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Sample records for chromatography-mass spectrometric determination

  1. Liquid chromatography-mass spectrometric and liquid chromatography-tandem mass spectrometric determination of hallucinogenic indoles psilocin and psilocybin in "magic mushroom" samples.

    Science.gov (United States)

    Kamata, Tooru; Nishikawa, Mayumi; Katagi, Munehiro; Tsuchihashi, Hitoshi

    2005-03-01

    Accurate and sensitive analytical methods for psilocin (PC) and psilocybin (PB), tryptamine-type hallucinogens contained in "magic mushrooms," were investigated using liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS). The chromatographic separation on an ODS column and mass spectral information gave complete discrimination between PC and PB without derivatization. The mass spectrometric detection had a high sensitivity, and the tandem mass spectrometric detection provided more specificity and accuracy, as well as high sensitivity. The detection limits ranged from 1 to 25 pg by LC-MS in the selected ion monitoring mode, and the intra- and inter-day coefficients of variation were estimated to be 4.21-5.93% by LC-MS-MS in the selected reaction monitoring mode. By applying the present LC-MS-MS technique to four real samples, the contents of PC and PB were found to vary over a wide range (0.60-1.4 and 0.18-3.8 mg/g dry wt. for PC and PB, respectively) between samples.

  2. Single-walled carbon nanotubes coated fibers for solid-phase microextraction and gas chromatography-mass spectrometric determination of pesticides in Tea samples.

    Science.gov (United States)

    Wu, Fang; Lu, Wanping; Chen, Jinghua; Liu, Wei; Zhang, Lan

    2010-08-15

    Using a single-walled carbon nanotubes (SWCNTs) as stationary phase of solid-phase microextraction (SPME) fibers, a simple, low cost and environmentally friendly method for extraction of 13 pesticides in Tea samples has been developed following gas chromatography-mass spectrometric determination. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction and desorption time, extraction temperature, stirring rate, solution pH and ionic strength. Under optimized conditions, the linearity of the developed method was in the range of 0.125-25 ng/mL with correlation coefficients greater than 0.9928 and the limits of detections (LODs) were 0.027-0.23 ng/mL (S/N=3). Meanwhile, the relative standard deviations (RSDs) for five successive measurements with single fiber, fiber-to-fiber, day-to-day were 2.3-13.0, 8.2-14.6 and 4.1-12.5%, respectively, indicating good reproducibility of the proposed method. The fiber had high extraction efficiency for studied pesticides in comparison with commercial poly(dimethylsiloxane) (PDMS) and polyacrylate (PA) fibers and could be used for more than 70 times without decrease of efficiency. The developed method was successfully applied for the analysis of real samples including green Tea, oolong Tea, white Tea, and flower Tea, and the recoveries of the pesticides spiked in these samples ranged from 75.1 to 118.4%. Chlorfenapyr and lambda-cyhalothrin were found in the Tea samples bought randomly from local market. The results demonstrated that the developed SWCNTs-SPME method was a simple, efficient pretreatment and enrichment procedure for pesticides in complex matrices. PMID:20678665

  3. Gas chromatography-mass spectrometric determination of polycyclic aromatic hydrocarbons in five species of fish from three sites in the Arabian Gulf.

    Science.gov (United States)

    Al-Saleh, Iman; Al-Doush, Inaam

    2002-06-01

    A gas chromatography-mass spectrmetroic (GC-MS) method was developed to measure six polycyclic aromatic hydrocarbons (PAHs) in 54 fish samples. Five fish species highly consumed by the local population (shrimps, Emperors, Rabbitfish, Doublebar Bream and Greasy Grouper) were selected from three different sites on the Gulf coast of Saudi Arabia where agricultural, municipal and petroleum industry activities take place. Variations in PAH levels among the three sites were not significant. Total concentrations of PAHs benzo(a)anthracene, chrysene, and benzo(b)fluoranthene ranged from non-detectable to 44.9 microg kg(-1). In this study, concentrations of benzo(a)anthracene, chrysene, benzo(b)fluoranthene and total PAHs greater than the acceptable tolerance limit (1 microg kg(-1)) were found in 68.5, 40.7, 51.9 and 83.3% of the fish samples, respectively. PAH contents in fish vary considerably with species; Doublebar bream contain the highest while shrimps contain the lowest. This pilot study clearly shows that the consumption of fish could be a source of exposure of the local population to PAHs. Since there is a consensus on the substantial contribution of PAHs to cancer in humans, it would be interesting to conduct further research in order to determine the magnitude of the problem along other coastal regions of Saudi Arabia.

  4. Applications of information theory and pattern recognition to gas chromatography-mass spectrometric analysis of toxic organic compounds in ambient air

    Energy Technology Data Exchange (ETDEWEB)

    Scott, D.R.

    1986-05-01

    The number of information channels contained in the gas-chromatographic, mass-spectrometric, and combined gas chromatography-mass spectrometric analysis of 78 toxic organic compounds was determined. The toxic compounds are those routinely monitored in ambient air samples using Tenax collection and gas chromatography-mass spectrometric analysis. The Shannon information content of the binary encoded and full-intensity mass spectra, of the gas-chromatographic retention times, and of the combined gas chromatographic-mass spectrometric spectra of the 78 compounds was calculated. The maximum binary information contents of the 35 channel gas chromatographic, 17 key channel mass spectral, and the 595 channel gas chromatographic-mass spectral methods were 6.4, 15.4, and < 21.8 bits, respectively. The 17 masses with the highest binary information content with regard to the 78 compounds were used with SIMCA pattern recognition to determine four classes among the 78 compounds. These included aromatics without chlorine substitution, chloroaromatics, bromoalkanes and alkenes, and chloroalkanes and alkenes.

  5. Comparison of two derivatization-based methods for solid-phase microextraction-gas chromatography-mass spectrometric determination of bisphenol A, bisphenol S and biphenol migrated from food cans.

    Science.gov (United States)

    Viñas, P; Campillo, N; Martínez-Castillo, N; Hernández-Córdoba, M

    2010-05-01

    An environmentally friendly sample pretreatment system based on solid-phase microextraction (SPME) for the sensitive determination of bisphenol A (BPA), bisphenol S (BPS) and biphenol (BP) is described. Two derivatisation reactions to obtain volatile derivatives are compared. Derivatisation with acetic anhydride (AA) was performed in situ in a 5-mM Na(2)CO(3)/NaHCO(3) buffer solution and analytes were extracted by direct immersion (DI) using a PA fibre (85 microm) at 90 degrees C for 40 min with stirring at 1,500 rpm. For derivatisation with bis-(trimethylsilyl)trifluoroacetamide (BSTFA), the analytes were first extracted by DI using the PA fibre at 70 degrees C for 40 min with stirring at 500 rpm. The fibre was then removed, dried in a nitrogen stream for 2 min and introduced into the headspace of BSTFA at 50 degrees C for 30 s. After derivatisation, the analytes were desorbed in the injection port of the GC in the splitless mode at 280 degrees C for 4 min. The separation was carried out by coupling gas chromatography with mass spectrometry in the selected ion monitoring mode, GC-MS(SIM). The method allowed the determination of the migrating levels of bisphenols found in food cans, and it was validated for linearity, detection and quantitation limits, selectivity, accuracy and precision. Detection limits ranged from 3 to 16 pg mL(-1), depending on the compound, at a signal-to-noise ratio of 3. Recoveries obtained for spiked samples were satisfactory for all compounds. Levels of BPA were higher than those of BPS and the lowest contents were found for BP.

  6. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Science.gov (United States)

    Tayade, Amol B; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chauhan, Rajinder S; Chaurasia, Om P; Srivastava, Ravi B

    2013-01-01

    Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo), belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS) technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S); 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl) phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl); α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful results in

  7. Systematic analysis of glycerol: colourimetric screening and gas chromatography-mass spectrometric confirmation.

    Science.gov (United States)

    Sardela, Vinícius F; Scalco, Fernanda B; Cavalcante, Karina M; Simoni, Ruth E; Silva, Deyvison R; Pereira, Henrique Marcelo G; de Oliveira, Maria Lúcia L Costa; Aquino Neto, Francisco R

    2015-10-01

    Glycerol is a naturally occurring polyol in the human body, essential for several metabolic processes. It is widely used in the food, pharmaceutical, and medical industries and in clinical practice as a plasma volume expander (PVE). Athletes, however, may use glycerol to mask the presence of forbidden substances or to enhance performance, inclusively through hyperhydration achieved by glycerol ingestion with added fluid. These practices are considered doping, and are prohibited by the World Anti-Doping Agency (WADA). Therefore, glycerol was introduced in the prohibited list. Doping through glycerol ingestion can readily be identified by detection of elevated glycerol concentrations in urine. In this paper, a protocol for the fast detection of glycerol in urine is proposed. It consists of a previous visual colourimetric screening, followed by a quantitative/qualitative confirmation analysis by mass spectrometry. The screening procedure involves a reaction in which polyhydric alcohols are oxidized by periodate to formic acid and formaldehyde, which is detected by the addition of a fuchsin solution. For the subsequent qualitative/quantitative confirmation analysis, a gas chromatography-mass spectrometry based approach with a non-deuterated internal standard and a drying step of only 10 min is proposed. The linear correlation was demonstrated within WADA´s threshold range. The calculated RSD were 2.1% for within-day precision and 2.8% for between-day precision. The uncertainty estimation was calculated, and a value of 2.7% was obtained. The procedure may also be used for the analysis of other polyols in urine, as for example the PVE mannitol. PMID:26112364

  8. Systematic analysis of glycerol: colourimetric screening and gas chromatography-mass spectrometric confirmation.

    Science.gov (United States)

    Sardela, Vinícius F; Scalco, Fernanda B; Cavalcante, Karina M; Simoni, Ruth E; Silva, Deyvison R; Pereira, Henrique Marcelo G; de Oliveira, Maria Lúcia L Costa; Aquino Neto, Francisco R

    2015-10-01

    Glycerol is a naturally occurring polyol in the human body, essential for several metabolic processes. It is widely used in the food, pharmaceutical, and medical industries and in clinical practice as a plasma volume expander (PVE). Athletes, however, may use glycerol to mask the presence of forbidden substances or to enhance performance, inclusively through hyperhydration achieved by glycerol ingestion with added fluid. These practices are considered doping, and are prohibited by the World Anti-Doping Agency (WADA). Therefore, glycerol was introduced in the prohibited list. Doping through glycerol ingestion can readily be identified by detection of elevated glycerol concentrations in urine. In this paper, a protocol for the fast detection of glycerol in urine is proposed. It consists of a previous visual colourimetric screening, followed by a quantitative/qualitative confirmation analysis by mass spectrometry. The screening procedure involves a reaction in which polyhydric alcohols are oxidized by periodate to formic acid and formaldehyde, which is detected by the addition of a fuchsin solution. For the subsequent qualitative/quantitative confirmation analysis, a gas chromatography-mass spectrometry based approach with a non-deuterated internal standard and a drying step of only 10 min is proposed. The linear correlation was demonstrated within WADA´s threshold range. The calculated RSD were 2.1% for within-day precision and 2.8% for between-day precision. The uncertainty estimation was calculated, and a value of 2.7% was obtained. The procedure may also be used for the analysis of other polyols in urine, as for example the PVE mannitol.

  9. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Directory of Open Access Journals (Sweden)

    Amol B Tayade

    Full Text Available Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo, belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S; 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl; α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful

  10. Gas chromatography-mass spectrometric analysis of bonded long chain fatty acids in a single zebrafish egg by ultrasound-assisted one-step transmethylation and extraction

    Energy Technology Data Exchange (ETDEWEB)

    Li Jianjian; Yue Yingxia; Li Tingting; Hu Xuejiao [Key Laboratory of Pesticides and Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, Hubei 430079 (China); Zhong Hongying, E-mail: hyzhong@mail.ccnu.edu.cn [Key Laboratory of Pesticides and Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, Hubei 430079 (China)

    2009-09-21

    Changes in the level of lipid composition in a single zebrafish egg have been involved in biological responses to chemical exposures. In this paper, an one-step transmethylation of lipids and simultaneous extraction of resultant fatty acid methyl esters followed by gas chromatography-mass spectrometric analysis was developed for the identification of bonded long chain fatty acids in a single zebrafish egg. The efficiency of transmethylation under different experimental conditions has been investigated. Dried egg homogenates were directly mixed with either 0.5 M NaOH or 1% H{sub 2}SO{sub 4} or 4% HCl solution of methanol and then an n-hexane solution was added on the top. Ultrasonication of this immiscible liquid-liquid-solid system produces high velocity impacts between solid particles and liquid phases and thus promotes mass transfer among phases. It was demonstrated that ultrasound irradiation has strong effect on the alkaline-catalyzed transmethylation of lipids but cannot significantly change the acid-catalyzed transmethylation of lipids. With the aid of ultrasonication, transmethylation can be combined with simultaneous extraction of the resultant fatty acid methyl esters into n-hexane phase. This approach simplifies the sample preparation procedure, shortens the reaction time but improves the efficiency of the transmethylation of lipids and reduces sample losses, especially for small size samples. It has been applied to determine bonded fatty acids in a single zebrafish egg. In total, 28 fatty acids from a single zebrafish egg have been identified reproducibly.

  11. Gas chromatography-mass spectrometric analysis of bonded long chain fatty acids in a single zebrafish egg by ultrasound-assisted one-step transmethylation and extraction

    International Nuclear Information System (INIS)

    Changes in the level of lipid composition in a single zebrafish egg have been involved in biological responses to chemical exposures. In this paper, an one-step transmethylation of lipids and simultaneous extraction of resultant fatty acid methyl esters followed by gas chromatography-mass spectrometric analysis was developed for the identification of bonded long chain fatty acids in a single zebrafish egg. The efficiency of transmethylation under different experimental conditions has been investigated. Dried egg homogenates were directly mixed with either 0.5 M NaOH or 1% H2SO4 or 4% HCl solution of methanol and then an n-hexane solution was added on the top. Ultrasonication of this immiscible liquid-liquid-solid system produces high velocity impacts between solid particles and liquid phases and thus promotes mass transfer among phases. It was demonstrated that ultrasound irradiation has strong effect on the alkaline-catalyzed transmethylation of lipids but cannot significantly change the acid-catalyzed transmethylation of lipids. With the aid of ultrasonication, transmethylation can be combined with simultaneous extraction of the resultant fatty acid methyl esters into n-hexane phase. This approach simplifies the sample preparation procedure, shortens the reaction time but improves the efficiency of the transmethylation of lipids and reduces sample losses, especially for small size samples. It has been applied to determine bonded fatty acids in a single zebrafish egg. In total, 28 fatty acids from a single zebrafish egg have been identified reproducibly.

