviation less than 10%. The optimized immunoassay was able to detect target mycotoxins at cut off levels equal to 80% of EU maximum permitted levels, i.e. 280, 400, 1400 and 3200 {mu}g kg{sup -1}, respectively, for zearalenone, T-2/HT-2 toxins, deoxynivalenol and fumonisins in maize, and 80, 400 and 1400 {mu}g kg{sup -1}, respectively, for zearalenone, T-2/HT-2 toxins and deoxynivalenol in wheat and oats. Analysis of naturally contaminated samples resulted in a good agreement between multiplex dipstick and validated confirmatory LC-MS/MS. The percentage of false positive results was less than or equal to 13%, whereas no false negative results were obtained. Data on the presence/absence of 6 mycotoxins at levels close to EU regulatory levels were obtained within 30 min. The proposed immunoassay protocol is rapid, inexpensive, easy-to-use and fit for purpose of rapid screening of mycotoxins

  8. Free lime quantitative determination by X ray diffraction, on anhiydrous and dried cement

    Directory of Open Access Journals (Sweden)

    Sagrera, J. L.

    1987-09-01

    Full Text Available In manufactured cements, and concerning the quality control, the fast determination of the contents of free lime is a necessary step. The measurement of the content is made taking the net altitude of one peak of the DRX which, on each case, is peculiar to the compound to be determined. So, a calibrating curve is drawn, using there synthetic samples prepared with original cement with addition of 1%, 3% and 5% in weight of calcium oxide prepared fusing at 1100 °C for two hours a Merkc precipitate calcium carbonate. This calibrating curve allows to know the free lime content in original cement, when the results obtained by X ray diffraction is carried to the calibrating curve.

    En la fabricación de cementos, y dentro del control de su calidad, la determinación rápida del contenido de cal libre es un dato necesario. Esta determinación, según normativa (*, debe hacerse usando la vía química. Como método alternativo existe la técnica de difracción de rayos X que, en pocos minutos, puede determinar el contenido de cal libre, sin posibles interferencias de otros compuestos. La medida del contenido se hace midiendo la altura de un pico del difractograma de rayos X que, para cada caso, es privativo del compuesto que se quiere determinar. En el presente artículo se trata de explicar, paso a paso, el procedimiento para determinar cuantitativamente el contenido de cal libre que existe en un cemento anhidro y desecado a 110 °C. Para ello, se construye una curva de calibrado utilizando tres muestras sintéticas preparadas en el laboratorio partiendo del cemento utilizado, al que se le añade el 1%, 3% y 5% en peso de OXIDO DE CALCIO preparado calcinando a 1.100 °C durante dos horas CARBONATO DE CALCIO precipitado Merck. Dicha curva de calibrado permite conocer el contenido de cal libre, del cemento de partida, cuando el resultado obtenido por difracción de rayos X se lleva a la curva patrón obtenida.

  9. Fuzzy hidden Markov chains segmentation for volume determination and quantitation in PET

    Science.gov (United States)

    Hatt, Mathieu; Lamare, Frédéric; Boussion, Nicolas; Roux, Christian; Turzo, Alexandre; Cheze-Lerest, Catherine; Jarritt, Peter; Carson, Kathryn; Salzenstein, Fabien; Collet, Christophe; Visvikis, Dimitris

    2007-01-01

    Accurate volume of interest (VOI) estimation in PET is crucial in different oncology applications such as response to therapy evaluation and radiotherapy treatment planning. The objective of our study was to evaluate the performance of the proposed algorithm for automatic lesion volume delineation; namely the Fuzzy Hidden Markov Chains (FHMC), with that of current state of the art in clinical practice threshold based techniques. As the classical Hidden Markov Chain (HMC) algorithm, FHMC takes into account noise, voxel’s intensity and spatial correlation, in order to classify a voxel as background or functional VOI. However the novelty of the fuzzy model consists of the inclusion of an estimation of imprecision, which should subsequently lead to a better modelling of the “fuzzy” nature of the object on interest boundaries in emission tomography data. The performance of the algorithms has been assessed on both simulated and acquired datasets of the IEC phantom, covering a large range of spherical lesion sizes (from 10 to 37mm), contrast ratios (4:1 and 8:1) and image noise levels. Both lesion activity recovery and VOI determination tasks were assessed in reconstructed images using two different voxel sizes (8mm3 and 64mm3). In order to account for both the functional volume location and its size, the concept of % classification errors was introduced in the evaluation of volume segmentation using the simulated datasets. Results reveal that FHMC performs substantially better than the threshold based methodology for functional volume determination or activity concentration recovery considering a contrast ratio of 4:1 and lesion sizes of <28mm. Furthermore differences between classification and volume estimation errors evaluated were smaller for the segmented volumes provided by the FHMC algorithm. Finally, the performance of the automatic algorithms was less susceptible to image noise levels in comparison to the threshold based techniques. The analysis of both

  10. Method for pretreating lignocellulosic biomass

    Science.gov (United States)

    Kuzhiyil, Najeeb M.; Brown, Robert C.; Dalluge, Dustin Lee

    2015-08-18

    The present invention relates to a method for pretreating lignocellulosic biomass containing alkali and/or alkaline earth metal (AAEM). The method comprises providing a lignocellulosic biomass containing AAEM; determining the amount of the AAEM present in the lignocellulosic biomass; identifying, based on said determining, the amount of a mineral acid sufficient to completely convert the AAEM in the lignocellulosic biomass to thermally-stable, catalytically-inert salts; and treating the lignocellulosic biomass with the identified amount of the mineral acid, wherein the treated lignocellulosic biomass contains thermally-stable, catalytically inert AAEM salts.

  11. Application of Scharer's quantitative method for the determination of residual alkaline phosphatase activity in standard Minas

    Directory of Open Access Journals (Sweden)

    C.F. Soares

    2013-08-01

    Full Text Available Milk pasteurization is a critical issue in the dairy industry, and failures in this process can affect final product safety. Scharer's enzymatic method is still traditionally used to verify pasteurization efficiency compliance, and it is based on screening for residual alkaline phosphatase in milk. Although several methods are used to quantify enzymatic activity to assess milk pasteurization efficiency, there is a small amount of published data regarding the use of these methods to quantify alkaline phosphatase in cheese. In this study, the Scharer's modified method was used to determine the levels of residual alkaline phosphatase in standard minas cheese, before and after 20 days of ripening. The cheeses were made using raw or pasteurized milk with the addition of different concentrations of raw milk (0; 0.05%; 0.10%; 0.20%; and 0.50%. In the fresh cheese samples, the method showed a sensitivity of only 0.50% with the addition of raw milk to the pasteurized milk used to make cheese. In addition, levels of up 0.20% of raw milk in pasteurized milk, the concentrations of phenol was inferior to 1μg phenol/g of dairy product which is the preconized indicator value for adequate pasteurization.

  12. Left ventricular ejection fraction determined by gated Tl-201 perfusion SPECT and quantitative software

    International Nuclear Information System (INIS)

    Hyun, In Young; Kim, Sung Eun; Seo, Jeong Kee; Hong, Eui Soo; Kwan, Jun; Park, Keum Soo; Lee, Woo Hyung

    2000-01-01

    We compared estimates of ejection fraction (EF) determined by gated Tl-201 perfusion SPECT (g-Tl-SPECT) with those by gated blood pool (GBP) scan. Eighteen subjects underwent g-Tl-SPECT and GBP scan. After reconstruction of g-Tl-SPECT, we measured EF with Cedars software. The comparison of the EF with g-Tl-SPECT and GBP scan was assessed by correlation analysis and Bland Altman plot. The estimates of EF were significantly different (p<0.05) with g-Tl-SPECT (40%±14%) and GBP scan (43%±14%). There was an excellent correlation of EF between g-Tl-SPECT and GBP scan (r=3D0.94, p<0.001). The mean difference of EF between GBP scan and g-Tl-SPECT was +3.2%. Ninety-five percent limits of agreement were ±9.8%. EF between g-Tl-SPECT and GBP scan were in poor agreement. The estimates of EF by g-Tl-SPECT was well correlated with those by GBP scan. However, EF of g-Tl-SPECT doesn't agree with EF of GBP scan. EF of g-Tl-SPECT can't be used interchangeably with EF of GBP scan.=20

  13. Quantitative determination of circulating endothelial cells in persons with low dose radioactivity exposure

    International Nuclear Information System (INIS)

    Al-Massarani, Gh.; Najjar, F.

    2013-04-01

    The aim of this study was to determine the risk of occupational exposure to low doses of ionizing radiation on the endothelium detachment through the quantification of circulating endothelial cells (CEC) in the peripheral blood of 63 workers in the Atomic Energy Commission in Syria (AECS) using a Magnetic Immuno-separation technique (IMS) and compare the results with 28 healthy (controls) is not exposed during their careers for any type of ionizing radiation. Our study showed for the first time the significantly increasing in the circulating endothelial cells count (P <0.0001) when employees are exposed to low doses of radiation less than 50 mSv. This result with previous studies about the late effects of radiation, assuming the existence of impact late radiation exposure on the cohesion of the endothelium, despite the lack of correlation with radiation dose measured during the past four years of work in AECS (between 2006-2010). This is due to several reasons, including the small sample size and lack of commitment by some workers develop individual control films during some periods of their work. The prospective studies for such workers can allow us to know if the rise in the number of CEC will be considered an early indicator for the risk of a cardiovascular disease when workers exposed to low-doses of ionizing radiation( tens of millisievert) that up to date are considered harmless (author).

  14. Quantitative Determination of Lercanidipine Enantiomers in Commercial Formulations by Capillary Electrophoresis

    Directory of Open Access Journals (Sweden)

    Luciana Pereira Lourenço

    2015-01-01

    Full Text Available An enantioselective method based on capillary electrophoresis (CE using cyclodextrin (CD as chiral selector was developed and validated for determination of lercanidipine (LER enantiomers, a drug calcium channel blocker which exerts antihypertensive effects of long duration, in a pharmaceutical formulation. Optimum separation of LER enantiomers was obtained on a 50 cm × 50 μm id capillary using a sodium acetate buffer solution 200 mmol/L pH 4.0 containing 10 mmol/L of 2,3,6-o-methyl-β-cyclodextrin (TM-β-CD as background electrolyte. The capillary temperature and voltage were 15°C and 25 kV, respectively, hydrodynamic injection and detection at 237 nm. Linearity was obtained in the range 12.5–100 μg/mL for both enantiomers (r≥0.995. The RSD (% and relative errors (E, % obtained in precision and accuracy studies (intraday and interday were lower than 5%. After validation, the method was applied to quantify the enantiomers of LER in commercial tablets and the results were satisfactory in terms of accuracy and precision, both less than 5%. Therefore, this method was found to be appropriate for enantioselective quality control of LER enantiomers in pharmaceutical formulations.

  15. Quantitative determination of arterial wall mechanics with pulse oximetric finger plethysmography.

    Science.gov (United States)

    Kato, R; Sato, J; Iuchi, T; Higuchi, Y

    1999-10-30

    The plethysmographic wave of pulse oximetry reflects arterial pulsation at the fingertip. Since arterial pressure and the pulsatile component of the arterial cross section represent the input and output of the fingertip arterial system, respectively, arterial wall mechanics may be delineated from their relationship. We aimed to construct a mathematical model of the fingertip arterial wall from the relationship between the plethysmographic wave and arterial pressure. The pulse oximetric plethysmographic signal at the forefinger and pressure at the ipsilateral radial artery were measured. Employing the data, simple mathematical models with one to four mechanical elements were tested in terms of the goodness of fit and the physiological implications. The determined model was applied to the data obtained during administration of vasoactive agents in anesthetized patients. The mathematical model suited for describing arterial wall mechanics was a four-element, two-compartment model. The two compartments represent passive mechanical and active contractile properties, respectively. In the application of the model to the anesthetized patients, the vasoactive agents produced changes in the model parameters that implied mechanical alterations in the arterial wall. These findings suggest the benefit of the four-element, two-compartment model in analyzing peripheral vascular wall mechanics influenced by various stimuli in intensive care and anesthesia.

  16. EXTRACTION AND QUANTITATIVE DETERMINATION OF ASCORBIC ACID FROM BANANA PEEL MUSA ACUMINATA ‘KEPOK’

    Directory of Open Access Journals (Sweden)

    Khairul Anwar Mohamad Said

    2016-04-01

    Full Text Available This paper discusses the extraction of an antioxidant compound, which is ascorbic acid or vitamin C, from a banana peel using an ultrasound-assisted extraction (UAE method. The type of banana used was Musa acuminata also known as “PisangKepok” in Malaysia. The investigation includes the effect of solvent/solid ratio (4.5, 5 g and 10  ml/g, sonication time (15, 30 and 45 mins and temperature variation (30 , 45  and 60oC on the extraction of ascorbic acid compounds from the banana peel to determine the best or optimum condition of the operation. Out of all extract samples analyzed by redox titration method using iodine solution, it was found that the highest yield was 0.04939 ± 0.00080 mg that resulted from an extraction at 30oC for 15 mins with 5 ml/g solvent-to-solute ratio.KEYWORDS:  Musa acuminata; ultrasound-assisted extraction; vitamin C; redox titration

  17. Studies on quantitative determination of total alkaloids and berberine in five origins of crude medicine "Sankezhen".

    Science.gov (United States)

    Li, Luyang; Long, Weifang; Wan, Xiangluan; Ding, Qi; Zhang, Fei; Wan, Dingrong

    2015-02-01

    The roots of Berberis plants are widely used as a traditional Chinese medicine called "Sankezhen", having the activities of antibacterial and anti-inflammatory, and the ingredients are alkaloids. This work aims to study and compare the total alkaloids and individual alkaloid (berberine) contents in roots and stems from five origins of Berberis plants (Berberis soulieana Schneid., B. henryana Schneid., B. triacanthophora Fedde, B. gagnepainii Schneid. and B. bergmanniae Schneid.) and provides some references for resource and quality evaluation of the medicine. Acid dye colorimetry and high-performance liquid chromatography were used in the determination. The results showed that the contents for the total alkaloids in root and stem samples were in the range of 1.60-4.72% and 0.76-2.70%, while those of the berberine were 0.70-2.92% and 0.23-1.07%. With higher contents of the total alkaloids and berberine, the roots of B. soulieana, B. gagnepainii and B. bergmanniae were good sources of "Sankezhen". Meanwhile, the contents were also high in stems of the three plants, indicating that the stems were likely to be alternative sources of "Sankezhen" after further research. As the results of precision, stability and recovery tests shown, the methods were simple, rapid and reliable, and provided valuable basis for quality evaluation and new resource investigation of "Sankezhen". © Crown copyright 2014.

  18. Extrusion Pretreatment of Lignocellulosic Biomass: A Review

    Directory of Open Access Journals (Sweden)

    Jun Zheng

    2014-10-01

    Full Text Available Bioconversion of lignocellulosic biomass to bioethanol has shown environmental, economic and energetic advantages in comparison to bioethanol produced from sugar or starch. However, the pretreatment process for increasing the enzymatic accessibility and improving the digestibility of cellulose is hindered by many physical-chemical, structural and compositional factors, which make these materials difficult to be used as feedstocks for ethanol production. A wide range of pretreatment methods has been developed to alter or remove structural and compositional impediments to (enzymatic hydrolysis over the last few decades; however, only a few of them can be used at commercial scale due to economic feasibility. This paper will give an overview of extrusion pretreatment for bioethanol production with a special focus on twin-screw extruders. An economic assessment of this pretreatment is also discussed to determine its feasibility for future industrial cellulosic ethanol plant designs.

  19. Use of radioimmunoassay for quantitative determination of progesterone in milk samples from dairy cows in Zimbabwe

    International Nuclear Information System (INIS)

    Freymark, P.J.; McCabe, C.T.

    1986-01-01

    A maximum 90-day service interval is an important economic factor in dairying. The determination of pregnancy at 21 to 26 days post-insemination can ensure that particular attention is paid to non-pregnant cows at subsequent heats, and thus help reduce this interval. In Zimbabwe a radioimmunoassay for milk progesterone using an iodinated tracer was developed in 1982 from a previously established assay for plasma progesterone. Progesterone antiserum is produced locally and the assay is used as an early pregnancy diagnosis test in dairy cattle. During 1983 two pilot schemes were instituted to investigate breed differences, logistics, and feasibility under the local conditions, and to identify constraints. Milk samples taken 24 days post-insemination were found to differentiate best between pregnant and non-pregnant cows for both major breeds in the country (Friesian/Holstein and Jersey). Pregnant cows had an average of 13.76 ng/mL (+-1.06) progesterone on day 24 while non-pregnant cows averaged 0.34 ng/mL (+-0.13) of progesterone. Apparently 12.2% of cows subsequently lost their embryos after day 24, and these cows averaged 9.98 ng/mL (+-1.52). Milk samples were also taken on the day of insemination; the results showed that 11% of cows were incorrectly inseminated when progesterone concentrations were high (2.59 ng/mL+-0.80). A National Early Pregnancy Diagnosis Scheme using milk progesterone was implemented in December 1984 and results to date are discussed in the paper. (author)

  20. Quantitative determination of tricalcicum aluminate in portland cement by X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Sagrera Moreno, José Luis

    1989-06-01

    Full Text Available Tricalcium aluminate (C3A is one of the constitutive phase of the cement-clinker. Its concentration influences the cement behaviour in sulphate aggressive soils. Therefore its quantification is very convenient and International standards fix its content when the concrete is used in contact with soils or liquids containing sulphate compounds. There are two possibilities in order to calculate the amount of C3A in clinker phases: one consist in a mathematical calculation from the results of the chemical analysis (Bogue formulae and the order is based in X-ray diffraction, using the height of the representative peak of the C3A phase. In the present note, the experimental procedure in order to determine the C3A content from X-ray test is presented.

    El aluminato tricáicico es una de las fases constitutivas del clinker de cemento portland. Su concentración en el cemento influye en el comportamiento de éste, en las obras sometidas a la posible agresividad de diferentes sulfatos cuando entran en contacto con las estructuras que se fabrican con él. Por ello la determinación de su concentración es un dato que puede invalidar su uso en una obra. De ahí que las normas internacionales fijen la cantidad de aluminato tricáicico según se clasifique la agresividad del entorno en el que una estructura será colocada. Existen fórmulas matemáticas para calcular la concentración de cada una de las fases del clinker a partir de las concentraciones de los elementos químicos de clinker expresados en forma de óxidos. Los posibles errores en los análisis químicos producen errores en los cálculos de las concentraciones de cada fase. Para determinar la concentración de dichas fases se puede emplear también la técnica de difracción de rayos X, basándose en la medida de la altura del pico representativo de la fase que se quiere determinar.

  1. Determination of CT number and density profile of binderless, pre-treated and tannin-based Rhizophora spp. particleboards using computed tomography imaging and electron density phantom

    Energy Technology Data Exchange (ETDEWEB)

    Yusof, Mohd Fahmi Mohd, E-mail: mfahmi@usm.my; Hamid, Puteri Nor Khatijah Abdul; Tajuddin, Abdul Aziz [School of Physics, Universiti Sains Malaysia, 11800 Penang (Malaysia); Bauk, Sabar [School of Distance Education, Universiti Sains Malaysia, 11800 Penang (Malaysia); Hashim, Rokiah [School of Industrial Technologies, Universiti Sains Malaysia, 11800 Penang (Malaysia)

    2015-04-29

    Plug density phantoms were constructed in accordance to CT density phantom model 062M CIRS using binderless, pre-treated and tannin-based Rhizophora Spp. particleboards. The Rhizophora Spp. plug phantoms were scanned along with the CT density phantom using Siemens Somatom Definition AS CT scanner at three CT energies of 80, 120 and 140 kVp. 15 slices of images with 1.0 mm thickness each were taken from the central axis of CT density phantom for CT number and CT density profile analysis. The values were compared to water substitute plug phantom from the CT density phantom. The tannin-based Rhizophora Spp. gave the nearest value of CT number to water substitute at 80 and 120 kVp CT energies with χ{sup 2} value of 0.011 and 0.014 respectively while the binderless Rhizphora Spp. gave the nearest CT number to water substitute at 140 kVp CT energy with χ{sup 2} value of 0.023. The tannin-based Rhizophora Spp. gave the nearest CT density profile to water substitute at all CT energies. This study indicated the suitability of Rhizophora Spp. particleboard as phantom material for the use in CT imaging studies.

  2. Determination of CT number and density profile of binderless, pre-treated and tannin-based Rhizophora spp. particleboards using computed tomography imaging and electron density phantom

    Science.gov (United States)

    Yusof, Mohd Fahmi Mohd; Hamid, Puteri Nor Khatijah Abdul; Bauk, Sabar; Hashim, Rokiah; Tajuddin, Abdul Aziz

    2015-04-01

    Plug density phantoms were constructed in accordance to CT density phantom model 062M CIRS using binderless, pre-treated and tannin-based Rhizophora Spp. particleboards. The Rhizophora Spp. plug phantoms were scanned along with the CT density phantom using Siemens Somatom Definition AS CT scanner at three CT energies of 80, 120 and 140 kVp. 15 slices of images with 1.0 mm thickness each were taken from the central axis of CT density phantom for CT number and CT density profile analysis. The values were compared to water substitute plug phantom from the CT density phantom. The tannin-based Rhizophora Spp. gave the nearest value of CT number to water substitute at 80 and 120 kVp CT energies with χ2 value of 0.011 and 0.014 respectively while the binderless Rhizphora Spp. gave the nearest CT number to water substitute at 140 kVp CT energy with χ2 value of 0.023. The tannin-based Rhizophora Spp. gave the nearest CT density profile to water substitute at all CT energies. This study indicated the suitability of Rhizophora Spp. particleboard as phantom material for the use in CT imaging studies.

  3. Determination of CT number and density profile of binderless, pre-treated and tannin-based Rhizophora spp. particleboards using computed tomography imaging and electron density phantom

    International Nuclear Information System (INIS)

    Yusof, Mohd Fahmi Mohd; Hamid, Puteri Nor Khatijah Abdul; Tajuddin, Abdul Aziz; Bauk, Sabar; Hashim, Rokiah

    2015-01-01

    Plug density phantoms were constructed in accordance to CT density phantom model 062M CIRS using binderless, pre-treated and tannin-based Rhizophora Spp. particleboards. The Rhizophora Spp. plug phantoms were scanned along with the CT density phantom using Siemens Somatom Definition AS CT scanner at three CT energies of 80, 120 and 140 kVp. 15 slices of images with 1.0 mm thickness each were taken from the central axis of CT density phantom for CT number and CT density profile analysis. The values were compared to water substitute plug phantom from the CT density phantom. The tannin-based Rhizophora Spp. gave the nearest value of CT number to water substitute at 80 and 120 kVp CT energies with χ 2 value of 0.011 and 0.014 respectively while the binderless Rhizphora Spp. gave the nearest CT number to water substitute at 140 kVp CT energy with χ 2 value of 0.023. The tannin-based Rhizophora Spp. gave the nearest CT density profile to water substitute at all CT energies. This study indicated the suitability of Rhizophora Spp. particleboard as phantom material for the use in CT imaging studies

  4. Quantitative determination of phases in ZrO2 (MgO) (Y2O3) using the Rietveld method

    International Nuclear Information System (INIS)

    Castro, Antonio Carlos de

    2007-01-01

    The key objective of this work is the crystallographic characterization of the zircon co-doped with Yttria and magnesium with the application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon monoclinic, tetragonal, and cubic). Samples of zircon polymorph were obtained from zircon doped with Yttria and magnesium at defined molar concentrations. The zircon polymorph stability during subeutetoid aging at 1350 deg C were investigated to determine ZrO 2 - MgO - Y 2 0 3 phases degradation and to define the solid solutions stability environment. ZrO 2 powders doped with 8 mol por cent of MgO and 1 mol por cent of Y 2 O 3 , and 9 mol por cent of MgO and 0 mol por cent of Y 2 O 3 have been prepared by chemical route using the co-precipitation method. These samples have been calcinate at 550 deg C, sintered at 1500 deg C and characterized by the Rietveld method using the X-ray diffraction data. The variation of the lattice parameter, changes in the phase composition and their microstructures are discussed. The application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon tetragonal and cubic) reveals no formation of tetragonal phase and indicating that the matrix is the cubic phase with low concentration of monoclinic phase.(author)

  5. An attempt to use immunohistochemical methods for semi-quantitative determination of surfactant in bronchial secretion after hyperbaric exposures

    Directory of Open Access Journals (Sweden)

    Piotr Siermontowski

    2015-12-01

    Full Text Available Background The most significant index of pulmonary oxygen toxicity is a decrease in vital capacity (VC dependent on the duration of exposure and partial pressure of oxygen. The only method to measure this decrease is spirometry performed directly after exposure. Objective The aim of the study was to check whether the extent of lung damage could be assessed by quantitative determination of pulmonary surfactant in bronchial secretion. Design Sputum samples were collected before, during and after hyperbaric air or oxygen exposures; histological preparations were prepared and stained immunohistochemically to visualize surfactant. Amongst 781 samples collected, only 209 contained sputum and only 126 were included in the study. In this group, only 64 preparations could be paired for comparison. Results The semi-quantitative method used and statistical findings have not demonstrated any significance. Conclusions The method suggested for assessing the extent of lung damage has been found unsuitable for practical use due to difficulties in obtaining the proper material; moreover, the study findings do not allow to draw conclusions concerning its effectiveness.

  6. Rapid quantitative determination of maltose and total sugars in sweet potato (Ipomoea batatas L. [Lam.]) varieties using HPTLC.

    Science.gov (United States)

    Lebot, Vincent

    2017-03-01

    When a raw sweet potato root is analysed, only sucrose, glucose and fructose are present but during cooking, starch is hydrolysed into maltose giving the sweet flavour to cooked roots. This study aimed at developing an HPTLC protocol for the rapid quantitative determination of maltose and total sugars in four commercial varieties and to compare them to 243 hybrids grouped by flesh colour (white, orange, purple). In commercial varieties, mean maltose content varied from 10.26 to 15.60% and total sugars from 17.83 to 27.77% on fresh weight basis. Hybrids showed significant variation in maltose content within each group, with means ranging from 7.65% for white-fleshed, to 8.53% in orange- and 11.98% in purple-fleshed. Total mean sugars content was 20.24, 22.11 and 26.84% respectively for white, orange and purple flesh hybrids. No significant correlations were detected between individual sugars but maltose and total sugars content were highly correlated. Compared to the best commercial variety ( Baby ), 25 hybrids (10.3%) presented a higher maltose content and 40 (16.5%) showed a higher total sugars content. HPTLC was observed as an attractive, cost efficient, high-throughput technique for quantitating maltose and total sugars in sweet potatoes. Perspectives for improving sweet potato quality for consumers' requirements are also discussed.

  7. Quantitative X-ray methods of amorphous content and crystallinity determination of SiO2, in Quartz and Opal mixture

    International Nuclear Information System (INIS)

    Ketabdari, M.R.; Ahmadi, K.; Esmaeilnia Shirvani, A.; Tofigh, A.

    2001-01-01

    X-ray diffraction technique is commonly used for qualitative analysis of minerals, and has also been successfully used for quantitative measurements. In this research, the matrix flushing and a new X-ray diffraction method have been used for the determination of crystallinity and amorphous content of Opal and Quartz mixture. The PCAPD is used to determine the quantitative analysis of these two minerals

  8. Methods to determine limit of detection and limit of quantification in quantitative real-time PCR (qPCR

    Directory of Open Access Journals (Sweden)

    Amin Forootan

    2017-06-01

    Full Text Available Quantitative Real-Time Polymerase Chain Reaction, better known as qPCR, is the most sensitive and specific technique we have for the detection of nucleic acids. Even though it has been around for more than 30 years and is preferred in research applications, it has yet to win broad acceptance in routine practice. This requires a means to unambiguously assess the performance of specific qPCR analyses. Here we present methods to determine the limit of detection (LoD and the limit of quantification (LoQ as applicable to qPCR. These are based on standard statistical methods as recommended by regulatory bodies adapted to qPCR and complemented with a novel approach to estimate the precision of LoD.

  9. Quantitative determination of anisotropic magnetoelectric coupling in BiFeO3-CoFe2O4 nanostructures

    Science.gov (United States)

    Oh, Yoon Seok; Crane, S.; Zheng, H.; Chu, Y. H.; Ramesh, R.; Kim, Kee Hoon

    2010-08-01

    The transverse and longitudinal magnetoelectric susceptibilities (MES) were quantitatively determined for (001) heteroepitaxial BiFeO3-CoFe2O4 nanostructures. Both of these MES values were sharply enhanced at magnetic fields below 6 kOe and revealed asymmetric line shapes with respect to the dc magnetic field, demonstrating the strain-induced magnetoelectric effect. The maximum transverse MES, which reached as high as ˜60 mV/cm Oe, was about five times larger than the longitudinal MES. This observation signifies that transverse magnetostriction of the CoFe2O4 nanopillars is enhanced more than the bulk value due to preferred magnetic domain alignment along the [001] direction coming from compressive, heteroepitaxial strain.

  10. Indication of recanalization therapy in acute ischemic stroke determined by quantitative evaluation of cerebral blood flow by SPECT

    International Nuclear Information System (INIS)

    Umemura, Atsushi; Suzuka, Tomonao; Nakamura, Akihiro

    1999-01-01

    Recanalization of occluded vessels has been attempted for the treatment of acute hemispheric ischemic stroke, but increases the risk of hemorrhage. The purpose of this study is to determine the indications for recanalization therapy in acute ischemic stroke by quantitative evaluation of cerebral blood flow by SPECT. We studied retrospectively the relationship between regional cerebral blood flow (rCBF) measured by 99m Tc-HM-PAO SPECT before treatment and the radiological final outcome in 9 patients, who had hemispheric ishemic strokes and underwent successful recanalization of the occluded artery by endovascular technique within 6 hours after onset. A noninvasive method described by Matsuda et al (Patlak plot) was used for the quantitative measurement of rCBF with SPECT. The results showed that the low value of rCBF before treatment correlated with the development of infarction after recanalization. When recanalization was achieved between 2 and 6 hours after onset, the critical level of rCBF to develop infarction was 25-30 ml/100 g/min. Despite early recanalization, one patient with a significant rCBF defect suffered from hemorrhagic transformation after recanalization. The measurement of rCBF by 99m Tc-HM-PAO SPECT is available for emergent cases and is very useful to determine the extent and the degree of ischemic insult in acute ischemic strokes. Our data indicate that if the residual rCBF, measured by SPECT, is over 25 ml/100 g/min, emergent recanalization therapy should be considered, while on the other hand, if the residual rCBF is severely reduced (below 20 ml/100 g/min), acute recanalization is contraindicated to avoid fatal hemorrhagic transformation. A prospective study to enhance our preliminary results is needed. (author)

  11. Quantitative determination of oil content in small quantity of oilseed rape by ultrasound-assisted extraction combined with gas chromatography.

    Science.gov (United States)

    Wei, Fang; Gao, Gui-Zhen; Wang, Xin-Fa; Dong, Xu-Yan; Li, Ping-Ping; Hua, Wei; Wang, Xu; Wu, Xiao-Ming; Chen, Hong

    2008-09-01

    Accurately quantitative determination of oil content in oilseed rape plays an important role in varieties breeding for improving oil content in seeds. However, large quantity of oilseeds were needed in order to obtain accuracy and precision results by using standard Soxhlet extraction method, which may be a handicap in analysis of small, rare and precious samples in plant breeding. In the present work, ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction method for the isolation of oil from small quantity of oilseed rape (oil of oilseed rape samples was extracted by ultrasound-assisted method, and then the fatty acids and total oil content of the seeds were qualitatively and quantitatively determined by gas chromatography (GC). Extraction efficiency of total oil obtained by ultrasound-assisted extraction through an orthogonal experiment (L(9) (3(4))) were investigated to get the best extraction conditions. Statistical analysis showed that the variable with the largest effect was the ultrasound-assisted extraction time which was followed by the ultrasound-assisted extraction power, and the liquid:solid ratio. A liquid:solid ratio of 1:4 (L:g), an ultrasound-assisted extraction time of 60 min and an ultrasound-assisted extraction power of 500 W were found to be optimal for oil extraction from oilseed rape. By comparing with the conventional method, it was found that the ultrasound-assisted extraction of oil from oilseed rape was about five times faster than the traditional extraction method. By the use of ultrasound-assisted extraction combined with GC analysis, the fatty acids and total oil content in small quantity of seeds (method.

  12. Indication of recanalization therapy in acute ischemic stroke determined by quantitative evaluation of cerebral blood flow by SPECT

    Energy Technology Data Exchange (ETDEWEB)

    Umemura, Atsushi; Suzuka, Tomonao; Nakamura, Akihiro [Hamamatsu Social Insurance Hospital, Shizuoka (Japan)

    1999-03-01

    Recanalization of occluded vessels has been attempted for the treatment of acute hemispheric ischemic stroke, but increases the risk of hemorrhage. The purpose of this study is to determine the indications for recanalization therapy in acute ischemic stroke by quantitative evaluation of cerebral blood flow by SPECT. We studied retrospectively the relationship between regional cerebral blood flow (rCBF) measured by {sup 99m}Tc-HM-PAO SPECT before treatment and the radiological final outcome in 9 patients, who had hemispheric ishemic strokes and underwent successful recanalization of the occluded artery by endovascular technique within 6 hours after onset. A noninvasive method described by Matsuda et al (Patlak plot) was used for the quantitative measurement of rCBF with SPECT. The results showed that the low value of rCBF before treatment correlated with the development of infarction after recanalization. When recanalization was achieved between 2 and 6 hours after onset, the critical level of rCBF to develop infarction was 25-30 ml/100 g/min. Despite early recanalization, one patient with a significant rCBF defect suffered from hemorrhagic transformation after recanalization. The measurement of rCBF by {sup 99m}Tc-HM-PAO SPECT is available for emergent cases and is very useful to determine the extent and the degree of ischemic insult in acute ischemic strokes. Our data indicate that if the residual rCBF, measured by SPECT, is over 25 ml/100 g/min, emergent recanalization therapy should be considered, while on the other hand, if the residual rCBF is severely reduced (below 20 ml/100 g/min), acute recanalization is contraindicated to avoid fatal hemorrhagic transformation. A prospective study to enhance our preliminary results is needed. (author)

  13. Quantitative determination of the neurotoxin β-N-methylamino-L-alanine (BMAA) by capillary electrophoresis-tandem mass spectrometry.

    Science.gov (United States)

    Kerrin, Elliott S; White, Robert L; Quilliam, Michael A

    2017-02-01

    Recent reports of the widespread occurrence of the neurotoxin β-N-methylamino-L-alanine (BMAA) in cyanobacteria and particularly seafood have raised concerns for public health. LC-MS/MS is currently the analytical method of choice for BMAA determinations but incomplete separation of isomeric and isobaric compounds, matrix suppression and conjugated forms are plausible limitations. In this study, capillary electrophoresis (CE) coupled with MS/MS has been developed as an alternative method for the quantitative determination of free BMAA. Using a bare fused silica capillary, a phosphate buffer (250 mM, pH 3.0) and UV detection, it was possible to separate BMAA from four isomers, but the limit of detection (LOD) of 0.25 μg mL -1 proved insufficient for analysis of typical samples. Coupling the CE to a triple quadrupole MS was accomplished using a custom sheath-flow interface. The best separation was achieved with a 5 M formic acid in water/acetonitrile (9:1) background electrolyte. Strong acid hydrolysis of lyophilized samples was used to release BMAA from conjugated forms. Field-amplified stacking after injection was achieved by lowering sample ionic strength with a cation-exchange cleanup procedure. Quantitation was accomplished using isotope dilution with deuterium-labelled BMAA as internal standard. An LOD for BMAA in solution of 0.8 ng mL -1 was attained, which was equivalent to 16 ng g -1 dry mass in samples using the specified extraction procedure. This was comparable with LC-MS/MS methods. The method displayed excellent resolution of amino acid isomers and had no interference from matrix components. The presence of BMAA in cycad, mussel and lobster samples was confirmed by CE-MS/MS, but not in an in-house cyanobacterial reference material, with quantitative results agreeing with those from LC-MS/MS. Graphical Abstract CE-MS separation and detection of BMAA, its isomers and the internal standard BMAA-d3.

  14. Effect on the K/sub m/ for radiosensitization at 00C of thiol depletion by diethylmaleate pretreatment: quantitative differences found using the radiation sensitizing agent misonidazole or oxygen

    International Nuclear Information System (INIS)

    Koch, C.J.; Stobbe, C.C.; Bump, E.A.

    1984-01-01

    Pretreatment of V79-WNRE cells with 150 μM diethylmaleate for 1 hr at 37 0 C caused a decrease in intracellular glutathione levels to approximately 10-15% of control levels. The cells could be washed free of diethylmaleate and held at 0 0 C for several hours without toxicity and with no increase in glutathione concentration, although the glutathione concentration rapidly increased to normal levels at higher temperatures. Glutathione depletion itself caused a small but consistent radiosensitization of hypoxic cells (dose enhancement ratio of 1.2). However glutathione depletion caused a profound change in the radiosensitizing efficiency of misonidazole, with a decrease in K/sub m/ of about sevenfold from 0.6 to 0.09 mM. In contrast, only a 2.5-fold decrease was found in the K/sub m/ for radiosensitization by oxygen with diethylmaleate pretreatment. These results suggest a fundamental problem with the conventional theory of radiosensitivity whereby one considers a first-order competition for reaction with target radicals between radical-fixing versus radical-repairing species. It also suggests difficulties in the interpretation of glutathione as the only endogenous protective species

  15. GREET Pretreatment Module

    Energy Technology Data Exchange (ETDEWEB)

    Adom, Felix K. [Argonne National Lab. (ANL), Argonne, IL (United States). Energy Systems Division; Dunn, Jennifer B. [Argonne National Lab. (ANL), Argonne, IL (United States). Energy Systems Division; Han, Jeongwoo [Argonne National Lab. (ANL), Argonne, IL (United States). Energy Systems Division

    2014-09-01

    A wide range of biofuels and biochemicals can be produced from cellulosic biomass via different pretreatment technologies that yield sugars. Process simulations of dilute acid and ammonia fiber expansion pretreatment processes and subsequent hydrolysis were developed in Aspen Plus for four lignocellulosic feedstocks (corn stover, miscanthus, switchgrass, and poplar). This processing yields sugars that can be subsequently converted to biofuels or biochemical. Material and energy consumption data from Aspen Plus were then compiled in a new Greenhouses Gases, Regulated Emissions, and Energy Use in Transportation (GREETTM) pretreatment module. The module estimates the cradle-to-gate fossil energy consumption (FEC) and greenhouse gas (GHG) emissions associated with producing fermentable sugars. This report documents the data and methodology used to develop this module and the cradle-to-gate FEC and GHG emissions that result from producing fermentable sugars.

  16. Ultratrace level determination and quantitative analysis of kidney injury biomarkers in patient samples attained by zinc oxide nanorods

    Science.gov (United States)

    Singh, Manpreet; Alabanza, Anginelle; Gonzalez, Lorelis E.; Wang, Weiwei; Reeves, W. Brian; Hahm, Jong-In

    2016-02-01

    Determining ultratrace amounts of protein biomarkers in patient samples in a straightforward and quantitative manner is extremely important for early disease diagnosis and treatment. Here, we successfully demonstrate the novel use of zinc oxide nanorods (ZnO NRs) in the ultrasensitive and quantitative detection of two acute kidney injury (AKI)-related protein biomarkers, tumor necrosis factor (TNF)-α and interleukin (IL)-8, directly from patient samples. We first validate the ZnO NRs-based IL-8 results via comparison with those obtained from using a conventional enzyme-linked immunosorbent method in samples from 38 individuals. We further assess the full detection capability of the ZnO NRs-based technique by quantifying TNF-α, whose levels in human urine are often below the detection limits of conventional methods. Using the ZnO NR platforms, we determine the TNF-α concentrations of all 46 patient samples tested, down to the fg per mL level. Subsequently, we screen for TNF-α levels in approximately 50 additional samples collected from different patient groups in order to demonstrate a potential use of the ZnO NRs-based assay in assessing cytokine levels useful for further clinical monitoring. Our research efforts demonstrate that ZnO NRs can be straightforwardly employed in the rapid, ultrasensitive, quantitative, and simultaneous detection of multiple AKI-related biomarkers directly in patient urine samples, providing an unparalleled detection capability beyond those of conventional analysis methods. Additional key advantages of the ZnO NRs-based approach include a fast detection speed, low-volume assay condition, multiplexing ability, and easy automation/integration capability to existing fluorescence instrumentation. Therefore, we anticipate that our ZnO NRs-based detection method will be highly beneficial for overcoming the frequent challenges in early biomarker development and treatment assessment, pertaining to the facile and ultrasensitive quantification

  17. Quantitative determination of pneumococcal capsular polysaccharide serotype 14 using a modification of phenol-sulfuric acid method.

    Science.gov (United States)

    Cuesta, Gabriela; Suarez, Norma; Bessio, Maria I; Ferreira, Fernando; Massaldi, Hugo

    2003-01-01

    The capsular polysaccharide of Streptococcus pneumoniae, serotype 14, is part of every pneumococcal vaccine presently in the market or under development. A strategy for the quantitative determination of this polysaccharide by the phenol-sulfuric acid method is described. The modality of acid addition is shown to be the critical step for obtaining reproducible test results between different technicians. Raising the incubation temperature above 80 degrees C increased the consistency of the method by more than 60% regardless of the acid addition modality, but at the expense of some loss of sensitivity. Incubation at 110 degrees C was found necessary to obtain reproducible results within 3% for this technique, which was used to follow the enrichment of the polysaccharide during the last steps of purification. A model mixture of the component polysaccharide sugars provided an adequate and economic standard to construct the calibration curve for this assay, with absorbance reading either in the reaction tubes or in a microplate. A similar procedure may be applied to the determination of other bacterial polysaccharides as well.

  18. Quantitative investigation on the critical thickness of the dielectric shell for metallic nanoparticles determined by the plasmon decay length

    Science.gov (United States)

    Li, Anran; Lim, Xinyi; Guo, Lin; Li, Shuzhou

    2018-04-01

    Inert dielectric shells coating the surface of metallic nanoparticles (NPs) are important for enhancing the NPs’ stability, biocompatibility, and realizing targeting detection, but they impair NPs’ sensing ability due to the electric fields damping. The dielectric shell not only determines the distance of the analyte from the NP surface, but also affects the field decay. From a practical point of view, it is extremely important to investigate the critical thickness of the shell, beyond which the NPs are no longer able to effectively detect the analytes. The plasmon decay length of the shell-coated NPs determines the critical thickness of the coating layer. Extracting from the exponential fitting results, we quantitatively demonstrate that the critical thickness of the shell exhibits a linear dependence on the NP volume and the dielectric constants of the shell and the surrounding medium, but only with a small variation influenced by the NP shape where the dipole resonance is dominated. We show the critical thickness increases with enlarging the NP sizes, or increasing the dielectric constant differences between the shell and surrounding medium. The findings are essential for applications of shell-coated NPs in plasmonic sensing.

  19. Quantitative determination by HPLC of ent-kaurenoic and grandiflorenic acids in aerial parts of Wedelia paludosa D.C.

    Directory of Open Access Journals (Sweden)

    R. Batista

    Full Text Available There are several reports of biological activity for kaurenoic acid (1, which is found in the aerial parts of Wedelia paludosa D.C., a herbaceous plant of the Asteraceae family abundant in Brazil, and that contains grandiflorenic acid (2 also. Both of these diterpenes were shown to cause lysis of trypomastigotes of the protozoa Trypanosoma cruzi, the causative agent of Chagas' disease (American trypanosomiasis. This paper reports the quantitative determination of these diterpene acids in the aerial parts of W. paludosa by an isocratic RP-HPLC method employing 60% acetonitrile in water and UV detection (220 nm. Kaurenoic acid (1 was found to be more abundant (0.85 ± 0.08% while the amount of grandiflorenic acid (2 determined was almost three times lower (0.32 ± 0.02%. No significant seasonal variation was observed for these compounds in W. paludosa growing in Belo Horizonte (MG, Brazil what points out to the aerial parts of this species are a good source of these biologically active diterpenes along all the year.

  20. The PEG-switch assay: a fast semi-quantitative method to determine protein reversible cysteine oxidation.

    Science.gov (United States)

    Burgoyne, Joseph Robert; Oviosu, Olujimi; Eaton, Philip

    2013-01-01

    Reversible protein cysteine oxidation is recognised as a pivotal post-transitional modification that transduces physiological as well as pathological signalling. Pharmacological interventions that target specific sources of oxidant formation are currently being trialled to ascertain their potential ability to prevent disease progression. To determine the selectivity of such pharmacological treatments and to indentify new drug targets, a suitable method is required to detect target cysteine oxidation. Using a polyethylene glycol (PEG)-based alkylating agent the reversible oxidation of target proteins can be determined using a novel switch method. After reduction and specific labelling of reversibly oxidised thiols with a 'heavy' PEG-tag, samples are resolved on sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) gels, Western blotted and immunostained for protein(s) of interest. A mobility shift in a target protein following PEG-alkylation correlates with the reversible oxidative modification. The oxidation of cAMP- and cGMP-dependent protein kinases was detected using the PEG-switch assay in Langendorff-perfused hearts after hydrogen peroxide was administered. The PEG-switch assay is a fast effective semi-quantitative method for measuring target reversible cysteine oxidation in complex protein mixtures derived from tissue or cultured cells. © 2013.

  1. Determination of Appropriate Service Delivery Level for Quantitative Attributes of Household Toilets in Rural Settlements of India from Users' Perspective

    Science.gov (United States)

    Rashid, Mohammad; Pandit, Debapratim

    2018-04-01

    Improvement of quality of sanitation services in rural settlements is an important development goal in developing countries including India and accordingly several strategies are adopted which promote the demand and use of household toilets through creating awareness and providing subsidies to poor people for construction of household toilets with service-level standards specified from experts' perspective. In many cases, users are unsatisfied with the quality of toilets constructed using subsidies and the same remain unused. Users' satisfaction depends on their perceptions of service quality of individual attributes and overall service quality of the household toilets, which is an important determinant of sustainability and sustained use of toilets. This study aims to assess and benchmark the appropriate service delivery level for quantitative attributes of rural household toilets based on user perception. The service quality is determined with the help of level of service (LOS) scales developed using successive interval scaling technique, the zone of tolerance (ZOT), and users satisfaction level (USL) which relates service delivery levels with user satisfaction directly. The study finds that the service quality of most of the attributes of household toilets constructed using subsidies is perceived as poor. The results also suggest that most of the users expect to have a toilet with the service level of attributes ranging between LOS A and LOS B.

  2. Automated and quantitative headspace in-tube extraction for the accurate determination of highly volatile compounds from wines and beers.

    Science.gov (United States)

    Zapata, Julián; Mateo-Vivaracho, Laura; Lopez, Ricardo; Ferreira, Vicente

    2012-03-23

    An automatic headspace in-tube extraction (ITEX) method for the accurate determination of acetaldehyde, ethyl acetate, diacetyl and other volatile compounds from wine and beer has been developed and validated. Method accuracy is based on the nearly quantitative transference of volatile compounds from the sample to the ITEX trap. For achieving that goal most methodological aspects and parameters have been carefully examined. The vial and sample sizes and the trapping materials were found to be critical due to the pernicious saturation effects of ethanol. Small 2 mL vials containing very small amounts of sample (20 μL of 1:10 diluted sample) and a trap filled with 22 mg of Bond Elut ENV resins could guarantee a complete trapping of sample vapors. The complete extraction requires 100 × 0.5 mL pumping strokes at 60 °C and takes 24 min. Analytes are further desorbed at 240 °C into the GC injector under a 1:5 split ratio. The proportion of analytes finally transferred to the trap ranged from 85 to 99%. The validation of the method showed satisfactory figures of merit. Determination coefficients were better than 0.995 in all cases and good repeatability was also obtained (better than 7% in all cases). Reproducibility was better than 8.3% except for acetaldehyde (13.1%). Detection limits were below the odor detection thresholds of these target compounds in wine and beer and well below the normal ranges of occurrence. Recoveries were not significantly different to 100%, except in the case of acetaldehyde. In such a case it could be determined that the method is not able to break some of the adducts that this compound forms with sulfites. However, such problem was avoided after incubating the sample with glyoxal. The method can constitute a general and reliable alternative for the analysis of very volatile compounds in other difficult matrixes. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Advances in aluminum pretreatment

    Energy Technology Data Exchange (ETDEWEB)

    Sudour, Michel; Maintier, Philippe [PPG Industries France, 3 Z.A.E. Les Dix Muids, B.P. 89, F-59583 Marly (France); Simpson, Mark [PPG Industries Inc., 1200 Piedmont Troy, Michigan 48083 (United States); Quaglia, Paolo [PPG Industries Italia, Via Garavelli 21, I-15028 Quattordio (Italy)

    2004-07-01

    As automotive manufacturers continue to look for ways to reduce vehicle weight, aluminum is finding more utility as a body panel component. The substitution of cold-rolled steel and zinc-coated substrates with aluminum has led to new challenges in vehicle pretreatment. As a result, changes to traditional pretreatment chemistries and operating practices are necessary in order to produce an acceptable coating on aluminum body panels. These changes result in increased sludging and other undesirable characteristics. In addition to the chemistry changes, there are also process-related problems to consider. Many existing automotive pretreatment lines simply were not designed to handle aluminum and its increased demands on filtration and circulation equipment. To retrofit such a system is capital intensive and in addition to requiring a significant amount of downtime, may not be totally effective. Thus, the complexities of pre-treating aluminum body panels have actually had a negative effect on efforts to introduce more aluminum into new vehicle design programs. Recent research into ways of reducing the negative effects has led to a new understanding of the nature of zinc phosphate bath -aluminum interactions. Many of the issues associated with the pretreatment of aluminum have been identified and can be mitigated with only minor changes to the zinc phosphate bath chemistry. The use of low levels of soluble Fe ions, together with free fluoride, has been shown to dramatically improve the efficiency of a zinc phosphate system processing aluminum. Appearance of zinc phosphate coatings, coating weights and sludge are all benefited by this chemistry change. (authors)

  4. Acetic acid pretreatment improves the hardness of cooked potato slices.

    Science.gov (United States)

    Zhao, Wenlin; Shehzad, Hussain; Yan, Shoulei; Li, Jie; Wang, Qingzhang

    2017-08-01

    The effects of acetic acid pretreatment on the texture of cooked potato slices were investigated in this work. Potato slices were pretreated with acetic acid immersion (AAI), distilled water immersion (DWI), or no immersion (NI). Subsequently, the cell wall material of the pretreated samples was isolated and fractioned to evaluate changes in the monosaccharide content and molar mass (MM), and the hardness and microscopic structure of the potato slices in different pretreatments before and after cooking were determined. The results showed that the highest firmness was obtained with more intact structure of the cell wall for cooked potato slices with AAI pretreatment. Furthermore, the MM and sugar ratio demonstrated that the AAI pretreated potato slices contained a higher content of the small molecular polysaccharides of cell walls, especially in the hemicellulose fraction. This work may provide a reference for potato processing. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Rapid and Quantitative Determination of S-Adenosyl-L-Methionine in the Fermentation Process by Surface-Enhanced Raman Scattering

    Directory of Open Access Journals (Sweden)

    Hairui Ren

    2016-01-01

    Full Text Available Concentrations of S-Adenosyl-L-Methionine (SAM in aqueous solution and fermentation liquids were quantitatively determined by surface-enhanced Raman scattering (SERS and verified by high-pressure liquid chromatography (HPLC. The Ag nanoparticle/silicon nanowire array substrate was fabricated and employed as an active SERS substrate to indirectly measure the SAM concentration. The linear relationship between the integrated intensity of peak centered at ~2920 cm−1 in SERS spectra and the SAM concentration was established, and the limit of detections of SAM concentrations was analyzed to be ~0.1 g/L. The concentration of SAM in real solution could be predicted by the linear relationship and verified by the HPLC detection method. The relative deviations (δ of the predicted SAM concentration are less than 13% and the correlation coefficient is 0.9998. Rolling-Circle Filter was utilized to subtract fluorescence background and the optimal results were obtained when the radius of the analyzing circle is 650 cm−1.

  6. Rapid and quantitative determination of 10 major active components in Lonicera japonica Thunb. by ultrahigh pressure extraction-HPLC/DAD

    Science.gov (United States)

    Fan, Li; Lin, Changhu; Duan, Wenjuan; Wang, Xiao; Liu, Jianhua; Liu, Feng

    2015-01-01

    An ultrahigh pressure extraction (UPE)-high performance liquid chromatography (HPLC)/diode array detector (DAD) method was established to evaluate the quality of Lonicera japonica Thunb. Ten active components, including neochlorogenic acid, chlorogenic acid, 4-dicaffeoylquinic acid, caffeic acid, rutin, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and quercetin, were qualitatively evaluated and quantitatively determined. Scanning electron microscope images elucidated the bud surface microstructure and extraction mechanism. The optimal extraction conditions of the UPE were 60% methanol solution, 400 MPa of extraction pressure, 3 min of extraction time, and 1:30 (g/mL) solid:liquid ratio. Under the optimized conditions, the total extraction yield of 10 active components was 57.62 mg/g. All the components showed good linearity (r2 ≥ 0.9994) and recoveries. This method was successfully applied to quantify 10 components in 22 batches of L. japonica samples from different areas. Compared with heat reflux extraction and ultrasonic-assisted extraction, UPE can be considered as an alternative extraction technique for fast extraction of active ingredient from L. japonica.

  7. Fracture threshold in the femur and tibia of people with spinal cord injury as determined by peripheral quantitative computed tomography.

    Science.gov (United States)

    Eser, Prisca; Frotzler, Angela; Zehnder, Yvonne; Denoth, Jachen

    2005-03-01

    To determine bone traits of the femur and tibia with peripheral quantitative computed tomography (pQCT) that best distinguish between spinal cord injury (SCI) subjects with and without fractures. Cross-sectional study. In- and outpatient paraplegic center in Switzerland. Ninety-nine motor complete SCI subjects (duration of paralysis, 2 mo-49 y), 21 of whom had sustained fractures of the femur or tibia. Not applicable. Subjects with SCI were questioned about the occurrence, location, and approximate date of fractures to their lower extremities. Trabecular and cortical bone mineral density (BMD), as well as bone geometric properties of distal epiphyses and midshafts of the femur and tibia, were measured by pQCT. Trabecular BMD of the femur and tibia distal epiphyses was found to distinguish best subjects with fractures from those without. Fractures occurred in subjects with trabecular BMD of less than 114 mg/cm 3 and less than 72 mg/cm 3 for the femoral and tibial distal epiphysis, respectively (corresponding to 46% and 29% of mean values of an able-bodied reference group). Approximately 50% of the subjects with chronic SCI (defined as time postinjury >5 y for femur data and >7 y for tibia data) had trabecular BMD values above the fracture threshold in the femur and about one third above the fracture threshold in the tibia. By using pQCT, it may be possible to identify subjects with SCI who are at risk of sustaining fractures of the femur and tibia through minor trauma.

  8. The Rapid and Sensitive Quantitative Determination of Galactose by Combined Enzymatic and Colorimetric Method: Application in Neonatal Screening.

    Science.gov (United States)

    Kianmehr, Anvarsadat; Mahrooz, Abdolkarim; Ansari, Javad; Oladnabi, Morteza; Shahbazmohammadi, Hamid

    2016-05-01

    The quantitative measurement of galactose in blood is essential for the early diagnosis, treatment, and dietary monitoring of galactosemia patients. In this communication, we aimed to develop a rapid, sensitive, and cost-effective combined method for galactose determination in dry blood spots. This procedure was based on the combination of enzymatic reactions of galactose dehydrogenase (GalDH), dihydrolipoyl dehydrogenase (DLD), and alkaline phosphates with a colorimetric system. The incubation time and the concentration of enzymes used in new method were also optimized. The analytical performance was studied by the precision, recovery, linearity, and sensitivity parameters. Statistical analysis was applied to method comparison experiment. The regression equation and correlation coefficient (R (2)) were Y = 0.0085x + 0.032 and R (2) = 0.998, respectively. This assay exhibited a recovery in the range of 91.7-114.3 % and had the limit detection of 0.5 mg/dl for galactose. The between-run coefficient of variation (CV) was between 2.6 and 11.1 %. The within-run CV was between 4.9 and 9.2 %. Our results indicated that the new and reference methods were in agreement because no significant biases exist between them. Briefly, a quick and reliable combined enzymatic and colorimetric assay was presented for application in newborn mass screening and monitoring of galactosemia patients.

  9. Quantitative determination of sulfur containing wine odorants at sub-ppb levels. 1. Synthesis of the deuterated analogues.

    Science.gov (United States)

    Kotseridis, Y; Ray, J L; Augier, C; Baumes, R

    2000-12-01

    [2H10]-4-Sulfanyl-4-methylpentan-2-one (d10-SMP), [2H2]-3-sulfanylhexan-1-ol (d2-3SH), and [2H5]-3-sulfanylhexyl acetate (d5-3SHAc), the labeled analogues of impact odorants of wines and other foods, were synthesized to be used for the quantitative determination of the natural compounds in white and red wines by stable isotope dilution assay. The sulfidation was achieved by Michael addition, on mesityl oxide or ethyl hex-2-enoate, respectively, of the sulfhydryl anion generated in situ from triphenylsilanethiol and potassium fluoride under phase transfer conditions. The labeling of 4-sulfanyl-4-methylpentan-2-one (SMP) was obtained from the commercial starting material, [2H6]acetone, so that this method could be used to synthesize 13C-labeled SMP from 13C-labeled acetone. The labeling of 3-sulfanylhexan-1-ol (3SH) and 3-sulfanylhexyl acetate (3SHAc) was obtained from reduction with lithium aluminum deuteride of the Michael adduct ethyl 3-sulfanylhexanoate and [2H3]-acetylation. During the synthesis, 3SH and 3SHAc were partially oxidized to their disulfide, which were reduced back to the thiols by an additional reduction step; the tertiary thiol SMP was less sensitive to this oxidation.

  10. A quantitative method for determining a representative detection limit of the forensic luminol test for latent bloodstains.

    Science.gov (United States)

    Cassidy, Brianna M; Lu, Zhenyu; Martin, Jennifer P; Tazik, Shawna K; Kellogg, Katie W; DeJong, Stephanie A; Belliveau, Elle O; Kilgore, Katherine E; Ervin, Samantha M; Meece-Rayle, Mackenzie; Abraham, Alyssa M; Myrick, Michael L; Morgan, Stephen L

    2017-09-01

    The luminol test has been used for over 60 years by forensic investigators for presumptive identification of blood and visualization of blood splatter patterns. Multiple studies have estimated the limit of detection (LD) for bloodstains when luminol is employed, with results ranging from 100× to 5,000,000× dilute. However, these studies typically have not identified and controlled important experimental variables which may affect the luminol LD for bloodstains. Without control of experimental parameters in the laboratory, variables which affect the potential of presumptive bloodstain test methods remain largely unknown, and comparisons required to establish new, more powerful detection methods are simply impossible. We have developed a quantitative method to determine the relationship between the amount of blood present and its reaction with luminol by measuring, under controlled conditions, the resulting chemiluminescent intensity with a video camera, combined with processing of the digital intensity data. The method resulted in an estimated LD for bloodstains on cotton fabric at ∼200,000× diluted blood with a specific luminol formulation. Although luminol is the focus of this study, the experimental protocol used could be modified to study effects of variables using other blood detection reagents. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Quantitative determination of optical and recombination losses in thin-film photovoltaic devices based on external quantum efficiency analysis

    Energy Technology Data Exchange (ETDEWEB)

    Nakane, Akihiro; Tamakoshi, Masato; Fujimoto, Shohei; Fujiwara, Hiroyuki, E-mail: fujiwara@gifu-u.ac.jp [Department of Electrical, Electronic and Computer Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193 (Japan); Tampo, Hitoshi; Kim, Kang Min; Kim, Shinho; Shibata, Hajime; Niki, Shigeru [Research Center for Photovoltaics, National Institute of Advanced Industrial Science and Technology (AIST), Central 2, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8568 (Japan)

    2016-08-14

    In developing photovoltaic devices with high efficiencies, quantitative determination of the carrier loss is crucial. In conventional solar-cell characterization techniques, however, photocurrent reduction originating from parasitic light absorption and carrier recombination within the light absorber cannot be assessed easily. Here, we develop a general analysis scheme in which the optical and recombination losses in submicron-textured solar cells are evaluated systematically from external quantum efficiency (EQE) spectra. In this method, the optical absorption in solar cells is first deduced by imposing the anti-reflection condition in the calculation of the absorptance spectrum, and the carrier extraction from the light absorber layer is then modeled by considering a carrier collection length from the absorber interface. Our analysis method is appropriate for a wide variety of photovoltaic devices, including kesterite solar cells [Cu{sub 2}ZnSnSe{sub 4}, Cu{sub 2}ZnSnS{sub 4}, and Cu{sub 2}ZnSn(S,Se){sub 4}], zincblende CdTe solar cells, and hybrid perovskite (CH{sub 3}NH{sub 3}PbI{sub 3}) solar cells, and provides excellent fitting to numerous EQE spectra reported earlier. Based on the results obtained from our EQE analyses, we discuss the effects of parasitic absorption and carrier recombination in different types of solar cells.

  12. Development and Validation of Quantitative (1)H NMR Spectroscopy for the Determination of Total Phytosterols in the Marine Seaweed Sargassum.

    Science.gov (United States)

    Zhang, Xiu-Li; Wang, Cong; Chen, Zhen; Zhang, Pei-Yu; Liu, Hong-Bing

    2016-08-10

    Knowledge of phytosterol (PS) contents in marine algae is currently lacking compared to those in terrestrial plants. The present studies developed a quantitative (1)H NMR method for the determination of the total PSs in Sargassum. The characteristic proton signal H-3α in PSs was used for quantification, and 2,3,4,5-tetrachloro-nitrobenzene was used as an internal standard. Seaweed samples could be recorded directly after total lipid extraction and saponification. The results showed that the PS contents in Sargassum fusiforme (788.89-2878.67 mg/kg) were significantly higher than those in Sargassum pallidum (585.33-1596.00 mg/kg). The variable contents in both species suggested that fixed raw materials are very important for future research and development. Orthogonal projection to latent structures discriminant analysis was carried out in the spectral region of δ 3.00-6.50 in the (1)H NMR spectrum. S. fusiforme and S. pallidum could be separated well, and the key sterol marker was fucosterol.

  13. Comparison of dilute mineral and organic acid pretreatment for enzymatic hydrolysis of wheat straw

    NARCIS (Netherlands)

    Kootstra, A.M.J.; Beeftink, H.H.; Scott, E.L.; Sanders, J.P.M.

    2009-01-01

    The efficiencies of fumaric, maleic, and sulfuric acid in wheat straw pretreatment were compared. As a measure for pretreatment efficiency, enzymatic digestibility of the lignocellulose was determined. Monomeric glucose and xylose concentrations were measured after subsequent enzymatic hydrolysis,

  14. Nonhazardous Urine Pretreatment Method

    Science.gov (United States)

    Akse, James R.; Holtsnider, John T.

    2012-01-01

    A method combines solid phase acidification with two non-toxic biocides to prevent ammonia volatilization and microbial proliferation. The safe, non-oxidizing biocide combination consists of a quaternary amine and a food preservative. This combination has exhibited excellent stabilization of both acidified and unacidified urine. During pretreatment tests, composite urine collected from donors was challenged with a microorganism known to proliferate in urine, and then was processed using the nonhazardous urine pre-treatment method. The challenge microorganisms included Escherichia coli, a common gram-negative bacteria; Enterococcus faecalis, a ureolytic gram-positive bacteria; Candida albicans, a yeast commonly found in urine; and Aspergillus niger, a problematic mold that resists urine pre-treatment. Urine processed in this manner remained microbially stable for over 57 days. Such effective urine stabilization was achieved using non-toxic, non-oxidizing biocides at higher pH (3.6 to 5.8) than previous methods in use or projected for use aboard the International Space Station (ISS). ISS urine pretreatment methods employ strong oxidants including ozone and hexavalent chromium (Cr(VI)), a carcinogenic material, under very acidic conditions (pH = 1.8 to 2.4). The method described here offers a much more benign chemical environment than previous pretreatment methods, and will lower equivalent system mass (ESM) by reducing containment volume and mass, system complexity, and crew time needed to handle pre-treatment chemicals. The biocides, being non-oxidizing, minimize the potential for chemical reactions with urine constituents to produce volatile, airborne contaminants such as cyanogen chloride. Additionally, the biocides are active under significantly less acidic conditions than those used in the current system, thereby reducing the degree of required acidification. A simple flow-through solid phase acidification (SPA) bed is employed to overcome the natural buffering

  15. Quantitative determination of carbonaceous particle mixing state in Paris using single-particle mass spectrometer and aerosol mass spectrometer measurements

    Directory of Open Access Journals (Sweden)

    R. M. Healy

    2013-09-01

    Full Text Available Single-particle mixing state information can be a powerful tool for assessing the relative impact of local and regional sources of ambient particulate matter in urban environments. However, quantitative mixing state data are challenging to obtain using single-particle mass spectrometers. In this study, the quantitative chemical composition of carbonaceous single particles has been determined using an aerosol time-of-flight mass spectrometer (ATOFMS as part of the MEGAPOLI 2010 winter campaign in Paris, France. Relative peak areas of marker ions for elemental carbon (EC, organic aerosol (OA, ammonium, nitrate, sulfate and potassium were compared with concurrent measurements from an Aerodyne high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS, a thermal–optical OCEC analyser and a particle into liquid sampler coupled with ion chromatography (PILS-IC. ATOFMS-derived estimated mass concentrations reproduced the variability of these species well (R2 = 0.67–0.78, and 10 discrete mixing states for carbonaceous particles were identified and quantified. The chemical mixing state of HR-ToF-AMS organic aerosol factors, resolved using positive matrix factorisation, was also investigated through comparison with the ATOFMS dataset. The results indicate that hydrocarbon-like OA (HOA detected in Paris is associated with two EC-rich mixing states which differ in their relative sulfate content, while fresh biomass burning OA (BBOA is associated with two mixing states which differ significantly in their OA / EC ratios. Aged biomass burning OA (OOA2-BBOA was found to be significantly internally mixed with nitrate, while secondary, oxidised OA (OOA was associated with five particle mixing states, each exhibiting different relative secondary inorganic ion content. Externally mixed secondary organic aerosol was not observed. These findings demonstrate the range of primary and secondary organic aerosol mixing states in Paris. Examination of the

  16. Effects of magnetic fields pretreatment of mungbean seeds on sprout ...

    African Journals Online (AJOL)

    Effects of magnetic fields pretreatment of mungbean seeds on sprout yield and quality. Yi-Ping Chen, Jun-Min He, Ran Li. Abstract. The aim of this investigation was to determine the effect of magnetic field pretreatment of mungbean seeds on the yield and quality of sprout. The sprout elongation, biomass and nutrition ...

  17. [Application of near infrared spectroscopy to qualitative identification and quantitative determination of Puccinia strii formis f. sp. tritici and P. recondita f. sp. tritici].

    Science.gov (United States)

    Li, Xiao-Long; Ma, Zhan-Hong; Zhao, Long-Lian; Li, Jun-Hui; Wang, Hai-Guang

    2014-03-01

    To realize qualitative identification and quantitative determination of Puccinia strii formis f. sp. tritici (Pst) and P. recondita f. sp. tritici (Prt), a qualitative identification model was built using near infrared reflectance spectroscopy (NIRS) combined with distinguished partial least squares (DPLS), and a quantitative determination model was built using NIRS combined with quantitative partial least squares (QPLS). In this study, 100 pure samples including 50 samples of Pst and 50 samples of Prt were obtained, and 120 mixed samples including three replicates of mixed urediospores of the two kinds of pathogen in different proportions (the content of Pst was within the range of 2. 5% 100% with 2. 5% as the gradient) were obtained. Then the spectra of the samples were collected using MPA spectrometer, respectively. Both pure samples and mixed samples were divided into training set and testing set with the ratio equal to 2:1. Qualitative identification model and quantitative determination model were built using internal cross-validation method in the spectral region 4,000--10,000 cm(-1) based on the training sets from pure samples and mixed samples, respectively. The results showed that the identification rates of the Pst-Prt qualitative identification model for training set and testing set were both up to 100. 00% when scatter correction was used as the preprocessing method of the spectra and the number of principal components was 3. When 'range normalization + scatter correction' was used as the preprocessing method of the spectra and the number of principal components was 6, determination coefficient (RZ), standard error of calibration (SEC) and average absolute relative deviation(AARD) of the Pst-Prt quantitative determination model for training set were 99.36%, 2.31% and 8.94%, respectively, and R2, standard error of prediction (SEP) and AARD for testing set were 99.37%, 2.29% and 5. 0%, respectively. The results indicated that qualitative identification

  18. Biomass shock pretreatment

    Science.gov (United States)

    Holtzapple, Mark T.; Madison, Maxine Jones; Ramirez, Rocio Sierra; Deimund, Mark A.; Falls, Matthew; Dunkelman, John J.