  12. DETERMINATION OF ACRYLAMIDE IN FOOD BY GAS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Michaela Vieriková

    2010-07-01

    Full Text Available  Acrylamide in food was determined by gas chromatography - mass spectrometry (GC-MS after bromination of acrylamide and underivatized acrylamide was quantified by ultra performance liquid chromatography -mass spectrometry (UPLC-MS. Two different sample preparation methods were used and optimised. The GC-MS method was used for various food matrices like breads, potato crisps, potato crackers, french fries. The UPLC-MS method was used for analysis of coffee. The limit of detection and limit of quantification for acrylamide were 7 µg.kg-1 and 20 µg.kg-1 by GC-MS, 9 µg.kg-1  and 30 µg.kg-1 by UPLC-MS. For both methods the reproducibility, given as relative standard deviation was    doi:10.5219/61  

  13. Determination of alkyl methanesulfonates in doxazosin mesylate by gas chromatography-mass spectrometer

    Directory of Open Access Journals (Sweden)

    C Sitaram

    2011-01-01

    Full Text Available High sensitive rapid gas chromatography-mass spectrometry method for the determination of four carcinogenic alkyl methanesulfonates viz. methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate in doxazosin mesylate has been presented by using selective ion monitoring mode. The optimum separation was achieved between methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate on a DB-5 (30 m×0.32 mm×1.0 μm capillary column under programming temperature. Acetonitrile, water and ammonia (90:9:1 v/v/v mixture was used as diluent. Various factors involved in the gas chromatography-mass spectrometry method development are also presented. This method was validated as per International Conference on Harmonization guidelines. The limit of quantitation of methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate is 6 ppm with respect to 30 mg/ml of doxazosin mesylate.

  14. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou;

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations acetone+acetoacetate levels (~25 to 8300 µM) and D-ß-hydroxybutyrate levels (~30 to 16500 µM). Recovery values varied...

  15. [Determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry].

    Science.gov (United States)

    Wang, Ghengyun; Zhang, Weiya; Li, Lixia; Shen, Yalei; Lin, Junfeng; Xie, Tangtang; Chu, Naiqing

    2014-08-01

    An effective method was established for the simultaneous determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry. Glycol ethers in leather and leather products were ultrasonically extracted at 45 °C, using ethyl acetate as the extraction solvent. The extracts were purified by solid phase extraction (SPE) columns, and then analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode. The content of each analyte was calibrated by external standard method. The limit of detection of ethylene glycol ethyl ether (EGEE) was 0. 10 mg/kg under the condition of signal to noise (S/N) of 3 and the limits of the other 11 glycol ethers were all less than 0.05 mg/kg. The spiked recoveries varied from 81. 2% to 95. 5% at three different spiked levels with the relative standard deviations (RSDs) ranged from 1.4% to 6. 6%. The proposed method is simple, rapid and accurate, with the limits of detection much less than the requirements of the Regulation Concerning Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) of European Union. It is applicable to the determination of residual glycol ethers in leather and leather products, and provides a reference for the relevant testing standards.

  16. The determination of 5-fluorouracil in human plasma by a gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    A gas chromatography-mass spectrometry method for the determination of 5-fluorouracil in human plasma is described. The method involves a single extraction procedure with 10 ml of isopropanol-eth-er(20:80) solution and pentafluoro-benzylation. Samples were injected using an automatic injector, followed by separation on a nonpolar capillary column and detection with a mass selective detector(MSD). No en-dogeneous compounds were found to interfere. The detection limit, based upon an assayed plasma volume of 0.5, was 3 ng/ml. The extraction yield was found to be above 80%. Plasma 5-FU concentrations were det-ermined by this method in about 500 plasma samples from cancer patients undergoing treatment with 5-FU. This method is suitable for monitoring of 5-FU in plasma of cancer patients

  17. Improved method for the determination of hydroxymethylfurfural in baby foods using liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Gökmen, Vural; Senyuva, Hamide Z

    2006-04-19

    An improved analytical method for the rapid, reliable, and sensitive determination of hydroxymethylfurfural (HMF) in baby foods is described. It entailed aqueous extraction from food matrix with simultaneous clarification using Carrez I and II reagents, solid-phase extraction cleanup using Oasis HLB, and analysis by liquid chromatography-mass spectrometry. A narrow-bore column allowed fast chromatographic separation with good resolution of HMF and matrix coextractives. In positive atmospheric pressure chemical ionization conditions, precursor and compound-specific ions were sensitively detected in selected ion monitoring mode. Sample preparation with efficient cleanup followed by fast chromatographic analysis allowed the analysis to be completed in <20 min. Recovery ranged between 91.8 and 94.7% for spiking levels of 0.25, 1.0, and 5.0 mg/kg HMF in cereal-based baby foods. The method was shown to be successful when using liquid chromatography coupled to ultraviolet detection at 285 nm. PMID:16608199

  18. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air. PMID:24370860

  19. Determination of Morphine and Codeine in Human Urine by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xiaoqian Zhang

    2013-01-01

    Full Text Available A sensitive and selective gas chromatography-mass spectrometry (GC-MS method was developed and validated for the determination of morphine and codeine in human urine. The GC-MS conditions were developed. The analysis was carried out on a HP-1MS column (30 m × 0.25 mm, 0.25 μm with temperature programming, and Helium was used as the carrier gas with a flow rate of 1.0 mL/min. Selected ion monitoring (SIM mode was used to quantify morphine and codeine. The derivation solvent, temperature, and time were optimized. A mixed solvent of propionic anhydride and pyridine (5 : 2 was finally used for the derivation at 80°C for 3 min. Linear calibration curves were obtained in the concentration range of 25–2000.0 ng/mL, with a lower limit of quantification of 25 ng/mL. The intra- and interday precision (RSD values were below 13%, and the accuracy was in the range 87.2–108.5%. This developed method was successfully used for the determination of morphine and codeine in human urine for forensic identification study.

  20. Determination of terpenes in tequila by solid phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Peña-Alvarez, Araceli; Capella, Santiago; Juárez, Rocío; Labastida, Carmen

    2006-11-17

    Solid phase microextraction and capillary gas chromatography-mass spectrometry were used for the determination of seven terpenes in tequila. The method was selected based on the following parameters: coating selection (PA, PDMS, CW/DVB, and PDMS/DVB), extraction temperature, addition of salt, and extraction time profile. The extraction conditions were: PDMS/DVB fiber, Headspace, 100% NaCl, 25 degrees C extraction temperature, 30 min extraction time and stirring at 1200 rpm. The calibration curves (50-1000 ng/ml) for the terpenes followed linear relationships with correlation coefficients (r) greater than 0.99, except for trans,trans-farnesol (r = 0.98). RSD values were smaller than 10% confirmed that the technique was precise. Samples from 18 different trade brands of "Aged" tequila analyzed with the developed method showed the same terpenes in different concentrations. The analytical procedure used is selective, robust (more than 100 analyses with the same fiber), fast and of low-cost.

  1. New Developments in Liquid Chromatography Mass Spectrometry for the Determination of Micropollutants

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    Zoraida Sosa-Ferrera

    2012-01-01

    Full Text Available The combination of liquid chromatography (LC with mass spectrometry (MS in the environmental field has appeared as a valuable tool for the determination of micropollutants. Several groups of compounds have been considered as particularly relevant (e.g., pharmaceuticals, hormones and other endocrine-disrupting, personal care products and their metabolites, flame retardants, surfactants, and plasticizers, among others since the same ones are continuously being released in the environment mainly as a result of the manufacturing processes, the disposal of unused or expired products, and the excreta. Because these micropollutants are not completely removed in the environment, very specific and sensitive analytical procedures are needed for their identification and quantification. High performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS (or LC-MS2 and especially time-of-flight mass spectrometry (TOF/MS, has allowed that many environmental contaminants that are highly polar or nonvolatile or have a high molecular weight to be analyzed or identified. In this work we present an overview focused on the developments of liquid chromatography mass spectrometry applied to the analysis of the main classes of micropollutants in aqueous and solid environmental samples. Various aspects of methodologies based on these techniques, including sample preparation (extraction/preconcentration and matrix effects, are discussed.

  2. Enantiomeric determination of DOPA in dietary supplements containing Mucuna pruriens by liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Hasegawa, Takashi; Takahashi, Kazunaga; Fukiwake, Tomohide; Saijo, Masaaki; Motoki, Yuji

    2013-01-01

    We developed a simple and rapid liquid chromatography/mass spectrometry (LC/MS) method for the enantiomeric determination of DOPA in dietary supplements containing Mucuna pruriens. L- and D-DOPA were ultrasonically extracted with 1% formic acid aqueous solution. The isolated extracts were analyzed by LC/MS using a Crownpak CR (-) column at 30℃. The mass spectrometer was operated in the positive mode of electrospray ionization, and the mobile phase was aqueous formic acid (pH 2.0). L-DOPA-ring-d3 was used as an internal standard. The method was validated for a dietary supplement spiked with L- and D-DOPA at 50 and 500 μg/g, respectively, and the recoveries of the DOPA enantiomers were between 97.5% and 101.3%. Relative standard deviation values of repeatability and intermediate precision were less than 7%. The method was applied to 14 dietary supplements. L-DOPA was detected in these supplements in the range of 0.88-12.8 mg/unit. D-DOPA was not detected. PMID:24190293

  3. Determination of phthalate esters in teas and tea infusions by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Du, Liping; Ma, Lijuan; Qiao, Yang; Lu, Yan; Xiao, Dongguang

    2016-04-15

    Phthalate esters (PAEs), a group of environmental pollutants which are carcinogenic to human body, have been detected in teas. In this work, five PAEs in teas and tea infusions were quantitatively determined by a modified simultaneous distillation extraction (SDE) coupled with gas chromatography-mass spectrometry. After the optimization of SDE, the proposed method afforded a wide range of linearity and high linear regression coefficients with the limits of detection range of 0.24-3.72 μg/kg. The average recoveries were 79.83-116.67% for tea samples and 78.22-101.64% for tea infusions with all the relative standard deviations below 20%. The total content of five PAEs in teas was 1.135-3.734 mg/kg and the total dissolving ratio of five PAEs from tea to infusion was 19.05-28.07% for the selected tea samples. The risk assessment result of all the selected tea samples demonstrated that the population with the habit of drinking tea won't cause risk to human health.

  4. Determination of endogenous ethanol in blood and breath by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jones, A W; Mårdh, G; Anggård, E

    1983-01-01

    We describe methods for the determination of endogenous ethanol in biological specimens from healthy abstaining subjects. The analytical methods were headspace gas chromatography (GC) for plasma samples and gas chromatography-mass spectometry (GC/MS) with deuterium labelled species 2H3-ethanol and 2H5-ethanol as internal standards for breath analysis. Ethanol in rebreathed air was about 10% higher than in directly analysed end-expired alveolar air. Known volumes of rebreathed air were passed through a liquid-N2 freeze trap and the volatile constituents of breath were concentrated prior to analysis by GC or GC/MS. Besides endogenous ethanol, peaks were seen on the chromatograms for methanol, acetone and acetaldehyde as well as several as yet unidentified substances. The endogenous alcohols ethanol and methanol were confirmed from their mass chromatograms and the GC/MS profile also indicated the presence of endogenous propan-1-ol. The concentration of endogenous ethanol in plasma showed wide inter-subject variations ranging from below detection limits to 1.6 micrograms/ml (34.8 mumol/l) and with mean +/- SD of 0.39 +/- 0.45 micrograms/ml (8.5 +/- 9.8 mumol/l). We aim to characterise further the role of endogenous ethanol with the main focus on dynamic aspects such as the rate of formation and turnover.

  5. Determination of fipronil by solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Vílchez, J L; Prieto, A; Araujo, L; Navalón, A

    2001-06-01

    A method for the determination of trace amounts of the insecticide fipronil was developed using solid-phase microextraction-gas chromatography-mass spectrometry and selected ion monitoring. Fipronil was extracted with a fused-silica fiber coated with 85 microm polyacrylate. The effects of pH, ionic strength, sample volume, extraction and desorption times as well as the extraction temperature were studied. Lindane was used as an internal standard. The linear concentration range of application was 0.3-100 ng ml(-1) of fipronil, with a relative standard deviation of 9.5% (for a level of 50 ng ml(-1)) and a detection limit of 0.08 ng ml(-1). The method was applied to check the eventual existence of fipronil above this limit in water and soil samples from Granada (Spain) as well as in human urine samples. The method validation was completed with spiked matrix samples. The method can be applied as a monitoring tool for water, soil and urine, in the investigation of environmental and occupational exposure to fipronil.

  6. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    International Nuclear Information System (INIS)

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4 degree C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range

  7. Determining the amount of Acrylamide in Potato Chips Using Xanthydrol as a Derivative Representative with Gas Chromatography-Mass Spectrometry

    OpenAIRE

    Maryam Zokaei; Marzieh Kamankesh; Saeideh Shojaei; Abdorreza Mohammadi

    2016-01-01

    Background and Objectives: In the production process of foods rich in carbohydrates and some other foods containing precursors of acrylamide formation, there is the possibility of acrylamide creation, which is a mutagen and carcinogen material. This study aims to introduce and optimize a new method for determining acrylamide in potato chips using xanthydrol as a derivative representative with gas chromatography-mass spectrometry. Materials and Methods: Important factors in the derivatizat...

  8. Determination of seven pyrethroids and six pyrethrins in water by liquid chromatography/mass spectrometry

    Science.gov (United States)

    ccanccapa, alexander; Masia, Ana; Pico, Yolanda

    2016-04-01

    Pyrethroids are the synthetic analogues of pyrethrins which were developed as pesticides from the extracts of dried and powdered flower heads of Chrysanthemum cinerariaefolium. They are increasingly used in agriculture due to their broad biological activity and slow development of pest resistance. Contamination of fresh-water ecosystems appears either because of the direct discharge of industrial and agricultural effluents or as a result of effluents from sewage treatment works; residues can thus accumulate in the surrounding biosphere [1, 2]. These substances, mostly determined by gas chromatography mass spectrometry (GC-MS) can be difficult to analyse due to their volatility and degradability. The purpose of this study is, as an alternative, to develop a fast and sensitive multi-residue method for the target analysis of 7 pyrethroids and the 6 natural pyrethrins currently used in water samples by liquid chromatography tandem mass spectrometry (LC-MS/MS). The compounds included in the study were acrinathrin, etofenprox, cyfluthrin, esfenvalerate, cyhalothrin, cypermethrin and flumethrin as pyrethroids and a commercial mix of pyrethrins containing Cinerin I, Jasmolin I, pyrethrin I, cinerin II, jasmolin II, pyrethrins II in different percentages. As a preliminary step, the ionization and fragmentation of the compounds were optimized injecting individual solutions of each analyte at 10 ppm in the system, using a gradient elution profile of water-methanol both with 10 mM ammonium formate. The ESI conditions were: capillary voltage 4000 V, nebulizer15 psi, source temperature 300◦C and gas flow 10 L min-1. [M+H]+, [M+Na]+ ,[M+NH3]+ ,[M+NH4+]+ were tested as precursor ions. The most intense signal was for ammonium adduct for all compounds. The optimal fragmentor range for product ions were between 20 to 80 ev and the collision energy ranged between 5 to 86 ev. The efficiency of the method was tested in water samples from Turia River without any known exposure to

  9. Determination of cocaine in brazilian paper currency by capillary gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Enrico Di Donato

    2007-01-01

    Full Text Available The presence of illicit drugs such as cocaine and marijuana in US paper currency is very well demonstrated. However, there is no published study describing the presence of cocaine and/or other illicit drugs in Brazilian paper currency. In this study, Brazilian banknotes were collected from nine cities, extracted and analyzed by capillary gas chromatography/mass spectrometry, in order to investigate the presence of cocaine. Bills were extracted with deionized water followed by ethyl acetate. Results showed that 93% of the bills presented cocaine in a concentration range of 2.38-275.10 µg/bill.