    2014-07-01

    Methods and apparatus for treating biomass that may include introducing a biomass to a chamber; exposing the biomass in the chamber to a shock event to produce a shocked biomass; and transferring the shocked biomass from the chamber. In some aspects, the method may include pretreating the biomass with a chemical before introducing the biomass to the chamber and/or after transferring shocked biomass from the chamber.

  19. Enzymatic hydrolysis of pretreated soybean straw

    International Nuclear Information System (INIS)

    Xu Zhong; Wang Qunhui; Jiang Zhaohua; Yang Xuexin; Ji Yongzhen

    2007-01-01

    In order to produce lactic acid, from agricultural residues such as soybean straw, which is a raw material for biodegradable plastic production, it is necessary to decompose the soybean straw into soluble sugars. Enzymatic hydrolysis is one of the methods in common use, while pretreatment is the effective way to increase the hydrolysis rate. The optimal conditions of pretreatment using ammonia and enzymatic hydrolysis of soybean straw were determined. Compared with the untreated straw, cellulose in straw pretreated by ammonia liquor (10%) soaking for 24 h at room temperature increased 70.27%, whereas hemicellulose and lignin in pretreated straw decreased to 41.45% and 30.16%, respectively. The results of infrared spectra (IR), scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis also showed that the structure and the surface of the straw were changed through pretreatment that is in favor of the following enzymatic hydrolysis. maximum enzymatic hydrolysis rate of 51.22% was achieved at a substrate concentration of 5% (w/v) at 50 deg. C and pH 4.8 using cellulase (50 fpu/g of substrate) for 36 h

  20. [Role of quantitative perfusion scintigraphy evaluation in determination of the efficiency of the procedure before lung volume reduction coil treatment for severe emphysema].

    Science.gov (United States)

    Yıldız, Fidan

    2017-06-01

    Lung volume reduction coil (LVRC) is a new treatment method which exercise capacities among the patients with severe emphysema. In order to determine the emphysema distribution before LVRC treatment, we examined the contribution of combination of the high resolution computed tomography (HRCT) of the lung and the quantitative perfusion scintigraphy to the efficiency of the procedure. The study was conducted retrospectively. The densitometry analysis and scores of emphysema areas of the patients who were found suitable for LVRC treatment in HRCT were determined. Before the procedure, the quantitative lung perfusion scintigraphies were taken. Lobes which had high emphysema score and in which a decrease perfusion was observed in quantitative perfusion scintigraphy were determined as treatment areas. A total of 22 patients were treated. In HRCT it was observed that perfusion decreased in lobes in which the emphysema damage scoring was high. A significant statistical difference was found between pre-and post- procedure measurements in terms of FEV 1 , RV, and TLC (pdifference was found as 45.4 ± 23.9 m (p= 0.000). No significant difference was determined between perfusion ratios before the procedure and perfusion ratios after the procedure. The quantitative perfusion scintigraphy taken before LVRC treatment in severe emphysema patients guides to determine the target lobe for treatment and makes contribution to the efficiency of the procedure.

  1. A new cineol derivative, polyphenols and norterpenoids from Saharan myrtle tea (Myrtus nivellei): Isolation, structure determination, quantitative determination and antioxidant activity.

    Science.gov (United States)

    Mansour, Amira; Celano, Rita; Mencherini, Teresa; Picerno, Patrizia; Piccinelli, Anna Lisa; Foudil-Cherif, Yazid; Csupor, Dezső; Rahili, Ghania; Yahi, Nassima; Nabavi, Seyed Mohammad; Aquino, Rita Patrizia; Rastrelli, Luca

    2017-06-01

    The phytochemical profile of decoction and infusion, obtained from the dried leaves of M. nivellei, consumed as tea in Saharan region, was characterized by UHPLC-PDA-HRMS. Fourteen compounds were characterized and, to confirm the proposed structures a preparative procedure followed by NMR spectroscopy was applied. Compound 3 (2-hydroxy-1,8-cineole disaccharide) was a never reported whereas a bicyclic monoterpenoid glucoside (2), two ionol glucosides (1 and 12), a tri-galloylquinic acid (4), two flavonol glycosides (5 and 9), and a tetra-galloylglucose (7), were reported in Myrtus spp. for the first time. Five flavonol O-glycosides (6, 8, 10-11, and 14) togheter a flavonol (13) were also identified. Quantitative determination of phenolic constituents from decoction and infusion has been performed by HPLC-UV-PDA. The phenolic content was found to be 150.5 and 102.6mg/g in decoction and infusion corresponding to 73.8 and 23.6mg/100mL of a single tea cup, respectively. Myricetin 3-O-β-d-(6″-galloyl)glucopyranoside (5), isomyricitrin (6) and myricitrin (8) were the compounds present in the highest concentration. The free-radical scavenging activities of teas and isolated compounds was measured by the DPPH assay and compared with the values of other commonly used herbal teas (green and black teas). Decoction displayed higher potency in scavenging free-radicals than the infusion and green and black teas. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. SNPs and real-time quantitative PCR method for constitutional allelic copy number determination, the VPREB1 marker case

    Directory of Open Access Journals (Sweden)

    Costa Elena

    2011-05-01

    Full Text Available Abstract Background 22q11.2 microdeletion is responsible for the DiGeorge Syndrome, characterized by heart defects, psychiatric disorders, endocrine and immune alterations and a 1 in 4000 live birth prevalence. Real-time quantitative PCR (qPCR approaches for allelic copy number determination have recently been investigated in 22q11.2 microdeletions detection. The qPCR method was performed for 22q11.2 microdeletions detection as a first-level screening approach in a genetically unknown series of patients with congenital heart defects. A technical issue related to the VPREB1 qPCR marker was pointed out. Methods A set of 100 unrelated Italian patients with congenital heart defects were tested for 22q11.2 microdeletions by a qPCR method using six different markers. Fluorescence In Situ Hybridization technique (FISH was used for confirmation. Results qPCR identified six patients harbouring the 22q11.2 microdeletion, confirmed by FISH. The VPREB1 gene marker presented with a pattern consistent with hemideletion in one 3 Mb deleted patient, suggestive for a long distal deletion, and in additional five non-deleted patients. The long distal 22q11.2 deletion was not confirmed by Comparative Genomic Hybridization. Indeed, the VPREB1 gene marker generated false positive results in association with the rs1320 G/A SNP, a polymorphism localized within the VPREB1 marker reverse primer sequence. Patients heterozygous for rs1320 SNP, showed a qPCR profile consistent with the presence of a hemideletion. Conclusions Though the qPCR technique showed advantages as a screening approach in terms of cost and time, the VPREB1 marker case revealed that single nucleotide polymorphisms can interfere with qPCR data generating erroneous allelic copy number interpretations.

  3. Quantitative Determination of Fatty Acids in Marine Fish and Shellfish from Warm Water of Straits of Malacca for Nutraceutical Purposes

    Directory of Open Access Journals (Sweden)

    Nurnadia Abd Aziz

    2013-01-01

    Full Text Available This study was conducted to quantitatively determine the fatty acid contents of 20 species of marine fish and four species of shellfish from Straits of Malacca. Most samples contained fairly high amounts of polyunsaturated fatty acids (PUFAs, especially alpha-linolenic acid (ALA, C18:3 n3, eicosapentaenoic acid (EPA, C20:5 n3, and docosahexaenoic acid (DHA, C22:6 n3. Longtail shad, yellowstripe scad, and moonfish contained significantly higher (P<0.05 amounts of eicosapentaenoic acid (EPA, docosahexaenoic acid (DHA, and alpha-linolenic acid (ALA, respectively. Meanwhile, fringescale sardinella, malabar red snapper, black pomfret, Japanese threadfin bream, giant seaperch, and sixbar grouper showed considerably high content (537.2–944.1 mg/100g wet sample of desirable omega-3 fatty acids. The polyunsaturated-fatty-acids/saturated-fatty-acids (P/S ratios for most samples were higher than that of Menhaden oil (P/S=0.58, a recommended PUFA supplement which may help to lower blood pressure. Yellowstripe scad (highest DHA, ω-3/ω-6=6.4, P/S=1.7, moonfish (highest ALA, ω-3/ω-6=1.9, P/S=1.0, and longtail shad (highest EPA, ω-3/ω-6=0.8, P/S=0.4 were the samples with an outstandingly desirable overall composition of fatty acids. Overall, the marine fish and shellfish from the area contained good composition of fatty acids which offer health benefits and may be used for nutraceutical purposes in the future.

  4. Quantitative trait loci mapping and gene network analysis implicate protocadherin-15 as a determinant of brain serotonin transporter expression.

    Science.gov (United States)

    Ye, R; Carneiro, A M D; Han, Q; Airey, D; Sanders-Bush, E; Zhang, B; Lu, L; Williams, R; Blakely, R D

    2014-03-01

    Presynaptic serotonin (5-hydroxytryptamine, 5-HT) transporters (SERT) regulate 5-HT signaling via antidepressant-sensitive clearance of released neurotransmitter. Polymorphisms in the human SERT gene (SLC6A4) have been linked to risk for multiple neuropsychiatric disorders, including depression, obsessive-compulsive disorder and autism. Using BXD recombinant inbred mice, a genetic reference population that can support the discovery of novel determinants of complex traits, merging collective trait assessments with bioinformatics approaches, we examine phenotypic and molecular networks associated with SERT gene and protein expression. Correlational analyses revealed a network of genes that significantly associated with SERT mRNA levels. We quantified SERT protein expression levels and identified region- and gender-specific quantitative trait loci (QTLs), one of which associated with male midbrain SERT protein expression, centered on the protocadherin-15 gene (Pcdh15), overlapped with a QTL for midbrain 5-HT levels. Pcdh15 was also the only QTL-associated gene whose midbrain mRNA expression significantly associated with both SERT protein and 5-HT traits, suggesting an unrecognized role of the cell adhesion protein in the development or function of 5-HT neurons. To test this hypothesis, we assessed SERT protein and 5-HT traits in the Pcdh15 functional null line (Pcdh15(av-) (3J) ), studies that revealed a strong, negative influence of Pcdh15 on these phenotypes. Together, our findings illustrate the power of multidimensional profiling of recombinant inbred lines in the analysis of molecular networks that support synaptic signaling, and that, as in the case of Pcdh15, can reveal novel relationships that may underlie risk for mental illness. © 2014 John Wiley & Sons Ltd and International Behavioural and Neural Genetics Society.

  5. Sample pre-treatment to eliminate cationic methylated arsenic for determining arsenite on an anion-exchange column by high performance liquid chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Huang, Jen-How; Ilgen, Gunter; Decker, Berryinne

    2008-03-17

    Co-elution of cationic methylated arsenic, e.g. arsenobetaine may interfere with the determination of arsenite on the Hamilton PRP-X100 anion-exchange column using a phosphate buffer isocratically. Therefore, a sample pre-treatment method with self-packed AG MP-50 cation-exchange cartridges was proposed, which enables the arsenite determination in samples containing arsenobetaine on a PRP-X100 column using a phosphate buffer (pH 5.6) isocratically. Methylated arsenic, including dimethylarsinic acid, trimethylarsine oxide, tetramethylarsonium ion, arsenobetaine and arsenocholine, with concentrations below 1000microgAsL(-1), may be completely retained in the AG MP-50 cartridge without any changes of arsenite, arsenate and monomethylarsonic acid speciation. Such retention was independent of the pH and matrix. It is proposed to be based on hydrophobic interaction. With the help of AG MP-50 cartridges, 11 arsenic species were detected in fish (DORM-2), mussels (BCR-477) and red algae (Porphyra tenera) in 10min on the PRP-X100 column using a phosphate buffer isocratically. Arsenite was the only minor species (up to 0.9%) among all water extractable arsenic species in fish, mussel and red algae.

  6. Quantitative determination and validation of octreotide acetate using1H-NMR spectroscopy with internal standard method.

    Science.gov (United States)

    Yu, Chen; Zhang, Qian; Xu, Peng-Yao; Bai, Yin; Shen, Wen-Bin; Di, Bin; Su, Meng-Xiang

    2018-01-01

    Quantitative nuclear magnetic resonance (qNMR) is a well-established technique in quantitative analysis. We presented a validated 1 H-qNMR method for assay of octreotide acetate, a kind of cyclic octopeptide. Deuterium oxide was used to remove the undesired exchangeable peaks, which was referred to as proton exchange, in order to make the quantitative signals isolated in the crowded spectrum of the peptide and ensure precise quantitative analysis. Gemcitabine hydrochloride was chosen as the suitable internal standard. Experimental conditions, including relaxation delay time, the numbers of scans, and pulse angle, were optimized first. Then method validation was carried out in terms of selectivity, stability, linearity, precision, and robustness. The assay result was compared with that by means of high performance liquid chromatography, which is provided by Chinese Pharmacopoeia. The statistical F test, Student's t test, and nonparametric test at 95% confidence level indicate that there was no significant difference between these two methods. qNMR is a simple and accurate quantitative tool with no need for specific corresponding reference standards. It has the potential of the quantitative analysis of other peptide drugs and standardization of the corresponding reference standards. Copyright © 2017 John Wiley & Sons, Ltd.

  7. Rapid and simple pretreatment of human body fluids using electromembrane extraction across supported liquid membrane for capillary electrophoretic determination of lithium.

    Science.gov (United States)

    Strieglerová, Lenka; Kubáň, Pavel; Boček, Petr

    2011-05-01

    Electromembrane extraction was used for simultaneous sample cleanup and preconcentration of lithium from untreated human body fluids. The sample of a body fluid was diluted 100 times with 0.5 mM Tris solution and lithium was extracted by electromigration through a supported liquid membrane composed of 1-octanol into 100 mM acetic acid acceptor solution. Matrix compounds, such as proteins, red blood cells, and other high-molecular-weight compounds were efficiently retained on the supported liquid membrane. The liquid membrane was anchored in pores of a short segment of a polypropylene hollow fiber, which represented a low cost, single use, disposable extraction unit and was discarded after each use. Acceptor solutions were analyzed using capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C(4) D) and baseline separation of lithium was achieved in a background electrolyte solution consisting of 18 mM L-histidine and 40 mM acetic acid at pH 4.6. Repeatability of the electromembrane extraction-CE-C(4) D method was evaluated for the determination of lithium in standard solutions and real samples and was better than 0.6 and 8.2% for migration times and peak areas, respectively. The concentration limit of detection of 9 nM was achieved. The developed method was applied to the determination of lithium in urine, blood serum, blood plasma, and whole blood at both endogenous and therapeutic concentration levels. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Pre-Treatment of Platinum Resistant Ovarian Cancer Cells with an MMP-9/MMP-2 Inhibitor Prior to Cisplatin Enhances Cytotoxicity as Determined by High Content Screening

    Directory of Open Access Journals (Sweden)

    John J. O'Leary

    2013-01-01

    Full Text Available Platinum resistance is a major cause of treatment failure in ovarian cancer. We previously identified matrix metalloproteinase 9 (MMP-9 as a potential therapeutic target of chemoresistant disease. A2780cis (cisplatin-resistant and A2780 (cisplatin-sensitive ovarian carcinoma cell lines were used. The cytotoxic effect of MMP-9/MMP-2 inhibitor, (2R-2-[(4-Biphenylsulfonyl amino]-3 phenylpropionic acid (C21H19NO4S alone or in combination with cisplatin was determined using high content screening. Protein expression was examined using immunohistochemistry and ELISA. Co-incubation of cisplatin and an MMP-9/MMP-2 inhibitor, (2R-2-[(4-Biphenylsulfonyl amino]-3 phenylpropionic acid (C21H19NO4S resulted in significantly greater cytotoxicity as compared to either treatment alone in a cisplatin resistant MMP-9 overexpressing cell line; A2780cis. In addition, pre-incubating with MMP-9i prior to cisplatin further enhances the cytotoxic effect. No significant difference was observed in MMP-9 protein in tissue but a trend towards increased MMP-9 was observed in recurrent serum. We propose that MMP-9/MMP-2i may be utilized in the treatment of recurrent/chemoresistant ovarian cancers that overexpress MMP-9 mRNA but its role in vivo remains to be evaluated.

  9. Fast Determination of Yttrium and Rare Earth Elements in Seawater by Inductively Coupled Plasma-Mass Spectrometry after Online Flow Injection Pretreatment

    Directory of Open Access Journals (Sweden)

    Zuhao Zhu

    2018-02-01

    Full Text Available A method for daily monitoring of yttrium and rare earth elements (YREEs in seawater using a cheap flow injection system online coupled to inductively coupled plasma-mass spectrometry is reported. Toyopearl AF Chelate 650M® resin permits separation and concentration of YREEs using a simple external calibration. A running cycle consumed 6 mL sample and took 5.3 min, providing a throughput of 11 samples per hour. Linear ranges were up to 200 ng kg−1 except Tm (100 ng kg−1. The precision of the method was <6% (RSDs, n = 5, and recoveries ranged from 93% to 106%. Limits of detection (LODs were in the range 0.002 ng kg−1 (Tm to 0.078 ng kg−1 (Ce. Good agreement between YREEs concentrations in CASS-4 and SLEW-3 obtained in this work and results from other studies was observed. The proposed method was applied to the determination of YREEs in seawater from the Jiulong River Estuary and the Taiwan Strait.

  10. Fast Determination of Yttrium and Rare Earth Elements in Seawater by Inductively Coupled Plasma-Mass Spectrometry after Online Flow Injection Pretreatment.

    Science.gov (United States)

    Zhu, Zuhao; Zheng, Airong

    2018-02-23

    A method for daily monitoring of yttrium and rare earth elements (YREEs) in seawater using a cheap flow injection system online coupled to inductively coupled plasma-mass spectrometry is reported. Toyopearl AF Chelate 650M ® resin permits separation and concentration of YREEs using a simple external calibration. A running cycle consumed 6 mL sample and took 5.3 min, providing a throughput of 11 samples per hour. Linear ranges were up to 200 ng kg -1 except Tm (100 ng kg -1 ). The precision of the method was <6% (RSDs, n = 5), and recoveries ranged from 93% to 106%. Limits of detection (LODs) were in the range 0.002 ng kg -1 (Tm) to 0.078 ng kg -1 (Ce). Good agreement between YREEs concentrations in CASS-4 and SLEW-3 obtained in this work and results from other studies was observed. The proposed method was applied to the determination of YREEs in seawater from the Jiulong River Estuary and the Taiwan Strait.

  11. Quantitative determination of conjugated linoleic acid and polyunsaturated fatty acids in milk with C17 as internal marker – Evaluation of different methylation procedures

    DEFF Research Database (Denmark)

    Lashkari, Saman; Jensen, Søren Krogh

    2017-01-01

    Fatty acids are commonly analysed by gas chromatography as their corresponding fatty acid (FA) methyl esters (FAME). For quantitative determination of individual FA an internal standard like C17:0 is necessary. Conjugated FA and polyunsaturated fatty acid (PUFA) represents a challenge in the meth...

  12. Music in Preschool Class: A Quantitative Study of Factors That Determine the Extent of Music in Daily Work in Swedish Preschool Classes

    Science.gov (United States)

    Ehrlin, Anna; Tivenius, Olle

    2018-01-01

    The aim of this article is to highlight what opportunities a six year old in preschool class in Sweden might have for participating in and being inspired by music. We ask the following question: What factors determine how music teaching is conceived and carried out in preschool class? The present study is quantitative in character, and data were…

  13. The role of NAA in the environmental studies. Quantitative determination of heavy metals pollutant on environmental samples

    International Nuclear Information System (INIS)

    Sutisna; Yusuf, Saeful; Fisli, Adel; Rukihati; Wardhani, Sri; Th Rina M

    2003-01-01

    The neutron activation analysis technique was applied in the elemental analysis of environmental samples to solve an environmental pollution problem. We focused our study in the analysis of heavy metal which has potentially become a pollutant. The environmental samples analyzed were some water, sediment and an air particulate matter. The tap water sample was collected from five samplings points located at region of Serpong and Muria. Meanwhile the river water samples were taken from five samplings points of Ciliwung River. Eight samplings points of Cisadane river estuary located at Tanjung Burung were selected to collect sediment samples. Air particulate samples were collected from Jakarta Metropolitan and Serpong using high volume air sampler. Trace elements analyses of water samples were done using a combination of INAA and pre-concentration stage prior irradiation. All samples were irradiated at GA. Siwabessy reactor located at Serpong using a thermal neutron flux of about 10 12 n.cm -2 .sec -1 . After cooling time, the samples irradiated were counted by a high resolution HPGe detector coupled to a multichannel analyzer. The quantitative analyses have been done using a comparative method to a fresh laboratory standard and we used some standard references materials to validate our analytical result. The obtained result from the tap water analysis show that the elements of As, Cr, Co, Cd, Mn, Sb and Zn could be determine quantitatively and they have a concentration range from about 0.02 μg/L to 103.9 μg/L. The analysis result of Ciliwung river water samples show that elements of Ag, As, Co, Cu, Fe, Hg, Mn, V and Zn are present in the range of 2.4 μg/L to about 1365.8 μg/L. Meanwhile some important elements were obtained in the sediments samples taken from Cisadane River estuary such as Ce (40.4 - 63.6 mg/kg), Co (15.2 - 40.2 mg/kg), Cr (21.6 - 57.8 mg/kg), Eu (1.2 - 1.8 mg/kg), Fe (7.0 - 16.8 mg/kg), Mn (887 - 1810 mg/kg) and V (160 - 558 mg/kg). Finally the

  14. Wet oxidation pretreatment of rape straw for ethanol production

    DEFF Research Database (Denmark)

    Arvaniti, Efthalia; Bjerre, Anne Belinda; Schmidt, Jens Ejbye

    2012-01-01

    Simultaneous Saccharification and Fermentation (SSF). To reduce the water use and increase the energy efficiency in WO pretreatment features like recycling liquid (filtrate), presoaking of rape straw in water or recycled filtrate before WO, skip washing pretreated solids (filter cake) after WO, or use of whole...... slurry (Filter cake + filtrate) in SSF were also tested. Except ethanol yields, pretreatment methods were evaluated based on achieved glucose yields, amount of water used, recovery of cellulose, hemicellulose, and lignin.The highest ethanol yield obtained was 67% after fermenting the whole slurry...... produced by WO at 205 °C for 3 min with 12 bar of oxygen gas pressure and featured with presoaking in water. At these conditions after pre-treatment, cellulose and hemicellulose was recovered quantitatively (100%) together with 86% of the lignin. WO treatments of 2–3 min at 205–210 °C with 12 bar of oxygen...

  15. PROJECT W-551 INTERIM PRETREATMENT SYSTEM TECHNOLOGY SELECTION SUMMARY DECISION REPORT AND RECOMMENDATION

    Energy Technology Data Exchange (ETDEWEB)

    CONRAD EA

    2008-08-12

    This report provides the conclusions of the tank farm interim pretreatment technology decision process. It documents the methodology, data, and results of the selection of cross-flow filtration and ion exchange technologies for implementation in project W-551, Interim Pretreatment System. This selection resulted from the evaluation of specific scope criteria using quantitative and qualitative analyses, group workshops, and technical expert personnel.

  16. PROJECT W-551 INTERIM PRETREATMENT SYSTEM TECHNOLOGY SELECTION SUMMARY DECISION REPORT AND RECOMMENDATION

    International Nuclear Information System (INIS)

    CONRAD EA

    2008-01-01

    This report provides the conclusions of the tank farm interim pretreatment technology decision process. It documents the methodology, data, and results of the selection of cross-flow filtration and ion exchange technologies for implementation in project W-551, Interim Pretreatment System. This selection resulted from the evaluation of specific scope criteria using quantitative and qualitative analyses, group workshops, and technical expert personnel

  17. Bacteriophage P22 and Staphylococcus aureus Attenuation on Nonporous Fomites as Determined by Plate Assay and Quantitative PCR▿

    Science.gov (United States)

    Masago, Yoshifumi; Shibata, Tomoyuki; Rose, Joan B.

    2008-01-01

    Decay rates of bacteriophage P22 and Staphylococcus aureus on six types of common household inanimate surfaces were evaluated based on cultivation and quantitative PCR. A much higher level of inactivation was observed using the plate assay, suggesting that detection of the pathogen genome in samples from fomites does not necessarily imply a health risk to humans. PMID:18621868

  18. Bacteriophage P22 and Staphylococcus aureus attenuation on nonporous fomites as determined by plate assay and quantitative PCR.

    Science.gov (United States)

    Masago, Yoshifumi; Shibata, Tomoyuki; Rose, Joan B

    2008-09-01

    Decay rates of bacteriophage P22 and Staphylococcus aureus on six types of common household inanimate surfaces were evaluated based on cultivation and quantitative PCR. A much higher level of inactivation was observed using the plate assay, suggesting that detection of the pathogen genome in samples from fomites does not necessarily imply a health risk to humans.

  19. iMet-Q: A User-Friendly Tool for Label-Free Metabolomics Quantitation Using Dynamic Peak-Width Determination.

    Directory of Open Access Journals (Sweden)

    Hui-Yin Chang

    Full Text Available Efficient and accurate quantitation of metabolites from LC-MS data has become an important topic. Here we present an automated tool, called iMet-Q (intelligent Metabolomic Quantitation, for label-free metabolomics quantitation from high-throughput MS1 data. By performing peak detection and peak alignment, iMet-Q provides a summary of quantitation results and reports ion abundance at both replicate level and sample level. Furthermore, it gives the charge states and isotope ratios of detected metabolite peaks to facilitate metabolite identification. An in-house standard mixture and a public Arabidopsis metabolome data set were analyzed by iMet-Q. Three public quantitation tools, including XCMS, MetAlign, and MZmine 2, were used for performance comparison. From the mixture data set, seven standard metabolites were detected by the four quantitation tools, for which iMet-Q had a smaller quantitation error of 12% in both profile and centroid data sets. Our tool also correctly determined the charge states of seven standard metabolites. By searching the mass values for those standard metabolites against Human Metabolome Database, we obtained a total of 183 metabolite candidates. With the isotope ratios calculated by iMet-Q, 49% (89 out of 183 metabolite candidates were filtered out. From the public Arabidopsis data set reported with two internal standards and 167 elucidated metabolites, iMet-Q detected all of the peaks corresponding to the internal standards and 167 metabolites. Meanwhile, our tool had small abundance variation (≤ 0.19 when quantifying the two internal standards and had higher abundance correlation (≥ 0.92 when quantifying the 167 metabolites. iMet-Q provides user-friendly interfaces and is publicly available for download at http://ms.iis.sinica.edu.tw/comics/Software_iMet-Q.html.

  20. Glycerol carbonate as green solvent for pretreatment of sugarcane bagasse

    Science.gov (United States)

    2013-01-01

    Background Pretreatment of lignocellulosic biomass is a prerequisite for effective saccharification to produce fermentable sugars. In this study, “green” solvent systems based on acidified mixtures of glycerol carbonate (GC) and glycerol were used to treat sugarcane bagasse and the roles of each solvent in deconstructing biomass were determined. Results Pretreatment of sugarcane bagasse at 90°C for only 30 min with acidified GC produced a solid residue having a glucan digestibility of 90% and a glucose yield of 80%, which were significantly higher than a glucan digestibility of 16% and a glucose yield of 15% obtained for bagasse pretreated with acidified ethylene carbonate (EC). Biomass compositional analyses showed that GC pretreatment removed more lignin than EC pretreatment (84% vs 54%). Scanning electron microscopy (SEM) showed that fluffy and size-reduced fibres were produced from GC pretreatment whereas EC pretreatment produced compact particles of reduced size. The maximal glucan digestibility and glucose yield of GC/glycerol systems were about 7% lower than those of EC/ethylene glycol (EG) systems. Replacing up to 50 wt% of GC with glycerol did not negatively affect glucan digestibility and glucose yield. The results from pretreatment of microcrystalline cellulose (MCC) showed that (1) pretreatment with acidified alkylene glycol (AG) alone increased enzymatic digestibility compared to pretreatments with acidified alkylene carbonate (AC) alone and acidified mixtures of AC and AG, (2) pretreatment with acidified GC alone slightly increased, but with acidified EC alone significantly decreased, enzymatic digestibility compared to untreated MCC, and (3) there was a good positive linear correlation of enzymatic digestibility of treated and untreated MCC samples with congo red (CR) adsorption capacity. Conclusions Acidified GC alone was a more effective solvent for pretreatment of sugarcane bagasse than acidified EC alone. The higher glucose yield obtained

  1. Determination of Quantitative Structure-Property Relationships of Solvent Resistance of Polycarbonate Copolymers Using a Resonant Multisensor System

    Science.gov (United States)

    Potyrailo, Radislav A.; Wroczynski, Ronald J.; McCloskey, Patrick J.; Morris, William G.

    In sensor and microfluidic applications, the need is to have an adequate solvent resistance of polymers to prevent degradation of the substrate surface upon deposition of sensor formilations, to prevent contamination of the solvent-containing sensor formulations or contamination of organic liquid reactions in microfluidic channels. Unfortunately, no comprehensive quantitative reference solubility data of unstressed copolymers is available to date. In this study, we evaluate solvent-resistance of several polycarbonate copolymers prepared from the reaction of hydroquinone (HQ), resorcinol (RS), and bisphenol A (BPA). Our high-throughput polymer evaluation approach permitted the construction of detailed solvent-resistance maps, the development of quantitative structure-property relationships for BPA-HQ-RS copolymers and provided new knowledge for the further development of the polymeric sensor and microfluidic components.

  2. NIST-Traceable NMR Method to Determine Quantitative Weight Percentage Purity of Nitrogen Mustard HN-1 Feedstock Samples

    Science.gov (United States)

    2014-06-01

    Aldrich), Part Number 74658- 5G , CAS No. 95-93-2, as a TraceCERT® certified reference material (CRM) standard for quantitative NMR. The...If the integration is incorrect, the spectrum can be manually integrated. In particular, Figure 2 shows that each peak has two 13C satellite peaks...0.55% of the center peak. The satellite peaks should be included in the integration of the central peak. (If the magnet is not well shimmed, the

  3. Quantitative HPLC analysis of sesquiterpene lactones and determination of chemotypes in Eremanthus seidelii MacLeish and Schumacher (Asteraceae)

    Energy Technology Data Exchange (ETDEWEB)

    Sakamoto, Humberto T. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Filosofia, Ciencias e Letras. Dept. de Quimica; Gobbo-Neto, Leonardo; Lopes, Norberto P.; Lopes, Joao L.C. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Fisica e Quimica]. E-mail: joaoluis@usp.br; npelopes@fcfrp.usp.br; Cavalheiro, Alberto J. [UNESP, Araraquara, SP (Brazil). Inst. de Quimica

    2005-11-15

    anthus seidelii MacLeish and Schumacher has a restricted occurrence to the Brazilian 'cerrado' surrounding the Furnas (MG) reservoir, in environments that have been seriously damaged by human activity. The present phytochemical investigation reveals that the sesquiterpene lactones (SL) 4{beta},5-dihydro-2',3'-dihydroxy-15-desoxy-goyazensolide (1) and 4{beta},5-dihydro-1',2'-epoxy-eremantholide-C (2) are the major secondary metabolites in E. seidelii leaves, and an HPLC method was developed for their quantitative analysis. HPLC analysis showed no significant seasonal variation in the concentrations of both SL. No qualitative differences were found in the SL patterns of all individuals sampled. However, there is a different SL quantitative pattern among the plants analyzed, pointing to the existence of three quantitative chemotypes of this species, with differences possibly originating from the activity of the enzymes that cyclize the goyazensolide type SL (1) to a eremantholide type SL (2). (author)

  4. Development and validation of an RP-HPLC method for quantitative determination of vanillin and related phenolic compounds in Vanilla planifolia.

    Science.gov (United States)

    Sinha, Arun Kumar; Verma, Subash Chandra; Sharma, Upendra Kumar

    2007-01-01

    A simple and fast method was developed using RP-HPLC for separation and quantitative determination of vanillin and related phenolic compounds in ethanolic extract of pods of Vanilla planifolia. Ten phenolic compounds, namely 4-hydroxybenzyl alcohol, vanillyl alcohol, 3,4-dihydroxybenzaldehyde, 4-hydroxybenzoic acid, vanillic acid, 4-hydroxybenzaldehyde, vanillin, p-coumaric acid, ferulic acid, and piperonal were quantitatively determined using ACN, methanol, and 0.2% acetic acid in water as a mobile phase with a gradient elution mode. The method showed good linearity, high precision, and good recovery of compounds of interest. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

  5. COMPARATIVE AND QUANTITATIVE DETERMINATION OF QUERCETIN AND RUTIN IN TRIBULUS TERRESTRIS L. FRUITS FROM DIFFERENT SEASONAL AND GEOGRAPHICAL POPULATIONS OF SOUTH INDIA

    OpenAIRE

    Suresh Reddy Yanala* and D. Sathyanarayana

    2018-01-01

    The objective of the present research work was comparative and quantitative determination of quercetin and rutin in Tribulus terrestirs fruits from different geographical regions and seasons by using HPLC. The Tribulus terrestris fruit samples collected from three different geographical regions of south India in June and December months. In the current HPLC analysis flavonoids in Tribulus terrestris Linn fruits were quantified at 360 nm with help of peak area by comparing to a calibration cur...