  10. Miniscale Liquid-Liquid Extraction Coupled with Full Evaporation Dynamic Headspace Extraction for the Gas Chromatography/Mass Spectrometric Analysis of Polycyclic Aromatic Hydrocarbons with 4000-to-14 000-fold Enrichment.

    Science.gov (United States)

    Liew, Christina Shu Min; Li, Xiao; Lee, Hian Kee

    2016-09-20

    A new sample preparation approach of combining a miniscale version of liquid-liquid extraction (LLE), termed miniscale-LLE (msLLE), with automated full evaporation dynamic headspace extraction (FEDHS) was developed. Its applicability was demonstrated in the extraction of several polycyclic aromatic hydrocarbons (PAHs) (acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene) from aqueous samples. In the first step, msLLE was conducted with 1.75 mL of n-hexane, and all of the extract was vaporized through a Tenax TA sorbent tube via a nitrogen gas flow, in the FEDHS step. Due to the stronger π-π interaction between the Tenax TA polymer and PAHs, only the latter, and not n-hexane, was adsorbed by the sorbent. This selectivity by the Tenax TA polymer allowed an effective concentration of PAHs while eliminating n-hexane by the FEDHS process. After that, thermal desorption was applied to the PAHs to channel them into a gas chromatography/mass spectrometric (GC/MS) system for analysis. Experimental parameters affecting msLLE (solvent volume and mixing duration) and FEDHS (temperature and duration) were optimized. The obtained results achieved low limits of detection (1.85-3.63 ng/L) with good linearity (r(2) > 0.9989) and high enrichment factors ranging from 4200 to 14 100. The optimized settings were applied to the analysis of canal water sampled from an industrial area and tap water, and this methodology was compared to stir-bar sorptive extraction (SBSE). This innovative combined extraction-concentration approach proved to be fast, effective, and efficient in determining low concentrations of PAHs in aqueous samples.

  11. Determination of naphthenic acid profile in Ghana's Jubilee Oil using gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Crude oil is the life-blood of the global economy. Its importance stems from the fact that it is a base product for a wide variety of goods [Drugs, Plastics, Liquefied Petroleum Gas (LPG)]. The oil discovery (over 3 billion barrel reserves in hydrocarbon and gas), about 60 km offshore between the Deepwater Tano and Cape Three Points Block in South western Ghana is a valuable natural asset and it has the potential of boosting the Ghanaian economy. During petroleum processing, various waste products are generated. One of such products is Naphthenic acids (NA). Naphthenic acids are organic acids naturally occurring in crude oil and a constituent of waste associated with oil refinery. Naphthenic acids serve as biomarkers for identification of the source of crude oil. The presence of Naphthenic acid in the aquatic environment causes toxic effects due to their weak biodegradable nature; the toxicity of Naphthenic acids depends on the class of Naphthenic acids present in the crude oil. The study assessed the profile of Naphthenic acids in Ghana’s Jubilee crude oil using Low Resolution Electron Impact – Gas Chromatography Mass Spectrometry (LREI-GCMS) after isolation of Naphthenic acids in the Jubilee oil by a modified Kupchan’s Partitioning Process. The Mass Spectrometric (MS) Work Station Software was used for the identification of the Naphthenic acids present in the Jubilee crude oil. The quality of the Jubilee oil was also evaluated through the use of some key physico-chemical parameters [Total Acid Number (TAN), Sulphur Content, Viscosity, Pour Point, Flashpoint, Water Content and Densities] based on the American Standards for Testing and Materials (ASTM, 2007). The Total Acid Number was determined by Colorimetric Titration (ASTM D974); Sulphur Content by X-ray Fluorescent Spectrometry (ASTM D4294); Pour Point by the use of the SETA cloud and Pour Point Refrigerator Technique (ASTM D97); Viscosity by Gravity Timed Method (ASTM D445); Density by the Hydrometer

  12. Determination of constituents of essential oil from Angelica sinensis by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    WU Ming-jian; SUN Xian-jun; DAI Yuan-hui; GUO Fang-qiu; HUANG Lan-fang; LIANG Yi-zeng

    2005-01-01

    Gas chromatography-mass spectrometry (GC-MS) coupled with chemometric resolution upon two-dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.

  13. Gas chromatography/mass spectrometry for the determination of nitrosamines in red wine.

    Science.gov (United States)

    Lona-Ramirez, Fernando J; Gonzalez-Alatorre, Guillermo; Rico-Ramírez, Vicente; Perez-Perez, Ma Cristina I; Castrejón-González, Edgar O

    2016-04-01

    N-nitrosamines (NAms) are highly active carcinogens that have been detected in food and beverages. Currently certain studies report their presence in red wine, while others fail to detect their presence. In this study the head space solid phase micro-extraction technique coupled to gas chromatography-mass spectrometry (HS-SPME-GC-MS) was applied to quantify four NAms in different types of red wine. The technique was found to be a simple, precise, fast and environmentally friendly alternative for the quantification of volatile NAms. A factorial analysis was carried out to evaluate the influence of the parameters on the HS-SPME technique. This is the first study that such analysis has been reported and where NAms in red wine have been quantified using HS-SPME-GC-MS. The method was validated by calculating the linearity, limit of detection and quantification. Two of the four NAms analyzed were found to be present in red wine samples.

  14. Determination of Synthetic Cathinones in Urine Using Gas Chromatography-Mass Spectrometry Techniques.

    Science.gov (United States)

    Hong, Wei-Yin; Ko, Ya-Chun; Lin, Mei-Chih; Wang, Po-Yu; Chen, Yu-Pen; Chiueh, Lih-Ching; Shih, Daniel Yang-Chih; Chou, Hsiu-Kuan; Cheng, Hwei-Fang

    2016-01-01

    In recent years, the abuse of synthetic cathinones has increased considerably. This study proposes a method, based on gas chromatography/mass spectrometry (GC-MS), to analyze and quantify six synthetic cathinones in urine samples: mephedrone (4-MMC), methylone (bk-MDMA), butylone, ethylone, pentylone and methylenedioxypyrovalerone (MDPV). In our procedure, the urine samples undergo solid-phase extraction (SPE) and derivatization prior to injection into the GC-MS device. Separation is performed using a HP-5MS capillary column. The use of selective ion monitoring (SIM mode) makes it is good sensitivity in this method, and the entire analysis process is within 18 min. In addition, the proposed method maintains linearity in the calibration curve from 50 to 2,000 ng/mL (r(2) > 0.995). The limit of detection of this method is 5 ng/mL, with the exception of MDPV (20 ng/mL); the limit of quantification is 20 ng/mL, with the exception of MDPV (50 ng/mL). In testing, the extraction performance of SPE was between 82.34 and 104.46%. Precision and accuracy results were satisfactory MDMA. Our results demonstrate the efficacy of the proposed method in the identification of synthetic cathinones in urine, with regard to the limits of detection and quantification. This method is highly repeatable and accurate. PMID:26410364

  15. Determination of volatile components in cut tobacco with gas chromatography-mass spectrometry and chemometric resolution

    Institute of Scientific and Technical Information of China (English)

    HUANG Lan-fang; WU Ming-jian; SUN Xian-jun; ZHONG Ke-jun; GUO Zi-ming; DAI Yun-hui; HUANG Ke-long; GUO Fang-qiu

    2007-01-01

    Chromatography-mass spectrometry (GC-MS) was used to analyze the volatile components of cut tobacco samples with the help of heuristic evolving latent projections (HELP). After extracting with simultaneous distillation and extraction method, the volatile components in cut tobacco were detected by GC-MS. Then the obtained original two-dimensional data were resolved into pure mass spectra and chromatograms. The qualitative analysis was performed by similarity searches in the national institute of standards and technology(NIST) mass database with the obtained pure mass spectrum of each component and the quantitative results were obtained by calculating the volume of total two-way response. The accuracy of qualitative and quantitative results were greatly improved by using the two-dimensional comprehensive information of chromatograms and mass spectra. 107 of 141 separated constituents in the total ion chromatogram of the volatile components were identified and quantified, accounting for about 88.01% of the total content. The result proves that the developed method is powerful for the analysis of complex cut tobacco samples.

  16. Simultaneous Determination of Hexoestrol, Diethylstilbestrol, Estrone and 17-Beta-estradiol in Feed by Gas Chromatography-mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Huo Feng; Li Ning; Lin Xiao-Li

    2016-01-01

    A method was developed for the simultaneous determination of four kinds of estrogens (hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol) in feed by gas chromatography-mass spectrometry (GC-MS). After the sample was extracted by ethyl ether and cleaned-up on HLB phase extraction column, four kinds of estrogens were derived and quantified in gas chromatography-mass spectrometry. The results showed that the linear detectable ranged from 2.5 ng•mL-1 to 250 ng•mL-1 for hexoestrol and from 5 ng•mL-1 to 500 ng•mL-1 for three other estrogens with the correlation coefficients (R2) were no less than 0.990. The recoveries were in the range of 76.34%-96.33% and the relative standard deviation was no more than 22.7%. The limits of quantitation (LOQ) for all analytics were between 10 ug•kg-1 and 20 ug•kg-1. The method was accurate and sensitive and could meet the actual requirements for the analyses of feed samples.

  17. Capillary ion chromatography-mass spectrometry for simultaneous determination of glucosylglycerol and sucrose in intracellular extracts of cyanobacteria.

    Science.gov (United States)

    Fa, Yun; Liang, Wenhui; Cui, He; Duan, Yangkai; Yang, Menglong; Gao, Jun; Liu, Huizhou

    2015-09-15

    A capillary ion chromatography-mass spectrometry (MS) method was proposed to determine glucosylglycerol (GG), sucrose, and five other carbohydrates. MS conditions and make-up flow parameters were optimized. This method is accurate and sensitive for simultaneous analysis of carbohydrates, with mean correlation coefficients of determination greater than 0.99, relative standard deviation of 0.91-2.81% for eight replicates, and average spiked recoveries of 97.3-104.9%. Limits of detection of sodium adduct were obtained with MS detection in selected ion mode for GG (0.006mg/L), sucrose (0.02mg/L), and other carbohydrates (0.03mg/L). This method was successfully applied to determine GG and sucrose in intracellular extracts of salt-stressed cyanobacteria.

  18. Rapid-resolution liquid chromatography/mass spectrometry for determination and quantitation of polyphenols in grape berries.

    Science.gov (United States)

    Cavaliere, Chiara; Foglia, Patrizia; Gubbiotti, Riccardo; Sacchetti, Paolo; Samperi, Roberto; Laganà, Aldo

    2008-10-01

    A rapid-resolution liquid chromatography/mass spectrometric (RRLC/MS) method for detection and quantitation of polyphenols in grape berry skins and seeds has been developed. Pulp-free berry skins were treated with liquid nitrogen and ground; seeds were also ground. Then, 3 g of samples were extracted with 30 mL of a mixture of methanol/water/formic acid 70:30:1 (v/v/v) under sonication and 1 microL of the final extract was injected into two 100 x 2.1 mm i.d., 1.8 microm Zorbax Eclipse plus C18 columns connected in series. Compounds were fractionated using a gradient elution of acidified acetonitrile/methanol 50:50 (v/v)/water. Columns were thermostatted at 70 degrees C. MS was carried out on an Agilent 6410 QqQ instrument equipped with an electrospray ionization source. Positive and negative MS/MS product ion scans were used for compound identification, whereas positive full scan MS in the m/z range 200-1400 was used for quantitation. By means of mass spectra comparison, various flavonols, flavan-3-ols, anthocyanins and stilbenes were identified. Quantitation was performed by external calibration, and concentration values were corrected for matrix effect that was evaluated in separate experiments. Semi-quantitative estimation was performed for compounds for which standards were not commercially available. Recoveries ranged from 90-102% with relative standard deviation (RSD) quality control. The developed method was applied to analyze the polyphenol content of three Vitis vinifera table cultivars at physiological maturity and after proper preservation for 6 weeks. Results demonstrated that during preservation about half of the polyphenol content was lost. PMID:18819110

  19. 氟乙酰胺中毒个案的气相色谱-质谱检验%Determination of Fluoroacetamide by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    郑珲; 张春水; 欧阳津

    2004-01-01

    A method of the determination of fluoroacetamide in a poison case was developed. Fluoroacetamide was extracted from stomach tissue, then was derived by PFBBr and determined by gas chromatography mass spectrometry(GC/MS). The results provided scientific proof for the justice identification.

  20. Determining the amount of Acrylamide in Potato Chips Using Xanthydrol as a Derivative Representative with Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Maryam Zokaei

    2016-02-01

    Full Text Available Background and Objectives: In the production process of foods rich in carbohydrates and some other foods containing precursors of acrylamide formation, there is the possibility of acrylamide creation, which is a mutagen and carcinogen material. This study aims to introduce and optimize a new method for determining acrylamide in potato chips using xanthydrol as a derivative representative with gas chromatography-mass spectrometry. Materials and Methods: Important factors in the derivatization and measurement processes were optimized using the one-factor-at-a-time method. The peak areas were assumed as the GC-MS response to evaluate the extraction efficiency of acrylamide, and optimization for all tests was performed two times. Figures of merit of the proposed method were evaluated. The amount of acrylamide in four potato chips samples, obtained from the market in Tehran city, was determined using the proposed method. Results: The optimum amounts of effective parameters, including derivatization temperature at 25oC, derivatization time (40 min, xanthydrol volume (40 µL, extracted solvent volume (500 µL and pH=7 were determined. The figures of merit for the proposed method were at the ideal range. The maximum and minimum amounts of acrylamide in the chip samples were also measured. Conclusions: The performance and reliability of proposed method as a simple, efficient and rapid method for determining acrylamide in potato chip samples were demonstrated.

  1. Rapid determination of polysaccharides in BianTi Soft extract by spectrophotometry coupled with gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Minxia Zheng

    2010-01-01

    Full Text Available A simple approach for the rapid determination of polysaccharides in BianTi Soft Extract using spectrophotometry coupled with gas chromatography-mass spectrometry (GC-MS was developed. The mixed standard solution composed of D-glucose, D-mannose, galactose and D-xylose in different proportions (1.00: 1.01: 0.12: 0.05 was prepared according to the monosaccharide composition analysis of the polysaccharides by GC-MS. The determination of polysaccharides by UV-Vis spectrophotometer was performed after 35-min color reaction, in which 1 ml 5% phenol and 4 ml sulfate was used. The assay of the method validation has shown that the method was stable, reliable and feasible. Furthermore, the proposed method was successfully applied in the preparation procedure of BianTi Soft Extract, selecting out optimal decoction conditions and suitable decoction container. It suggests that the convenient method could be useful for the quality control of BianTi Soft Extract. Meanwhile, it may be an alternative for polysaccharides determination of other formulations.

  2. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review.

    Science.gov (United States)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. PMID:27566339

  3. Simultaneous Determination of 10 Photoinitiators in Milk by Solid-Phase Microextraction Coupled with Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Liu, Pengyan; Zhao, Chunxia; Zhang, Yajing; Chen, Yanjie

    2016-05-01

    Photoinitiators (PIs) are widely used in food packaging materials, can migrate easily from packaging materials to food, and cause food contamination. It is essential to establish a method of determining PIs residues in food. A new method for simultaneously determining 10 kinds of PIs in milk has been established by using solid-phase microextraction (SPME) combined with a simple method of protein precipitation as the pretreatment approach and gas chromatography/mass spectrometry as the detecting technique. The limits of detection for 10 PIs in different milks were between 0.05 and 1.4 μg/L (skimmed milk), between 0.07 and 2.2 μg/L (semi-skimmed milk), between 0.11 and 4.4 μg/L (whole milk), respectively. The recoveries were from 71.5% to 133.5%, and the relative standard deviations were less than 15%. Twelve kinds of packed milk with different brands and fat contents were determined using this method. PMID:27010861

  4. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review.

    Science.gov (United States)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS.

  5. METHOD 530 DETERMINATION OF SELECT SEMIVOLATILE ORGANIC CHEMICALS IN DRINKING WATER BY SOLID PHASE EXTRACTION AND GAS CHROMATOGRAPHY/ MASS SPECTROMETRY (GC/MS)

    Science.gov (United States)

    1.1. This is a gas chromatography/mass spectrometry (GC/MS) method for the determination of selected semivolatile organic compounds in drinking waters. Accuracy and precision data have been generated in reagent water, and in finished ground and surface waters for the compounds li...

  6. Dual dispersive liquid-liquid microextraction for determination of phenylpropenes in oils by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Tsai, Chia-Ju; Li, Jih-Heng; Feng, Chia-Hsien

    2015-09-01

    A novel, simple and quick sample preparation method was developed and used for pre-concentration and extraction of six phenylpropenes, including anethole, estragole, eugenol, methyl eugenol, safrole and myristicin, from oil samples by dual dispersive liquid-liquid microextraction. Gas chromatography-mass spectrometry was used for determination and separation of compounds. Several experimental parameters affecting extraction efficiency were evaluated and optimized, including forward-extractant type and volume, surfactant type and concentration, water volume, and back-extractant type and volume. For all analytes (10-1000ng/mL), the limits of detection (S/N≧3) ranged from 1.0 to 3.0ng/mL; the limits of quantification (S/N≧10) ranged from 2.5 to 10.0ng/mL; and enrichment factors ranged from 3.2 to 37.1 times. Within-run and between-run relative standard deviations (n=6) were less than 2.61% and less than 4.33%, respectively. Linearity was excellent with determination coefficients (r(2)) above 0.9977. The experiments showed that the proposed method is a simple, effective, and environmentally friendly method of analyzing phenylpropenes in oil samples.

  7. [Simultaneous determination of 16 organic acids in feed additives by on-line enrichment and ion chromatography-mass spectrometry].

    Science.gov (United States)

    Xiong, Zhiyu; Dong, Ying; Zhou, Hongbin; Yu, Yang; Li, Jing; Sun, Li

    2014-02-01

    A novel analytical method for simultaneous determination of sixteen organic acids by on-line enrichment and ion chromatography-mass spectrometry (IC-MS) was developed. Online enrichment and separation of the organic acids were performed by ion chromatography on a homemade enrichment column and a homemade separation column. The qualitative and quantitative analyses of the organic acids were performed by mass spectrometry in selected ion monitoring (SIM) mode on the basis of atmospheric pressure chemical ionization (APCI) source in negative mode. The sample of 200 microL was injected for the analysis, and the on-line enrichment time was 3 min. The sodium hydroxide solution was used as a gradient elution system. The two columns made it possible to have a low limit of detection due to the good enrichment and separation capability. The sixteen organic acids were separated completely within 30 min. All curves showed good linearity within the test concentration ranges. The limits of detection (LODs) were between 0.01 and 0.22 mg/L, and the average recoveries were between 70.6% and 110.8%. The relative standard deviations (RSDs) were less than 6.3%. The results indicate that this method is simple, rapid, sensitive and accurate for the determination of the organic acids in feed additives.

  8. Determination of Panthenol, Cholecalciferol and Tocopherol in Cosmetic Products by Gas Chromatography-Mass Spectrometry in SIM Mode.

    Science.gov (United States)

    Jeong, H J; Lee, M H; Ro, K W; Hur, C W; Kim, J W

    1999-02-01

    A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry (GC-MS) has been developed. Three vitamins (panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran (ThF), and silylated with bis-trimethylsilyltri-fluoroacetamide- trichloromethylsilane (BSTFA). Silylated vitamins were separated on a fused-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring (SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50 pg of panthenol, 285 pg of cholecalciferol and 130 pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product (i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, convenient and exact determination of panthenol, cholecalciferol and tocopherol. PMID:18505529

  9. [Determination of bisphenol A from toys and food contact materials by derivatization and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Gao, Yonggang; Zhang, Yanyan; Gao, Jianguo; Zhang, Huiling; Zheng, Lisha; Chen, Jing

    2012-10-01

    A method was developed for the determination of bisphenol A (BPA) in toys and food contact materials. The BPA was extracted with Soxhlet extraction method from the sample and reacted with acetic anhydride. The final product was determined by gas chromatography-mass spectrometry (GC-MS). To achieve the optimum derivatization performance, the derivatization time and dosage of derivatization reagent etc. were investigated. Under the optimized experimental conditions, the final product was stable and the peak shape was good. The linearity of the derivative was good in the range of 0.05 to 50 mg/L with the correlation coefficient (r2) above 0.999. The recoveries ranged from 80% to 93% at the spiked levels of 0.05, 1.00, 10.00 mg/kg with the relative standard deviations (RSDs) less than 3.7%. The limit of detection (S/N = 3) was 10 microg/kg. The method is accurate and has high recovery. The method is suitable for the inspection of bisphenol A in toys and food contact materials.

  10. [Determination of short chain chlorinated paraffins in leather products by solid phase extraction coupled with gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhang, Weiya; Wan, Xin; Li, Lixia; Wang, Chengyun; Jin, Shupei; Xing, Jun

    2014-10-01

    The short chain chlorinated paraffins (SCCPs) are the additives frequently used in the leather production in China, but they have been put into the list of forbidden chemicals issued by European Union recently. In fact, there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thor- oughly separated from the analyte of the SCCPs on a home-made solid phase extraction (SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chloride (2:1, v/v). With this method, the recoveries for the SCCPs spiked in the real leather samples varied from 90.47% to 99.00% with the relative standard deviations (RSDs) less than 6.7%, and the limits of detection (LODs) were between 0.069 and 0.110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.

  11. Simultaneous determination of 76 micropollutants in water samples by headspace solid phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martínez, C; Ramírez, N; Gómez, V; Pocurull, E; Borrull, F

    2013-11-15

    This study focuses on the development of an analytical method based on headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of 76 micropollutants in water samples. The selected micropollutants include volatile organic compounds (VOCs) (e.g. chlorobenzenes, chloroalkanes), endocrine disrupting compounds (EDCs) (e.g. bisphenol A and tributyl phosphate), odour compounds (e.g. limonene, phenol), fragrance allergens (e.g. geraniol, eugenol) and some pesticides (e.g. heptachlor, terbutryn). The experimental conditions affecting their extraction, such as the type of fibre, temperature and time of extraction, sample volume and ionic strength of the samples were optimized using HS-SPME. The method showed good linear range, reproducibility between days, repeatability and low detection limits (at ng L(-1) levels). The validated method has been applied to determine the target organic micropollutants in aqueous samples from different experimental research units of surface water, sea water, waste water and those effluents of advance membrane treatments. The optimized method showed good performance in the different types of samples studied. The analysis revealed the presence of several micropollutants at concentrations between 20 and 5000 μg L(-1), such as ethylbenzene, o-xylene, p-isopropilbenzene, D-limonene, citral and isoeugenol, due to the fact that these species are commonly used in domestic and industrial applications. PMID:24148498

  12. Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Xie Zhiyong [GKSS Research Centre, Institute for Coastal Research, Department of Environmental Chemistry, Max-Planck-Str. 1, D-21502 Geesthacht (Germany) and Johann Wolfgang Goethe-University Frankfurt at Main, Institute of Atmospheric and Environmental Sciences, Department of Analytical Environmental Chemistry, Georg-Voigt-Str. 14, 60054 Frankfurt (Germany)]. E-mail: zhiyong.xie@gkss.de; Ebinghaus, Ralf [GKSS Research Centre, Institute for Coastal Research, Department of Environmental Chemistry, Max-Planck-Str. 1, D-21502 Geesthacht (Germany); Lohmann, Rainer [Graduate School of Oceanography, University of Rhode Island, Narragansett, RI 02882-1197 (United States); Heemken, Olaf [LAVES, Philosophenweg 36/38, D-26121 Oldenburg (Germany); Caba, Armando [GKSS Research Centre, Institute for Coastal Research, Department of Environmental Chemistry, Max-Planck-Str. 1, D-21502 Geesthacht (Germany); Puettmann, Wilhelm [Johann Wolfgang Goethe-University Frankfurt at Main, Institute of Atmospheric and Environmental Sciences, Department of Analytical Environmental Chemistry, Georg-Voigt-Str. 14, 60054 Frankfurt (Germany)

    2007-02-19

    A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79 {+-} 1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC-MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pg m{sup -3} and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pg m{sup -3}) to 0.85 pg m{sup -3}. A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential.

  13. Determination of seventeen polar/thermolabile pesticides in apples and apricots by liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Zrostlíková, Jitka; Hajslová, Jana; Kovalczuk, Tomás; Stĕpán, Radim; Poustka, Jan

    2003-01-01

    A simple liquid chromatography/mass spectrometry (LC/MS) approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated. The group of pesticides comprised benzimidazoles and azoles (carbendazim, thiabendazole, imazalil, propiconazole, prochloraz, epoxiconazole, flusilazole, tebuconazole, bitertanol); N-methylcarbamates (carbaryl, carbofuran, methiocarb); and phenylureas and benzoylphenylureas (linuron, diflubenzuron, triflumuron, teflubenzuron, flufenoxuron). Matrixes (apple, apricot) were extracted with acetonitrile and crude extracts were cleaned up by solid-phase extraction (SPE) using either mixed cation exchange or hydrophilic lipophilic balance cartridges. LC separation of pesticides was performed on a reversed-phase column, Discovery C18. Electrospray ionization and ion trap MS/MS detection were applied. For most pesticides, overall recoveries ranged from 75 to 122%, and repeatability (as relative standard deviation) from 5 repetitive determinations of recovery ranged from 3 to 21%. Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step. Limits of detection were 0.1-3 microg/kg for benzimidazole and azole fungicides and carbamate insecticides. For urea insecticides, detection limits were slightly higher (3-10 microg/kg). PMID:12852583

  14. Determination of organotin compounds in-water by headspace solid phase microextraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Chou, Chi-Chi; Lee, Maw-Rong

    2005-01-28

    This investigation evaluates headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) to determine trace levels of organotins in water. The organotins were derivatized in situ with sodium tetraethylborate and adsorbed on a poly(dimethysiloxane) (PDMS)-coated fused silica fiber. The SPME experimental procedures to extract organotins in water were at pH 5, with extraction and derivatization simultaneously at 45 degrees C for 30 min in a 2% sodium tetraethylborate solution and a sample solution volume in the ratio of 1:1, and desorption in the splitless injection port of the GC at 260 degrees C for 2 min. Detection limits are determined to be in the low ng/L range. According to the analysis, the linearity range is from 10 to 10,000 ng/L with R.S.D. values below 12% except triphenyltin (24%). The proposed method was tested by analyzing surface seawater from the harbors on the Taiwanese coast for organotins residues. Some organotins studied were detected in the analyzed samples. Results of this study demonstrate the adequacy of the headspace SPME-GC-MS method for analyzing organotins in sea water samples. PMID:15729814

  15. Determination of daminozide in apples and apple leaves by liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Mol, H.G.J.; Dam, R.C.J. van; Vreeken, R.J.; Steijger, O.M.

    1999-01-01

    A straightforward and efficient method was developed for the determination of intact daminozide in apples and apple leaves. After extraction with methanol and a clean-up step using a graphitized carbon cartridge, the extract was analysed by ion-trap liquid chromatography-tandem mass spectrometry (LC

  16. New Developments in Liquid Chromatography Mass Spectrometry for the Determination of Micropollutants

    OpenAIRE

    Zoraida Sosa-Ferrera; Cristina Mahugo-Santana; José Juan Santana-Rodríguez

    2012-01-01

    The combination of liquid chromatography (LC) with mass spectrometry (MS) in the environmental field has appeared as a valuable tool for the determination of micropollutants. Several groups of compounds have been considered as particularly relevant (e.g., pharmaceuticals, hormones and other endocrine-disrupting, personal care products and their metabolites, flame retardants, surfactants, and plasticizers, among others) since the same ones are continuously being released in the environment mai...

  17. Perchloroethylene Analysis by Chemical Oxidation and Determination of Intermediate Products by Gas Chromatography, Mass Spectrometry

    OpenAIRE

    Sadeghi, M. (PhD; Naddafi, K. (PhD; Nabizadeh, R. (PhD

    2014-01-01

    Background and Objective: Perchloroethylene (PCE) is a chlorinated hydrocarbon used as a solvent in many industrial processes. In contaminated water and soil a great deal of PCE is found. This study aimed to determine the rate of decomposition of PCE occurred after advanced oxidation. Material and Methods: In this descriptive-analytic study conducted (2011) in public health faculty of Tehran University of medical sciences, gas chromatographic was used to measure PCE and gas chromatography - m...