  6. Investigation of Pleurotus ostreatus pretreatment on switchgrass for ethanol production

    Science.gov (United States)

    Slavens, Shelyn Gehle

    Fungal pretreatment using the white-rot fungus Pleurotus ostreatus on switchgrass for ethanol production was studied. In a small-scale storage study, small switchgrass bales were inoculated with fungal spawn and automatically watered to maintain moisture. Sampled at 25, 53, and 81 d, the switchgrass composition was determined and liquid hot water (LHW) pretreatment was conducted. Fungal pretreatment significantly decreased the xylan and lignin content; glucan was not significantly affected by fungal loading. The glucan, xylan, and lignin contents significantly decreased with increased fungal pretreatment time. The effects of the fungal pretreatment were not highly evident after the LHW pretreatment, showing only changes based on sampling time. Although other biological activity within the bales increased cellulose degradation, the fungal pretreatment successfully reduced the switchgrass lignin and hemicellulose contents. In a laboratory-scale nutrient supplementation study, copper, manganese, glucose, or water was added to switchgrass to induce production of ligninolytic enzymes by P. ostreatus. After 40 d, ligninolytic enzyme activities and biomass composition were determined and simultaneous saccharification and fermentation (SSF) was conducted to determine ethanol yield. Laccase activity was similar for all supplements and manganese peroxidase (MnP) activity was significantly less in copper-treated samples than in the other fungal-inoculated samples. The fungal pretreatment reduced glucan, xylan, and lignin content, while increasing extractable sugars content. The lowest lignin contents occurred in the water-fungal treated samples and produced the greatest ethanol yields. The greatest lignin contents occurred in the copper-fungal treated samples and produced the lowest ethanol yields. Manganese-fungal and glucose-fungal treated samples had similar, intermediate lignin contents and produced similar, intermediate ethanol yields. Ethanol yields from switchgrass

  7. Lime pretreatment and fermentation of enzymatically hydrolyzed sugarcane bagasse.

    Science.gov (United States)

    Rabelo, Sarita C; Maciel Filho, Rubens; Costa, Aline C

    2013-03-01

    Sugarcane bagasse was subjected to lime (calcium hydroxide) pretreatment and enzymatic hydrolysis for second-generation ethanol production. A central composite factorial design was performed to determine the best combination of pretreatment time, temperature, and lime loading, as well as to evaluate the influence of enzymatic loadings on hydrolysis conversion. The influence of increasing solids loading in the pretreatment and enzymatic hydrolysis stages was also determined. The hydrolysate was fermented using Saccharomyces cerevisiae in batch and continuous mode. In the continuous fermentation, the hydrolysates were concentrated with molasses. Lime pretreatment significantly increased the enzymatic digestibility of sugarcane bagasse without the need for prior particle size reduction. In the optimal pretreatment conditions (90 h, 90 °C, 0.47 glime/g bagasse) and industrially realistic conditions of hydrolysis (12.7 FPU/g of cellulase and 7.3 CBU/g of β-glucosidase), 139.6 kglignin/ton raw bagasse and 126.0 kg hemicellulose in the pretreatment liquor per ton raw bagasse were obtained. The hydrolysate from lime pretreated sugarcane bagasse presented low amounts of inhibitors, leading to ethanol yield of 164.1 kgethanol/ton raw bagasse.

  8. Rigour in quantitative research.

    Science.gov (United States)

    Claydon, Leica Sarah

    2015-07-22

    This article which forms part of the research series addresses scientific rigour in quantitative research. It explores the basis and use of quantitative research and the nature of scientific rigour. It examines how the reader may determine whether quantitative research results are accurate, the questions that should be asked to determine accuracy and the checklists that may be used in this process. Quantitative research has advantages in nursing, since it can provide numerical data to help answer questions encountered in everyday practice.

  9. Infrared Spectroscopy as a Versatile Analytical Tool for the Quantitative Determination of Antioxidants in Agricultural Products, Foods and Plants

    Science.gov (United States)

    Cozzolino, Daniel

    2015-01-01

    Spectroscopic methods provide with very useful qualitative and quantitative information about the biochemistry and chemistry of antioxidants. Near infrared (NIR) and mid infrared (MIR) spectroscopy are considered as powerful, fast, accurate and non-destructive analytical tools that can be considered as a replacement of traditional chemical analysis. In recent years, several reports can be found in the literature demonstrating the usefulness of these methods in the analysis of antioxidants in different organic matrices. This article reviews recent applications of infrared (NIR and MIR) spectroscopy in the analysis of antioxidant compounds in a wide range of samples such as agricultural products, foods and plants. PMID:26783838

  10. Quantitative surface characterization of silicon spheres by combined XRF and XPS analysis for the determination of the Avogadro constant

    Science.gov (United States)

    Müller, Matthias; Beckhoff, Burkhard; Beyer, Edyta; Darlatt, Erik; Fliegauf, Rolf; Ulm, Gerhard; Kolbe, Michael

    2017-10-01

    For the quantitative surface characterization of a monocrystalline silicon sphere, PTB has constructed and put into operation an analytical instrument, which combines x-ray fluorescence and x-ray photoelectron spectroscopy techniques. The main objective of this novel instrument is the characterization of the oxide layer and unintentional contaminations, e.g. from hydrocarbons. It is equipped with a ball manipulator allowing measurements at each point on the surface of ball-shaped samples with a diameter of about 93.7 mm. Monocrystalline silicon spheres with this diameter allow a realization of the SI base unit of mass.

  11. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study DNA was extracted either directly or following freeze storage of three homogenized human fecal...... samples using three different extraction methods. No consistent differences were observed in DNA yields between extractions on fresh and frozen samples, however differences were observed between extraction methods. Quantitative PCR analysis was subsequently performed on all DNA samples using six different...

  12. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    2012-01-01

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study, DNA was extracted either directly or following freeze storage of three homogenized human fecal...... samples using three different extraction methods. No consistent differences were observed in DNA yields between extractions on fresh and frozen samples; however, differences were observed between extraction methods. Quantitative PCR analysis was subsequently performed on all DNA samples using six...

  13. Simultaneous, simple and rapid determination of five bioactive free anthraquinones in Radix et Rhizoma Rhei by quantitative {sup 1}H NMR

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Jian-Wei; Cai, Le; Fang, Yun-Shan; Duan, Wei-He; Li, Zhen-Jie; Ding, Zhong-Tao, E-mail: ztding@ynu.edu.cn, E-mail: caile@ynu.edu.cn [Key Laboratory of Medicinal Chemistry for Natural Resource, Ministry of Education, School of Chemical Science and Technology, Yunnan University, Kunming (China)

    2016-07-01

    Radix et Rhizoma Rhei has been recognized for centuries in traditional medicine for its multiple pharmacological actions. The free anthraquinones including physcion, chrysophanol, emodin, rhein, and aloe-emodin are the main bioactive components in Radix et Rhizoma Rhei. In the present study, a fast quantitative {sup 1}H nuclear magnetic resonance (q-HNMR) method for the determination and quantitation of five free anthraquinones in Radix et Rhizoma Rhei was developed. Validation of the quantitative method was performed in terms of specificity, accuracy, precision, and stability. The results showed that the solvent acetone-d{sub 6} enabled satisfactory separation of the signals to be integrated. Five anthraquinones in Radix et Rhizoma Rhei could be quantified accurately using featured signals from {sup 1}H NMR. This work implied that q-HNMR represents a feasible alternative to high-performance liquid chromatography (HPLC)-based methods for quantitation of anthraquinones in Radix et Rhizoma Rhei and is suitable for the quality control of Radix et Rhizoma Rhei. (author)

  14. Quantitative determination of BAF312, a S1P-R modulator, in human urine by LC-MS/MS: prevention and recovery of lost analyte due to container surface adsorption.

    Science.gov (United States)

    Li, Wenkui; Luo, Suyi; Smith, Harold T; Tse, Francis L S

    2010-02-15

    Analyte loss due to non-specific binding, especially container surface adsorption, is not uncommon in the quantitative analysis of urine samples. In developing a sensitive LC-MS/MS method for the determination of a drug candidate, BAF312, in human urine, a simple procedure was outlined for identification, confirmation and prevention of analyte non-specific binding to a container surface and to recover the 'non-specific loss' of an analyte, if no transfer has occurred to the original urine samples. Non-specific binding or container surface adsorption can be quickly identified by using freshly spiked urine calibration standards and pre-pooled QC samples during a LC-MS/MS feasibility run. The resulting low recovery of an analyte in urine samples can be prevented through the use of additives, such as the non-ionic surfactant Tween-80, CHAPS and others, to the container prior to urine sample collection. If the urine samples have not been transferred from the bulk container, the 'non-specific binding' of an analyte to the container surface can be reversed by the addition of a specified amount of CHAPS, Tween-80 or bovine serum albumin, followed by appropriate mixing. Among the above agents, Tween-80 is the most cost-effective. beta-cyclodextrin may be suitable in stabilizing the analyte of interest in urine via pre-treating the matrix with the agent. However, post-addition of beta-cyclodextrin to untreated urine samples does not recover the 'lost' analyte due to non-specific binding or container surface adsorption. In the case of BAF312, a dynamic range of 0.0200-20.0 ng/ml in human urine was validated with an overall accuracy and precision for QC sample results ranging from -3.2 to 5.1% (bias) and 3.9 to 10.2% (CV), respectively. Pre- and post-addition of 0.5% (v/v) Tween-80 to the container provided excellent overall analyte recovery and minimal MS signal suppression when a liquid-liquid extraction in combination with an isocratic LC separation was employed. The

  15. Quantitative determination of methanol and ethanol with synthetic calibration spectra in passive Fourier transform infrared remote sensing measurements.

    Science.gov (United States)

    Guo, Qiaohan; Small, Gary W

    2013-08-01

    A spectral synthesis strategy is introduced to help obtain estimates of path-integrated concentrations in passive Fourier transform infrared (FT-IR) remote sensing measurements conducted during field-monitoring experiments. Obtaining quantitative information from passive infrared data is challenging because of the joint effects of temperature and concentration on spectral intensities. The collection of calibration data for use in modeling spectral intensities for a given set of experimental conditions is also costly and labor intensive. In the work presented here, a radiance model is defined for use in synthesizing calibration spectra that serve as inputs to partial least-squares (PLS) models that relate spectral intensities to path-integrated concentrations. The field data for which quantitative estimates are desired are used to estimate the background temperature associated with a given time and set of experimental conditions. Sample temperatures can be obtained through either experimental measurement or by estimating one calibration release. Given these temperatures, calibration data can be synthesized and the PLS model developed. This methodology is tested with stack monitoring data obtained from controlled releases of pure and mixture samples of heated ethanol and methanol. Experiments were conducted across 6 days with stack temperatures of 150 to 200 °C and with path-integrated concentrations in the range of 10 to 300 parts per million meters. Median relative errors in the estimates of path-integrated concentration were typically in the range of 20% or less, with the best results observed at the higher stack temperatures.

  16. Quantitative determination of 21-hydroxy-deflazacort in human plasma using gradient semi-microbore liquid chromatography.

    Science.gov (United States)

    Reynolds, D L; Burmaster, S D; Eichmeier, L S

    1994-01-01

    A sensitive and selective liquid chromatographic procedure to quantitate the deflazacort metabolite 21-hydroxy-deflazacort (DF-21OH) in human plasma was developed and validated. DF-21OH and fludrocortisone acetate (internal standard, IS) were isolated from human plasma (2 mL) by solid-phase extraction onto C-18 cartridges. Potential interferences were selectively removed and analytes were eluted with ethyl acetate. Following evaporation, the residue was reconstituted for HPLC analysis. Separation was achieved by gradient elution using a 5 microns YMC Basic column (2.0 x 100 mm) with mobile phases consisting of 20% methanol and 50% acetonitrile in 50 mM phosphate buffer (pH 3) at a temperature of 50 degrees C. Flow rate was maintained at 0.3 mL/min., and analytes were quantified spectrophotometrically at 246 nm. The assay was validated over the range 1.0 to 500 ng/mL DF-21OH. Calibration curves were prepared using a weighted (1/concentration) nonlinear quadratic regression algorithm. Peak-height ratios were proportional to the amount of DF-21OH added to plasma. Assay precision (%RSD) ranged from 4.2 to 11%, with a corresponding assay accuracy (% relative error) of +/- 2.8%. Absolute recovery of DF-21OH from plasma was 78-86% over the concentration range. The minimum quantitation limit was 1.0 ng/mL.

  17. Systematic approach to optimize a pretreatment method for ultrasensitive liquid chromatography with tandem mass spectrometry analysis of multiple target compounds in biological samples.

    Science.gov (United States)

    Togashi, Kazutaka; Mutaguchi, Kuninori; Komuro, Setsuko; Kataoka, Makoto; Yamazaki, Hiroshi; Yamashita, Shinji

    2016-08-01

    In current approaches for new drug development, highly sensitive and robust analytical methods for the determination of test compounds in biological samples are essential. These analytical methods should be optimized for every target compound. However, for biological samples that contain multiple compounds as new drug candidates obtained by cassette dosing tests, it would be preferable to develop a single method that allows the determination of all compounds at once. This study aims to establish a systematic approach that enables a selection of the most appropriate pretreatment method for multiple target compounds without the use of their chemical information. We investigated the retention times of 27 known compounds under different mobile phase conditions and determined the required pretreatment of human plasma samples using several solid-phase and liquid-liquid extractions. From the relationship between retention time and recovery in a principal component analysis, appropriate pretreatments were categorized into several types. Based on the category, we have optimized a pretreatment method for the identification of three calcium channel blockers in human plasma. Plasma concentrations of these drugs in a cassette-dose clinical study at microdose level were successfully determined with a lower limit of quantitation of 0.2 pg/mL for diltiazem, 1 pg/mL for nicardipine, and 2 pg/mL for nifedipine. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Effects of Pretreatments in Convective Dehydration of Rosehip (Rosa eglanteria

    Directory of Open Access Journals (Sweden)

    Alejandra Mabellini

    2012-04-01

    Full Text Available The aim of this work was to experimentally determine drying curves for thin layer and bed drying of rosehip fruits, with and without pretreatments, to reduce processing times as a function of drying air operating variables, to propose dehydration kinetics of fruits and to determine its kinetic parameters for further use within drying simulation software. Fruits were pre-treated both chemically and mechanically, which included dipping the fruits in NaOH and ethyl oleate solutions; and cutting or perforating the fruit cuticle, respectively. Simulation models were then adopted to fit the kinetics drying data considering fruit volume shrinkage. These simple models minimized the calculation time during the simulation of deep-bed driers. Results show that pre-treatments reduced processing times up to 57%, and evaluated models satisfactorily predicted the drying of rosehip fruit. Effective mass diffusion coefficients were up to 4-fold greater when fruit was submitted to mechanical pretreatments.

  19. Development and validation of a quantitative method for determination of carmine (E120) in foodstuffs by liquid chromatography: NMKL Collaborative Study.

    Science.gov (United States)

    Merino, L; Edberg, U; Tidriks, H

    1997-01-01

    A liquid chromatographic method for quantitative determination of carmine (E120) in different foodstuffs is described. Qualitative and semiquantitative methods for analysis of carmine and other related dyes are well established. However, quantitative methods available are based mainly on enzymatic reactions that are time-consuming or specific for analysis of carminic acid in yoghurt. In the method developed and validated here, carminic acid is extracted by boiling the sample with HCl, purified on a solid-phase extraction cartridge, and injected on a C18 analytical column. The method was evaluated by an internal analytical quality control and a collaborative study in which 11 laboratories from the Nordic countries participated. The food samples analyzed were fruit jelly, liqueur, juice, yoghurt, and ice cream. Materials were distributed to participants as uniform level and split level. Validation showed that the proposed method is well suited for quantitative determination of carmine. The detection limit is 0.1 mg/L. The mean relative standard deviation for reproducibility varies from 7.9 to 11.7%. The proposed method is simple and relatively fast compared with previously published methods.

  20. Quantitative size-dependent structure and strain determination of CdSe nanoparticles using atomic pair distribution function analysis

    International Nuclear Information System (INIS)

    Masadeh, A. S.; Bozin, E. S.; Farrow, C. L.; Paglia, G.; Juhas, P.; Billinge, S. J. L.; Karkamkar, A.; Kanatzidis, M. G.

    2007-01-01

    The size-dependent structure of CdSe nanoparticles, with diameters ranging from 2 to 4 nm, has been studied using the atomic pair distribution function (PDF) method. The core structure of the measured CdSe nanoparticles can be described in terms of the wurtzite atomic structure with extensive stacking faults. The density of faults in the nanoparticles is ∼50%. The diameter of the core region was extracted directly from the PDF data and is in good agreement with the diameter obtained from standard characterization methods, suggesting that there is little surface amorphous region. A compressive strain was measured in the Cd-Se bond length that increases with decreasing particle size being 0.5% with respect to bulk CdSe for the 2 nm diameter particles. This study demonstrates the size-dependent quantitative structural information that can be obtained even from very small nanoparticles using the PDF approach

  1. Quantitative size-dependent structure and strain determination of CdSe nanoparticles using atomic pair distribution function analysis

    Science.gov (United States)

    Masadeh, A. S.; Božin, E. S.; Farrow, C. L.; Paglia, G.; Juhas, P.; Billinge, S. J. L.; Karkamkar, A.; Kanatzidis, M. G.

    2007-09-01

    The size-dependent structure of CdSe nanoparticles, with diameters ranging from 2to4nm , has been studied using the atomic pair distribution function (PDF) method. The core structure of the measured CdSe nanoparticles can be described in terms of the wurtzite atomic structure with extensive stacking faults. The density of faults in the nanoparticles is ˜50% . The diameter of the core region was extracted directly from the PDF data and is in good agreement with the diameter obtained from standard characterization methods, suggesting that there is little surface amorphous region. A compressive strain was measured in the Cd-Se bond length that increases with decreasing particle size being 0.5% with respect to bulk CdSe for the 2nm diameter particles. This study demonstrates the size-dependent quantitative structural information that can be obtained even from very small nanoparticles using the PDF approach.

  2. Active auxin uptake by zucchini membrane vesicles: quantitation using ESR volume and delta pH determinations

    International Nuclear Information System (INIS)

    Lomax, T.L.; Mehlhorn, R.J.; Briggs, W.R.

    1985-01-01

    Closed and pH-tight membrane vesicles prepared from hypocotyls of 5-day-old dark-grown seedlings of Cucurbita pepo accumulate the plant growth hormone indole-3-acetic acid along an imposed proton gradient (pH low outside, high inside). The use of electron paramagnetic spin probes permitted quantitation both of apparent vesicle volume and magnitude of the pH gradient. Under the experimental conditions used, hormone accumulation was at minimum 20-fold, a value 4 times larger than what one would predict if accumulation reflected only diffusional equilibrium at the measured pH gradient. It is concluded that hormone uptake is an active process, with each protonated molecule of hormone accompanied by an additional proton. Experiments with ionophores confirm that it is the pH gradient itself which drives the uptake

  3. Deferasirox, deferiprone and desferrioxamine treatment in thalassemia major patients: cardiac iron and function comparison determined by quantitative magnetic resonance imaging

    Science.gov (United States)

    Pepe, Alessia; Meloni, Antonella; Capra, Marcello; Cianciulli, Paolo; Prossomariti, Luciano; Malaventura, Cristina; Putti, Maria Caterina; Lippi, Alma; Romeo, Maria Antonietta; Bisconte, Maria Grazia; Filosa, Aldo; Caruso, Vincenzo; Quarta, Antonella; Pitrolo, Lorella; Missere, Massimiliano; Midiri, Massimo; Rossi, Giuseppe; Positano, Vincenzo; Lombardi, Massimo; Maggio, Aurelio

    2011-01-01

    Background Oral deferiprone was suggested to be more effective than subcutaneous desferrioxamine for removing heart iron. Oral once-daily chelator deferasirox has recently been made commercially available but its long-term efficacy on cardiac iron and function has not yet been established. Our study aimed to compare the effectiveness of deferasirox, deferiprone and desferrioxamine on myocardial and liver iron concentrations and bi-ventricular function in thalassemia major patients by means of quantitative magnetic resonance imaging. Design and Methods From the first 550 thalassemia subjects enrolled in the Myocardial Iron Overload in Thalassemia network, we retrospectively selected thalassemia major patients who had been receiving one chelator alone for longer than one year. We identified three groups of patients: 24 treated with deferasirox, 42 treated with deferiprone and 89 treated with desferrioxamine. Myocardial iron concentrations were measured by T2* multislice multiecho technique. Biventricular function parameters were quantitatively evaluated by cine images. Liver iron concentrations were measured by T2* multiecho technique. Results The global heart T2* value was significantly higher in the deferiprone (34±11ms) than in the deferasirox (21±12 ms) and the desferrioxamine groups (27±11 ms) (P=0.0001). We found higher left ventricular ejection fractions in the deferiprone and the desferrioxamine versus the deferasirox group (P=0.010). Liver iron concentration, measured as T2* signal, was significantly lower in the desferrioxamine versus the deferiprone and the deferasirox group (P=0.004). Conclusions The cohort of patients treated with oral deferiprone showed less myocardial iron burden and better global systolic ventricular function compared to the patients treated with oral deferasirox or subcutaneous desferrioxamine. PMID:20884710

  4. Development of a liquid chromatography-electrospray-tandem mass spectrometry method for the quantitative determination of benzoxazinone derivatives in plants.

    Science.gov (United States)

    Bonnington, Lea; Eljarrat, Ethel; Guillamón, Miriam; Eichhorn, Peter; Taberner, Andreu; Barceló, Damià

    2003-07-01

    A new method for the quantification of benzoxazinone derivatives in extracts of wheat foliage and root samples using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) is described. Using this method, the characterization, separation, and quantitative detection of a mixture of six naturally occurring 1,4-benzoxazin-3(4H)-one derivatives, including the hydroxamic acids (DIMBOA, DIBOA), lactams (HBOA, and HMBOA), benzoxazilinones (BOA, MBOA), and two synthetic methoxylated variations of DIBOA and HBOA, was achieved. The application of a novel, highly modified reversed-phase LC column, the dodecyl (C12) TMS end-capped Synergi MAX-RP, enhanced the on-line chromatographic separation through improvements to component resolution, analyte stability and peak shape and also to the column lifetime. The complete ESI-MS-MS precursor-product ion fragmentation pathways for the benzoxazinone derivatives are described for the first time and used to deduce a generic fragmentation pattern for the compound class. Characteristic transitions for the benzoxazinones were thus used in the developed analytical method enabling reliable quantification with simultaneous screening for other potentially present derivatives, while eliminating interferences from other coeluting contaminants from the complex plant extract matrix. Quantitative analysis was done in the multiple reaction monitoring mode, using two specific combinations of a precursor-product ion transitions for each compound. The ESI-MS-MS detection method offered improvements to the sensitivity and selectivity, as compared with previously applied LC methods, with detection limits down to 0.002-0.023 ng/microL. The developed method was demonstrated by analyzing foliages and roots of six different wheat cultivars using pressurized liquid extraction-solid-phase extraction cleanup-LC-ESI-MS-MS. The analytes were detected in the range of 0.7-207 microg/g of dry weight.

  5. Application of a quantitative1H-NMR (1H-qNMR) method for the determination of geniposidic acid and acteoside in Plantaginis semen.

    Science.gov (United States)

    Tanaka, Rie; Inagaki, Risa; Sugimoto, Naoki; Akiyama, Hiroshi; Nagatsu, Akito

    2017-01-01

    A quantitative 1 H-NMR method ( 1 H-qNMR) was developed to determine the concentration of acteoside and geniposidic acid in Plantaginis semen, which is an important crude drug for diuretic purposes. The purity of geniposidic acid and acteoside was determined by the ratio of the intensity of the H-3 signal at δ 7.51 ppm or the H-7″ signal at δ 7.58 ppm in methanol-d 4 to that of a hexamethyldisilane (HMD) signal at 0.04 ppm, respectively. The concentration of HMD was corrected with the International System of Units traceability using potassium hydrogen phthalate of certified reference material grade. The geniposidic acid content in two batches of Plantaginis semen as determined by 1 H-qNMR was found to be 0.84 and 1.00 %, and the acteoside content was determined to be 0.80 and 0.93 %. We demonstrated that this method is useful for the quantitative analysis of geniposidic acid and acteoside in Plantainis semen.

  6. Development of a quantitative method for trace elements determination in ores by XRF: an application to phosphorite from Olinda (PE), Brazil

    International Nuclear Information System (INIS)

    Imakuma, K.; Sato, I.M.; Cretella Neto, J.; Costa, M.I.

    1976-01-01

    A quantitative analytical method by means of X-Ray Fluorescence intended to determine Zn, Cu and Ni trace amounts in a phosphorite ore from Olinda, PE-Brazil was established. The double dilution method with borax as the melting flux was the one choosed because ores diluted in borax in the form of melted samples show matrix effects with respect to the element to be analysed; it was possible to identify the elements already presented in the ore that caused interference in the Zn, Cu and Ni determinations. Such elements were Ca and their quantities were subsequently determined. The addition of appropriate quantities of Fe and Ca to standards allowed us to minimize the matrix effects without the undersired introduction of extraneous elements in the ore, moreover, the urge of knowing the exact amounts of Fe and Cu present in the ore drove us towards a simultaneous development of another analytical method suitable to measure medium to high contents. This method also made use of the technique of dilution with melting. These methods present advantages such as: a quantitative analysis with great reproducibility of results; the extension of the method to routine determination, to all kinds of ores. The main sources of error can be controlled, allowing an accuracy as high as +- 1 ppm for Cu, +- 4 ppm for Ni, +- 6 ppm for Zn and +- 1% for both Fe can Ca under the most unfavorable conditions

  7. Pretreatment of Dioscorea zingiberensis for Microbial Transformation

    Directory of Open Access Journals (Sweden)

    Tianxiang Zheng

    2014-09-01

    Full Text Available The influences of five pretreatments on fungal growth and enzyme production during microbial transformation of Dioscorea zingiberensis (DZW were studied. The biomass, α-rhamnase and β-glucosidase activities in the fermentation system were employed in the study to determine how each method affected the efficiency of microbial transformation. The fungal strain grew better on the substrate which contained easily utilized carbon source. While lack of carbon source induced the strain produce more glucosidase. Among five pretreatment methods, complex enzymatic hydrolyzation can remove 84.3% starch and 76.5% fibre from DZW in form of sugar, which resulted in high α-rhamnase activity of 2.89 IU/mL and β-glucosidase activity of 8.17 IU/mL in fermentation broth.

  8. Using Quantitative Reverse Transcriptase PCR and Cell Culture Plaque Assays to Determine Resistance of Toxoplasma gondii Oocysts to Chemical Sanitizers

    Science.gov (United States)

    Toxoplasma gondii oocysts are highly resistant to many chemical sanitizers. Current methods used to determine oocyst infectivity have relied exclusively on mouse, chicken, and feline bioassays. Although considered gold standards, they only provide a qualitative assessment of oocyst infectivity. I...

  9. Quantitative determination of copper in a glass matrix using double pulse laser induced breakdown and electron paramagnetic resonance spectroscopic techniques.

    Science.gov (United States)

    Khalil, Ahmed A I; Morsy, Mohamed A

    2016-07-01

    A series of lithium-lead-borate glasses of a variable copper oxide loading were quantitatively analyzed in this work using two distinct spectroscopic techniques, namely double pulse laser induced breakdown spectroscopy (DP-LIBS) and electron paramagnetic resonance (EPR). DP-LIBS results measured upon a combined nanosecond lasers irradiation running at 266nm and 1064nm pulses of a collinear configuration directed to the surface of borate glass samples with a known composition. This arrangement was employed to predict the electron's temperature (Te) and density (Ne) of the excited plasma from the recorded spectra. The intensity of elements' responses using this scheme is higher than that of single-pulse laser induced breakdown spectroscopy (SP-LIBS) setup under the same experimental conditions. On the other hand, the EPR data shows typical Cu (II) EPR-signals in the borate glass system that is networked at a distorted tetragonal Borate-arrangement. The signal intensity of the Cu (II) peak at g⊥=2.0596 has been used to quantify the Cu-content accurately in the glass matrix. Both techniques produced linear calibration curves of Cu-metals in glasses with excellent linear regression coefficient (R(2)) values. This study establishes a good correlation between DP-LIBS analysis of glass and the results obtained using EPR spectroscopy. The proposed protocols prove the great advantage of DP-LIBS system for the detection of a trace copper on the surface of glasses. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Alternative method for the quantitative determination of Rashba- and Dresselhaus spin–orbit interaction using the magnetization

    International Nuclear Information System (INIS)

    Wilde, M A; Grundler, D

    2013-01-01

    The quantum oscillatory magnetization M of a two-dimensional electron system in a magnetic field B is found to provide quantitative information on both the Rashba- and Dresselhaus spin–orbit interaction (SOI). This is shown by first numerically solving the model Hamiltonian including the linear Rashba- and Dresselhaus SOI and the Zeeman term in particular in a doubly tilted magnetic field and second evaluating the intrinsically anisotropic magnetization for different directions of the in-plane magnetic field component. The amplitude of specific magnetic quantum oscillations in M(B) is found to be a direct measure of the SOI strength at fields B where SOI-induced Landau level anticrossings occur. The anisotropic M allows one to quantify the magnitude of both contributions as well as their relative sign. The influence of cubic Dresselhaus SOI on the results is discussed. We use realistic sample parameters and show that recently reported experimental techniques provide a sensitivity which allows for the detection of the predicted phenomena. (paper)

  11. Quantitative Determination of Alkaloids in Lotus Flower (Flower Buds of Nelumbo nucifera and Their Melanogenesis Inhibitory Activity

    Directory of Open Access Journals (Sweden)

    Toshio Morikawa

    2016-07-01

    Full Text Available A quantitative analytical method for five aporphine alkaloids, nuciferine (1, nornuciferine (2, N-methylasimilobine (3, asimilobine (4, and pronuciferine (5, and five benzylisoquinoline alkaloids, armepavine (6, norarmepavine (7, N-methylcoclaurine (8, coclaurine (9, and norjuziphine (10, identified as the constituents responsible for the melanogenesis inhibitory activity of the extracts of lotus flowers (the flower buds of Nelumbo nucifera, has been developed using liquid chromatography-mass spectrometry. The optimum conditions for separation and detection of these 10 alkaloids were achieved on a πNAP column, a reversed-phase column with naphthylethyl group-bonded silica packing material, with CH3CN–0.2% aqueous acetic acid as the mobile phase and using mass spectrometry equipped with a positive-mode electrospray ionization source. According to the protocol established, distributions of these 10 alkaloids in the petal, receptacle, and stamen parts, which were separated from the whole flower, were examined. As expected, excellent correlations were observed between the total alkaloid content and melanogenesis inhibitory activity. Among the active alkaloids, nornuciferine (2 was found to give a carbamate salt (2′′ via formation of an unstable carbamic acid (2′ by absorption of carbon dioxide from the air.

  12. Determining the best extractant and extraction conditions for fulvic acid through qualitative and quantitative analysis of vermicompost

    Directory of Open Access Journals (Sweden)

    Omid Shabnani Moghadam

    2015-06-01

    Full Text Available Fulvic acid is a natural tampon and an appropriate chelating agent that has high ion-exchange ability and increasing absorption of minerals in plants. This paper examined the effects of extractants (sodium hydroxide, sodium polyphosphate, urea and EDTA and the extraction time (1, 7 and 9 days on the physicochemical properties of vermicompost-produced fulvic acid. Finally, various methods were compared to the universal method of humic substances. Different qualitative and quantitative analysis such as detecting the functional groups (FTIR, measurement of functional groups, spectrophotometric ratios and humification indices were carried out on fulvic acid. Results showed that the highest and lowest amounts of fulvic acid were extracted by the sodium hydroxide and urea, respectively. Various extractants made negligible changes in the type and quality of the Fulvic acid functional groups. Results indicated that sodium hydroxide was the best extractant and the minimum amounts of fulvic acid were extracted by the urea. Urea-extracted fulvic acid had the most functional groups of total acidity and phenolic OH. The most carboxyl functional groups and spectrophotometric ratios were detected in EDTA solution. At the end, by the comparison of various methods, universal method despite the low extraction amount had more functional groups and higher efficiencies compare to others.

  13. An approach for determining quantitative measures for bone volume and bone mass in the pediatric spina bifida population.

    Science.gov (United States)

    Horenstein, Rachel E; Shefelbine, Sandra J; Mueske, Nicole M; Fisher, Carissa L; Wren, Tishya A L

    2015-08-01

    The pediatric spina bifida population suffers from decreased mobility and recurrent fractures. This study aimed to develop a method for quantifying bone mass along the entire tibia in youth with spina bifida. This will provide information about all potential sites of bone deficiencies. Computed tomography images of the tibia for 257 children (n=80 ambulatory spina bifida, n=10 non-ambulatory spina bifida, n=167 typically developing) were analyzed. Bone area was calculated at regular intervals along the entire tibia length and then weighted by calibrated pixel intensity for density weighted bone area. Integrals of density weighted bone area were used to quantify bone mass in the proximal and distal epiphyses and diaphysis. Group differences were evaluated using analysis of variance. Non-ambulatory children suffer from decreased bone mass in the diaphysis and proximal and distal epiphyses compared to ambulatory and control children (P≤0.001). Ambulatory children with spina bifida showed statistically insignificant differences in bone mass in comparison to typically developing children at these sites (P>0.5). This method provides insight into tibial bone mass distribution in the pediatric spina bifida population by incorporating information along the whole length of the bone, thereby providing more information than dual-energy x-ray absorptiometry and peripheral quantitative computed tomography. This method can be applied to any population to assess bone mass distribution across the length of any long bone. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Quantitative determination of methamphetamine in oral fluid by liquid-liquid extraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bahmanabadi, L; Akhgari, M; Jokar, F; Sadeghi, H B

    2017-02-01

    Methamphetamine abuse is one of the most medical and social problems many countries face. In spite of the ban on the use of methamphetamine, it is widely available in Iran's drug black market. There are many analytical methods for the detection of methamphetamine in biological specimen. Oral fluid has become a popular specimen to test for the presence of methamphetamine. The purpose of the present study was to develop a method for the extraction and detection of methamphetamine in oral fluid samples using liquid-liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS) methods. An analytical study was designed in that blank and 50 authentic oral fluid samples were collected to be first extracted by LLE and subsequently analysed by GC/MS. The method was fully validated and showed an excellent intra- and inter-assay precision (reflex sympathetic dystrophy ˂ 10%) for external quality control samples. Recovery with LLE methods was 96%. Limit of detection and limit of quantitation were 5 and 15 ng/mL, respectively. The method showed high selectivity, no additional peak due to interfering substances in samples was observed. The introduced method was sensitive, accurate and precise enough for the extraction of methamphetamine from oral fluid samples in forensic toxicology laboratories.

  15. Metabolism of ticlopidine in rats: identification and quantitative determination of some its metabolites in plasma, urine and bile.

    Science.gov (United States)

    Tuong, A; Bouyssou, A; Paret, J; Cuong, T G

    1981-01-01

    The fate of Ticlopidine, a new inhibitor of platelet aggregation, has been studied in rats following single oral doses. The compound was quickly absorbed as evaluated by the time of the peak plasma concentration. The metabolism of Ticlopidine involved N-oxidation, cleavage of the N-C bond, oxidation of aliphatic carbon followed by glycine conjugation. Methods for quantitation of Ticlopidine and of its metabolites, Ticlopidine-N-oxide, Tetrahydrothienopyridine, 2-cloro-hippuric acid, and the metabolite named Ticlopidine-M, are reported. Urinary excretion took place essentially in the first 24 hours and biliary excretion was most pronounced in the hour following dosing. Small amounts of Ticlopidine were excreted unchanged. The major urinary metabolites were 2-chlorohippuric acid (16% of the dose) and tetrahydrothienopyridine (8%), while Ticlopidine-M predominated in the bile (2% in 0.5h). The peak plasma concentration of Ticlopidine occurred at 0.5 hour. The plasma concentration/time curve displayed a biphasic profile and the terminal half-life of Ticlopidine was tentatively estimated to be 6-10 h in the rat. Ticlopidine-N-oxide was also quantified in plasma: the levels were inferior to those of Ticlopidine throughout the experimental period.

  16. Processes for pretreating lignocellulosic biomass: A review

    Energy Technology Data Exchange (ETDEWEB)

    McMillan, J.D.

    1992-11-01

    This paper reviews existing and proposed pretreatment processes for biomass. The focus is on the mechanisms by which the various pretreatments act and the influence of biomass structure and composition on the efficacy of particular pretreatment techniques. This analysis is used to identify pretreatment technologies and issues that warrant further research.

  17. Pretreatment Characteristics of Waste Oak Wood by Ammonia Percolation

    Science.gov (United States)

    Kim, Jun-Seok; Kim, Hyunjoon; Lee, Jin-Suk; Lee, Joon-Pyo; Park, Soon-Chul

    A log of waste oak wood collected from a Korean mushroom farm has been tested for ammonia percolation pretreatment. The waste log has different physical characteristics from that of virgin oak wood. The density of the waste wood was 30% lower than that of virgin oak wood. However, there is little difference in the chemical compositions between the woods. Due to the difference in physical characteristics, the optimal pretreatment conditions were also quite different. While for waste oak the optimum temperature was determined to be 130°C, for virgin oak wood the optimum pretreatment was only achieved at 170°C. Presoaking for 12 h with ammonia solution before pretreatment was helpful to increase the delignification efficiency.

  18. Reducing the V2O3(0001) surface through electron bombardment – a quantitative structure determination with I/V-LEED

    OpenAIRE

    Feiten, F.; Kuhlenbeck, H.; Freund, H.

    2016-01-01

    The (0001) surface of vanadium sesquioxide, V2O3, is terminated by vanadyl groups under standard ultra high vacuum preparation conditions. Reduction with electrons results in a chemically highly active surface with a well-defined LEED pattern indicating a high degree of order. In this work we report the first quantitative structure determination of a reduced V2O3(0001) surface. We identify two distinct surface phases by STM, one well ordered and one less well ordered. I/V-LEED shows the order...

  19. Evaluation of Real-Time Quantitative PCR as a Standard Cytogenetic Diagnostic Tool for Confirmation of Microarray (aCGH) Results and Determination of Inheritance

    OpenAIRE

    Wang, Rubin; Carter, Jenny; Lench, Nicholas

    2013-01-01

    Aim: To evaluate the use of real-time quantitative PCR (qPCR) as a diagnostic tool for follow up of abnormal microarray (aCGH) results. Method: qPCR was performed on 207 samples with known aCGH results to detect chromosomal abnormality and determine the capability of qPCR. Eighty-four samples were processed and the results compared with the original aCGH result and with one or more of the alternative follow-up methods: aCGH, fluorescence in situ hybridization (FISH), or karyotyping. A separat...

  20. Quantitative analysis of mineral powders by DRIFTS: Determination of SrCO3 in superconductor precursor powders

    DEFF Research Database (Denmark)

    Bak, J.; Kindl, B.

    1997-01-01

    An application of diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) has been demonstrated to be able to determine small concentrations, down to the 100-ppm level, of carbonates in powdery superconductor (SPC) precursor samples, The detection of carbonates in SPC precursor powders...

  1. Quantitative method to determine the regional drinking water odorant regulation goals based on odor sensitivity distribution: illustrated using 2-MIB.

    Science.gov (United States)

    Yu, Jianwei; An, Wei; Cao, Nan; Yang, Min; Gu, Junong; Zhang, Dong; Lu, Ning

    2014-07-01

    Taste and odor (T/O) in drinking water often cause consumer complaints and are thus regulated in many countries. However, people in different regions may exhibit different sensitivities toward T/O. This study proposed a method to determine the regional drinking water odorant regulation goals (ORGs) based on the odor sensitivity distribution of the local population. The distribution of odor sensitivity to 2-methylisoborneol (2-MIB) by the local population in Beijing, China was revealed by using a normal distribution function/model to describe the odor complaint response to a 2-MIB episode in 2005, and a 2-MIB concentration of 12.9 ng/L and FPA (flavor profile analysis) intensity of 2.5 was found to be the critical point to cause odor complaints. Thus the Beijing ORG for 2-MIB was determined to be 12.9 ng/L. Based on the assumption that the local FPA panel can represent the local population in terms of sensitivity to odor, and that the critical FPA intensity causing odor complaints was 2.5, this study tried to determine the ORGs for seven other cities of China by performing FPA tests using an FPA panel from the corresponding city. ORG values between 12.9 and 31.6 ng/L were determined, showing that a unified ORG may not be suitable for drinking water odor regulations. This study presents a novel approach for setting drinking water odor regulations. Copyright © 2014. Published by Elsevier B.V.

  2. Radioimmunoassay for the quantitative determination of human anti-meningococcal antibodies. Annual report 1 Feb 78-30 Apr 79

    International Nuclear Information System (INIS)

    Gotschlich, E.C.

    1979-01-01

    During the last year of contract support, we have performed a large number of antibody determinations on sera of children vaccinated with Group A or Group C meningococcal polysaccharide. In addition, a number of sera from monkeys vaccinated with different preparations of Group C were also studied. These sera were provided through the efforts of the staff of NIAID and also from other sources

  3. Determinants of Perceived Learning and Satisfaction in Online Business Courses: An Extension to Evaluate Differences between Qualitative and Quantitative Courses

    Science.gov (United States)

    Eastman, Jacqueline K.; Aviles, Maria; Hanna, Mark D.

    2017-01-01

    This study examined the determinants of perceived learning and satisfaction in online courses and the moderating effect of course type. For perceived learning outcomes, those students who perceive a higher level of interaction and those students who are satisfied will report higher levels of learning outcomes. There were significant differences…

  4. QUANTITATIVE-DETERMINATION OF THE DOPAMINE AGONIST LISURIDE IN PLASMA USING HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH FLUORESCENCE DETECTION

    NARCIS (Netherlands)

    WOLTHERS, BG; KAMERBEEK, WDJV; VANBEUSEKOM, CM; ELSHOF, F; BUITENHUIS, AWD; BRUNT, EPR; LAKKE, JPWF

    1993-01-01

    An HPLC method for the determination of lisuride hydrogen maleate in plasma is described. After addition of ergotamine tartrate as internal standard, plasma is extracted with diethyl ether. Following evaporation of the solvent and redissolving in methanol the extract is injected on a silica HPLC

  5. Determination of glutamate dehydrogenase activity and its kinetics in mouse tissues using metabolic mapping (quantitative enzyme histochemistry)

    NARCIS (Netherlands)

    Botman, Dennis; Tigchelaar, Wikky; van Noorden, Cornelis J. F.

    2014-01-01

    Glutamate dehydrogenase (GDH) catalyses the reversible conversion of glutamate into α-ketoglutarate with the concomitant reduction of NAD(P)(+) to NAD(P)H or vice versa. GDH activity is subject to complex allosteric regulation including substrate inhibition. To determine GDH kinetics in situ, we

  6. Thyroglobulin (Tg) recovery testing with quantitative Tg antibody measurement for determining interference in serum Tg assays in differentiated thyroid carcinoma.

    Science.gov (United States)

    Persoon, Adrienne C M; Links, Thera P; Wilde, Juergen; Sluiter, Wim J; Wolffenbuttel, Bruce H R; van den Ouweland, Johannes M W

    2006-06-01

    Thyroglobulin (Tg) measurements are complicated by interference from Tg autoantibodies (TgAbs) or heterophilic antibodies (HAMAs). We used a new automated immunochemiluminometric assay (ICMA) with Tg recovery (TgR) on the Nichols Advantage platform to reassess the clinical utility of recovery testing in detecting interference in serum Tg measurement in patients with differentiated thyroid carcinoma. We used 2 TgAb methods to detect Tg measurement interference with TgR and quantitative TgAb measurement in sera from 127 patients. In a limited number of samples, we used an RIA as comparison method because it appeared to be minimally affected by TgAb. Prevalence of TgAbs was 13% (17 of 127) in either 1 or both TgAb assays. A compromised TgR ( or =70%) corresponded with TgAb negativity in both assays for 95 of 101 samples (94%). In 6 TgAb-positive sera with TgR within the reference interval, there were no discrepancies between RIA and ICMA results. We obtained discordant RIA and ICMA results for 6 of 9 TgAb-positive sera with decreased TgR. In 1 TgAb-negative sample, the Tg result was falsely increased because of interference by HAMAs, as shown by an overrecovery of 126%. The Nichols Advantage TgR assay is a valuable complementary method to overcome the technical problem of interference by TgAbs or HAMAs in TgAb assays. Further studies are needed to confirm the potential added value of this TgR assay.

  7. Threshold microsclerotial inoculum for cotton verticillium wilt determined through wet-sieving and real-time quantitative PCR.

    Science.gov (United States)

    Wei, Feng; Fan, Rong; Dong, Haitao; Shang, Wenjing; Xu, Xiangming; Zhu, Heqin; Yang, Jiarong; Hu, Xiaoping

    2015-02-01

    Quantification of Verticillium dahliae microsclerotia is an important component of wilt management on a range of crops. Estimation of microsclerotia by dry or wet sieving and plating of soil samples on semiselective medium is a commonly used technique but this method is resource-intensive. We developed a new molecular quantification method based on Synergy Brands (SYBR) Green real-time quantitative polymerase chain reaction of wet-sieving samples (wet-sieving qPCR). This method can detect V. dahliae microsclerotia as low as 0.5 CFU g(-1) of soil. There was a high correlation (r=0.98) between the estimates of conventional plating analysis and the new wet-sieving qPCR method for 40 soil samples. To estimate the inoculum threshold for cotton wilt, >400 soil samples were taken from the rhizosphere of individual plants with or without visual wilt symptoms in experimental and commercial cotton fields at the boll-forming stage. Wilt inoculum was estimated using the wet-sieving qPCR method and related to wilt development. The estimated inoculum threshold varied with cultivar, ranging from 4.0 and 7.0 CFU g(-1) of soil for susceptible and resistant cultivars, respectively. In addition, there was an overall relationship of wilt incidence with inoculum density across 31 commercial fields where a single composite soil sample was taken at each field, with an estimated inoculum threshold of 11 CFU g(-1) of soil. These results suggest that wilt risk can be predicted from the estimated soil inoculum density using the new wet-sieving qPCR method. We recommend the use of 4.0 and 7.0 CFU g(-1) as an inoculum threshold on susceptible and resistant cultivars, respectively, in practical risk prediction schemes.

  8. Neuroanatomical patterns of the mu, delta, and kappa opioid receptors of rat brain as determined by quantitative in vitro autoradiography

    International Nuclear Information System (INIS)

    Tempel, A.; Zukin, R.S.

    1987-01-01

    Highly specific radioligands and quantitative autoradiography reveal strikingly different neuroanatomical patterns for the mu, delta, and kappa opioid receptors of rat brain. The mu receptors are most densely localized in patches in the striatum, layers I and III of the cortex, the pyramidal cell layer of the hippocampal formation, specific nuclei of the thalamus, the pars reticulata of the substantia nigra, the interpeduncular nucleus, and the locus coeruleus. In contrast, delta receptors are highly confined, exhibiting selective localization in layers I, II, and VIa of the neocortex, a diffuse pattern in the striatum, and moderate concentration in the pars reticulata of the substantia nigra and in the interpeduncular nucleus. delta receptors are absent in most other brain structures. This distribution is unexpected in that the enkephalins, the putative endogenous ligands of the delta receptor, occur essentially throughout the brain. The kappa receptors of rat brain exhibit a third pattern distinct from that of the mu and delta receptors. kappa receptors occur at low density in patches in the striatum and at particularly high density in the nucleus accumbens, along the pyramidal and molecular layers of the hippocampus, in the granular cell layer of the dentate gyrus, specific midline nuclei of the thalamus, and hindbrain regions. kappa receptors appear to be uniformly distributed across regions in the neocortex with the exception of layer III, which revealed only trace levels of binding. An important conclusion of the present study is that delta receptors occur at high density only in the forebrain and in two midbrain structures, whereas mu and kappa receptors exhibit discrete patterns in most major brain regions

  9. Quantitative Determination of Lattice Fluoride Effects on the Solubility and Crystallinity of Carbonated Apatites with Incorporated Fluoride

    Science.gov (United States)

    Yan, Guang; Moribe, Kunikazu; Otsuka, Makoto; Papangkorn, Kongnara; Higuchi, William I.

    2013-01-01

    The purpose of this study was to evaluate quantitatively the effects of fluoride on the solubility and crystallinity of carbonated apatites (CAPs) after its incorporation into the crystal lattice using the metastable equilibrium solubility (MES) distribution method. Fluoride incorporated CAPs (F-CAPs) of two different carbonate levels (3% and 5%) and fluoride contents from 0 to 20,000 μg/g were synthesized. X-ray diffraction experiments and Rietveld analysis were conducted to obtain crystallite microstrain and unit cell parameters. Acetate buffer MES solution media were prepared at two solution fluoride concentrations (0.2 mg/L and 2.0 mg/L) and at two pHs (5.0 and 5.7). The unit cell a-axis values of the F-CAPs were found to decrease as the fluoride content increased; consistent with the fluoride being incorporated into the crystal lattice. The fluoride concentrations in the MES solution media were high enough to provide a “swamping” effect such that the fluoride released from the F-CAPs during dissolution was minimal in changing the solution fluoride concentration. Employing the MES distribution superposition method, it was shown that the surface complex possessing the fluorapatite (FAP) stoichiometry (Ca10(PO4)6F2) accounted for the MES distribution behavior of all experiments. In addition, the mean pIFAP [the value of −log(aca 10PO46aF2) calculated from ionic activity product based on FAP stoichiometry of the MES dissolution media in which 50% of the F-CAP had dissolved] correlated well with the crystallite microstrain parameters of the F-CAPs. The incorporated fluoride in the F-CAPs showed only modest effects on F-CAP crystallinity and solubility. PMID:23235353

  10. A liquid chromatography-tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables.

    Science.gov (United States)

    Wang, Chao; Riedl, Ken M; Schwartz, Steven J

    2010-11-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC-MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with (13)C(5) 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C(18) column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1-9% RSD, recovery 84-91%, limit of detection 64-658 fmol and limit of quantitation 193-1994 fmol. Herein we describe a rapid, sensitive and selective HPLC-MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  11. A liquid chromatography–tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables

    Science.gov (United States)

    Wang, Chao; Riedl, Ken M.; Schwartz, Steven J.

    2013-01-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC–MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with 13C5 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C18 column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1–9% RSD, recovery 84–91%, limit of detection 64–658 fmol and limit of quantitation 193–1994 fmol. Herein we describe a rapid, sensitive and selective HPLC–MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  12. Quantitative determination of dopamine in single rat pheochromocytoma cells by microchip electrophoresis with only one high-voltage power supply.

    Science.gov (United States)

    Sha, Cuicui; Fan, Yuejuan; Cheng, Jieke; Cheng, Han

    2015-07-01

    We developed a method for the direct identification of dopamine in single cultured rat pheochromocytoma cells by capillary electrophoresis using an end-channel carbon fiber nanoelectrode amperometric detector. The operation mode was designed to achieve single-cell injection and lysis in microfluidic chip electrophoresis with only one high-voltage power supply. The separation and detection conditions were optimized. Four catecholamines were baseline-separated and determined with this system, and the cell density and liquid height of the reservoirs were accommodated for single cell loading, docking and analysis. The microchip capillary electrophoresis system was successfully applied to determine dopamine in single cultured rat pheochromocytoma cells. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. The use of Fourier-transform infrared spectroscopy for the quantitative determination of glucose concentration in whole blood

    International Nuclear Information System (INIS)

    Shen, Y C; Davies, A G; Linfield, E H; Elsey, T S; Taday, P F; Arnone, D D

    2003-01-01

    Fourier-transform infrared transmission spectroscopy has been used for the determination of glucose concentration in whole blood samples from 28 patients. A 4-vector partial least-squares calibration model, using the spectral range 950-1200 cm -1 , yielded a standard-error-of-prediction of 0.59 mM for an independent test set. For blood samples from a single patient, we found that the glucose concentration was proportional to the difference between the values of the second derivative spectrum at 1082 cm -1 and 1093 cm -1 . This indicates that spectroscopy at these two specific wavenumbers alone could be used to determine the glucose concentration in blood plasma samples from a single patient, with a prediction error of 0.95 mM

  14. A Study to Identify the Determinants of Patient Satisfaction at Martin Army Community Hospital Using Quantitative and Qualitative Methods

    Science.gov (United States)

    1990-06-01

    1988). Psychographic segmentation for marketing success, Healthcare Executive, March/April, 26-29. Oliver 87 Friedman, John (1989). Applied marketing ...the statistical calculations presented in this paper. X The Marketing Committee of MACH for their 0 involvement in determining the questions to be...services available at the Oliver 14 hospital--capitalizing on one of the best consumer marketing opportunities available in hospitals today. However

  15. Quantitative determination of total and individual flavonoids in stems and leaves of Buddleja davidii and Buddleja albiflora

    OpenAIRE

    Ying, Cheng; Wan, Dingrong

    2012-01-01

    Background: Buddleja davidii and B. albiflora are two different original plants of the famous crude medicine "Diaoyangchen." Materials and Methods: An ultraviolet-visible spectrophotometric method and a HPLC method were used for the determination of total and individual flavonoids (luteolin and apigenin) contents from their stems and leaves for the first time. Results: From the comparative evaluation, remarkable differences in flavonoids contents were observed between different origins and di...

  16. Validation of an analytical method for the quantitative determination of selenium in bacterial biomass by ultraviolet-visible spectrophotometry.

    Science.gov (United States)

    Mörschbächer, Ana Paula; Dullius, Anja; Dullius, Carlos Henrique; Bandt, Cassiano Ricardo; Kuhn, Daniel; Brietzke, Débora Tairini; Malmann Kuffel, Fernando José; Etgeton, Henrique Pretto; Altmayer, Taciélen; Gonçalves, Tamara Engelmann; Oreste, Eliézer Quadro; Ribeiro, Anderson Schwingel; de Souza, Claucia Fernanda Volken; Hoehne, Lucélia

    2018-07-30

    The present paper describes the validation of a spectrophotometry method involving molecular absorption in the visible ultraviolet-visible (UV-Vis) region for selenium (Se) determination in the bacterial biomass produced by lactic acid bacteria (LAB). The method was found to be suitable for the target application and presented a linearity range from 0.025 to 0.250 mg/L Se. The angular and linear coefficients of the linear equation were 1.0678 and 0.0197 mg/L Se, respectively, and the linear correlation coefficient (R 2 ) was 0.9991. Analyte recovery exceeded 96% with a relative standard deviation (RSD) below 3%. The Se contents in LAB ranged from 0.01 to 20 mg/g. The Se contents in the bacterial biomass determined by UV-Vis were not significantly different (p > 0.05) those determined by graphite furnace atomic absorption spectrometry. Thus, Se can be quantified in LAB biomass using this relatively simpler technique. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. Study on the method for determination of the nuclear fuel elements burnout by the quantitative analysis of 148Nd

    International Nuclear Information System (INIS)

    Enoshita, Margarida

    1978-01-01

    The scope of present work to study the precision and accuracy of a method for separation and determination of the.stable isotope 148 Nd. The extraction chromatography and ion exchange techniques were used for the separation of fission products and uranium. Kieselguhr and di(2-ethyl-hexyl)phosphoric acid were used as inert support and stationary phase, respectively, in the steps of the separation procedure where the extraction chromatography technique was applied, and anionic resin mixed with Pb0 2 was used for the ion exchange operation. The behaviour of each element in the separation procedure was verified by means of radioactive tracers, namely, 147 Nd, 141 Ce and 137 Cs. Use was made of the thermal neutron activation analysis in order to determine the 148 Nd percentage recovered after the separation procedure was run. On the other hand, the radioactive isotope 147 Nd was used to find chemical yield achieved for the separation procedure. Student's t test applied to verify the accuracy of the method used whose acceptability was verified by using the criterion recommended by McFarren and also taking into account the suggestion proposed by Eckschlager. The precision of the method was verified by means of the standard deviation of the several determinations. (author)

  18. Determination of glutamate dehydrogenase activity and its kinetics in mouse tissues using metabolic mapping (quantitative enzyme histochemistry).

    Science.gov (United States)

    Botman, Dennis; Tigchelaar, Wikky; Van Noorden, Cornelis J F

    2014-11-01

    Glutamate dehydrogenase (GDH) catalyses the reversible conversion of glutamate into α-ketoglutarate with the concomitant reduction of NAD(P)(+) to NAD(P)H or vice versa. GDH activity is subject to complex allosteric regulation including substrate inhibition. To determine GDH kinetics in situ, we assessed the effects of various glutamate concentrations in combination with either the coenzyme NAD(+) or NADP(+) on GDH activity in mouse liver cryostat sections using metabolic mapping. NAD(+)-dependent GDH V(max) was 2.5-fold higher than NADP(+)-dependent V(max), whereas the K(m) was similar, 1.92 mM versus 1.66 mM, when NAD(+) or NADP(+) was used, respectively. With either coenzyme, V(max) was determined at 10 mM glutamate and substrate inhibition was observed at higher glutamate concentrations with a K(i) of 12.2 and 3.95 for NAD(+) and NADP(+) used as coenzyme, respectively. NAD(+)- and NADP(+)-dependent GDH activities were examined in various mouse tissues. GDH activity was highest in liver and much lower in other tissues. In all tissues, the highest activity was found when NAD(+) was used as a coenzyme. In conclusion, GDH activity in mice is highest in the liver with NAD(+) as a coenzyme and highest GDH activity was determined at a glutamate concentration of 10 mM. © The Author(s) 2014.

  19. Differential effects of a post-anthesis fertilizer regimen on the wheat flour proteome determined by quantitative 2-DE

    Directory of Open Access Journals (Sweden)

    Altenbach Susan B

    2011-08-01

    Full Text Available Abstract Background Mineral nutrition during wheat grain development has large effects on wheat flour protein content and composition, which in turn affect flour quality and immunogenic potential for a commodity of great economic value. However, it has been difficult to define the precise effects of mineral nutrition on protein composition because of the complexity of the wheat flour proteome. Recent improvements in the identification of flour proteins by tandem mass spectrometry (MS/MS and the availability of a comprehensive proteome map of flour from the US wheat Butte 86 now make it possible to document changes in the proportions of individual flour proteins that result from the application of mineral nutrition. Results Plants of Triticum aestivum 'Butte 86' were grown with or without post-anthesis fertilization (PAF and quantitative 2-dimensional gel electrophoresis (2-DE was used to analyze protein composition of the resulting flour. Significant changes in the proportions of 54 unique proteins were observed as a result of the treatment. Most omega-gliadins, high molecular weight glutenin subunits (HMW-GS and serpins as well as some alpha-gliadins increased in proportion with PAF. In contrast, alpha-amylase/protease inhibitors, farinins, purinins and puroindolines decreased in proportion. Decreases were also observed in several low molecular weight glutenin subunits (LMW-GS, globulins, defense proteins and enzymes. The ratio of HMW-GS to LMW-GS in the flour increased from 0.61 to 0.95 and the ratio of gliadins to glutenins increased from 1.02 to 1.30 with PAF. Because flour protein content doubled with PAF from 7 to 14%, most protein types actually increased in absolute amount (μg/mg flour protein. Data further suggest that flour proteins change with PAF according to their content of sulfur-containing amino acids Cys + Met. Conclusions A 2-DE approach revealed changes in the wheat flour proteome due to PAF that are important for flour

  20. Assessment of goals and priorities in patients with a chronic condition: a secondary quantitative analysis of determinants across 11 countries.

    Science.gov (United States)

    Vermunt, Neeltje P C A; Westert, Gert P; Olde Rikkert, Marcel G M; Faber, Marjan J

    2018-03-01

    To assess the impact of patient characteristics, patient-professional engagement, communication and context on the probability that healthcare professionals will discuss goals or priorities with older patients. Secondary analysis of cross-sectional data from the 2014 Commonwealth Fund International Health Policy Survey of Older Adults. 11 western countries. Community-dwelling adults, aged 55 or older. Assessment of goals and priorities. The final sample size consisted of 17,222 respondents, 54% of whom reported an assessment of their goals and priorities (AGP) by healthcare professionals. In logistic regression model 1, which was used to analyse the entire population, the determinants found to have moderate to large effects on the likelihood of AGP were information exchange on stress, diet or exercise, or both. Country (living in Sweden) and continuity of care (no regular professional or organisation) had moderate to large negative effects on the likelihood of AGP. In model 2, which focussed on respondents who experienced continuity of care, country and information exchange on stress and lifestyle were the main determinants of AGP, with comparable odds ratios to model 1. Furthermore, a professional asking questions also increased the likelihood of AGP. Continuity of care and information exchange is associated with a higher probability of AGP, while people living in Sweden are less likely to experience these assessments. Further study is required to determine whether increasing information exchange and professionals asking more questions may improve goal setting with older patients. Key points   A patient goal-oriented approach can be beneficial for older patients with chronic conditions or multimorbidity; however, discussing goals with these patients is not a common practice. The likelihood of discussing goals varies by country, occurring most commonly in the USA, and least often in Sweden. Country-level differences in continuity of care and questions asked by a

  1. Identification and quantitative determination of carbohydrates in ethanolic extracts of two conifers using 13C NMR spectroscopy.

    Science.gov (United States)

    Duquesnoy, Emilie; Castola, Vincent; Casanova, Joseph

    2008-04-07

    We developed a method for the direct identification and quantification of carbohydrates in raw vegetable extracts using (13)C NMR spectroscopy without any preliminary step of precipitation or reduction of the components. This method has been validated (accuracy, precision and response linearity) using pure compounds and artificial mixtures before being applied to authentic ethanolic extracts of pine needles, pine wood and pine cones and fir twigs. We determined that carbohydrates represented from 15% to 35% of the crude extracts in which pinitol was the principal constituent accompanied by arabinitol, mannitol, glucose and fructose.

  2. Quantitative determination of uranium and thorum contents of some rock samples in Nigeria using natural calibration sources

    International Nuclear Information System (INIS)

    Uwah, E.J.; Ajakaiye, D.E.

    1987-01-01

    Three natural multiple-source standards were used to estimate eU and eTh concentrations in rock samples collected during in-situ reconnaissance surveys in the Sokoto Basin of Nigeria. The standards were those previously analyzed by Delayed neutron counting (DNC) and X0ray Fluoresence (DRF) techniques (Uwah and Ajakaiye, 1986). Regression analysis of the data from twelve of the samples analyzed by DNC and XRF techniques enabled a quick approximate determination of eU and eTh in many samples in the survey area, containing about 50 ppm U and above

  3. Quantitative determination of cucurbitane-type triterpenes and triterpene glycosides in dietary supplements containing bitter melon (Momordica charantia) by HPLC-MS/MS.

    Science.gov (United States)

    Ma, Jun; Krynitsky, Alexander J; Grundel, Erich; Rader, Jeanne I

    2012-01-01

    Momordica charantia L. (Cucurbitaceae), commonly known as bitter melon, is widely cultivated in many tropical and subtropical areas of the world. It is a common food staple; its fruits, leaves, seeds, stems, and roots also have a long history of use in traditional medicine. In the United States, dietary supplements labeled as containing bitter melon can be purchased over-the-counter and from Internet suppliers. Currently, no quantitative analytical method is available for monitoring the content of cucurbitane-type triterpenes and triterpene glycosides, the major constituents of bitter melon, in such supplements. We investigated the use of HPLC-electrospray ionization (ESI)-MS/MS for the quantitative determination of such compounds in dietary supplements containing bitter melon. Values for each compound obtained from external calibration were compared with those obtained from the method of standard additions to address matrix effects associated with ESI. In addition, the cucurbitane-type triterpene and triterpene glycoside contents of two dietary supplements determined by the HPLC-ESI-MS/MS method with standard additions were compared with those measured by an HPLC method with evaporative light scattering detection, which was recently developed for quantification of such compounds in dried fruits of M. charantia. The contents of five cucurbitane-type triterpenes and triterpene glycosides in 10 dietary supplements were measured using the HPLC-ESI-MS/MS method with standard additions. The total contents of the five compounds ranged from 17 to 3464 microg/serving.

  4. Application of Near-Infrared Spectroscopy to Quantitatively Determine Relative Content of Puccnia striiformis f. sp. tritici DNA in Wheat Leaves in Incubation Period

    Directory of Open Access Journals (Sweden)

    Yaqiong Zhao

    2017-01-01

    Full Text Available Stripe rust caused by Puccinia striiformis f. sp. tritici (Pst is a devastating wheat disease worldwide. Potential application of near-infrared spectroscopy (NIRS in detection of pathogen amounts in latently Pst-infected wheat leaves was investigated for disease prediction and control. A total of 300 near-infrared spectra were acquired from the Pst-infected leaf samples in an incubation period, and relative contents of Pst DNA in the samples were obtained using duplex TaqMan real-time PCR arrays. Determination models of the relative contents of Pst DNA in the samples were built using quantitative partial least squares (QPLS, support vector regression (SVR, and a method integrated with QPLS and SVR. The results showed that the kQPLS-SVR model built with a ratio of training set to testing set equal to 3 : 1 based on the original spectra, when the number of the randomly selected wavelength points was 700, the number of principal components was 8, and the number of the built QPLS models was 5, was the best. The results indicated that quantitative detection of Pst DNA in leaves in the incubation period could be implemented using NIRS. A novel method for determination of latent infection levels of Pst and early detection of stripe rust was provided.

  5. Validation of an Ultraviolet-visible (UV-Vis) technique for the quantitative determination of curcumin in poly(L-lactic acid) nanoparticles.

    Science.gov (United States)

    Silva-Buzanello, Rosana Aparecida da; Ferro, Ana Caroline; Bona, Evandro; Cardozo-Filho, Lúcio; Araújo, Pedro Henrique Hermes de; Leimann, Fernanda Vitória; Gonçalves, Odinei Hess

    2015-04-01

    Curcumin is a natural yellow-orange pigment extracted from turmeric and is a potential substitute of health-dangerous artificial dyes. Nanoencapsulation in biodegradable polymers is a promising alternative to improve curcumin stability and water solubility but curcumin concentration inside the nanoparticles must be precisely known. A reliable method to determine the actual curcumin concentration must be validated since the validation procedures warrant that the method is adequate and sufficient for the specific application involved. This work describes the validation parameters given by the International Conference on Harmonisation (ICH) guidelines to adopt an analytical method based on Ultraviolet-visible spectroscopy for the quantitative determination of curcumin encapsulated in poly(l-lactic acid) nanoparticles. This method was validated in respect to linearity, detection limit, quantification limit, accuracy and precision. Studies on the analytical procedure validation warranted safety in final results obtained for the curcumin concentration in the nanoparticles. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. New method for determination of quantitative indices of zooplankton feeding with the use of phosphorus isotopes under close to ''in situ'' conditions

    International Nuclear Information System (INIS)

    Zesenko, A.Ja.; Pavlovskaya, T.V.

    1985-01-01

    A new method determining food rations, duration of food digestion and elements of food balance in case of zooplankton fed on natural plankton was elaborated. A feature of radioactive mineral phosphorus entering into all components of plankton in natural marine water is a basis of this method. Fractionating the natural plankton according to the size of food particles with determination of specific radioactivity in them give a possibility to elucidate selectivity of feeding in zooplankton, its role in grazing and transforming the matter as well as regeneration of mineral phosphorus in pelagial ecosystems. High sensitivity (1 x 10 -4 μg P/indiv.) of the method allows to carry out experiments on separate individuals and estimate quantitatively variability of their food rations and separate elements of food balance. 28 refs., 3 figs., 3 tabs. (author)

  7. A method for volume determination of the orbit and its contents by high resolution axial tomography and quantitative digital image analysis.

    Science.gov (United States)

    Cooper, W C

    1985-01-01

    The various congenital and acquired conditions which alter orbital volume are reviewed. Previous investigative work to determine orbital capacity is summarized. Since these studies were confined to postmortem evaluations, the need for a technique to measure orbital volume in the living state is presented. A method for volume determination of the orbit and its contents by high-resolution axial tomography and quantitative digital image analysis is reported. This procedure has proven to be accurate (the discrepancy between direct and computed measurements ranged from 0.2% to 4%) and reproducible (greater than 98%). The application of this method to representative clinical problems is presented and discussed. The establishment of a diagnostic system versatile enough to expand the usefulness of computerized axial tomography and polytomography should add a new dimension to ophthalmic investigation and treatment.