  18. Simultaneous determination of five anti-epilepsy drugs in human plasma using liquid chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    STEFANIE; WeiBig

    2010-01-01

    A new liquid chromatography-mass spectrometry method for the determination of carbamazepine,clonazepam,alprazolam,estazolam and phenytoin in human plasma has been developed by using diazepam as an internal standard.Chromatographic separation was performed on a Zorbax SB-C18 column(30 mm × 2.1 mm,3.5 ?m) with a mobile phase consisting of methanol and aqueous 25 mM ammonium acetate using gradient elution.A diethyl ether extraction method was used for the extraction of five anti-epilepsy drugs.The final extract was injected for analysis by LC-MS/MS.The method was validated within the concentration range of 50-5000 ng mL-1 for five anti-epilepsy drugs.The precision of the assay(RSD%) was less than 10% at all concentration levels within the tested range.The method recoveries for all samples were more than 90%.The results indicate that the method is specific,sensitive and accurate,and suitable to study the pharmacokinetics,to adjust the dosage for individual administration,and to monitor the drug-concentration and drug abuse of the five anti-epilepsy drugs.

  19. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  20. Determining the Levels of Volatile Organic Pollutants in Urban Air Using a Gas Chromatography-Mass Spectrometry Method

    Directory of Open Access Journals (Sweden)

    Simona Nicoara

    2009-01-01

    Full Text Available The paper presents the application of a method based on coupled gas chromatography-mass spectrometry, using an isotopically labelled internal standard for the quantitative analysis of benzene (B, toluene (T, ethyl benzene (E, and o-, m-, p-xylenes (X. Their atmospheric concentrations were determined based on short-term sampling, in different sites of Cluj-Napoca, a highly populated urban centre in N-W Romania, with numerous and diversified road vehicles with internal combustion engines. The method is relatively inexpensive and simple and shows good precision and linearity in the ranges of 7–60 μg/m3 (B, 13–90 μg/m3 (T, 7–50 μg/m3 (E, 10–70 μg/m3 (X-m,p, and 20–130 μg/m3 (X-o. The limits of quantitation/detection of the method LOQ/LOD are of 10/5 μg/m3 (Xo, 5/3 μg/m3 (B, E, X-m,p, and of 3/1 μg/m3 (T, respectively.

  1. Simultaneous enantioselective determination of amphetamine and congeners in hair specimens by negative chemical ionization gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martins, Liliane; Yegles, Michel; Chung, Heesun; Wennig, Robert

    2005-10-15

    Enantioselective quantification of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA) enantiomers in hair using gas chromatography-mass spectrometry (GC-MS) is described. Hair specimens were digested with 1M sodium hydroxide at 100 degrees C for 30 min and extracted by a solid phase procedure using Cleanscreen ZSDAU020. Extracted analytes were derivatised with (S)-heptafluorobutyrylprolyl chloride and the resulting diastereoisomers were quantified by GC-MS operating in the negative chemical ionization mode. Extraction yields were between 73.0 and 97.9%. Limits of detection varied in the range of 2.1-45.9 pg/mg hair, whereas the lowest limits of quantification varied between 4.3 and 91.8 pg/mg hair. Intra- and inter-assay precision and respective accuracy were acceptable. The enantiomeric ratios (R versus S) of AM, MA, MDA, MDMA and MDEA were determined in hair from suspected amphetamine abusers. Only MA and AM enantiomers were detectable in this collective and the quantification data showed in most cases higher concentrations of (R)-MA and (R)-AM than those of the corresponding (S)-enantiomers. PMID:16154523

  2. Molecular species composition of plant cardiolipin determined by liquid chromatography mass spectrometry.

    Science.gov (United States)

    Zhou, Yonghong; Peisker, Helga; Dörmann, Peter

    2016-07-01

    Cardiolipin (CL), an anionic phospholipid of the inner mitochondrial membrane, provides essential functions for stabilizing respiratory complexes and is involved in mitochondrial morphogenesis and programmed cell death in animals. The role of CL and its metabolism in plants are less well understood. The measurement of CL in plants, including its molecular species composition, is hampered by the fact that CL is of extremely low abundance, and that plants contain large amounts of interfering compounds including galactolipids, neutral lipids, and pigments. We used solid phase extraction by anion exchange chromatography to purify CL from crude plant lipid extracts. LC/MS was used to determine the content and molecular species composition of CL. Thus, up to 23 different molecular species of CL were detected in different plant species, including Arabidopsis, mung bean, spinach, barley, and tobacco. Similar to animals, plant CL is dominated by highly unsaturated species, mostly containing linoleic and linolenic acid. During phosphate deprivation or exposure to an extended dark period, the amount of CL decreased in Arabidopsis, accompanied with an increased degree in unsaturation. The mechanism of CL remodeling during stress, and the function of highly unsaturated CL molecular species, remains to be defined. PMID:27179363

  3. Improved sensitivity gas chromatography-mass spectrometry determination of parabens in waters using ionic liquids.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2016-01-01

    A new procedure for the introduction of ionic liquid samples in gas chromatography (GC) is proposed. This procedure, based on microvial insert thermal desorption, allows the direct analysis of the compounds preconcentrated by ionic liquid based liquid-liquid microextraction (IL-LLME) using the combination of a thermal desorption unit (TDU) and a programmed temperature vaporization injector (PTV). Two different IL-LLME methodologies, one based on the formation of a microdroplet emulsion by dispersive liquid-liquid microextraction (DLLME) and other through ultrasound-assisted emulsification microextraction (USAEME) were studied and evaluated. IL-DLLME proved advantageous and consequently, it was adopted for preconcentration purposes. This easy to apply approach was used for the determination of five parabens (methyl-, ethyl-, propyl-, butyl- and isobutyl paraben) in swimming pool waters, after in situ acetylation. The optimized conditions of TDU/PTV allowed the analytes contained in 20 µL of the enriched IL to be transferred to the capillary column. Quantification of the samples was carried out against aqueous standards, and quantification limits of between 4.3 and 8.1 ng L(-1) were obtained, depending on the compound. Concentrations of between 9 and 47 ng L(-1) for some analytes were obtained in the analysis of ten samples. PMID:26695305

  4. Determination of omeprazole and its metabolites in human plasma by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Kanazawa, Hideko; Okada, Akiko; Matsushima, Yoshikazu; Yokota, Hiromitsu; Okubo, Shigeo; Mashige, Fumiko; Nakahara, Kazuhiko

    2002-03-01

    Omeprazole is a benzimidazole compound that acts as a proton-pump inhibitor. Because the metabolism of omeprazole is mainly catalyzed by cytochrome P-450 (CYP) 3A4 and CYP2C19. the genetic polymorphism of CYP2C19 could be of clinical concern in the treatment of acid-related diseases with omeprazole. Therefore, a reliable method for omeprazole phenotyping is desirable in clinical situations. This study has demonstrated the determination of omeprazole and its metabolites in human plasma by liquid chromatography-three-dimensional quadrupole mass spectrometry with a sonic spray ionization interface. The analytical column was YMC-Pack Pro C18(50x2.0 mm I.D.) using acetonitrile-50 mM ammonium acetate (pH 7.25) (1:4) at a flow-rate of 0.2 ml/min. The drift voltage was 30 V. The sampling aperture was heated at 110 degrees C and Shield temperature was 230 degrees C. In the mass spectrum, the molecular ions of omeprazole, hydroxyomeprazole and omeprazole sulfone were clearly observed as base peaks. This method is sufficiently sensitive and accurate for pharmacokinetic studies of omeprazol. PMID:11999727

  5. Determination of fenbendazole and oxfendazole in liver and muscle using liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Blanchflower, W J; Cannavan, A; Kennedy, D G

    1994-06-01

    A method has been developed for the determination of the anthelmintics fenbendazole and oxfendazole in liver and muscle samples using liquid chromatography-thermospray mass spectrometry (LC-MS). The samples were homogenized with water, sonicated with methanol and centrifuged. The supernatants were washed with light petroleum and extracted with diethyl ether-ethyl acetate. The extracts were evaporated to dryness, dissolved in mobile phase and injected into the LC-MS system. Fenbendazole and oxfendazole were measured separately using two different mobile phases. Single-ion monitoring of the positive ion at m/z 300 was used for fenbendazole and of m/z 316 for oxfendazole. The detection limits for the assay were 0.05 microgram g-1 for fenbendazole and 0.1 microgram g-1 for oxfendazole. The mean recoveries were 91% for fenbendazole and 86% for oxfendazole. The assay has been used for statutory testing purposes and for measuring the levels of fenbendazole and oxfendazole in liver and muscle from sheep after dosing with a commercial anthelmintic containing fenbendazole.

  6. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle L.; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  7. Determination of alkyl amines in atmospheric aerosol particles: a comparison of gas chromatography-mass spectrometry and ion chromatography approaches

    Directory of Open Access Journals (Sweden)

    R.-J. Huang

    2014-03-01

    Full Text Available In recent years low molecular weight alkyl amines have been recognized to play an important role in particle formation and growth in the lower atmosphere. However, major uncertainties are associated with their atmospheric processes, sources and sinks, mostly due to the lack of ambient measurements and the difficulties in accurate quantification of alkyl amines at trace level. In this study, we present the evaluation and optimization of two analytical approaches, i.e., gas chromatography-mass spectrometry (GC-MS and ion chromatography (IC, for the determination of alkyl amines in aerosol particles. Alkyl amines were converted to carbamates through derivatization with isobutyl chloroformate for GC-MS determination. A set of parameters affecting the analytical performances of the GC-MS approach, including reagent amount, reaction time and pH value, was evaluated and optimized. The accuracy is 84.3–99.1%, and the limits of detection obtained are 1.8–3.9 pg. For the IC approach, a solid phase extraction (SPE column was used to separate alkyl amines from interfering cations before IC analysis. 1–2% (v/v of acetone (or 2–4% (v/v of acetonitrile was added to the eluent to improve the separation of alkyl amines on the IC column. The limits of detection obtained are 2.1–15.9 ng and the accuracy is 55.1–103.4%. The lower accuracy can be attributed to evaporation losses of amines during the sample concentration procedure. Measurements of ambient aerosol particle samples collected in Hong Kong show that the GC-MS approach is superior to the IC approach for the quantification of primary and secondary alkyl amines due to its lower detection limits and higher accuracy.

  8. Introducing Students to Gas Chromatography-Mass Spectrometry Analysis and Determination of Kerosene Components in a Complex Mixture

    Science.gov (United States)

    Pacot, Giselle Mae M.; Lee, Lyn May; Chin, Sung-Tong; Marriott, Philip J.

    2016-01-01

    Gas chromatography-mass spectrometry (GC-MS) and GC-tandem MS (GC-MS/MS) are useful in many separation and characterization procedures. GC-MS is now a common tool in industry and research, and increasingly, GC-MS/MS is applied to the measurement of trace components in complex mixtures. This report describes an upper-level undergraduate experiment…

  9. THE DETERMINATION OF DELTA-5-ANDROSTENEDIOL AND ITS SULFATE IN SERUM AND URINE BY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

    NARCIS (Netherlands)

    DIKKESCHEI, LD; WOLTHERS, BG; WILLEMSE, PHB; VANDERPOL, H; DERUYTERBUITENHUIS, AW; NAGEL, GT

    1993-01-01

    OBJECTIVES We developed an assay for delta-5-androstenediol (adiol) and delta-5-androstenediol-3-sulphate (adiol-3S) in serum and adiol and total adiol sulphate (adiol-S) in urine. DESIGN An analytical procedure using HPLC and gas chromatography-mass spectrometry was devised and tested for its relia

  10. Determination of thyroid hormones in mouse tissues by isotope-dilution microflow liquid chromatography-mass spectrometry method.

    Science.gov (United States)

    De Angelis, Meri; Giesert, Florian; Finan, Brian; Clemmensen, Christoffer; Müller, Timo D; Vogt-Weisenhorn, Daniela; Tschöp, Matthias H; Schramm, Karl-Werner

    2016-10-15

    Thyroid hormones (THs) play a critical role in the regulation of many biological processes such as growth, metabolism and development both in humans and wildlife. In general, TH levels are measured by immunoassay (IA) methods but the specificity of the antibodies used in these assays limits selectivity. In the last decade, several analytical methods using liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (LC-MS/MS) have been developed to measure THs. These new techniques proved to be more accurate than the IA analysis and they were widely used for the determination of TH level in different human and animal tissues. A large part of LC-MS/MS methods described in literature employed between 200 and 500mg of sample, however this quantity can be considered too high especially when preclinical studies are conducted using mice as test subjects. Thus an analytical method that reduces the amount of tissue is essential. In this study, we developed a procedure for the analysis of six THs; L-thyroxine (T4), 3,3',5-triiodo-l-thyronine (T3), 3,3',5'-triiodo-l-thyronine (rT3), 3,5-diiodo-l-thyronine (rT2), 3,3'-diiodo-l-thyronine (T2), 3-iodo-l-thyronine (T1) using isotope ((13)C6-T4, (13)C6-T3, (13)C6-rT3, (13)C6-T2) dilution liquid chromatography-mass spectrometry. The major difference with previously described methods lies in the utilization of a nano-UPLC (Ultra Performance Liquid Chromatography) system in micro configuration. This approach leads to a reduction compared to the published methods, of column internal diameter, flow rate, and injected volume. The result of all these improvements is a decrease in the amount of sample necessary for the analysis. The method was tested on six different mouse tissues: liver, heart, kidney, muscle, lung and brown adipose tissue (BAT). The nano-UPLC system was interfaced with a quadrupole time-of-flight mass spectrometer (Q-TOF2-MS) using the positive ion mode electrospray ionization. In our analytical method

  11. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine:Method validation and application to real samples

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    A fast screening protocol was developed for the simultaneous determination of nine antiestrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/ mass spectrometry (...