  8. Use of quantitative real-time PCR to determine viability of Streptococcus equi subspecies equi in respiratory secretions from horses with strangles.

    Science.gov (United States)

    Pusterla, N; Leutenegger, C M; Barnum, S M; Byrne, B A

    2018-01-17

    In recent years, molecular approaches have been able to characterise the viability of equine upper respiratory tract pathogens using absolute molecular quantitation as well as detection of transcripts for virulence genes. The objective of this study was to investigate molecular surrogates for S. equi subspecies equi (S. equi) viability in biological samples from horses with strangles. Retrospective cross-sectional study. S. equi culture-positive and culture-negative upper airway secretions were assessed by qPCR at the genomic (gDNA) and complimentary DNA (cDNA) level for various target genes (SeM, SEQ2190, eqbE and szpSe). Absolute quantitation was performed using standard curves, and the results were expressed as number of S. equi target genes per μl of gDNA or cDNA. Additionally, the presence or absence of S. equi gene expression for the various target genes was assessed and compared with the culture results. While all 21 culture-positive samples tested S. equiqPCR positive, up to 43.7 and 18.9% of 64 culture-negative samples tested qPCR positive at the gDNA and cDNA level, respectively. Significant differences in absolute quantitation for S. equi at the gDNA level were found between culture-positive and culture-negative samples. When absolute quantitation of S. equi target genes at the gDNA level was assessed with the presence or absence of transcripts, there was a significantly higher S. equi target gene number in samples with expression of transcripts compared with samples with no expression of transcripts. The lack of standardisation of samples collected in the field and the delay from sample collection to samples processing may have negatively affected the cultivability of S. equi and mRNA quality. Molecular viability for S. equi can be investigated by determining absolute quantitation and/or by detecting mRNA for specific target genes. However, veterinarians have to be cautioned that any qPCR-positive result for S. equi needs to be taken

  9. Quantitative determination of the dopamine agonist lisuride in plasma using high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Wolthers, B G; Verhagen Kamerbeek, W D; van Beusekom, C M; Elshof, F; de Ruyter Buitenhuis, A W; Brunt, E P; Lakke, J P

    1993-12-08

    An HPLC method for the determination of lisuride hydrogen maleate in plasma is described. After addition of ergotamine tartrate as internal standard, plasma is extracted with diethyl ether. Following evaporation of the solvent and redissolving in methanol the extract is injected on a silica HPLC column and lisuride is monitored by fluorescence detection using an excitation wavelength of 322 nm and an emission wavelength of 405 nm. The method is sufficiently accurate and precise with a detection limit of 20 pg/ml lisuride in plasma. The usefulness of the method is demonstrated by measurements of lisuride levels after oral intake of a 0.6 mg dose of the drug by a healthy male volunteer, showing a peak level of 1266 pg/ml, 45 min after intake.

  10. Quantitative determination of metaxalone in human plasma by LC-MS and its application in a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Lanting Zhao

    2016-10-01

    Full Text Available A simple and rapid method using liquid chromatography–mass spectrometry (LC-MS for the determination of metaxalone in human plasma has been developed and validated. Letrozole was used as the internal standard (IS. The plasma samples were simply treated with acetonitrile which allowed the precipitation of plasma proteins. The chromatographic separation was achieved on a Sapphire C18 (2.1 mm × 150 mm, 5 µm, Newark, USA column using the mobile phase (5 mM ammonium acetate containing 0.01% formic acid: acetonitrile (45:55, v/v at a flow rate of 0.3 ml/min. The selected ion monitoring (SIM in the positive mode was used for the determination of [M + H]+ m/z 222.1 and 286.1 for metaxalone and letrozole, respectively. The standard curve obtained was linear (r2 ≥ 0.99 over the concentration range of 30.24−5040 ng/ml. Meanwhile, no interfering peaks or matrix effect was observed. The method established was simple and successfully applied to a pharmacokinetic study of metaxalone in healthy Chinese volunteers after a single oral dose administration of 800 mg metaxalone. The main pharmacokinetic parameters of metaxalone were as follow: Cmax, (1664 ± 1208 ng/ml and (2063 ± 907 ng/ml; AUC0−36, (13925 ± 6590 ng/ml h and (18620 ± 5717 ng/ml h; t1/2, (13.6 ± 7.7 h and (20.3 ± 7.7 h for the reference and test tablets, respectively. These pharmacokinetic parameters of metaxalone in healthy Chinese volunteers were reported for the first time.

  11. An automated FTIR method for the routine quantitative determination of moisture in lubricants: An alternative to Karl Fischer titration.

    Science.gov (United States)

    van de Voort, Frederik R; Sedman, Jacqueline; Cocciardi, Robert; Juneau, Steve

    2007-04-15

    An accurate primary Fourier transform infrared (FTIR) method for the determination of moisture in mineral and ester based lubricants has been developed based on the extraction of moisture into dry acetonitrile. FTIR evaluation of acetonitrile extracts from new and used lubricants as well as common lubricant additives and contaminants which might co-extract indicated that phenolic constituents interfered significantly with moisture measurements. By measuring moisture at 3676cm(-1) on the shoulder of the asymmetric OH stretching band, spectral interferences from extracted phenolic constituents were minimized. The spectra of calibration standards (0-2100ppm), prepared by gravimetric addition of water to dry acetonitrile, were recorded in a 1000-mum CaF(2) transmission flow cell and produced linear standard curves having an S.D. of approximately +/-20ppm. Lubricant sample preparation involved the vigorous shaking (20min) of a 1:1.5 (w/v) mixture of lubricant and dry acetonitrile, centrifugation to separate the phases, acquisition of the FTIR spectrum of the upper acetonitrile layer, and subtraction of the spectrum of the dry acetonitrile used for extraction. A Continuous Oil Analyzer and Treatment (COAT((R))) FTIR system was programmed to allow the automated analysis of acetonitrile extracts, and the methodology was validated by analyzing 58 new and used oils, independently analyzed by the Karl Fischer (KF) method. Linear regression of FTIR versus KF results for these oils produced a linear plot with a between-method S.D. of +/-80ppm. As implemented on the COAT((R)) system, this FTIR method is capable of analyzing 72 acetonitrile extracts/h and provides a high-speed alternative to the KF titrimetric procedures for the determination of water in lubricants.

  12. Quantitative texture determination in pressure tube (Zr-2.5 Wt% Nb alloy) material as a function of cold work

    International Nuclear Information System (INIS)

    Dey, G.K.; Tewari, R.; Srivastava, D.; De, P.K.; Banerjee, S.; Kiran Kumar, M.; Samajdar, I.

    2003-06-01

    The texture studies on the pressure tube Zr-2.5 Nb alloy have mainly been confined to the determination of the basal pole distribution along certain direction or the inverse pole presentation in the material. This information though useful does not provide an insight into micro-textural development upon cold working. In the present study, complete bulk as well as micro texture development as a function of cold work has been obtained by determining orientation distribution function. In this work, two distinct starting microstructures of Zr-2.5 wt% Nb have been used -(a) single-phase α(hcp) martensitic structure and (b) two-phase, β(bcc) + α, Widmanstaetten structure. In the second case, the α phase was present in lamellar morphology and β stringers were sandwiched between these a lamella. In some instances single-phase α were present. However, both microstructures had similar starting crystallographic texture. Samples were deformed by unidirectional and cross rolling at room temperature. In the two-phase structure the changes in the bulk texture on cold rolling was found to be insignificant, while in the single-phase material noticeable textural changes were observed. Taylor type deformation texture models predicted textural changes in single-phase structure but failed to predict the observed lack of textural development in the two-phase material. Microtexture observations showed that a plates remained approximately single crystalline after cold rolling, while the β matrix underwent significant orientational changes. Based on microstructural and microtextural observations, a simple model is proposed in which the plastic flow is mainly confined to the β matrix within which the α plates are subjected to in-plane rigid body rotation. The model explains the observed lack of textural developments in the two-phase structure. (author)

  13. Tank Focus Area pretreatment activities

    International Nuclear Information System (INIS)

    McGinnis, C.P.; Welch, T.D.; Manke, K.L.

    1997-01-01

    Plans call for the high-level wastes to be retrieved from the tanks and immobilized in a stable waste form suitable for long-term isolation. Chemistry and chemical engineering operations are required to retrieve the wastes, to condition the wastes for subsequent steps, and to reduce the costs of the waste management enterprise. Pretreatment includes those processes between retrieval and immobilization, and includes preparation of suitable feed material for immobilization and separations to partition the waste into streams that yield lower life-cycle costs. Some of the technologies being developed by the Tank Focus Area (TFA) to process these wastes are described. These technologies fall roughly into three areas: (1) solid/liquid separation (SLS), (2) sludge pretreatment, and (3) supernate pretreatment

  14. Enhanced biogas production from penicillin bacterial residue by thermal-alkaline pretreatment

    International Nuclear Information System (INIS)

    Zhong, Weizhang; Li, Guixia; Gao, Yan; Li, Zaixing; Geng, Xiaoling; Li, Yubing; Yang, Jingliang; Zhou, Chonghui

    2015-01-01

    In this study, the orthogonal experimental design was used to determine the optimum conditions for the effect of thermal alkaline; pretreatment on the anaerobic digestion of penicillin bacterial residue. The biodegradability of the penicillin; bacterial residue was evaluated by biochemical methane potential tests in laboratory. The optimum values of temperature,; alkali concentration, pretreatment time and moisture content for the thermal-alkaline pretreatment were determined as; 70 °C, 6% (w/v), 30 min, and 85%, respectively. Thermal-alkaline pretreatment could significantly enhance the soluble; chemical oxygen demand solubilization, the suspended solid solubilization and the biodegradability. Biogas production; was enhanced by the thermal-alkaline pretreatment, probably as a result of the breakdown of cell walls and membranes of; micro-organisms, which may facilitate the contact between organic molecules and anaerobic microorganisms.; Keywords: penicillin bacterial residue; anaerobic digestion; biochemical methane potential tests; pretreatment

  15. Determination of quantitative food consumption levels for use in microbial risk assessments: cheddar cheese as an example.

    Science.gov (United States)

    Bahk, Gyung-Jin; Todd, Ewen C D

    2007-01-01

    Microbial risk assessment (MRA) is becoming increasingly used in the management of food safety because it can be used to quantify risks and help rank intervention strategies. The exposure assessment components of the assessments have become complex with many aspects of the contamination, survival, and growth of a pathogen in a food being taken into consideration. Insufficient consumption data constitutes an important data gap and consequently one of many sources of uncertainty in MRA even though the effects of uncertainty are smaller than those affecting bacterial concentration in foods. Therefore, food consumption data also play an important role in exposure assessment of MRA. In the United States, there are large-scale, nationwide sets of consumption data available for use in MRA, i.e., the National Health and Nutrition Examination Survey (NHANES). Newly released dietary interview data in the NHANES 2001 to 2002 survey show that it has been redesigned and that the data were sufficiently updated from previous versions to have more value for MRAs. We propose a model that can effectively use the new data sets and be incorporated into MRAs, using as an example consumption of Cheddar cheese/American-type cheese. This model included the prevalence of food eaten as well as the amount and frequency. We determined the amount of Cheddar/American cheese consumed per day with probability distribution (e.g., lognormal distribution). These could be further determined by gender, age, pregnancy, and combination food type, which we plan to do in the future. The frequency of the range of serving numbers for Cheddar/American cheese consumed per person per day and prevalence as the proportion of a population (e.g., survey respondents) eating a certain food in a day are also presented. Unlike traditional published mean values, the results of this model provide probability distribution intakes that can be compared with mean and median intakes. This allows values in the upper

  16. Development of an open source software of quantitative analysis for radionuclide determination by gamma-ray spectrometry using semiconductor detectors

    International Nuclear Information System (INIS)

    Maduar, Marcelo Francis

    2010-01-01

    Radioactivity quantification of gamma-ray emitter radionuclides in samples measured by HPGe gamma-ray spectrometry relies on the analysis of the photopeaks present in the spectra, especially on the accurate determination of their net areas. Such a task is usually performed with the aid of proprietary software tools. This work presents a methodology, algorithm descriptions and an open source application, called OpenGamma, for the peak search and analysis in order to obtain the relevant peaks parameters and radionuclides activities. The computational implementation is released entirely in open-source license for the main code and with the use of open software packages for interface design and mathematical libraries. The procedure for the peak search is performed on a three step approach. Firstly a preliminary search is done by using the second-difference method, consisting in the generation of a derived spectrum in order to find candidate peaks. In the second step, the experimental peaks widths are assessed and well formed and isolated ones are chosen to obtain a FWHM vs. channel relationship, by application of the Levenberg-Marquardt minimization method for non-linear fitting. Lastly, regions of the spectrum with grouped peaks are marked and a non-linear fit is again applied to each region to obtain baseline and photopeaks terms; from these terms, peaks net areas are then assessed. (author)

  17. Deep Eutectic Solvents as Novel and Effective Extraction Media for Quantitative Determination of Ochratoxin A in Wheat and Derived Products

    Directory of Open Access Journals (Sweden)

    Luca Piemontese

    2017-01-01

    Full Text Available An unprecedented, environmentally friendly, and faster method for the determination of Ochratoxin A (OTA (a mycotoxin produced by several species of Aspergillus and Penicillium and largely widespread in nature, in wheat and derived products has, for the first time, been set up and validated using choline chloride (ChCl-based deep eutectic solvents (DESs (e.g., ChCl/glycerol (1:2 and ChCl/ urea (1:2 up to 40% (w/w water as privileged, green, and biodegradable extraction solvents. This also reduces worker exposure to toxic chemicals. Results are comparable to those obtained using conventional, hazardous and volatile organic solvents (VOCs typical of the standard and official methods. OTA recovery from spiked durum wheat samples, in particular, was to up to 89% versus 93% using the traditional acetonitrile-water mixture with a repeatability of the results (RSDr of 7%. Compatibility of the DES mixture with the antibodies of the immunoaffinity column was excellent as it was able to retain up to 96% of the OTA. Recovery and repeatability for durum wheat, bread crumbs, and biscuits proved to be within the specifications required by the current European Commission (EC regulation. Good results in terms of accuracy and precision were achieved with mean recoveries between 70% (durum wheat and 88% (bread crumbs and an RSDr between 2% (biscuits and 7% (bread.

  18. Quantitative determination of carboxylic acids, amino acids, carbohydrates, ethanol and hydroxymethylfurfural in honey by (1)H NMR.

    Science.gov (United States)

    del Campo, Gloria; Zuriarrain, Juan; Zuriarrain, Andoni; Berregi, Iñaki

    2016-04-01

    A method using (1)H NMR spectroscopy has been developed to quantify simultaneously thirteen analytes in honeys without previous separation or pre-concentration steps. The method has been successfully applied to determine carboxylic acids (acetic, formic, lactic, malic and succinic acids), amino acids (alanine, phenylalanine, proline and tyrosine), carbohydrates (α- and β-glucose and fructose), ethanol and hydroxymethylfurfural in eucalyptus, heather, lavender, orange blossom, thyme and rosemary honeys. Quantification was performed by using the area of the signal of each analyte in the honey spectra, together with external standards. The regression analysis of the signal area against concentration plots, used for the calibration of each analyte, indicates a good linearity over the concentration ranges found in honeys, with correlation coefficients higher than 0.985 for the thirteen quantified analytes. The recovery studies give values over the 93.7-105.4% range with relative standard deviations lower than 7.4%. Good precision, with relative standard deviations over the range of 0.78-5.21% is obtained. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Mamona: determinação quantitativa do teor de óleo Quantitive determination of castor oil

    Directory of Open Access Journals (Sweden)

    Míriam Bottiglia Tambascia

    1986-01-01

    Full Text Available Foi desenvolvida uma metodologia para quantificar o teor de óleo em sementes de mamona, a partir da determinação do índice de refração de soluções etanólicas de diferentes concentrações a diferentes temperaturas. Os resultados mostraram um comportamento linear entre índice de refração e concentração de óleo para cada temperatura, com um excelente coeficiente de correlação, permitindo, assim, a quantificação do teor de óleo de mamona por metodologia bastante rápida e precisa.A methodology was developed to quantify the castor oil seed content, through the determination of refractive index of ethanolic solutions with different oil concentrations and temperatures. The results showed a nearly linear relationship between the refractive index and oil concentration for each temperature. This correlation permits to quantify castor oil content of ethanolic solutions by calculation from the quickly and accurate measurement of refractive index.

  20. HPLC-QTOF-MS method for quantitative determination of active compounds in an anti-cellulite herbal compress

    Directory of Open Access Journals (Sweden)

    Ngamrayu Ngamdokmai

    2017-08-01

    Full Text Available A herbal compress used in Thai massage has been modified for use in cellulite treatment. Its main active ingredients were ginger, black pepper, java long pepper, tea and coffee. The objective of this study was to develop and validate an HPLCQTOF-MS method for determining its active compounds, i.e., caffeine, 6-gingerol, and piperine in raw materials as well as in the formulation together with the flavouring agent, camphor. The four compounds were chromatographically separated. The analytical method was validated through selectivity, intra-, inter day precision, accuracy and matrix effect. The results showed that the herbal compress contained caffeine (2.16 mg/g, camphor (106.15 mg/g, 6-gingerol (0.76 mg/g, and piperine (4.19 mg/g. The chemical stability study revealed that herbal compresses retained >80% of their active compounds after 1 month of storage at ambient conditions. Our method can be used for quality control of the herbal compress and its raw materials.

  1. Quantitative determination of sediment movement at the landward spoil ground in the Yangtze Estuary with radioactive tracer

    International Nuclear Information System (INIS)

    Li Zhangsu

    1993-01-01

    A radioactive tracer experiment was carried out at the landward spoil ground of the North Passage in the Yangtze Estuary in June of 1991. The scandium-46 was selected as the tracer, the total activity released is 17.95 x 10 10 Bq(4.85 Ci), the amount of the scandium-46 glass is 495 g. The purpose of the experiment is to determine the sediment movement direction, path, velocity and transport rate. The experiment provides the direct evidence for using the landward spoil ground in the future. The experiment results show the sediment movement was governed by the ebb tide current during the period of middle and neap tides when the radioactive tracer was injected both on the flood and ebb tides, and the sediment moved from the injection points to the middle of the North Passage near the navigation buoy No. 269. The direction of the sediment movement is 110 degree, the particle velocity is 758 m/d, and the sediment transport rate per unit width is 47.8 m 3 /md

  2. QUANTITATIVE DETERMINATION OF MAIN GROUPS OF SUBSTANCES IN GRANULES ON THE BASIS OF MEDICINAL VEGETABLE RAW MATERIAL FOR TREATING GASTROINTESTINAL DISEASES

    Directory of Open Access Journals (Sweden)

    Spiridonov S.V.

    2014-12-01

    Full Text Available In the last time a significant increasing of gastrointestinal tract diseases has been observed. The poor quality and irrational feeding, environmental pollution, psychological and other factors is the causes of this. Very often the gastrointestinal tract has a multifactorial pathological effects, also affecting the hepatosphere organs and urogenital system. Also a great importance have accompanying disorders of the central nervous system. Thus we must to require a comprehensive approach to the creation of drugs for use in gastroenterology, the assortment range of which should be expanded. Advantageous position in this case takes a phytotherapy using drugs based on medicinal plant raw material, which acting on the main areas of the pathological process. For this purpose the scientists from the National University of Pharmacy (Kharkov, Ukraine was created a complex herbal drug in the form of granules under the code name "Poligerbagastrin", includes the following types of medicinal plant raw material powders: helichrysum arenarium flowers, corn stigmas, horsetail grass, knotweed grass, horse chestnut seeds, licorice roots and wheat bran. Materials and methods To determine the quantity of biologically active substances the method of spectrophotometry in the visible and UV spectral region was used. This method is well studied and available, equipped with high-precision hardware. He also described in the Ukrainian normative documents and contained in the world's leading pharmacopoeias. For determination was used the unifieds methods, which shown in pharmacopoeia monographs and other reference literature. Determination was carried out with a spectrophotometer HP 8543 UV-VIZ of «Hewlett Packard» company, USA. Results and discussion For the quantitative determination of flavonoids was used a methodology, which based on the complexation reaction of isolated by acid hydrolysis and extraction with ethylacetate hydrolysis products with aluminum chloride in

  3. The sentinel lymph node spread determines quantitatively melanoma seeding to non-sentinel lymph nodes and survival.

    Science.gov (United States)

    Ulmer, Anja; Dietz, Klaus; Werner-Klein, Melanie; Häfner, Hans-Martin; Schulz, Claudia; Renner, Philipp; Weber, Florian; Breuninger, Helmut; Röcken, Martin; Garbe, Claus; Fierlbeck, Gerhard; Klein, Christoph A

    2018-03-01

    Complete lymph node dissection (CLND) after a positive sentinel node (SN) biopsy provides important prognostic information in melanoma patients but has been questioned for therapeutic use recently. We explored whether quantification of the tumour spread to SNs may replace histopathology of non-sentinel nodes (NSNs) for staging purposes. We quantified melanoma spread in SNs and NSNs in 128 patients undergoing CLND for a positive SN. In addition to routine histopathology, one-half of each of all 1496 SNs and NSNs was disaggregated into a single cell suspension and stained immunocytochemically to determine the number of melanoma cells per 10 6 lymph node cells, i.e. the disseminated cancer cell density (DCCD). We uncovered melanoma spread to NSNs in the majority of patients; however, the tumour load and the proportion of positive nodes were significantly lower in NSNs than in SNs. The relation between SN and NSN spread could be described by a mathematical function with DCCD NSN  = DCCD SN c /10 1 - c (c = 0.69; 95% confidence interval [CI]: 0.62-0.76). At a median follow-up of 67 months, multivariable Cox regression analyses revealed that DCCD SN (p = 0.02; HR 1.34, 95% CI: 1.05-1.71) and the total number of pathologically positive nodes (p = 0.02; HR 1.53, 95% CI: 1.07-2.22) were significant risk factors after controlling for age, gender, thickness of melanoma and ulceration status. A prognostic model based on DCCD SN and melanoma thickness predicted outcome as accurately as a model including pathological information of both SNs and NSNs. The assessment of DCCD SN renders CLND for staging purposes unnecessary. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Quantitative determination, Metal analysis and Antiulcer evaluation of Methanol seeds extract of Citrullus lanatus Thunb (Cucurbitaceae in Rats

    Directory of Open Access Journals (Sweden)

    Okunrobo O. Lucky

    2012-10-01

    Full Text Available Objective: The use of herbs in treatment of diseases is gradually becoming universally accepted especially in non industrialized societies. Citrullus lanatus Thunb (Cucurbitaceae commonly called water melon is widely consumed in this part of the world as food and medicine. This work was conducted to investigate the phytochemical composition, proximate and metal content analysis of the seed of Citrullus lanatus and to determine the antiulcer action of the methanol seed extract. Methods: Phytochemical screening, proximate and metal content analysis was done using the standard procedures and the antiulcer activity was evaluated against acetylsalicylic acid-induced ulcers. Results: The results revealed the presence of the following phytochemicals; flavonoids, saponins, tannins, alkaloids, glycosides. Proximate analysis indicated high concentration of carbohydrate, protein and fat while metal analysis showed the presence of sodium, calcium, zinc, magnesium at levels within the recommended dietary intake. Antiulcer potential of the extract against acetylsalicylic acid induced ulceration of gastric mucosa of Wister rats was evaluated at three doses (200mg/kg, 400mg/kg, and 800mg/kg. The ulcer parameters investigated included ulcer number, ulcer severity, ulcer index and percentage ulcer protection. The antiulcer activity was compared against ranitidine at 20mg/kg. The extract exhibited a dose related antiulcer activity with maximum activity at 800mg/kg (P<0.001. Conclusions: Proximate and metal content analysis of the seeds provides information that the consumption of the seeds of Citrullus lanatus is safe. This present study also provides preliminary data for the first time that the seeds of Citrullus lanatus possesses antiulcer activity in animal model.

  5. Quantitative determination of the enantiomers of methadone in human plasma and saliva by chiral column chromatography coupled with mass spectrometric detection.

    Science.gov (United States)

    George, Rani; Lobb, Michael; Haywood, Alison; Khan, Sohil; Hardy, Janet; Good, Phillip; Hennig, Stefanie; Norris, Ross

    2016-01-01

    Methadone is a potent lipophilic synthetic opioid that is effective in the treatment of cancer pain and perceived benefit in difficult pain control scenarios (especially in cases of neuropathic pain). The use of methadone in clinical practice is challenging however, due to the narrow therapeutic window and large inter- and intra-individual variability in therapeutic response. Quantitation of the enantiomers d- and l-methadone (d- and l-MTD) in plasma and saliva provides a basis for studying its pharmacokinetics in patients with cancer and for monitoring efficacy, toxicity and side-effects. This assay involves quantitation of the enantiomers of methadone using their respective deuterated internal standards, in plasma and saliva matrices with no impact of ion suppression in either matrix. The analytical recoveries of d- and l-MTD from the saliva collection devices (Salivette®) are optimised in this novel method with an accurate and simple extraction method employing dichloromethane. Optimal enantioselective separations were achieved using an α1-acid glycoprotein chiral stationary phase and triple quadrupole tandem mass spectrometer. Linearity was demonstrated over 0.05-1000µg/L for both enantiomers in plasma and in saliva with correlation coefficients greater than 0.998. The lower limit of quantitation (LLOQ) was determined to be 0.1µg/L in plasma and saliva for d- and l-MTD. Accuracy of the method ranges from 100% to 106% even at the LLOQ and total precision, expressed as the coefficient of variation, was between 0.2% and 4.4% for both analytes in both matrices. A simple one step extraction procedure resulted in recoveries greater than 95% for both analytes, at concentrations as low as 0.5µg/L, from the Salivette®. The validated method was applied successfully in 14 paired plasma and saliva samples obtained from adult patients with cancer pain receiving methadone. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Quantitative Trait Locus Based Virulence Determinant Mapping of the HSV-1 Genome in Murine Ocular Infection: Genes Involved in Viral Regulatory and Innate Immune Networks Contribute to Virulence.

    Directory of Open Access Journals (Sweden)

    Aaron W Kolb

    2016-03-01

    Full Text Available Herpes simplex virus type 1 causes mucocutaneous lesions, and is the leading cause of infectious blindness in the United States. Animal studies have shown that the severity of HSV-1 ocular disease is influenced by three main factors; innate immunity, host immune response and viral strain. We previously showed that mixed infection with two avirulent HSV-1 strains (OD4 and CJ994 resulted in recombinants that exhibit a range of disease phenotypes from severe to avirulent, suggesting epistatic interactions were involved. The goal of this study was to develop a quantitative trait locus (QTL analysis of HSV-1 ocular virulence determinants and to identify virulence associated SNPs. Blepharitis and stromal keratitis quantitative scores were characterized for 40 OD4:CJ994 recombinants. Viral titers in the eye were also measured. Virulence quantitative trait locus mapping (vQTLmap was performed using the Lasso, Random Forest, and Ridge regression methods to identify significant phenotypically meaningful regions for each ocular disease parameter. The most predictive Ridge regression model identified several phenotypically meaningful SNPs for blepharitis and stromal keratitis. Notably, phenotypically meaningful nonsynonymous variations were detected in the UL24, UL29 (ICP8, UL41 (VHS, UL53 (gK, UL54 (ICP27, UL56, ICP4, US1 (ICP22, US3 and gG genes. Network analysis revealed that many of these variations were in HSV-1 regulatory networks and viral genes that affect innate immunity. Several genes previously implicated in virulence were identified, validating this approach, while other genes were novel. Several novel polymorphisms were also identified in these genes. This approach provides a framework that will be useful for identifying virulence genes in other pathogenic viruses, as well as epistatic effects that affect HSV-1 ocular virulence.

  7. Quantitative trait loci involved in sex determination and body growth in the gilthead sea bream (Sparus aurata L. through targeted genome scan.

    Directory of Open Access Journals (Sweden)

    Dimitrios Loukovitis

    Full Text Available Among vertebrates, teleost fish exhibit a considerably wide range of sex determination patterns that may be influenced by extrinsic parameters. However even for model fish species like the zebrafish Danio rerio the precise mechanisms involved in primary sex determination have not been studied extensively. The zebrafish, a gonochoristic species, is lacking discernible sex chromosomes and the sex of juvenile fish is difficult to determine. Sequential protandrous hermaphrodite species provide distinct determination of the gender and allow studying the sex determination process by looking at the mechanism of sex reversal. This is the first attempt to understand the genetic basis of phenotypic variation for sex determination and body weight in a sequential protandrous hermaphrodite species, the gilthead sea bream (Sparus aurata. This work demonstrates a fast and efficient strategy for Quantitative Trait Loci (QTL detection in the gilthead sea bream, a non-model but target hermaphrodite fish species. Therefore a comparative mapping approach was performed to query syntenies against two other Perciformes, the European sea bass (Dicentrarchus labrax, a gonochoristic species and the Asian sea bass (Lates calcarifer a protandrous hermaphrodite. In this manner two significant QTLs, one QTL affecting both body weight and sex and one QTL affecting sex, were detected on the same linkage group. The co-segregation of the two QTLs provides a genomic base to the observed genetic correlation between these two traits in sea bream as well as in other teleosts. The identification of QTLs linked to sex reversal and growth, will contribute significantly to a better understanding of the complex nature of sex determination in S. aurata where most individuals reverse to the female sex at the age of two years through development and maturation of the ovarian portion of the gonad and regression of the testicular area. [Genomic sequences reported in this manuscript have been

  8. Development of new quantitative mass spectrometry and semi-automatic isofocusing methods for the determination of Apolipoprotein E typing.

    Science.gov (United States)

    Hirtz, Christophe; Vialaret, Jerome; Nouadje, Georges; Schraen, Susanna; Benlian, Pascale; Mary, Sandrine; Philibert, Pascal; Tiers, Laurent; Bros, Pauline; Delaby, Constance; Gabelle, Audrey; Lehmann, Sylvain

    2016-02-15

    Apolipoprotein E (Apo E) is a 36 Kda glycoprotein involved in lipid transport. It exists in 3 major isoforms: E2, E3 and E4. ApoE status is known to be a major risk factor for late-onset Alzheimer's and cardiovascular diseases. Genotyping is commonly used to obtain ApoE status but can show technical issues with ambiguous determinations. Phenotyping can be an alternative, not requiring genetic material. We evaluated the ability to accurately type ApoE isoforms by 2 phenotyping tests in comparison with genotyping. Two phenotyping techniques were used: (1) LC-MS/MS detection of 4 ApoE specific peptides (6490 Agilent triple quadripole): After its denaturation, serum was either reduced and alkylated, or only diluted, and then trypsin digested. Before analysis, desalting, evaporation and resuspension were performed. (2) Isoelectric focusing and immunoprecipitation: serum samples were neuraminidase digested, delipidated and electrophoresed on Hydragel ApoE (Sebia agarose gel) using Hydrasys 2 Scan instrument (Sebia, Lisses, France). ApoE isoforms bands were directly immunofixed in the gel using a polyclonal anti human ApoE antibody. Then, incubation of the gel with HRP secondary antibody followed by TTF1/TTF2 substrate allowed the visualization of ApoE bands. The results of the two techniques were compared to genotyping. Sera from 35 patients previously genotyped were analyzed with the 2 phenotyping techniques. 100% concordance between both phenotyping assays was obtained for the tested phenotypes (E2/E2, E2/E3, E2/E4, E3/E3, E3/E4, E4/E4). When compared to genotyping, 3 samples were discordant. After reanalyzing them by both phenotyping tests and DNA sequencing, 2/3 discrepancies were confirmed. Those can be explained by variants or rare ApoE alleles or by unidentified technical issues. 102 additional samples were then tested on LC-MS/MS only and compared to genotyping. The data showed 100% concordance. Our 2 phenotyping methods represent a valuable alternative to

  9. Determination of Cytochrome P450 2D6 (CYP2D6 Gene Copy Number by Real-Time Quantitative PCR

    Directory of Open Access Journals (Sweden)

    Laurent Bodin

    2005-01-01

    Full Text Available Gene dosage by real-time quantitative PCR has proved to be accurate for measuring gene copy number. The aim of this study was to apply this approach to the CYP2D6 gene to allow for rapid identification of poor and ultrarapid metabolizers (0, 1, or more than 2 gene copy number. Using the 2−ΔΔCt calculation method and a duplex reaction, the number of CYP2D6 gene copies was determined. Quantitative PCR was performed on 43 samples previously analyzed by Southern blotting and long PCR including 20 samples with a heterozygous deletion, 11 with normal copy number (2 copies, and 12 samples with duplicated genes. The average ratio ranged from 1.02 to 1.28, 1.85 to 2.21, and 2.55 to 3.30, respectively, for the samples with 1 copy, 2 copies, and 3 copies. This study shows that this method is sensitive enough to detect either a heterozygous gene deletion or duplication.

  10. Determination of the limits of identification and quantitation of selected organochlorine and organophosphorous pesticide residues in surface water by full-scan gas chromatography/mass spectrometry.

    Science.gov (United States)

    Tahboub, Yahya R; Zaater, Mohammad F; Al-Talla, Zeiad A

    2005-12-09

    In this work, we report a reliable method for quantitation and determination of the limits of identification of 14 organochlorine and organophosphorous pesticide (OPP) residues in surface water. The method features the simultaneous identification and quantitation of targeted pesticides and the possibility of identification of any other eluting compounds. The method is based on liquid-liquid extraction (LLE) with a mixture of petroleum ether and dichloromethane (70:30, v/v) followed by gas chromatographic separation and a full-scan mass spectrometric detection (GC-MS). The method presents a new validation parameter, limit of identification (LOI) which is defined for our purpose as the lowest analyte concentration that yields a library searchable mass spectrum. The method is linear over the range 0.048-1.20microgL(-1) for nine pesticides and 0.024-0.60microgL(-1) for the other five pesticides. Correlation coefficients vary between 0.988 and 0.998. Limits of detection (LODs) vary between 0.005 and 0.05microgL(-1) for 4,4'-DDT and LOIs vary between 0.012 and 0.048microgL(-1).

  11. Qualitative and quantitative determination of YiXinShu Tablet using ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry.

    Science.gov (United States)

    Sun, Zhi; Li, Zhuolun; Zuo, Lihua; Wang, Zhenhui; Zhou, Lin; Shi, Yingying; Kang, Jian; Zhu, Zhenfeng; Zhang, Xiaojian

    2017-11-01

    To clarify and quantify the chemical profile of YiXinShu Tablet rapidly, a feasible and accurate strategy was developed by applying ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry. A total of 105 components were identified, including 25 phenanthraquinones, 11 lactones, 19 lignans, 24 acids, and 26 other compounds. Among them, 26 major compounds were unambiguously detected by comparing with reference standards. And 19 of these compounds in three batches of YiXinShu Tablet were selected for quantitative determination. (Z)-Ligustilide, salvianic acid A, salvianolic acid A, salvianolic acid B, and rosmarinic acid were abundant in these three batches with contents over 1 mg/g. The established analysis methods were examined to be accurate and feasible. The results show that the ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry method has a powerful qualitative ability and promising quantitative application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Development and validation of a modified ultrasound-assisted extraction method and a HPLC method for the quantitative determination of two triterpenic acids in Hedyotis diffusa.

    Science.gov (United States)

    Yang, Yu-Chiao; Wei, Ming-Chi; Chiu, Hui-Fen; Huang, Ting-Chia

    2013-12-01

    In the present study, the oleanolic acid (OA) and ursolic acid (UA) contents ofHedyotis diffusa and H. corymbosa were determined by a rapid, selective and accurate method combining modified ultrasound-assisted extraction (MUAE) and HPLC. Compared with traditional extraction methods, MUAE reduced the extraction time, the extraction temperature and the solvent consumption and maximized the extraction yields of OA and UA. Furthermore, the combined MUAE-HPLC method was applied to quantitate OA and UA in plant samples and exhibited good repeatability, reproducibility and stability. The mean recovery studies (one extraction cycle) for OA and UA were between 91.3 and 91.7% with RSD values less than 4.5%. The pioneer method was further applied to quantitate OA and UA in six samples of H. diffusa and five samples of H. corymbosa. The results showed that the OA and UA content in the samples from different sources were significantly different. This report is valuable for the application of H. diffusa and H. corymbosa obtained from different regions in clinical research and pharmacology.

  13. Liquid chromatography-tandem mass spectrometric assay for the quantitative determination of the tyrosine kinase inhibitor quizartinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Retmana, Irene A; Wang, Jing; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2017-01-01

    A bioanalytical assay for quizartinib -a potent, and selective FLT3 tyrosine kinase inhibitor- in mouse plasma was developed and validated. Salting-out assisted liquid-liquid extraction (SALLE), using acetonitrile and magnesium sulfate, was selected as sample pretreatment with deuterated quizartinib

  14. Development of a genus-specific next generation sequencing approach for sensitive and quantitative determination of the Legionella microbiome in freshwater systems.

    Science.gov (United States)

    Pereira, Rui P A; Peplies, Jörg; Brettar, Ingrid; Höfle, Manfred G

    2017-03-31

    Next Generation Sequencing (NGS) has revolutionized the analysis of natural and man-made microbial communities by using universal primers for bacteria in a PCR based approach targeting the 16S rRNA gene. In our study we narrowed primer specificity to a single, monophyletic genus because for many questions in microbiology only a specific part of the whole microbiome is of interest. We have chosen the genus Legionella, comprising more than 20 pathogenic species, due to its high relevance for water-based respiratory infections. A new NGS-based approach was designed by sequencing 16S rRNA gene amplicons specific for the genus Legionella using the Illumina MiSeq technology. This approach was validated and applied to a set of representative freshwater samples. Our results revealed that the generated libraries presented a low average raw error rate per base (approach also showed high in situ specificity (>95%) and very good repeatability. Only in samples in which the gammabacterial clade SAR86 was present more than 1% non-Legionella sequences were observed. Next-generation sequencing read counts did not reveal considerable amplification/sequencing biases and showed a sensitive as well as precise quantification of L. pneumophila along a dilution range using a spiked-in, certified genome standard. The genome standard and a mock community consisting of six different Legionella species demonstrated that the developed NGS approach was quantitative and specific at the level of individual species, including L. pneumophila. The sensitivity of our genus-specific approach was at least one order of magnitude higher compared to the universal NGS approach. Comparison of quantification by real-time PCR showed consistency with the NGS data. Overall, our NGS approach can determine the quantitative abundances of Legionella species, i. e. the complete Legionella microbiome, without the need for species-specific primers. The developed NGS approach provides a new molecular surveillance tool

  15. Energy consumption modeling during dairy sewage pretreatment

    Science.gov (United States)

    Dąbrowski, Wojciech; Żyłka, Radosław; Malinowski, Paweł; Boruszko, Dariusz

    2017-11-01

    The research was conducted in a dairy WWTP located in north-eastern Poland with the average flow of 546 m3d-1 and PE 11500 in 2016. Energy consumption was measured with the help of Lumel 3-phase network parameter transducers installed within the plant. The modeling was conducted based on the quantity and quality of raw sewage, after its screening, averaging and dissolved air flotation. The following parameters were determined: BOD5, COD. N-total and P-total. During the research period. 15 measurement series were carried out. Pollution loads removed in primary treatment varied from 167.0 to 803.5 kgO2d-1 and 1205.9 to 10032 kgO2d-1 for BOD5 and COD respectively. The energy consumption share during dairy pretreatment in relation to the total energy consumption was in the range from 13.8 to 28.5% with the mean value of 18.7% during the research period. Energy consumption indicators relating to removed pollution loads for primary treatment were established with the mean values of 0.74 and 0.83 kWhkg-1d-1 for BOD5 and COD respectively. An attempt was made to determine the influence of raw sewage characteristics and pretreatment efficiency on energy consumption of the object. A model of energy consumption during pretreatment was estimated according to the experimental data obtained in the research period. It was modeled using the linear regression model and principal component analysis.

  16. Energy consumption modeling during dairy sewage pretreatment

    Directory of Open Access Journals (Sweden)

    Dąbrowski Wojciech

    2017-01-01

    Full Text Available The research was conducted in a dairy WWTP located in north-eastern Poland with the average flow of 546 m3d-1 and PE 11500 in 2016. Energy consumption was measured with the help of Lumel 3-phase network parameter transducers installed within the plant. The modeling was conducted based on the quantity and quality of raw sewage, after its screening, averaging and dissolved air flotation. The following parameters were determined: BOD5, COD. N-total and P-total. During the research period. 15 measurement series were carried out. Pollution loads removed in primary treatment varied from 167.0 to 803.5 kgO2d-1 and 1205.9 to 10032 kgO2d-1 for BOD5 and COD respectively. The energy consumption share during dairy pretreatment in relation to the total energy consumption was in the range from 13.8 to 28.5% with the mean value of 18.7% during the research period. Energy consumption indicators relating to removed pollution loads for primary treatment were established with the mean values of 0.74 and 0.83 kWhkg-1d-1 for BOD5 and COD respectively. An attempt was made to determine the influence of raw sewage characteristics and pretreatment efficiency on energy consumption of the object. A model of energy consumption during pretreatment was estimated according to the experimental data obtained in the research period. It was modeled using the linear regression model and principal component analysis.

  17. Social determinants of health and seasonal influenza vaccination in adults ≥65 years: a systematic review of qualitative and quantitative data

    Science.gov (United States)

    2013-01-01

    Background Vaccination against influenza is considered the most important public health intervention to prevent unnecessary hospitalizations and premature deaths related to influenza in the elderly, though there are significant inequities among global influenza vaccine resources, capacities, and policies. The objective of this study was to assess the social determinants of health preventing adults ≥65 years old from accessing and accepting seasonal influenza vaccination. Methods A systematic search was performed in January 2011 using MEDLINE, ISI – Web of Science, PsycINFO, and CINAHL (1980–2011). Reference lists of articles were also examined. Selection criteria included qualitative and quantitative studies written in English that examined social determinants of and barriers against seasonal influenza vaccination among adults≥65 years. Two authors performed the quality assessment and data extraction. Thematic analysis was the main approach for joint synthesis, using identification and juxtaposition of themes associated with vaccination. Results Overall, 58 studies were analyzed. Structural social determinants such as age, gender, marital status, education, ethnicity, socio-economic status, social and cultural values, as well as intermediary determinants including housing-place of residence, behavioral beliefs, social influences, previous vaccine experiences, perceived susceptibility, sources of information, and perceived health status influenced seasonal influenza vaccination. Healthcare system related factors including accessibility, affordability, knowledge and attitudes about vaccination, and physicians’ advice were also important determinants of vaccination. Conclusions Our results demonstrate that the ability of adults ≥65 years to receive seasonal influenza vaccine is influenced by structural, intermediate, and healthcare-related social determinants which have an impact at the health system, provider, and individual levels. PMID:23617788

  18. Promise of combined hydrothermal/chemical and mechanical refining for pretreatment of woody and herbaceous biomass.

    Science.gov (United States)

    Kim, Sun Min; Dien, Bruce S; Singh, Vijay

    2016-01-01

    Production of advanced biofuels from woody and herbaceous feedstocks is moving into commercialization. Biomass needs to be pretreated to overcome the physicochemical properties of biomass that hinder enzyme accessibility, impeding the conversion of the plant cell walls to fermentable sugars. Pretreatment also remains one of the most costly unit operations in the process and among the most critical because it is the source of chemicals that inhibit enzymes and microorganisms and largely determines enzyme loading and sugar yields. Pretreatments are categorized into hydrothermal (aqueous)/chemical, physical, and biological pretreatments, and the mechanistic details of which are briefly outlined in this review. To leverage the synergistic effects of different pretreatment methods, conducting two or more pretreatments consecutively has gained attention. Especially, combining hydrothermal/chemical pretreatment and mechanical refining, a type of physical pretreatment, has the potential to be applied to an industrial plant. Here, the effects of the combined pretreatment (combined hydrothermal/chemical pretreatment and mechanical refining) on energy consumption, physical structure, sugar yields, and enzyme dosage are summarized.

  19. The enzymatic hydrolysis of pretreated pulp fibers predominantly involves "peeling/erosion" modes of action.

    Science.gov (United States)

    Arantes, Valdeir; Gourlay, Keith; Saddler, Jack N

    2014-01-01

    There is still considerable debate regarding the actual mechanism by which a "cellulase mixture" deconstructs cellulosic materials, with accessibility to the substrate at the microscopic level being one of the major restrictions that limits fast, complete cellulose hydrolysis. In the work reported here we tried to determine the predominant mode of action, at the fiber level, of how a cellulase mixture deconstructs pretreated softwood and hardwood pulp fibers. Quantitative changes in the pulp fibers derived from different pretreated biomass substrates were monitored throughout the course of enzymatic hydrolysis to see if the dominant mechanisms involved either the fragmentation/cutting of longer fibers to shorter fibers or their "peeling/delamination/erosion," or if both cutting and peeling mechanisms occurred simultaneously. Regardless of the source of biomass, the type of pretreatment and the chemical composition of the substrate, under typical hydrolysis conditions (50°C, pH 4.8, mixing) longer pulp fibers (fiber length >200 μm) were rapidly broken down until a relatively constant fiber length of 130 to 160 μm was reached. In contrast, shorter fibers with an initial average fiber length of 130 to 160 μm showed no significant change in length despite their substantial hydrolysis. The fragmentation/cutting mode of deconstruction was only observed on longer fibers at early stages of hydrolysis. Although the fiber fragmentation mode of deconstruction was not greatly influenced by enzyme loading, it was significantly inhibited by glucose and was mainly observed during initial mixing of the enzyme and substrate. In contrast, significant changes in the fiber width occurred throughout the course of hydrolysis for all of the substrates, suggesting that fiber width may limit the rate and extent of cellulose hydrolysis. It appears that, at the fiber level, pretreated pulp fibers are hydrolyzed through a two-step mode of action involving an initial rapid

  20. DEVELOPMENT OF REAL-TIME MULTIPLEX PCR FOR THE QUANTITATIVE DETERMINATION OF TREC'S AND KREC'S IN WHOLE BLOOD AND IN DRIED BLOOD SPOTS

    Directory of Open Access Journals (Sweden)

    M. A. Gordukova

    2015-01-01

    Full Text Available Primary immunodeficiencies (PID such as severe combined immunodeficiency (SCID and X-linked agammaglobulinemia are characterized by the lack of functional Tand B-cells, respectively. Without early diagnosis and prompt treatment children with PID suffer from severe infectious diseases, leading to their death or disability. Our purpose was developing of simple, inexpensive, high throughput technique based on the quantitative determination of TREC and KREC molecules by real-time PCR, and its validation in a group of children with a verified diagnosis of SCID and X-linked agammaglobulinemia.In this study, we developed and validated multiplex real-time PCR for the TREC’s and KREC’s quantitative analysis. We have shown that linear range of Ct changes depending on the concentrations of targets with a correlation coefficient R2 not worse than 0.98 was observed at concentrations from 109 to 5 × 104 copies per ml. The lowest amount of targets reliably detected in a reaction volume was 10 TREC’s copies, 5 KREC ‘s copies and 5 copies of internal control (IL17RA. We determined the age-depended reference values of TRECs and KRECs in whole blood in 29 boys and 27 girls with normal immunological parameters. The normal cut-offs for TRECs and KRECs were defined in dry blood spots depending on the method of extraction.The proposed method showed 100% diagnostic sensitivity and specificity in the studied group. The method can be proposed as a screening tool for the diagnosis of SCID and X-linked agammaglobulinemia both in whole blood and in the dry blood spots. The further investigation is required with larger number of samples. 

  1. Superiority of quantitative exercise thallium-201 variables in determining long-term prognosis in ambulatory patients with chest pain: a comparison with cardiac catheterization

    International Nuclear Information System (INIS)

    Kaul, S.; Finkelstein, D.M.; Homma, S.; Leavitt, M.; Okada, R.D.; Boucher, C.A.

    1988-01-01

    The purpose of this study was to determine the prognostic utility of quantitative exercise thallium-201 imaging and compare it with that of cardiac catheterization in ambulatory patients. Accordingly, long-term (4 to 9 years) follow-up was obtained in 293 patients who underwent both tests for the evaluation of chest pain: 89 had undergone coronary artery bypass graft surgery within 3 months of testing and were excluded from analysis, 119 experienced no cardiac events and 91 had an event (death in 20, nonfatal myocardial infarction in 21 and coronary artery bypass operations performed greater than 3 months after cardiac catheterization in 50). When all variables were analyzed using Cox regression analysis, the quantitatively assessed lung/heart ratio of thallium-201 activity was the most important predictor of a future cardiac event (chi 2 = 40.21). Other significant predictors were the number of diseased vessels (chi 2 = 17.11), patient gender (chi 2 = 9.43) and change in heart rate from rest to exercise (chi 2 = 4.19). Whereas the number of diseased vessels was an important independent predictor of cardiac events, it did not add significantly to the overall ability of the exercise thallium-201 test to predict events. Furthermore, information obtained from thallium-201 imaging alone was marginally superior to that obtained from cardiac catheterization alone (p = 0.04) and significantly superior to that obtained from exercise testing alone (p = 0.02) in determining the occurrence of events. In addition, unlike the exercise thallium-201 test, which could predict the occurrence of all categories of events, catheterization data were not able to predict the occurrence of nonfatal myocardial infarction. The exclusion of bypass surgery and previous myocardial infarction did not alter the results

  2. Quantitative assessment of source contributions to PM2.5 on the west coast of Peninsular Malaysia to determine the burden of Indonesian peatland fire

    Science.gov (United States)

    Fujii, Yusuke; Tohno, Susumu; Amil, Norhaniza; Latif, Mohd Talib

    2017-12-01

    Almost every dry season, peatland fires occur in Sumatra and Kalimantan Inlands. Dense smoke haze from Indonesian peatland fires (IPFs) causes impacts on health, visibility, transport and regional climate in Southeast Asian countries such as Indonesia, Malaysia, and Singapore. Quantitative knowledge of IPF source contribution to ambient aerosols in Southeast Asia (SEA) is so useful to make appropriate suggestions to policy makers to mitigate IPF-induced haze pollution. However, its quantitative contribution to ambient aerosols in SEA remains unclarified. In this study, the source contributions to PM2.5 were determined by the Positive Matrix Factorization (PMF) model with annual comprehensive observation data at Petaling Jaya on the west coast of Peninsular Malaysia, which is downwind of the IPF areas in Sumatra Island, during the dry (southwest monsoon: June-September) season. The average PM2.5 mass concentration during the whole sampling periods (Aug 2011-Jul 2012) based on the PMF and chemical mass closure models was determined as 20-21 μg m-3. Throughout the sampling periods, IPF contributed (on average) 6.1-7.0 μg m-3 to the PM2.5, or ∼30% of the retrieved PM2.5 concentration. In particular, the PM2.5 was dominantly sourced from IPF during the southwest monsoon season (51-55% of the total PM2.5 concentration on average). Thus, reducing the IPF burden in the PM2.5 levels would drastically improve the air quality (especially during the southwest monsoon season) around the west coast of Peninsular Malaysia.

  3. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Directory of Open Access Journals (Sweden)

    Brahmi Fatiha

    2014-12-01

    Full Text Available Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata, Mentha pulegium L. and Mentha rotundifolia (L. Huds by high performance thin layer chromatography (HPTLC-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method. Results: Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1 000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively. The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox® equivalents as a natural source for inhibitors of lipid peroxidation. Conclusions: Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  4. Determination of the spectral dependence of reduced scattering and quantitative second-harmonic generation imaging for detection of fibrillary changes in ovarian cancer

    Science.gov (United States)

    Campbell, Kirby R.; Tilbury, Karissa B.; Campagnola, Paul J.

    2015-03-01

    Here, we examine ovarian cancer extracellular matrix (ECM) modification by measuring the wavelength dependence of optical scattering measurements and quantitative second-harmonic generation (SHG) imaging metrics in the range of 800-1100 nm in order to determine fibrillary changes in ex vivo normal ovary, type I, and type II ovarian cancer. Mass fractals of the collagen fiber structure is analyzed based on a power law correlation function using spectral dependence measurements of the reduced scattering coefficient μs' where the mass fractal dimension is related to the power. Values of μs' are measured using independent methods of determining the values of μs and g by on-axis attenuation measurements using the Beer-Lambert Law and by fitting the angular distribution of scattering to the Henyey-Greenstein phase function, respectively. Quantitativespectral SHG imaging on the same tissues determines FSHG/BSHG creation ratios related to size and harmonophore distributions. Both techniques probe fibril packing order, but the optical scattering probes structures of sizes from about 50-2000 nm where SHG imaging - although only able to resolve individual fibers - builds contrast from the assembly of fibrils. Our findings suggest that type I ovarian tumor structure has the most ordered collagen fibers followed by normal ovary then type II tumors showing the least order.

  5. Effect of pretreating of host oil on coprocessing

    Energy Technology Data Exchange (ETDEWEB)

    Hajdu, P.E.; Tierney, J.W.; Wender, I. [Univ. of Pittsburgh, PA (United States)

    1995-12-31

    The principal objective of this research was to determine if coprocessing performance (i.e., coal conversion and oil yield) could be significantly improved by pretreating the heavy resid prior to reacting it with coal. For this purpose, two petroleum vacuum resids (1000{degrees}F+), one from the Amoco Co. and another from the Citgo Co., were used as such and after they had been pretreated by catalytic hydrogenation and hydrocracking reactions. The pretreatments were aimed at improving the host oil by; (1) converting any aromatic structures in the petroleum to hydroaromatic compounds capable of donating hydrogen, (2) cracking the heavy oil to lower molecular weight material that might serve as a better solvent, (3) reducing the coking propensity of the heavy oil through the hydrogenation of polynuclear aromatic compounds, and (4) removing metals and heteroatoms that might poison a coprocessing catalyst. Highly dispersed catalysts, including fine particle Fe- and Mo-based, and dicobalt octacarbonyl, Co{sub 2}(CO){sub 8}, were used in this study. The untreated and pretreated resids were extensively characterized in order to determine chemical changes brought about by the pretreatments. The modified heavy oils were then coprocessed with an Illinois No. 6 coal as well as with a Wyodak coal, and compared to coprocessing with untreated resids under the same hydroliquefaction conditions. The amount of oil derived from coal was estimated by measuring the level of phenolic oxygen (derived mainly from coal) present in the oil products. Results are presented and discussed.

  6. [DNA quantification of blood samples pre-treated with pyramidon].

    Science.gov (United States)

    Zhu, Chuan-Hong; Zheng, Dao-Li; Ni, Rao-Zhi; Wang, Hai-Sheng; Ning, Ping; Fang, Hui; Liu, Yan

    2014-06-01

    To study DNA quantification and STR typing of samples pre-treated with pyramidon. The blood samples of ten unrelated individuals were anticoagulated in EDTA. The blood stains were made on the filter paper. The experimental groups were divided into six groups in accordance with the storage time, 30 min, 1 h, 3 h, 6 h, 12 h and 24h after pre-treated with pyramidon. DNA was extracted by three methods: magnetic bead-based extraction, QIAcube DNA purification method and Chelex-100 method. The quantification of DNA was made by fluorescent quantitative PCR. STR typing was detected by PCR-STR fluorescent technology. In the same DNA extraction method, the sample DNA decreased gradually with times after pre-treatment with pyramidon. In the same storage time, the DNA quantification in different extraction methods had significant differences. Sixteen loci DNA typing were detected in 90.56% of samples. Pyramidon pre-treatment could cause DNA degradation, but effective STR typing can be achieved within 24 h. The magnetic bead-based extraction is the best method for STR profiling and DNA extraction.

  7. The pretreatment of corn stover with Gloeophyllum trabeum KU-41 for enzymatic hydrolysis

    Directory of Open Access Journals (Sweden)

    Gao Ziqing

    2012-05-01

    Full Text Available Abstract Background Pretreatment is an essential step in the enzymatic hydrolysis of biomass for bio-ethanol production. The dominant concern in this step is how to decrease the high cost of pretreatment while achieving a high sugar yield. Fungal pretreatment of biomass was previously reported to be effective, with the advantage of having a low energy requirement and requiring no application of additional chemicals. In this work, Gloeophyllum trabeum KU-41 was chosen for corn stover pretreatment through screening with 40 strains of wood-rot fungi. The objective of the current work is to find out which characteristics of corn stover pretreated with G. trabeum KU-41 determine the pretreatment method to be successful and worthwhile to apply. This will be done by determining the lignin content, structural carbohydrate, cellulose crystallinity, initial adsorption capacity of cellulase and specific surface area of pretreated corn stover. Results The content of xylan in pretreated corn stover was decreased by 43% in comparison to the untreated corn stover. The initial cellulase adsorption capacity and the specific surface area of corn stover pretreated with G. trabeum were increased by 7.0- and 2.5-fold, respectively. Also there was little increase in the cellulose crystallinity of pretreated corn stover. Conclusion G. trabeum has an efficient degradation system, and the results indicated that the conversion of cellulose to glucose increases as the accessibility of cellulose increases due to the partial removal of xylan and the structure breakage of the cell wall. This pretreatment method can be further explored as an alternative to the thermochemical pretreatment method.

  8. Evaluation of Real-Time Quantitative Polymerase Chain Reaction (qPCR) to Determine Escherichia coli Concentrations at Two Lake Erie Beaches

    Science.gov (United States)

    Kephart, Christopher M.; Bushon, Rebecca N.

    2009-01-01

    During the recreational seasons of 2006 and 2007, the quantitative polymerase chain reaction (qPCR) method was used to determine Escherichia coli (E. coli) concentrations in samples from two Lake Erie beaches. Results from the qPCR method were compared to those obtained by traditional culturing on modified mTEC agar. Regression analysis showed strong, statistically significant correlations between results from the two methods for both years. Correlation coefficients at Edgewater and Villa Angela Beaches were 0.626 and 0.789 for 2006 and 0.667 and 0.829 for 2007, respectively. Linear regression analyses were done to determine how well E. coli concentrations could have been predicted from qPCR results. These hypothetical predictions were compared to the current practice of determining recreational water quality from E. coli concentrations determined for samples collected on the previous day. The qPCR method resulted in a greater percentage of correct predictions of water-quality exceedances than the current method for both beaches and both years. However, because regression equations differed somewhat between both sites and both years, the study did not result in any single relation reliable enough to use for actual real-time prediction of water-quality exceedances for either beach; therefore, a posterior analysis of data was done. Additional years of data may be needed to develop such a relation. Results from this study support the continued development and testing of a qPCR method for providing rapid and accurate estimates of E. coli concentrations for monitoring recreational water quality.

  9. Semiautomatic determination of arterial input functions for quantitative dynamic contrast-enhanced magnetic resonance imaging in non-small cell lung cancer patients.

    Science.gov (United States)

    Chung, Julius; Kim, Jae-Hun; Lee, Eun Ju; Kim, Yoo Na; Yi, Chin A

    2015-03-01

    The aim of this study was to validate a semiautomatic detection method for the arterial input functions (AIFs) using Kendall coefficient of concordance (KCC) for quantitative analysis of dynamic contrast-enhanced magnetic resonance imaging in non-small cell lung cancer patients. We prospectively enrolled 28 patients (17 men, 11 women; mean age, 62 years) who had biopsy-proven non-small cell lung cancer. All enrolled patients underwent dynamic contrast-enhanced magnetic resonance imaging of the entire thorax. For the quantitative measurement of pharmacokinetic parameters, K and ve, of the lung cancers, AIFs were determined in 2 different ways: a manual method that involved 3 independent thoracic radiologists selecting a region of interest (ROI) within the aortic arch in the 2D coronal plane and a semiautomatic method that used in-house software to establish a KCC score, which provided a measure of similarity to typical AIF pattern. Three independent readers selected voxel clusters with high KCC scores calculated 3-dimensionally across planes in the data set. K and ve were correlated using intraclass correlation coefficients (ICCs), and Bland-Altman plots were used to examine agreement across methods and reproducibility within a method. Arterial input functions were determined using the data from ROI volumes that were significantly larger in the semiautomatic method (mean ± SD, 3360 ± 768 mm) than in the manual method (677 ± 380 mm) (P < 0.001). K showed very strong agreement (ICC, 0.927) and ve showed moderately strong agreement (ICC, 0.718) between the semiautomatic and manual methods. The reproducibility for K (ICCmanual, 0.813 and ICCsemiautomatic, 0.998; P < 0.001) and ve (ICCmanual, 0.455 and ICCsemiautomatic, 0.985, P < 0.001) was significantly better with the semiautomatic method than the manual method. We found semiautomated detection using KCC to be a robust method for determining the AIF. This method allows for larger ROIs specified in 3D across planes

  10. Quantitative determination of caffeine and alcohol in energy drinks and the potential to produce positive transdermal alcohol concentrations in human subjects.

    Science.gov (United States)

    Ayala, Jessica; Simons, Kelsie; Kerrigan, Sarah

    2009-01-01

    The purpose of this study was to determine whether non-alcoholic energy drinks could result in positive "alcohol alerts" based on transdermal alcohol concentration (TAC) using a commercially available electrochemical monitoring device. Eleven energy drinks were quantitatively assayed for both ethanol and caffeine. Ethanol concentrations for all of the non-alcoholic energy drinks ranged in concentration from 0.03 to 0.230% (w/v) and caffeine content per 8-oz serving ranged from 65 to 126 mg. A total of 15 human subjects participated in the study. Subjects consumed between 6 and 8 energy drinks over an 8-h period. The SCRAM II monitoring device was used to determine TACs every 30 min before, during, and after the study. None of the subjects produced TAC readings that resulted in positive "alcohol alerts". TAC measurements for all subjects before, during and after the energy drink study period (16 h total) were energy drink that greatly exceeds what would be considered typical. Based on these results, it appears that energy drink consumption is an unlikely explanation for elevated TACs that might be identified as potential drinking episodes or "alcohol alerts" using this device.

  11. [Quantitative determination of trans-fatty acids in oils and fats by capillary gas chromatography: results of a JOCS collaborative study].

    Science.gov (United States)

    Shirasawa, Seiichi; Shiota, Makoto; Arakawa, Hiroshi; Shigematsu, Yasuhiko; Yokomizo, Kazuhisa; Shionoya, Noriko; Okamoto, Takahisa; Miyazaki, Yousuke; Takahashi, Shigeyuki; Himata, Katsuichi

    2007-01-01

    Excessive intake of trans-fatty acids increases the risk of cardiovascular disease. Much attention is drawn to the consumption of trans-fatty acids worldwide, and regulations for trans-fatty acids are instituted in several countries. Precise and convenient methods for determination of trans-fatty acid level are required, but there is no standard method using capillary Gas Chromatography in Japan. Therefore, for the new standard method, collaborative studies were carried out. The results were as follows: 1) Heptadecanoate (C17:0 free fatty acid) was chosen for internal standard substance. 2) Two Gas Chromatography columns, SP2560 (100 m) column (100% cyanopropyl polysiloxane liquid phase) and TC-70 (60 m) column (70% cyanopropyl polysilphenylene-siloxane liquid phase), were examined in the collaborative studies. We measured the edible oil samples containing 2-45 g/100 g of trans-fatty acids, and trans-fatty acid contents were quantitatively the same with both columns. The range of reproducibility coefficient of variation were below 10%. 3) Fats and oils sampled were soybean, rapeseed, palm, palm kernel, beef tallow, pork fat and their hydrogenated forms, for which good peak resolution was achieved. From the above results, the technique evaluated in the present study was considered to be suitable for determination of the content of trans-fatty acids in fats and oils exclusive of fish oil and milk fat.

  12. Quantitative determination of lateral concentration and depth profile of histidine-tagged recombinant proteins probed by grazing incidence X-ray fluorescence.

    Science.gov (United States)

    Körner, Alexander; Abuillan, Wasim; Deichmann, Christina; Rossetti, Fernanda F; Köhler, Almut; Konovalov, Oleg V; Wedlich, Doris; Tanaka, Motomu

    2013-05-02

    We have demonstrated that the complementary combination of grazing incidence X-ray fluorescence (GIXF) with specular X-ray reflectivity (XRR) can be used to quantitatively determine the density profiles of Ni(2)(+) ions complexed with chelator headgroups as well as S atoms in recombinant proteins anchored to lipid monolayers at the air/water interface. First, we prepared phospholipid monolayers incorporating chelator lipid anchors at different molar fractions at the air/water interface. The fine-structures perpendicular to the global plane of monolayers were characterized by XRR in the presence of Ni(2)(+) ions, yielding the thickness, roughness, and electron density of the stratified lipid monolayers. X-ray fluorescence intensities from Ni Kα core levels recorded at the incidence angles below and above the critical angle of total reflection allow for the determination of the position and lateral density of Ni(2)(+) ions associated with chelator headgroups with a high spatial accuracy (±5 Å). The coupling of histidine-tagged Xenopus cadherin 11 (Xcad-11) can also be identified by changes in the fines-structures using XRR. Although fluorescence intensities from S Kα level were much weaker than Ni Kα signals, we could detect the location of S atoms in recombinant Xcad-11 proteins.

  13. Dual-energy CT iodine maps as an alternative quantitative imaging biomarker to abdominal CT perfusion: determination of appropriate trigger delays for acquisition using bolus tracking.

    Science.gov (United States)

    Skornitzke, Stephan; Fritz, Franziska; Mayer, Philipp; Koell, Marco; Hansen, Jens; Pahn, Gregor; Hackert, Thilo; Kauczor, Hans-Ulrich; Stiller, Wolfram

    2018-03-07

    Quantitative evaluation of different bolus tracking trigger delays for acquisition of dual energy (DE) CT iodine maps as an alternative to CT perfusion. Prior to this retrospective analysis of prospectively acquired data, DECT perfusion sequences were dynamically acquired in 22 patients with pancreatic carcinoma using dual source CT at 80/140 kV p with tin filtration. After deformable motion-correction, perfusion maps of blood flow (BF) were calculated from 80 kV p image series of DECT, and iodine maps were calculated for each of the 34 DECT acquisitions per patient. BF and iodine concentrations were measured in healthy pancreatic tissue and carcinoma. To evaluate potential DECT acquisition triggered by bolus tracking, measured iodine concentrations from the 34 DECT acquisitions per patient corresponding to different trigger delays were assessed for correlation to BF and intergroup differences between tissue types depending on acquisition time. Average BF measured in healthy pancreatic tissue and carcinoma was 87.6 ± 28.4 and 38.6 ± 22.2 ml/100 ml min -1 , respectively. Correlation between iodine concentrations and BF was statistically significant for bolus tracking with trigger delay greater than 0 s (r max = 0.89; p alternative to CT perfusion measurements of BF. Advances in knowledge: After clinical validation, DECT iodine maps of pancreas acquired using bolus tracking with appropriate trigger delay as determined in this study could offer an alternative quantitative imaging biomarker providing functional information for tumor assessment at reduced patient radiation exposure compared to CT perfusion measurements of BF.

  14. The development of 1,3-diphenylisobenzofuran as a highly selective probe for the detection and quantitative determination of hydrogen peroxide.

    Science.gov (United States)

    Żamojć, Krzysztof; Zdrowowicz, Magdalena; Rudnicki-Velasquez, Paweł Błażej; Krzymiński, Karol; Zaborowski, Bartłomiej; Niedziałkowski, Paweł; Jacewicz, Dagmara; Chmurzyński, Lech

    2017-01-01

    1,3-Diphenylisobenzofuran (DPBF) has been developed as a selective probe for the detection and quantitative determination of hydrogen peroxide in samples containing different reactive nitrogen and oxygen species (RNOS). DPBF is a fluorescent probe which, for almost 20 years, was believed to react in a highly specific manner toward some reactive oxygen species (ROS) such as singlet oxygen and hydroxy, alkyloxy or alkylperoxy radicals. Under the action of these individuals DPBF has been rapidly transformed to 1,2-dibenzoylbenzene (DBB). In order to check if DPBF can act as a unique indicator of the total amount of different RNOS, as well as oxidative stress caused by an overproduction of these individuals, a series of experiments was carried out, in which DPBF reacted with peroxynitrite anion, superoxide anion, hydrogen peroxide, hypochlorite anion, and anions commonly present under biological conditions, namely nitrite and nitrate. In all cases, except for hydrogen peroxide, the product of the reaction is DBB. Only under the action of H 2 O 2 9-hydroxyanthracen-10(9H)-one (oxanthrone) is formed. This product has been identified with the use of fluorescence spectroscopy, NMR spectroscopy, high performance liquid chromatography coupled with mass spectrometry, infrared spectroscopy, elemental analysis, and cyclic voltammetry (CV). A linear relationship was found between a decrease in the fluorescence intensity of DPBF and the concentration of hydrogen peroxide in the range of concentrations of 0.196-3.941 mM. DPBF responds to hydrogen peroxide in a very specific way with the limits of detection and quantitation of 88 and 122.8 μM, respectively. The kinetics of the reaction between DBBF and H 2 O 2 was also studied.