  12. Determination of N-acetyl-S-(N-methylcarbamoyl)cysteine (AMCC) in the general population using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Käfferlein, H U; Angerer, J

    1999-10-01

    Carbamoylation of glutathione, peptides and DNA is thought to be one of the most important reactions occurring in an organism after exposure to nitrosoureas, methylformamides or isocyanates. The carcinogenic effects of carbamoylation are not yet fully clarified. Although carbamoylation is known to occur after occupational exposure, it has never been reported in the general population. To clarify the situation, we investigated the levels of N-acetyl-S-(N-methylcarbamoyl)cysteine (AMCC) in urine samples from persons without occupational exposure using a sensitive and specific method (gas chromatography-mass spectrometry, GC-MS). AMCC is the degradation product of N-methylcarbamoylated glutathione. The clean-up procedure of urine samples includes two liquid-liquid extraction steps and solid phase extraction using a cation-exchange resin to separate AMCC from other urinary components. N,N-Dimethylpropionic acid amide (DMPA) is used as internal standard. During the preparation of the samples, AMCC is converted to ethyl-N-methylcarbamate (EMC) in the presence of anhydrous potassium carbonate (K2CO3) and ethanol. The reliability and accuracy of this method have been proven in detail. The relative standard deviation for the within-series imprecision for three different concentrations was determined to be between 10.9% and 14.3%, while the relative standard deviation for the between-day imprecision was between 11.3% and 14.8%. The mean recovery for AMCC was determined to be between 79.2% and 85.6%. The limit of detection for the simultaneous measurement of two fragment masses was 30 micrograms L-1. Using this GC-MS method, we analysed urine samples from 42 individuals of the general population in order to determine their urinary excretion of AMCC. It was identified in 40 samples. The mean concentration was 40 micrograms L-1. AMCC can be formed in two ways. The first possibility is the dietary intake of isothiocyanates, especially methyl isothiocyanate, which is a component

  13. Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Margalho, Cláudia; Castanheira, Alice; Real, Francisco Corte; Gallardo, Eugenia; López-Rivadulla, Manuel

    2016-05-01

    Despite worldwide efforts aiming to ban the marketing and subsequent abuse of psychoactive substances such as synthetic cathinones and phenethylamines, there has been an alarming growth of both in recent years. Different compounds similar to those already existing are continuously appearing in the market in order to circumvent the legislation. An analytical methodology has been validated for qualitative and quantitative determinations of D-cathine (D-norpseudoehedrine), ephedrine, methcathinone, 1-(4-methoxyphenyl)-propan-2-amine (PMA), mephedrone, methedrone, 2,5-dimethoxy-4-methylamphetamine (DOM), 4-bromo-2,5-dimethoxyamphetamine (DOB), 2,5-dimethoxyphenethylamine (2C-H), 4-bromo-2,5-dimethoxyphenethylamine (2C-B), 4-iodo-2,5-dimethoxyphenethylamine (2C-I), 2-[2,5-dimethoxy-4-(ethylthio)phenyl]ethanamine (2C-T-2), 2,5-dimethoxy-4-isopropylthiophenethylamine (2C-T-4) and 2-[2,5-dimethoxy-4-(propylthio)phenyl]ethanamine (2C-T-7), in low volumes of vitreous humor (100 μL), pericardial fluid (250 μL) and whole blood (250 μL), using deutered amphetamine, ephedrine and mephedrone as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantification, intra- and interday precision and trueness, recovery and stability. The method included mixed-mode solid phase extraction, followed by microwave fast derivatization and analysis by gas chromatography-mass spectrometry operated in selected ion monitoring mode. The procedure was linear between 5 and 600 ng/mL, with determination coefficients higher than 0.99 for all analytes. Intra- and interday precision ranged from 0.1 to 13.6%, while accuracy variability was within 80-120% interval from the nominal concentration at all studied levels. The extraction efficiencies ranged from 76.6 to 112.8%. Stability was considered acceptable for all compounds in the studied matrices. The developed assay was applied to authentic samples of the Laboratory of Chemistry and Forensic

  14. Flavonoid content and antioxidant capacity of spinach genotypes determined by high-performance liquid chromatography/mass spectrometry

    Science.gov (United States)

    Flavonoids in different spinach genotypes were separated, identified, and quantified by a high-performance liquid chromatographic method with photodiode array and mass spectrometric detection. The antioxidant capacities of the genotypes were also measured using two antioxidant assays - oxygen radica...

  15. Identification of alkylated phosphates by gas chromatography-mass spectrometric investigations with different ionization principles of a thermally aged commercial lithium ion battery electrolyte.

    Science.gov (United States)

    Weber, Waldemar; Kraft, Vadim; Grützke, Martin; Wagner, Ralf; Winter, Martin; Nowak, Sascha

    2015-05-15

    The thermal aging process of a commercial LiPF6 based lithium ion battery electrolyte has been investigated in view of the formation of volatile phosphorus-containing degradation products. Aging products were analyzed by GC-MS. Structure determination of the products was performed by support of chemical ionization MS in positive and negative modes. A fraction of the discovered compounds belongs to the group of fluorophosphates (phosphorofluoridates) which are in suspect of potential toxicity. This is well known for relative derivatives, e.g. diisopropyl fluorophosphate. Another fraction of the identified compounds belongs to the group of trialkyl phosphates. These compounds may provide a positive impact on the thermal and electrochemical performance of Li-based batteries as repeatedly described in the literature.

  16. GC- MS法同时测定食品中35种常见的农残%Simultaneous Determination of 35 Kinds of Pesticide Residues in Food by Gas Chromatography - mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    沈平; 潘磊; 彭进; 谢朝梅; 谢燕湘; 刘玉萍

    2011-01-01

    Objective To establish a gas chromatography - mass spectrometric method for simultaneous determination of 35 kinds of pesticide residues in food samples. Methods Samples were extracted using acetonitrile and then evaporated nearly to dryness with a rotary evaporator. The concentrated extract was dissolved with acetone and methylene chloride mixture and dehydrated with anhydrous Na2SO4 and finally purified with Carb/NH2 column and silicon magnesium column. The purified solution was concentrated before analysis by gas chromatography - mass spectrometry. Results The results showed that the detection limit was 0.005-0.05 mg/L, the recoveries of standard addition were 70.6%- 113.5%, and the RSD wasl.5%~7.8%. The linear coefficients were ≥0. 995. Conclusions This method is able to determine 35 kinds of pesticide residues in food safety risk monitoring samples in 2011 at the same chromatographic and mass spectrometric conditions. It is sensitive and reproducible, and of high accuracy and precision, which can be used in the actual testing analysis.%目的 建立用GC-MS同时检测食品中35种常见农药的方法. 方法 样品中所含农药残留用乙腈一并提取,浓缩近干,经丙酮和二氯甲烷混合液溶解,无水Na2SO4脱水,过Carb/NH2柱、硅镁柱净化,浓缩待测定. 结果 实验结果显示最低检出限为0.005~0.05 mg/ L,加标回收率为70.6%~113.5%,RSD为1.5%~7.8%,标准曲线r值均≥0.995. 结论 该方法能够将食品中常见的35种农残在同一色谱及质谱条件下检测,能实现良好的分离,定性定量准确、灵敏、重现性良好,可用于实际样品检测分析.

  17. Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

    Science.gov (United States)

    Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

    2016-09-08

    Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days

  18. Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces

  19. Method development for the determination of wood preservatives in commercially treated wood using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Šťávová, Jana; Sedgeman, Carl A; Smith, Zachary T; Frink, Lillian A; Hart, Jessica A; Niri, Vadoud H; Kubátová, Alena

    2011-09-30

    Fungicides and insecticides are commonly used preservatives to protect wood products against microbiological degradations. Currently, there is a lack of analytical methods addressing the quantitative determination of a wide range of wood preserving species in wood matrices. In this study, a reliable method was developed for the determination of a mixture of wood preserving agents with differing chemical structures (i.e., properties), including tebuconazole (TAZ), propiconazole (PAZ), 3-iodo-2-propynyl butylcarbamate (IPBC), and permethrin (PER), in pine wood. The analyte recoveries obtained by Soxhlet and multiple-stage sonication extractions were compared. While both extraction methods yielded similar results (80-100%), Soxhlet extraction was found to be less labor-intensive and thus preferred providing also lower RSDs of 1-6%. In comparison to methanol, commonly used as an extraction solvent for triazoles, acetone yielded similar extraction efficiencies for all analytes while reducing the time of sample concentration. The solid phase extraction method for triazoles was adapted to allow for a separation of IPBC and PER from the wood matrix. As opposed to previous studies, three recovery standards were employed, which enabled the correction of individual analyte losses during the sample preparation. The matrix-affected limits of detection (LODs) using gas chromatography with mass spectrometric detection were nearly the same for triazoles 0.07 and 0.21 ng g(-1) for PAZ and TAZ in sapwood and 0.18 and 0.21 ng g(-1) in heartwood, respectively. Higher LODs were observed for IPBC and PER: 3.9 and 1.7 ng g(-1) in sapwood, and 2.0 and 6.0 ng g(-1) in heartwood, respectively. The recoveries in the wood submitted to commercial sample treatment showed gradient distribution of analytes depending on the penetration of the treatment.

  20. Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

    Science.gov (United States)

    Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

    2015-12-24

    A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). PMID:26684593

  1. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Daniele Z., E-mail: daniele.dzs@dpf.gov.br [Setor Tecnico-Cientifico, Superintendencia Regional do Departamento de Policia Federal no Rio Grande do Sul, 1365 Ipiranga Avenue, Azenha, Zip Code 90160-093 Porto Alegre, Rio Grande do Sul (Brazil); Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Pechansky, Flavio [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Duarte, Paulina C.A.V. [Secretaria Nacional de Politicas sobre Drogas (SENAD), Esplanada dos Ministerios, Block ' A' , 5th floor, Zip Code 70050-907 Brasilia, Distrito Federal (Brazil); De Boni, Raquel [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Froehlich, Pedro E.; Limberger, Renata P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil)

    2011-06-24

    Graphical abstract: Highlights: > Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. > Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. > Linear range 2(4)-256 ng mL{sup -1}, detection limits 0.5-2 ng mL{sup -1}. > Accuracy 98-112%, precision <15% of RSD, recovery 77-112%. > Importance of residual evaluation in checking model goodness-of-fit. - Abstract: A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal{sup TM} device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL{sup -1} (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL{sup -1}. The detection limits were 0.5 ng mL{sup -1} (MET), 1 ng mL{sup -1} (MPH) and 2 ng mL{sup -1} (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal{sup TM} device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

  2. Gas chromatography mass spectrometry computer analysis of volatile halogenated hydrocarbons in man and his environment--A multimedia environmental study.

    Science.gov (United States)

    Barkley, J; Bunch, J; Bursey, J T; Castillo, N; Cooper, S D; Davis, J M; Erickson, M D; Harris, B S; Kirkpatrick, M; Michael, L C; Parks, S P; Pellizzari, E D; Ray, M; Smith, D; Tomer, K B; Wagner, R; Zweidinger, R A

    1980-04-01

    As part of a study to make a comparative analysis of selected halogenated compounds in man and the environmental media, a quantitative gas chromatography mass spectrometric analysis of the levels of the halogenated compounds found in the breath, blood and urine of an exposed population (Old Love Canal area, Niagara, New York) and their immediate environment (air and water) was undertaken. In addition, levels of halogenated hydrocarbons in air samples taken in the general Buffalo, Niagara Falls area were determined.

  3. Gas chromatography mass spectrometry computer analysis of volatile halogenated hydrocarbons in man and his environment--A multimedia environmental study.

    Science.gov (United States)

    Barkley, J; Bunch, J; Bursey, J T; Castillo, N; Cooper, S D; Davis, J M; Erickson, M D; Harris, B S; Kirkpatrick, M; Michael, L C; Parks, S P; Pellizzari, E D; Ray, M; Smith, D; Tomer, K B; Wagner, R; Zweidinger, R A

    1980-04-01

    As part of a study to make a comparative analysis of selected halogenated compounds in man and the environmental media, a quantitative gas chromatography mass spectrometric analysis of the levels of the halogenated compounds found in the breath, blood and urine of an exposed population (Old Love Canal area, Niagara, New York) and their immediate environment (air and water) was undertaken. In addition, levels of halogenated hydrocarbons in air samples taken in the general Buffalo, Niagara Falls area were determined. PMID:7448328

  4. Determination of dimethyl trisulfide in rabbit blood using stir bar sorptive extraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    Manandhar, Erica; Maslamani, Nujud; Petrikovics, Ilona; Rockwood, Gary A; Logue, Brian A

    2016-08-26

    Cyanide poisoning by accidental or intentional exposure poses a severe health risk. The current Food and Drug Administration approved antidotes for cyanide poisoning can be effective, but each suffers from specific major limitations concerning large effective dosage, delayed onset of action, or dependence on enzymes generally confined to specific organs. Dimethyl trisulfide (DMTS), a sulfur donor that detoxifies cyanide by converting it into thiocyanate (a relatively nontoxic cyanide metabolite), is a promising next generation cyanide antidote. Although a validated analytical method to analyze DMTS from any matrix is not currently available, one will be vital for the approval of DMTS as a therapeutic agent against cyanide poisoning. Hence, a stir bar sorptive extraction (SBSE) gas chromatography - mass spectrometry (GC-MS) method was developed and validated for the analysis of DMTS from rabbit whole blood. Following acid denaturation of blood, DMTS was extracted into a polydimethylsiloxane-coated stir bar. The DMTS was then thermally desorbed from the stir bar and analyzed by GC-MS. The limit of detection of DMTS using this method was 0.06μM with dynamic range from 0.5-100μM. For quality control standards, the precision, as measured by percent relative standard deviation, was below 10%, and the accuracy was within 15% of the nominal concentration. The method described here will allow further investigations of DMTS as a promising antidote for cyanide poisoning. PMID:27477518

  5. [Determination of 21 organophosphorus pesticides in tea by gas chromatography-mass spectrometry coupled with hydroxylated multi-walled carbon nanotubes based on dispersive solid-phase extraction].

    Science.gov (United States)

    Rong, Jiefeng; Wei, Hang; Li, Yijun; Huang, Huoshui; Xu, Meizhu

    2016-02-01

    A rapid determination method of 21 organophosphorus pesticides in tea was developed by QuEChERS method using modified multi-walled carbon nanotubes (MWCNTs-OH), primary-secondary amine (PSA) and MgSO4 coupled with gas chromatography-mass spectrometry. The pesticide residues in tea were extracted with a hexane-acetone (2:1, v/v) mixture, and cleaned up by dispersive solid-phase extraction using MWCNTs-OH and primary-secondary amine (PSA) as the sorbents. After centrifugation and filtration, the target compounds were analyzed by gas chromatography-mass spectrometry and quantified by the external standard method. Under the optimized conditions, good linearities were obtained in the range of 0. 01- 0. 50 mg/kg. The average recoveries were in the range of 81. 5% -109. 4% at three spiked levels, with relative standard deviations (RSDs, n = 5 ) of 2. 3% - 10. 6%. The limits of quantification were 0. 001-0. 040 mg/kg. This method is simple, fast, sensitive, cheap, and can meet the requirements of the rapid detection of organophosphorus pesticides in tea.

  6. [Determination of 21 organophosphorus pesticides in tea by gas chromatography-mass spectrometry coupled with hydroxylated multi-walled carbon nanotubes based on dispersive solid-phase extraction].

    Science.gov (United States)

    Rong, Jiefeng; Wei, Hang; Li, Yijun; Huang, Huoshui; Xu, Meizhu

    2016-02-01

    A rapid determination method of 21 organophosphorus pesticides in tea was developed by QuEChERS method using modified multi-walled carbon nanotubes (MWCNTs-OH), primary-secondary amine (PSA) and MgSO4 coupled with gas chromatography-mass spectrometry. The pesticide residues in tea were extracted with a hexane-acetone (2:1, v/v) mixture, and cleaned up by dispersive solid-phase extraction using MWCNTs-OH and primary-secondary amine (PSA) as the sorbents. After centrifugation and filtration, the target compounds were analyzed by gas chromatography-mass spectrometry and quantified by the external standard method. Under the optimized conditions, good linearities were obtained in the range of 0. 01- 0. 50 mg/kg. The average recoveries were in the range of 81. 5% -109. 4% at three spiked levels, with relative standard deviations (RSDs, n = 5 ) of 2. 3% - 10. 6%. The limits of quantification were 0. 001-0. 040 mg/kg. This method is simple, fast, sensitive, cheap, and can meet the requirements of the rapid detection of organophosphorus pesticides in tea. PMID:27382726

  7. Simultaneous determination of 4-tert-octylphenol,4-nonylphenol and bisphenol A in Guanting Reservoir using gas chromatography-mass spectrometry with selected ion monitoring

    Institute of Scientific and Technical Information of China (English)

    JIN Xing-long; HUANG Guo-lan; JIANG Gui-bin; ZHOU Qun-fang; LIU Jing-fu

    2004-01-01

    The wide occurrence of estrogenic compounds 4-tert-octylphenol, 4-nonylphenol, bisphenol A in surface water of Guanting Reservoir was successfully determined. The target compounds in water samples were preconcentrated by liquid-liquid extraction with dichloromethane, derivatized by trifluoroacetic anhydride, and quantified by gas chromatography-mass spectrometry(GC-MS) with selected ion monitoring(SIM). In the selected seven sampling sites(S1-S7), the concentrations of NP in sample S7 were significantly higher than the other in reservoir. The pollution status in S3 and S7 were much more serious. The concentrations of OP, NP and BPA were in the range of 44.5-48.8, 221.6-349.6 and 30.2-82.7 ng/L, respectively. The pollution were mainly inputted from the upper river and released from sediments in Guanting Reservoir.

  8. Determination of musty odorants, 2-methylisoborneol and geosmin, in environmental water by headspace solid-phase microextraction and gas chromatography--mass spectrometry.

    Science.gov (United States)

    Saito, Keita; Okamura, Kota; Kataoka, Hiroyuki

    2008-04-01

    A simple and sensitive method for the determination of musty odorants, 2-methylisoborneol (MIB) and geosmin (GSM), in environmental water was developed by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry. MIB and GSM were separated within 10 min using a DB-1 capillary column and detected in the selective ion monitoring mode. HS-SPME using a polydimethylsiloxane/divinylbenzene fiber provided effective sample enrichment, and was carried out by fiber exposition at 70 degrees C for 30 min. Using this method, the calibration curves of MIB and GSM were linear in the range of 0-500 pg/mL, with a correlation coefficient above 0.9977 (n=24). The detection limits (S/N=3) of MIB and GSM were 0.9 and 0.6 pg/mL, respectively. This method was successfully applied to the analysis of environmental water samples without interference peaks.

  9. A salting out-acetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics.

    Science.gov (United States)

    Dong, Hao; Guo, Xindong; Xian, Yanping; Luo, Haiying; Wang, Bin; Wu, Yuluan

    2015-11-27

    A sensitive gas chromatography-mass spectrometry method was established for the simultaneous determination of thirteen N-nitrosamines (NAs) in skin care cosmetics. The cosmetics samples were firstly dispersed by water and subsequently extracted and purified using salting out-acetonitrile homogeneous extraction method. Finally, the extracting solution was concentrated by slow nitrogen gas blowing. All of the samples were separated by INNOWAX capillary chromatographic column, and detected by selected ion monitoring (SIM) mode of gas chromatography-mass spectrometry (GC-MS) and quantified by isotope internal standard method. The method was validated for linearity and range, accuracy, precision and sensitivity. Under the optimized condition, the calibration curves were linear over the selected concentration ranges of 2-500μg/L for all the thirteen analytes, with calculated coefficients of determination (R(2)) of greater than 0.996. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 3-15μg/kg and 10-50μg/kg, respectively. Recoveries were calculated at three levels of concentration spiked in two kinds of cosmetics (skin care cream and water). The values were found between 93.8% and 121.0% with relative standard deviation (RSD) values of 2.5-7.2% for intra-day precision (n=6) and 3.3-6.7% for inter-day precision (n=5). The method was successfully applied to analyze twenty-two cosmetics samples and N-nitrosodimethylamine (NDMA) was detected in one sample with the concentration of 207μg/kg.

  10. A salting out-acetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics.

    Science.gov (United States)

    Dong, Hao; Guo, Xindong; Xian, Yanping; Luo, Haiying; Wang, Bin; Wu, Yuluan

    2015-11-27

    A sensitive gas chromatography-mass spectrometry method was established for the simultaneous determination of thirteen N-nitrosamines (NAs) in skin care cosmetics. The cosmetics samples were firstly dispersed by water and subsequently extracted and purified using salting out-acetonitrile homogeneous extraction method. Finally, the extracting solution was concentrated by slow nitrogen gas blowing. All of the samples were separated by INNOWAX capillary chromatographic column, and detected by selected ion monitoring (SIM) mode of gas chromatography-mass spectrometry (GC-MS) and quantified by isotope internal standard method. The method was validated for linearity and range, accuracy, precision and sensitivity. Under the optimized condition, the calibration curves were linear over the selected concentration ranges of 2-500μg/L for all the thirteen analytes, with calculated coefficients of determination (R(2)) of greater than 0.996. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 3-15μg/kg and 10-50μg/kg, respectively. Recoveries were calculated at three levels of concentration spiked in two kinds of cosmetics (skin care cream and water). The values were found between 93.8% and 121.0% with relative standard deviation (RSD) values of 2.5-7.2% for intra-day precision (n=6) and 3.3-6.7% for inter-day precision (n=5). The method was successfully applied to analyze twenty-two cosmetics samples and N-nitrosodimethylamine (NDMA) was detected in one sample with the concentration of 207μg/kg. PMID:26518490

  11. Analysis of Volatile Metabolites Released by Staphylococcus Aureus using Gas Chromatography-Mass Spectrometry and Determination of its Antifungal Activity

    Directory of Open Access Journals (Sweden)

    Hayfaa Hussein Jaddoa

    2016-08-01

    Full Text Available Bacterial volatile organic compounds (VOCs have been considered as sensitive and specific biomarkers for bacterial detection in human specimens and culture media. The possibility of using VOCs markers as one of the largest groups of bacterial metabolites would open a new frontier for developing more efficient techniques in the diagnosis of bacterial infections. The aims of this research were analysis of the bioactive chemical products and evaluation of antibacterial and antifungal activity. Bioactives (chemical compounds often referred to as secondary metabolites were analyzed using gas chromatography-mass spectroscopy (GC-MS techniques, then the in vitro antibacterial and antifungal activity of the methanolic extract was evaluated. Thirty five bioactive compounds were identified in the methanolic extract of Staphylococcus aureus. GC-MS analysis of Staphylococcus aureus revealed the existence of the: Hexanoic acid , 2-methyl, 12,15-Octadecadiynoic acid , methyl ester, 1-Aminononadecane ,N-trifluoroacetyl-, N-[3-[N-Aziridyl]propylidene]hexylamine, N-(2,5-Dicyano-3,4-dihydro-2H-pyrrol-2-yl-acetamide, 3-Cyclohex-3-enyl-propionic acid, 1-Methyl-4-[nitromethyl]-4-piperidinol, 3-Azonia-5-hexyn-1-ol , N,N-dimethyl-O-acetyl-,bromide, 1-Hexadecanol -2-methyl-, 1-Propyl-3,6-diazahomoadamantan, 9-Borabicyclo[3.3.1]nonane , 9-mercapto-, Benzyl methyl ketone, L-Aspartic acid ,N-glycyl-, Aminoacetamide , N-methyl-N-[4-(1-pyrrolidinyl-2-butynyl]-, Tertbutyloxyformamide , N-methyl-N-[4-(1-pyrrolidinyl-2-butyn, 5,7-Dodecadiyn-1,12-diol, Deoxyspergualin, D-Streptamine , O-6-deoxy-α-D-glucopyranosyl-(1-4, dl-Citrulline, N-[3-Diethylaminopropyl]-4-oxo-1,2,3,4,5,6,7,8-octahydroqui, N-Propionyl-D-glucoseamine, Cystine, 3,4-Dihydrocoumarin ,6-fluoro-4,4-dimethyl-, 4-(2,5-Dihydro-3-methoxyphenylbutylamine, 3-methoxy-2-(1-methylethyl-5-(2-methylpropylpyrazine, Uric acid, Thiocyanic acid 4-methoxy-2,6-dimethyl-3-pyridyl ester, 12-Dimethylamino-10-oxododecanoic acid

  12. EPA Method 525.3 - Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

    Science.gov (United States)

    Method 525.3 is an analytical method that uses solid phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) for the identification and quantitation of 125 selected semi-volatile organic chemicals in drinking water.

  13. Simultaneous determination of amoxicillin and clavulanic acid in the human plasma by high performance liquid chromatography: Mass spectrometry (UPLC/MS

    Directory of Open Access Journals (Sweden)

    Ćirić Biljana

    2010-01-01

    Full Text Available Background/Aim. Quantitative analysis of amoxicillin and clavulanic acid in biological matrices requires sensitive and specific methods which allow determination of therapeutic concentration in μg/mL range. Analytical methods for determination of their concentrations in body fluids described in literature include high performance liquid chromatography coupled to UV detector (HPLC-UV and liquid chromatography-mass spectrometry (LC-MS. The aim of this study was to develop sensitive and specific ultra performance liquid chromatography/ mass spectrometry (UPLC/MS method which could be used for the spectral identification and quantification of the low concentrations of amoxicillin and clavulanic acid in the human plasma. Method. A sensitive and specific UPLC/MS method for amoxicillin and clavulanic acid determination was developed in this study. The samples were taken from the adult healthy volunteers receiving per os one tablet of amoxicillin (875 mg in combination with clavulanic acid (125 mg. Results. Plasma samples were pretreated by direct deproteinization with perchloric acid. Quantification limit of 0.01 μg/ml for both amoxicillin and clavulanic acid was achieved. The method was reproducible day by day (RSD < 7 %. Analytical recoveries for amoxicillin ranged from 98.82% to 100.9% (for concentrations of 1, 5 and 20 μg/mL, and recoveries for clavulanic acid were 99,89% to 100.1% (for concentrations of 1, 2 and 5 μg/mL. This assay was successfully applied to a pilot pharmacokinetic study in healthy volunteers after a single-oral administration of amoxicillin/ clavulanic combination. The determined plasma concentrations of both amoxicillin and clavulanic acid were in the range of the expected values upon the literature data for HPLC-UV and LC-MS methods. Conclusion. The described method provided a few advantages comparing with LC/MS-MS method. The method is faster using running time of 5 minute, has lower limit of quantification (LOQ and it

  14. Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 69 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals on aquatic organisms in wastewater. This method also is useful for evaluating the effects of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are indicators of wastewater or have endocrine-disrupting potential. These compounds include the alkylphenol ethoxylate nonionic surfactants, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Wastewater compounds in whole-water samples were extracted using continuous liquid-liquid extractors and methylene chloride solvent, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 0.5 microgram per liter averaged 72 percent ? 8 percent relative standard deviation. The concentration of 21 compounds is always reported as estimated because method recovery was less than 60 percent, variability was greater than 25 percent relative standard deviation, or standard reference compounds were prepared from technical mixtures. Initial method detection limits averaged 0.18 microgram per liter. Samples were preserved by adding 60 grams of sodium chloride and stored at 4 degrees Celsius. The laboratory established a sample holding-time limit prior to sample extraction of 14 days from the date of collection.

  15. Determination of volatile components of saffron by optimised ultrasound-assisted extraction in tandem with dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sereshti, Hassan; Heidari, Reza; Samadi, Soheila

    2014-01-15

    In the present research, a combined extraction method of ultrasound-assisted extraction (UAE) in conjunction with dispersive liquid-liquid microextraction (DLLME) was applied to isolation and enrichment of saffron volatiles. The extracted components of the saffron were separated and determined by gas chromatography-mass spectrometry (GC-MS) technique. The mixture of methanol/acetonitrile was chosen for the extraction of the compounds and chloroform was used at the preconcentration stage. The important parameters, such as composition of extraction solvent, volume of preconcentration solvent, ultrasonic applying time, and salt concentration were optimised by using a half-fraction factorial central composite design (CCD). Under the optimal conditions, the linear dynamic ranges (LDRs) were 10-10,000mgL(-)(1). The determination coefficients (R(2)) were from 0.9990 to 0.9997. The limits of detection (LODs) and limits of quantification (LOQs) for the extracted compounds were 6-123mgL(-)(1) and 20-406mgL(-)(1), respectively. The relative standard deviations (RSDs) were 2.48-9.82% (n=3). The enhancement factors (EFs) were 3.6-41.3. PMID:24054273

  16. [Determination of 46 plasticizers in food contact polyvinyl chloride packaging materials and their migration into food simulants by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Guo, Chunhai; Bo, Haibo; Duan, Wenzhong; Jia, Haitao; Chen, Ruichun; Ma, Yusong; Ai, Lianfeng

    2011-01-01

    A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 46 plasticizers in food contact polyvinyl chloride (PVC) packaging materials and their migration into food simulants, i. e. water, 3% acetic acid, 10% ethanol and olive oil. Plasticizers in the PVC packaging materials, aqueous food simulants and olive oil food simulants were extracted by the dissolution-precipitation, liquid-liquid extraction and gel permeation chromatography (GPC) approaches, respectively. The extracts were analyzed by GC-MS in selective ion monitoring (SIM) mode and quantified using the external standard method. The cal-ibration curves were linear in the ranges of 0.1-2.0 mg/L with the correlation coefficients of 0.9910-0. 999 9. The limits of detection were from 0. 005 mg/kg to 0. 05 mg/kg ( S/N = 5 ). The recoveries at 3 spiked levels were 69.51%-107. 21% and the relative standard deviations (RSDs n = 6) ranged from 3.53% to 18.95%. These results show that this method is fast, sensitive and accurate for the qualitative and quantitative determination of plasticizers in food contact plastic products and 4 types of food simulants. PMID:21574398

  17. [Simultaneous determination of 23 ester compounds in cigarette water-borne adhesives by liquid-liquid extraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Gong, Shuguo; Kong, Bo; Tuo, Suxing; Dai, Yunhui; Wu, Mingjian; Tan, Liquan; Liu, Wei

    2013-10-01

    A method of gas chromatography-mass spectrometry (GC-MS) with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds including acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 microm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column (60 m x 0.25 mm x 0.25 microm), and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4-50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8%-109.1%, and the relative standard deviations (RSDs, n = 5) were less than 4%. The limits of detection (LODs) and limits of quantification (LOQs were in the ranges of 0.02-0.76 mg/kg and 0.04-2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.

  18. Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 μg kg-1, respectively. This validated method was successfully applied to the determination of melamine in real samples from market.