  15. Identifying quantitative trait loci and determining closely related stalk traits for rind penetrometer resistance in a high-oil maize population.

    Science.gov (United States)

    Hu, Haixiao; Meng, Yujie; Wang, Hongwu; Liu, Hai; Chen, Shaojiang

    2012-05-01

    Stalk lodging in maize causes annual yield losses between 5 and 20% worldwide. Many studies have indicated that maize stalk strength significantly negatively correlates with lodging observed in the field. Rind penetrometer resistance (RPR) measurements can be used to effectively evaluate maize stalk strength, but little is known about the genetic basis of this parameter. The objective of this study was to explore a genetic model and detect quantitative trait loci (QTL) of RPR and determine relationships between RPR and other stalk traits, especially cell wall chemical components. RPR is quantitative trait in nature, and both additive and non-additive effects may be important to consider for the improvement of RPR. Nine additive-effect QTLs covering nine chromosomes, except chromosome 5, and one pair of epistatic QTLs were detected for RPR. CeSA11 involved in cellulose synthesis and colorless2 involved in lignin synthesis were identified as possible candidate genes for RPR. Internode diameter (InD), fresh weight of internode (FreW), dry weight of internode (DryW), fresh weight and dry weight as well as cell wall components per unit volume significantly positively correlated with RPR. The internode water content (InW) significantly negatively correlated with RPR. Notably, these traits significantly correlated with RPR, and the QTLs of these traits co-localized with those of RPR. The corresponding results obtained from correlation analysis and QTL mapping suggested the presence of pleitropism or linkage between genes and indicated that these different approaches may be used for cross authentication of relationships between different traits.

  16. Quantitative Determination of Δ9-THC, CBG, CBD, Their Acid Precursors and Five Other Neutral Cannabinoids by UHPLC-UV-MS.

    Science.gov (United States)

    Wang, Yan-Hong; Avula, Bharathi; ElSohly, Mahmoud A; Radwan, Mohamed M; Wang, Mei; Wanas, Amira S; Mehmedic, Zlatko; Khan, Ikhlas A

    2018-03-01

    Cannabinoids are a group of terpenophenolic compounds in the medicinal plant Cannabis sativa (Cannabaceae family). Cannabigerolic acid, Δ 9 -tetrahydrocannabinolic acid A, cannabidiolic acid, Δ 9 -tetrahydrocannabinol, cannabigerol, cannabidiol, cannabichromene, and tetrahydrocannabivarin are major metabolites in the classification of different strains of C. sativa . Degradation or artifact cannabinoids cannabinol, cannabicyclol, and Δ 8 -tetrahydrocannabinol are formed under the influence of heat and light during processing and storage of the plant sample. An ultrahigh-performance liquid chromatographic method coupled with photodiode array and single quadruple mass spectrometry detectors was developed and validated for quantitative determination of 11 cannabinoids in different C. sativa samples. Compounds 1:  - 11: were baseline separated with an acetonitrile (with 0.05% formic acid) and water (with 0.05% formic acid) gradient at a flow rate of 0.25 mL/min on a Waters Cortec UPLC C18 column (100 mm × 2.1 mm I. D., 1.6 µm). The limits of detection and limits of quantitation of the 11 cannabinoids were below 0.2 and 0.5 µg/mL, respectively. The relative standard deviation for the precision test was below 2.4%. A mixture of acetonitrile and methanol (80 : 20, v / v ) was proven to be the best solvent system for the sample preparation. The recovery of all analytes was in the range of 97 - 105%. A total of 32 Cannabis samples including hashish, leaves, and flower buds were analyzed. Georg Thieme Verlag KG Stuttgart · New York.

  17. Quantitative lead determination in coating paint on children's outwear by LA-ICP-MS: a practical calibration strategy for solid samples.

    Science.gov (United States)

    Mercan, Selda; Ellez, Sevinç Zeynep; Türkmen, Zeynep; Yayla, Murat; Cengiz, Salih

    2015-01-01

    Lead is a hazardous compound that affects the central nervous system in people, particularly children, and may cause some reversible and irreversible diseases. Legal regulations try to prevent the exposure from products especially produced for children such as coating paints, jewelry, toys, bed linen, textile, etc. The aim of this study was to determine the lead levels of coating paints on children׳s outwear selling in district bazaar by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and to specify the percent of non-complying samples. Here we described the solid matrix calibration method and confirmed the results with the microwave-assisted acid digestion method. Both comparative methods were validated by analysis of the certified reference materials (NIST SRM-612 glass matrix, NIST SRM-2582 powdered paint and ERM-EC681k) and bias% for accuracy and RSD% for precision were calculated lower than 6.8% and 7.3%, respectively. The recovery ranges of laser ablation and microwave-assisted acid digestion method for Pb were found to be between 88.2-98.1% and 95.3-101.3%, respectively. The limits of detection values were determined as 0.162 mg kg(-1) for direct sampling in the ablation chamber and 0.002 ng mL(-1) for aqueous solutions. Correlation result of 16 samples (r=0.99) examined in both methods was satisfactory. In coating paint samples, 14.65% of 198 (n=29) did not comply with the 90 mg kg(-1) lead limit according to regulation. Validated quantitative laser ablation method may be preferred to quickly and reliably determine the Pb levels in other solid samples as well as coating paints. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Pretreatment Solution for Water Recovery Systems

    Science.gov (United States)

    Muirhead, Dean (Inventor)

    2018-01-01

    Chemical pretreatments are used to produce usable water by treating a water source with a chemical pretreatment that contains a hexavalent chromium and an acid to generate a treated water source, wherein the concentration of sulfate compounds in the acid is negligible, and wherein the treated water source remains substantially free of precipitates after the addition of the chemical pretreatment. Other methods include reducing the pH in urine to be distilled for potable water extraction by pretreating the urine before distillation with a pretreatment solution comprising one or more acid sources selected from a group consisting of phosphoric acid, hydrochloric acid, and nitric acid, wherein the urine remains substantially precipitate free after the addition of the pretreatment solution. Another method described comprises a process for reducing precipitation in urine to be processed for water extraction by mixing the urine with a pretreatment solution comprising hexavalent chromium compound and phosphoric acid.

  19. Aromatic inhibitors derived from ammonia-pretreated lignocellulose hinder bacterial ethanologenesis by activating regulatory circuits controlling inhibitor efflux and detoxification

    Directory of Open Access Journals (Sweden)

    David H. Keating

    2014-08-01

    Full Text Available Efficient microbial conversion of lignocellulosic hydrolysates to biofuels is a key barrier to the economically viable deployment of lignocellulosic biofuels. A chief contributor to this barrier is the impact on microbial processes and energy metabolism of lignocellulose-derived inhibitors, including phenolic carboxylates, phenolic amides (for ammonia-pretreated biomass, phenolic aldehydes, and furfurals. To understand the bacterial pathways induced by inhibitors present in ammonia-pretreated biomass hydrolysates, which are less well studied than acid-pretreated biomass hydrolysates, we developed and exploited synthetic mimics of ammonia-pretreated corn stover hydrolysate (ACSH. To determine regulatory responses to the inhibitors normally present in ACSH, we measured transcript and protein levels in an Escherichia coli ethanologen using RNA-seq and quantitative proteomics during fermentation to ethanol of synthetic hydrolysates containing or lacking the inhibitors. Our study identified four major regulators mediating these responses, the MarA/SoxS/Rob network, AaeR, FrmR, and YqhC. Induction of these regulons was correlated with a reduced rate of ethanol production, buildup of pyruvate, depletion of ATP and NAD(PH, and an inhibition of xylose conversion. The aromatic aldehyde inhibitor 5-hydroxymethylfurfural appeared to be reduced to its alcohol form by the ethanologen during fermentation, whereas phenolic acid and amide inhibitors were not metabolized. Together, our findings establish that the major regulatory responses to lignocellulose-derived inhibitors are mediated by transcriptional rather than translational regulators, suggest that energy consumed for inhibitor efflux and detoxification may limit biofuel production, and identify a network of regulators for future synthetic biology efforts.

  20. Development and validation of a liquid chromatography-tandem mass spectrometry method for the quantitative determination of gamithromycin in animal plasma, lung tissue and pulmonary epithelial lining fluid.

    Science.gov (United States)

    De Baere, Siegrid; Devreese, Mathias; Watteyn, Anneleen; Wyns, Heidi; Plessers, Elke; De Backer, Patrick; Croubels, Siska

    2015-06-12

    A sensitive and specific method for the quantitative determination of gamithromycin in animal plasma, lung tissue and pulmonary epithelial lining fluid (PELF) using liquid chromatography combined with heated electrospray ionization tandem mass spectrometry (LC-MS/MS) was developed. The sample preparation was rapid, straightforward and consisted of a deproteinization and phospholipid removal step using an Oasis(®) Ostro™ 96-well plate (chicken, turkey and calf plasma) or HybridSPE(®)-Phospholipid SPE cartridges (pig plasma and turkey lung tissue), while a liquid-liquid extraction with diethyl ether in alkaline medium was used for PELF of turkey poults. Chromatography was performed on a C18 Hypersil GOLD column using 0.01M ammonium acetate in water with a pH of 9, and acetonitrile as mobile phases. The MS/MS instrument was operated in the positive electrospray ionization mode and the following selected reaction monitoring transitions were monitored for gamithromycin (protonated molecule>product ion): m/z 777.45>619.35 and m/z 777.45>157.80 for quantification and identification, respectively. The method was validated in-house: matrix-matched calibration graphs were prepared and good linearity (r≥0.99) was achieved over the concentration ranges tested (2.5-10,000ngmL(-1) for chicken, pig and calf plasma; 5.0-2500ngmL(-1) for turkey plasma; 50-10,000ngg(-1) for turkey lung tissue and 20-1000ngmL(-1) for turkey PELF). Limits of quantification (LOQ) were 2.5ngmL(-1) for chicken, pig and calf plasma and 5.0ngmL(-1) for turkey plasma, while the limits of detection (LOD) ranged between 0.007 and 0.07ngmL(-1). For lung tissue and PELF, respective LOQ and LOD values of 50ngg(-1) and 0.76ngg(-1) (lung tissue) and 20ngmL(-1) and 0.1ngmL(-1) (PELF) were obtained. The results for the within-day and between-day precision, expressed as relative standard deviation (RSD), fell within the maximal RSD values. The accuracy fell within -30% to +10% (concentrations 1-10ngmL(-1)) or

  1. Potential of potassium hydroxide pretreatment of switchgrass for fermentable sugar production.

    Science.gov (United States)

    Sharma, Rajat; Palled, Vijaykumar; Sharma-Shivappa, Ratna R; Osborne, Jason

    2013-02-01

    Chemical pretreatment of lignocellulosic biomass has been extensively investigated for sugar generation and subsequent fuel production. Alkaline pretreatment has emerged as one of the popular chemical pretreatment methods, but most attempts thus far have utilized NaOH for the pretreatment process. This study aimed at investigating the potential of potassium hydroxide (KOH) as a viable alternative alkaline reagent for lignocellulosic pretreatment based on its different reactivity patterns compared to NaOH. Performer switchgrass was pretreated at KOH concentrations of 0.5-2% for varying treatment times of 6-48 h, 6-24 h, and 0.25-1 h at 21, 50, and 121 °C, respectively. The pretreatments resulted in the highest percent sugar retention of 99.26% at 0.5%, 21 °C, 12 h while delignification up to 55.4% was observed with 2% KOH, 121 °C, 1 h. Six pretreatment conditions were selected for subsequent enzymatic hydrolysis with Cellic CTec2® for sugar generation. The pretreatment condition of 0.5% KOH, 24 h, 21 °C was determined to be the most effective as it utilized the least amount of KOH while generating 582.4 mg sugar/g raw biomass for a corresponding percent carbohydrate conversion of 91.8%.

  2. X-ray magnetic dichroism: from quantitative determination of magnetic moments to imaging of magnetization dynamics; Dichroisme magnetique des rayons X: de la determination quantitative des moments magnetiques a l'imagerie de la dynamique de l'aimantation

    Energy Technology Data Exchange (ETDEWEB)

    Vogel, J

    2006-03-15

    In this document, I use some results of my research activities of the last ten years to show the power of x-ray magnetic dichroism for determining magnetic properties of thin layers, multilayers and nano-structures. The use of sum rules for x-ray dichroism allows a quantitative determination of the spin and orbital contributions to the magnetic moment, for each element of a heterogeneous material separately. Used in a qualitative way, x-ray dichroism allows monitoring the magnetization of the different layers in a multilayer material as a function of applied field. In combination with the temporal structure of synchrotron radiation, it is possible to study fast magnetization reversal with element selectivity, which is important for devices like spin valves and magnetic tunnel junctions. Adding the spatial resolution of a photoelectron emission microscope (PEEM), it becomes possible to study all the details of the fast magnetization reversal in complex magnetic systems. (author)

  3. Quantitative determination of occupation sites of trace Co substituted for multiple Fe sites in M-type hexagonal ferrite using statistical beam-rocking TEM-EDXS analysis.

    Science.gov (United States)

    Ohtsuka, Masahiro; Muto, Shunsuke; Tatsumi, Kazuyoshi; Kobayashi, Yoshinori; Kawata, Tsunehiro

    2016-04-01

    The occupation sites and the occupancies of trace dopants in La/Co co-doped Sr-M-type ferrite, SrFe12O19, were quantitatively and precisely determined by beam-rocking energy-dispersive X-ray spectroscopy (EDXS) on the basis of electron-channeling effects. Because the Co atoms, in particular, should be partially substituted for the five crystallographically inequivalent sites, which could be key parameters in improving the magneto-crystalline anisotropy, it is difficult yet intriguing to discover their occupation sites and occupancies without using the methods of large-scale facilities, such as neutron diffraction and synchrotron radiation. In the present study, we tackled this problem by applying an extended statistical atom location by channeling enhanced microanalysis method, using conventional transmission electron microscopy, EDXS and dynamical electron elastic/inelastic scattering theories. The results show that the key occupation sites of Co were the 2a, 4f1 and 12k sites. The quantified occupancies of Co were consistent with those of the previous study, which involved a combination of neutron diffraction and extended X-ray absorption fine structure analysis, as well as energetics considerations based on by first-principles calculations. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  4. A novel non-destructive manner for quantitative determination of plumpness of live Eriocheir sinensis using low-field nuclear magnetic resonance.

    Science.gov (United States)

    Song, Lingling; Zhang, Hongcai; Chen, Shunsheng

    2018-03-01

    The present study investigated the quantitative and non-destructive determination of Eriocheir sinensis' plumpness during four mature stages using low field-nuclear magnetic resonance (LF- 1 H NMR). Normalized lipid volume of live E. sinensis was calculated from Sept to Dec using 3D LF- 1 H nuclear magnetic imaging (MRI) and the validity of proposed technique was compared and verified with traditional Soxhlet extraction and live dissection method, respectively. The results showed the plumpness of female E. sinensis was higher than that of male ones from Sept to Dec and the highest plumpness of male and female E. sinensis reached 99,436.44 and 109,207.15mm 3 in Oct. The normalized lipid volume of live male and female E. sinensis had a positive correlation with lipid content. This proposed method with short assay time, favorable selectivity, and accuracy demonstrated its application potential in grading regulation and quality evaluation of live E. sinensis. Copyright © 2017. Published by Elsevier Ltd.

  5. Quantitative determination of uranium distribution homogeneity in MTR fuel type plates; Determinacao quantitativa da homogeneidade da distribuicao de uranio em combustiveis nucleares tipo placa

    Energy Technology Data Exchange (ETDEWEB)

    Ferrufino, Felipe Bonito Jaldin

    2011-07-01

    IPEN/CNEN-SP produces the fuel to supply its nuclear research reactor IEA-R1. The fuel is assembled with fuel plates containing an U{sub 3}Si{sub 2}-Al composite meat. A good homogeneity in the uranium distribution inside the fuel plate meat is important from the standpoint of irradiation performance. Considering the lower power of reactor IEA-R1, the uranium distribution in the fuel plate has been evaluated only by visual inspection of radiographs. However, with the possibility of IPEN to manufacture the fuel for the new Brazilian Multipurpose Reactor (RMB), with higher power, it urges to develop a methodology to determine quantitatively the uranium distribution into the fuel. This paper presents a methodology based on X-ray attenuation, in order to quantify the uranium concentration distribution in the meat of the fuel plate by using optical densities in radiographs and comparison with standards. The results demonstrated the inapplicability of the method, considering the current specification for the fuel plates due to the high intrinsic error to the method. However, the study of the errors involved in the methodology, seeking to increase their accuracy and precision, can enable the application of the method to qualify the final product. (author)

  6. Quantitative determination of seven chemical constituents and chemo-type differentiation of chamomiles using high-performance thin-layer chromatography.

    Science.gov (United States)

    Sagi, Satyanarayanaraju; Avula, Bharathi; Wang, Yan-Hong; Zhao, Jianping; Khan, Ikhlas A

    2014-10-01

    A simple and rapid high-performance thin-layer chromatographic method was developed for the separation and determination of six flavonoids (rutin, luteolin-7-O-β-glucoside, chamaemeloside, apigenin-7-O-β-glucoside, luteolin, apigenin) and one coumarin, umbelliferone from chamomile plant samples and dietary supplements. The separation was achieved on amino silica stationary phase using dichloromethane/acetonitrile/ethyl formate/glacial acetic acid/formic acid (11:2.5:3:1.25:1.25 v/v/v/v/v) as the mobile phase. The quantitation of each compound was carried out using densitometric reflection/absorption mode at their respective absorbance maxima after postchromatographic derivatization using natural products reagent (1% w/v methanolic solution of diphenylboric acid-β-ethylamino ester). The method was validated for specificity, limits of detection and quantification, precision (intra- and interday) and accuracy. The limits of detection and quantification were found to be in the range from 6-18 and 16-55 ng/band for six flavonoids and one coumarin, respectively. The intra- and interday precision was found to be 90%. The data acquired from high-performance thin-layer chromatography was processed by principal component analysis using XLSTAT statistical software. Application of principal component analysis and agglomerative hierarchial clustering was successfully able to differentiate two chamomiles (German and Roman) and Chrysanthemum. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Evaluation of flow-injection tandem mass spectrometry for rapid and high-throughput quantitative determination of B vitamins in nutritional supplements.

    Science.gov (United States)

    Bhandari, Deepak; Van Berkel, Gary J

    2012-08-29

    The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B vitamins, viz., B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed. Automated flow injection introduced 1 μL of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and SRM 3280. The quantity determined for each B vitamin in SRM 3280 was within the statistical range provided for the respective certified values. This approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B vitamins, as evidenced by an agreement with the label values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.

  8. Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Deepak [ORNL; Van Berkel, Gary J [ORNL

    2012-01-01

    The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45 min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.

  9. Reducing the V2O3(0001) surface through electron bombardment--a quantitative structure determination with I/V-LEED.

    Science.gov (United States)

    Feiten, Felix E; Kuhlenbeck, Helmut; Freund, Hans-Joachim

    2016-01-28

    The (0001) surface of vanadium sesquioxide, V2O3, is terminated by vanadyl groups under standard ultra high vacuum preparation conditions. Reduction with electrons results in a chemically highly active surface with a well-defined LEED pattern indicating a high degree of order. In this work we report the first quantitative structure determination of a reduced V2O3(0001) surface. We identify two distinct surface phases by STM, one well ordered and one less well ordered. I/V-LEED shows the ordered phase to be terminated by a single vanadium atom per surface unit cell on a quasi-hexagonal oxygen layer with three atoms per two-dimensional unit cell. Furthermore we compare the method of surface reduction via electron bombardment with the deposition of V onto a vanadyl terminated film. The latter procedure was previously proposed to result in a structure with three surface vanadium atoms in the 2D unit cell and we confirm this with simulated STM images.

  10. The development of a method for the qualitative and quantitative determination of petroleum hydrocarbon components using thin-layer chromatography with flame ionization detection.

    Science.gov (United States)

    Wang, Shijie; Guo, Guanlin; Yan, Zengguang; Lu, Guilan; Wang, Qunhui; Li, Fasheng

    2010-01-15

    An analytical scheme to determine groups of petroleum hydrocarbon compounds in crude oil was developed and used for the qualitative and quantitative characterization of crude oil samples from the Shengli oilfield, the second largest oilfield in China. Crude oil samples were fractionated and analyzed by thin-layer chromatography with flame ionization detection (TLC-FID). Relative standard deviation (RSD) values for retention time, peak height and half peak width were less than 5.2% for all classes of compounds, based on nine independent replicates. The crude oil light fraction was further analyzed by GC-MS and the majority of identified compounds were methyl- or hydro-derivatives of long-chain hydrocarbons and aromatic compounds. The external standard method used in the present study can lower detection limits of petroleum hydrocarbon compound classes to 20.0 mg L(-1), and the crude oil concentration in the range of 30 and 35,000 mg L(-1) has a high linear correlation (r(2)>0.97, Poil contaminated soils of 50, 80, 200 and 300 mg g(-1). The tested TLC-FID method showed a 10% higher recovery for total extractable materials than the reference EC method. The calibration factor was fraction-dependent and varied with the recovery rate of TLC/EC. Regarding the tested extraction procedures, accelerated solvent extraction (ASE) had a higher extraction efficiency for crude oil contaminated soils than Soxhlet and ultrasonic extractions. 2009 Elsevier B.V. All rights reserved.

  11. Determinants of the process and outcomes of household participation in collaborative forest management in Ghana: a quantitative test of a community resilience model.

    Science.gov (United States)

    Akamani, Kofi; Hall, Troy Elizabeth

    2015-01-01

    This study tested a proposed community resilience model by investigating the role of institutions, capital assets, community and socio-demographic variables as determinants of households' participation in Ghana's collaborative forest management (CFM) program and outcomes of the program. Quantitative survey data were gathered from 209 randomly selected households from two forest-dependent communities. Regression analysis shows that households' participation in the CFM program was predicted by community location, past connections with institutions, and past bonding social capital. Community location and past capitals were the strongest predictors of the outcomes of the CFM program as judged by current levels of capitals. Participation in the CFM program also had a positive effect on human capital but had minimal impact on the other capitals influencing household well-being and resilience, suggesting that the impact of co-management on household resilience may be modest. In all, the findings highlight the need for co-management policies to pay attention to the historical context of community interaction processes influencing access to capital assets and local institutions to successfully promote equitable resilience. Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. Feasibility and extension of universal quantitative models for moisture content determination in beta-lactam powder injections by near-infrared spectroscopy.

    Science.gov (United States)

    Zhang, Xue-Bo; Feng, Yan-Chun; Hu, Chang-Qin

    2008-12-23

    In present work, we investigated the feasibility of universal calibration models for moisture content determination of a much complicated products system of powder injections to simulate the process of building universal models for drug preparations with same INN (International Nonproprietary Name) from diverse formulations and sources. We also extended the applicability of universal model by model updating and calibration transfer. Firstly, a moisture content quantitative model for ceftriaxone sodium for injection was developed, the results show that calibration model established for products of some manufacturers is also available for the products of others. Then, we further constructed a multiplex calibration model for seven cephalosporins for injection ranging from 0.40 to 9.90%, yielding RMSECV and RMSEP of 0.283 and 0.261, respectively. However, this multiplex model could not predict samples of another cephalosporin (ceftezole sodium) and one penicillins (penicillin G procaine) for injection accurately. With regard to such limits and the extension of universal models, two solutions are proposed: model updating (MU) and calibration transfer. Overall, model updating is a robust method for the analytical problem under consideration. When timely model updating is impractical, piecewise direct standardization (PDS) algorithm is more desirable and applied to transfer calibration model between different powder injections. Both two solutions have proven to be effective to extend the applicability of original universal models for the new products emerging.

  13. Quantitative determination of antidepressants and their select degradates by liquid chromatography/electrospray ionization tandem mass spectrometry in biosolids destined for land application.

    Science.gov (United States)

    Niemi, Lydia M; Stencel, Katherine A; Murphy, Madigan J; Schultz, Melissa M

    2013-08-06

    Antidepressants are one of the most widely dispensed classes of pharmaceuticals in the United States. As wastewater treatment plants are a primary source of pharmaceuticals in the environment, the use of biosolids as fertilizer is a potential route for antidepressants to enter the terrestrial environment. A microsolvent extraction method, utilizing green chemistry, was developed for extraction of the target antidepressants and degradation products from biosolids, or more specifically lagoon biosolids. Liquid chromatography/tandem mass spectrometry was used for quantitative determination of antidepressants in the lagoon biosolid extracts. Recoveries from matrix spiking experiments for the individual antidepressants had an average of 96%. The limits of detection for antidepressant pharmaceuticals and degradates ranged from 0.36 to 8.0 ng/kg wet weight. The method was applied to biosolids destined for land application. A suite of antidepressants was consistently detected in the lagoon biosolid samples, and thus antidepressants are being introduced to terrestrial environments through the land application of these biosolids. Sertraline and norsertraline were the most abundant antidepressant and degradation product detected in the biosolid samples. Detected, individual antidepressant concentrations ranged from 8.5 ng/kg (norfluoxetine) to 420 ng/kg wet weight (norsertraline).

  14. Determinants of activity at human Toll-like receptors 7 and 8: quantitative structure-activity relationship (QSAR) of diverse heterocyclic scaffolds.

    Science.gov (United States)

    Yoo, Euna; Salunke, Deepak B; Sil, Diptesh; Guo, Xiaoqiang; Salyer, Alex C D; Hermanson, Alec R; Kumar, Manoj; Malladi, Subbalakshmi S; Balakrishna, Rajalakshmi; Thompson, Ward H; Tanji, Hiromi; Ohto, Umeharu; Shimizu, Toshiyuki; David, Sunil A

    2014-10-09

    Toll-like receptor (TLR) 7 and 8 agonists are potential vaccine adjuvants, since they directly activate APCs and enhance Th1-driven immune responses. Previous SAR investigations in several scaffolds of small molecule TLR7/8 activators pointed to the strict dependence of the selectivity for TLR7 vis-à-vis TLR8 on the electronic configurations of the heterocyclic systems, which we sought to examine quantitatively with the goal of developing "heuristics" to define structural requisites governing activity at TLR7 and/or TLR8. We undertook a scaffold-hopping approach, entailing the syntheses and biological evaluations of 13 different chemotypes. Crystal structures of TLR8 in complex with the two most active compounds confirmed important binding interactions playing a key role in ligand occupancy and biological activity. Density functional theory based quantum chemical calculations on these compounds followed by linear discriminant analyses permitted the classification of inactive, TLR8-active, and TLR7/8 dual-active compounds, confirming the critical role of partial charges in determining biological activity.

  15. Development and evaluation of a standard method for the quantitative determination of elements in float glass samples by LA-ICP-MS.

    Science.gov (United States)

    Latkoczy, Christopher; Becker, Stefan; Dücking, Marc; Günther, Detlef; Hoogewerff, Jurian A; Almirall, Jose R; Buscaglia, JoAnn; Dobney, Andrew; Koons, Robert D; Montero, Shirly; van der Peijl, Gerard J Q; Stoecklein, Wilfried R S; Trejos, Tatiana; Watling, John R; Zdanowicz, Vincent S

    2005-11-01

    Forensic analysis of glass samples was performed in different laboratories within the NITE-CRIME (Natural Isotopes and Trace Elements in Criminalistics and Environmental Forensics) European Network, using a variety of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) systems. The main objective of the interlaboratory tests was to cross-validate the different combinations of laser ablation systems with different ICP-MS instruments. A first study using widely available samples, such as the NIST SRM 610 and NIST SRM 612 reference glasses, led to deviations in the determined concentrations for trace elements amongst the laboratories up to 60%. Extensive discussion among the laboratories and the production of new glass reference standards (FGS 1 and FGS 2) established an improved analytical protocol, which was tested on a well-characterized float glass sample (FG 10-1 from the BKA Wiesbaden collection). Subsequently, interlaboratory tests produced improved results for nearly all elements with a deviation of < 10%, demonstrating that LA-ICP-MS can deliver absolute quantitative measurements on major, minor and trace elements in float glass samples for forensic and other purposes.

  16. Comprehensive qualitative and quantitative determination of pesticides and veterinary drugs in honey using liquid chromatography-Orbitrap high resolution mass spectrometry.

    Science.gov (United States)

    Gómez-Pérez, María Luz; Plaza-Bolaños, Patricia; Romero-González, Roberto; Martínez-Vidal, José Luis; Garrido-Frenich, Antonia

    2012-07-27

    A database has been created for the simultaneous analysis of more than 350 pesticides and veterinary drugs (including antibiotics) using ultra-high performance liquid chromatography coupled to high resolution Orbitrap mass spectrometry (UHPLC-Orbitrap-MS). This is a comprehensive exact mass database built using the Exactive-Orbitrap analyzer. The developed database includes exact masses of the target ions and retention time data, and allows the automatic search of the included compounds. Generic chromatographic and MS conditions have been applied. The presented database is suitable for qualitative analysis, and it was also evaluated for quantitative purposes in routine analysis, after the optimization and validation of a generic extraction method in honey samples. Adequate recovery and precision values for most of the studied analytes were obtained and the limits of detection (LOD) ranged from 1 to 50 μg kg(-1). For pesticides, LODs were always lower than the MRLs established by European Union in honey, except for a few compounds. This method was applied to the analysis of 26 real honey samples and some pesticides (azoxystrobin, coumaphos, dimethoate and thiacloprid) were detected in 4 samples. Azoxystrobin and coumaphos were determined in two different samples (organic honey) at 1.5 μg kg(-1) and 5.1 μg kg(-1). Veterinary drugs were not detected in the analyzed samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Influence of coefficient of variation in determining significant difference of quantitative values obtained from 28-day repeated-dose toxicity studies in rats.

    Science.gov (United States)

    Kobayashi, Katsumi; Sakuratani, Yuki; Abe, Takemaru; Yamazaki, Kazuko; Nishikawa, Satoshi; Yamada, Jun; Hirose, Akihiko; Kamata, Eiichi; Hayashi, Makoto

    2011-01-01

    In order to understand the influence of coefficient of variation (CV) in determining significant difference of quantitative values of 28-day repeated-dose toxicity studies, we examined 59 parameters of 153 studies conducted in accordance with Chemical Substance Control Law in 12 test facilities. Sex difference was observed in 12 parameters and 10 parameters showed large CV in females. The minimum CV was 0.74% for sodium. CV of electrolytes was comparatively small, whereas enzymes had large CV. Large differences in CV were observed for major parameters among 7-8 test facilities. The changes in CV were grossly classified into 11. Our study revealed that a statistical significant difference is usually detected if there is a difference of 7% in mean values between the groups and the groups have a CV of about 7%. A parameter with a CV as high as 30% may be significantly different, if the difference of the mean between the groups is 30%. It would be ideal to use median value to assess the treatment-related effect, rather than mean, when the CV is very high. We recommend using CV of the body weight as a standard to judge the adverse effect level.

  18. Chemical characterization of the aroma of Grenache rosé wines: aroma extract dilution analysis, quantitative determination, and sensory reconstitution studies.

    Science.gov (United States)

    Ferreira, Vicente; Ortín, Natalia; Escudero, Ana; López, Ricardo; Cacho, Juan

    2002-07-03

    The aroma of a Grenache rosé wine from Calatayud (Zaragoza, Spain) has been elucidated following a strategy consisting of an aroma extract dilution analysis (AEDA), followed by the quantitative analysis of the main odorants and the determination of odor activities values (OAVs) and, finally, by a series of reconstitution and omission tests with synthetic aroma models. Thirty-eight aroma compounds were found in the AEDA study, 35 of which were identified. Twenty-one compounds were at concentrations higher than their corresponding odor thresholds. An aroma model prepared by mixing the 24 compounds with OAV > 0.5 in a synthetic wine showed a high qualitative similarity with the aroma of the rosé wine. The addition of compounds with OAV 10 was very different from that of the wine. Omission tests revealed that the most important odorant of this Grenache rosé wine was 3-mercapto-1-hexanol, with a deep impact on the wine fruity and citric notes. The synergic action of Furaneol and homofuraneol also had an important impact on wine aroma, particularly in its fruity and caramel notes. The omission of beta-damascenone, which had the second highest OAV, caused only a slight decrease on the intensity of the aroma model. Still weaker was the sensory effect caused by the omission of 10 other compounds, such as fatty acids and their ethyl esters, isoamyl acetate, and higher alcohols.

  19. Protein standardization III: Method optimization basic principles for quantitative determination of human serum proteins on automated instruments based on turbidimetry or nephelometry.

    Science.gov (United States)

    Blirup-Jensen, S

    2001-11-01

    Quantitative protein determinations in routine laboratories are today most often carried out using automated instruments. However, slight variations in the assay principle, in the programming of the instrument or in the reagents may lead to different results. This has led to the prerequisite of method optimization and standardization. The basic principles of turbidimetry and nephelometry are discussed. The different reading principles are illustrated and investigated. Various problems are identified and a suggestion is made for an integrated, fast and convenient test system for the determination of a number of different proteins on the same instrument. An optimized test system for turbidimetry and nephelometry should comprise high-quality antibodies, calibrators, controls, and buffers and a protocol with detailed parameter settings in order to program the instrument correctly. A good user program takes full advantage of the optimal reading principles for the different instruments. This implies--for all suitable instruments--sample preincubation followed by real sample blanking, which automatically corrects for initial turbidity in the sample. Likewise it is recommended to measure the reagent blank, which represents any turbidity caused by the antibody itself. By correcting all signals with these two blank values the best possible signal is obtained for the specific analyte. An optimized test system should preferably offer a wide measuring range combined with a wide security range, which for the user means few re-runs and maximum security against antigen excess. A non-linear calibration curve based on six standards is obtained using a suitable mathematical fitting model, which normally is part of the instrument software.