  19. Simultaneous determination of three classes of antibiotics in the suspended solids of swine wastewater by ultrasonic extraction, solid-phase extraction and liquid chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Xun Pan; Zhimin Qiang; Weiwei Ben; Meixue Chen

    2011-01-01

    This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids (SS) of swine wastewater,including five sulfonamides,three tetracyclines and one macrolide (tiamulin).The entire procedures for sample pretreatment,ultrasonic extraction (USE),solid-phase extraction (SPE),and liquid chromatography-mass spectrometry (LC-MS) quantification were examined and optimized.The recovery efficiencies were found to be 76%-104% for sulfonamides,81%-112% for tetracyclines,and 51%4% for tiamulin at three spiking levels.The intra-day and inter-day precisions,as expressed by the relative standard deviation (RSD),were below 17%.The method detection limits (MDLs) were between 0.14 and 7.14 μg/kg,depending on a specific antibiotic studied.The developed method was applied to field samples collected from three concentrated swine feeding plants located in Beijing,Shanghai and Shandong province of China.All the investigated antibiotics were detected in both SS and liquid phase of swine wastewater,with partition coefficients (logKd) ranging from 0.49 to 2.30.This study demonstrates that the SS can not be ignored when determining the concentrations of antibiotics in swine wastewater.

  20. Determination of aromatic amines in hair dye and henna samples by ion-pair extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Akyüz, Mehmet; Ata, Sevket

    2008-05-12

    A gas chromatography-mass spectrometry (GC-MS) method has been proposed for the determination of carcinogenic and toxic aromatic amines in hair dye, henna and dyed hair samples. The method includes ion-pair extraction of aromatic amines from aqueous samples with bis-2-ethylhexylphosphate (BEHPA) released after solving the samples in acidic solution followed by sonication, derivatisation of compounds with isobutyl chloroformate (IBCF) and their GC-MS analysis in both electron impact (EI) and positive and negative ion chemical ionisation (PNICI) mode as their isobutyloxycarbonyl (isoBOC) derivatives. The obtained recoveries of aromatic amines ranged from 92.2 to 98.4% and the precision of this method, as indicated by the relative standard deviations (RSDs) was within the range of 0.7-4.2%. The detection limits obtained from calculations by using GC-MS results based on signal-to-noise ratio (S/N)=3 were within the range from 0.02 to 0.20 ng/g. In the present study, the commercially available 54 permanent hair dye, 35 modified or natural henna and 15 dyed hair samples were analysed for the aromatic amines by the proposed method and the method was shown to be suitable to determine the aromatic amine ingredients and metabolites of these commercial products. PMID:18280687

  1. [Determination of 46 plasticizers in food contact polyvinyl chloride packaging materials and their migration into food simulants by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Guo, Chunhai; Bo, Haibo; Duan, Wenzhong; Jia, Haitao; Chen, Ruichun; Ma, Yusong; Ai, Lianfeng

    2011-01-01

    A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 46 plasticizers in food contact polyvinyl chloride (PVC) packaging materials and their migration into food simulants, i. e. water, 3% acetic acid, 10% ethanol and olive oil. Plasticizers in the PVC packaging materials, aqueous food simulants and olive oil food simulants were extracted by the dissolution-precipitation, liquid-liquid extraction and gel permeation chromatography (GPC) approaches, respectively. The extracts were analyzed by GC-MS in selective ion monitoring (SIM) mode and quantified using the external standard method. The cal-ibration curves were linear in the ranges of 0.1-2.0 mg/L with the correlation coefficients of 0.9910-0. 999 9. The limits of detection were from 0. 005 mg/kg to 0. 05 mg/kg ( S/N = 5 ). The recoveries at 3 spiked levels were 69.51%-107. 21% and the relative standard deviations (RSDs n = 6) ranged from 3.53% to 18.95%. These results show that this method is fast, sensitive and accurate for the qualitative and quantitative determination of plasticizers in food contact plastic products and 4 types of food simulants.

  2. [Determination of 28 organochlorine and pyrethroid pesticides in pine nuts using solid-phase extraction and on-line gel permeation chromatography-gas chromatography/mass spectrometry].

    Science.gov (United States)

    Kang, Qinghe; Wu, Yan; Gao, Kaiyang; Li, Zhibin

    2009-03-01

    An analytical method has been developed for the determination of 28 organochlorine pesticides and pyrethroid pesticides in pine nuts. The sample was extracted With acetonitrile-water (4:1, v/v) as the extraction solution by means of high-speed homogenization. The crude extract was purified by an Aluminium-N solid phase extraction column to remove most of the fat and sterols in the sample, then on-line gel permeation chromatography-gas chromatography/ mass spectrometry (GPC-GC/MS) analysis was performed. The recoveries for the most of pesticides in the sample spiked with the standards of 0.05 mg/kg were 70%-120%, and the relative standard deviations were less than 15%. The limits of detection of 28 organochlorine pesti- and pyrethroid pesticides were 0.002-0.05 mg/kg. The linear relationship and the recovery results were satisfactory. The method is rapid, accurate, highly senstive, and can be used for the simultaneous determination of pesticide residues in pine nuts.

  3. Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ho, Tse-Tsung; Chen, Chung-Yu [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); Li Zuguang [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, Zhejiang (China); Yang, Thomas Ching-Cherng [Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 82444, Taiwan (China); Lee, Maw-Rong, E-mail: mrlee@dragon.nchu.edu.tw [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China)

    2012-01-27

    Highlights: Black-Right-Pointing-Pointer Ionic liquid (IL), ([C{sub 4}MIM][PF{sub 6}]), was rapid synthesized by microwave radiation. Black-Right-Pointing-Pointer Trace chlorophenols in landfill leachate were extract by SPME coated IL. Black-Right-Pointing-Pointer The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 Degree-Sign C for 4 min. Linearity was observed from 0.1 to 1000 {mu}g L{sup -1} with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 {mu}g L{sup -1}. The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 {mu}g L{sup -1}. The results demonstrate that the IL-SPME-GC/MS method is highly effective in

  4. Determination of BROMATE AT PARTS-PER-TRILLION LEVELS BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY WITH NEGATIVE CHEMICAL IONIZATION

    Science.gov (United States)

    The ozonation of bromide-containing source waters produces bromate as a class 2B carcinogenic disinfection by-product. The present work describes the determination of bromate by gas chromatography-negative chemical ionization mass spectrometry (GC-NCIMS) following a bromate react...

  5. Tequila volatile characterization and ethyl ester determination by solid phase microextraction gas chromatography/mass spectrometry analysis.

    Science.gov (United States)

    Vallejo-Cordoba, Belinda; González-Córdova, Aarón Fernando; del Carmen Estrada-Montoya, María

    2004-09-01

    Solid phase microextraction (SPME) and gas chromatography were used for tequila volatile characterization and ethyl ester quantitation. Several factors determined the differences in tequila volatile profiles obtained by the SPME technique, namely, sampling mode, fiber coating, and fiber exposure time. Each of these factors determined the most suitable conditions for the analysis of volatile profiles in tequila. Volatile extraction consisted of placing 40 mL of tequila in a sealed vial kept at 40 degrees C. A poly(dimethylsiloxane) fiber was immersed in the liquid for 60 min and desorbed for 5 min into the gas chromatograph. The identified volatiles by mass spectrometry were mainly alcohols, esters, and ketones. The calibration curves for ethyl hexanoate, octanoate, and decanoate followed linear relationships with highly significant (p tequila samples. Quantitative differences in ethyl esters were found for the four most commonly known tequila types: silver, gold, aged, and extra-aged.

  6. The determination of sulfonamides in honey by high performance liquid chromatography--mass spectrometry method (LC/MS).

    Science.gov (United States)

    Krivohlavek, Adela; Smit, Zdenko; Bastinac, Martina; Zuntar, Irena; Plavic-Plavsic, Franjo

    2005-08-01

    The sulfonamides (SAs) are stable chemotherapeutics used against the bacterial disease affecting bees, known as American foulbrood (Bacillus larvae), so their residues could appear in the honey of treated bees. Their presence at a concentration above the limit value could be a potential danger to human health. Therefore, a simple, rapid, and reliable method for determination of 11 available SAs in honey was optimized. The samples were homogenized and cleaned with extraction on solid phase by means of Chromabond C18 end-capped cartridge followed by LC/MS analyses. A detection limit of 25 microg/kg was achieved for all analytes. The repeatability of the method was proven and the optimal parameters for temperature and pH of the mobile phase and acetic buffer, respectively, were determined. In this study, 20 samples of domestic honey were included. Six of the analyzed samples were positive, but all results were below the Croatian permissible limit value (100 microg/kg).

  7. Determination of volatile aroma compounds of Ganoderma lucidum by gas chromatography mass spectrometry (HS-GC/MS).

    Science.gov (United States)

    Taşkın, Hatıra; Kafkas, Ebru; Çakıroğlu, Özgün; Büyükalaca, Saadet

    2013-01-01

    This study was conducted at Horticulture Department of Cukurova University, Adana, Turkey during 2010-2011. Fresh sample of Ganoderma lucidum collected from Mersin province of Turkey was used as material. Volatile aroma compounds were performed by Headspace Gas Chromatography (HS-GC/MS). Alcohols, aldehydes, acids, phenol, L-Alanine, d-Alanine, 3Methyl, 2-Butanamine, 2-Propanamine were determined. 1-Octen-3-ol (Alcohol) and 3-methyl butanal (Aldehyde) were identified as major aroma compounds.

  8. Novel determination of polychlorinated naphthalenes in water by liquid chromatography-mass spectrometry with atmospheric pressure photoionization.

    Science.gov (United States)

    Moukas, Athanasios I; Thomaidis, Nikolaos S; Calokerinos, Antony C

    2016-01-01

    This study presents the development, optimization, and validation of a novel method for the determination of polychlorinated naphthalenes (PCNs) by liquid chromatography-atmospheric pressure photoionization (APPI), using toluene as dopant. The mass spectra of PCN 52, 54, 66, 67, 73, and 75 were recorded in negative ionization. The base ions corresponded to [M-Cl+O](-), where M is the analyte molecule. A strategy, which includes designs of experiments, for the development, the evaluation, and the optimization of the LC-APPI-MS/MS methods is also described. Finally, a highly sensitive method with low instrumental limits of detection (LoDs), ranging from 0.8 pg for PCN 75 to 16 pg for PCN 54 on column, was validated. A Thermo Hypersil Green PAH (100 mm × 2.1 mm, 3 μm) column was used with acetonitrile/water/methanol as mobile phase. The method was applied for the determination of the selected PCNs in surface and tap water samples. A simple liquid-liquid extraction method for the extraction of PCNs from water samples was used. Method LoQs ranged from 29 ng L(-1), for PCN 73, to 63 ng L(-1), for PCN 54, and the recoveries ranged from 97 to 99%, for all congeners. This is the first LC-APPI-MS/MS method for the determination of PCNs in water samples.

  9. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  10. Determination of Dimethylfumarate in Leather and Footwear by Solid-Phase micro Extraction and Gas Chromatography-Mass Spectrometry

    OpenAIRE

    Cuadros Domènech, Rosa Maria; Font Vallès, Joaquim; Reyes Reyes, Maria; Ollé Otero, Lluís; Marsal Monge, Agustín

    2010-01-01

    In the last two years, Europe has experienced a rise in skin allery and dermatitis due to goods and Asian provenance that have been treacted with dimethylfumarate (DMFU). Accordingly,laboratories in the leather and foodwear sectors have been obliged to develop analytical methods to determine the presence of this substance given de absence of an official method. The ban on DMFU as laid down in Decision 2009/251 of the European Union establishes a maximun concentration of DMFU in products of 0....

  11. An in situ derivatization - dispersive liquid-liquid microextraction combined with gas-chromatography - mass spectrometry for determining biogenic amines in home-made fermented alcoholic drinks.

    Science.gov (United States)

    Płotka-Wasylka, Justyna; Simeonov, Vasil; Namieśnik, Jacek

    2016-07-01

    A novel dispersive liquid-liquid microextraction (DLLME) gas chromatography mass-spectrometry (GC-MS) method was developed for the determination of 13 biogenic amines in home-made wine samples. The method allows to simultaneous extraction and derivatization of the amines providing a simple and fast mode of extract enrichment. During the study, two different procedures were examined. Statistical analysis was performed to choose better procedure, as well as the conditions of derivatization reaction. At least, a mixture of methanol (dispersive solvent; 215μL), chloroform (extractive solvent; 400μL), and isobutyl choloroformate (derivatizing reagent; 90μL) was used as extractive/derivatizing reagent, added to 5mL of sample. The addition of mixture of pyridine and HCl was necessary to eliminate the by-products. The proposed method showed good linearity (correlation coefficients >0.9961), good recoveries (from 77 to 105%), and good intra-day precision (below 13%) and inter-day precision (below 10%). Moreover, detection limits were never over 4.1μg/L. The developed method was successfully applied to the analysis of 17 home-made wine samples not regulated by law. All of the biogenic amines analyzed were found in most of the wines.

  12. Up-and-down-shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry for the determination of fungicides in wine.

    Science.gov (United States)

    Chu, Shang-Ping; Tseng, Wan-Chi; Kong, Po-Hsin; Huang, Chun-Kai; Chen, Jung-Hsuan; Chen, Pai-Shan; Huang, Shang-Da

    2015-10-15

    An up-and-down-shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME) method coupled with gas chromatography-mass spectrometry was developed for the determination of fungicides (cyprodinil, procymidone, fludioxonil, flusilazole, benalaxyl, and tebuconazole) in wine. The developed method requires 11 μL of 1-octanol without the need for dispersive solvents. The total extraction time was approximately 3 min. Under optimum conditions, the linear range of the method was 0.05-100 μg L(-1) for all fungicides and the limit of detection was 0.007-0.025 μg L(-1). The absolute and relative recoveries were 31-83% and 83-107% for white wine, respectively, and 32-85% and 83-108% for red wine, respectively. The intra-day and inter-day precision were 0.5-7.5% and 0.7-6.1%, respectively. Our developed method had good sensitivity and high extraction efficiency. UDSA-DLLME is a desirable method in terms of performance and speed.

  13. Determination of phthalates in wine by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry: fibre comparison and selection.

    Science.gov (United States)

    Carrillo, J D; Salazar, C; Moreta, C; Tena, M T

    2007-09-14

    This paper describes the development of a headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for determining phthalates in wine. The HS-SPME conditions were thoroughly studied: first, the performance of six fibres at three temperature values and two sample volumes was surveyed by means of a 6 x 3 x 2 multi-factor categorical experimental design. From this study, three fibres - carbowax-divinylbenzene (CW-DVB), polyacrylate (PA) and polydimethylsiloxane-divinylbenzene (PDMS-DVB) - were selected. Then, temperature, sample volume and sodium chloride concentration were optimised using a central composite design and the overall desirability function for each fibre. The optimal values were 70 degrees C, a NaCl concentration of 2.6, 3.6 and 5.5M for PA, CW-DVB and PDMS-DVB fibres, respectively, and sample volumes of 4.0, 3.5 and 3.0 mL. Next, the performance characteristics of the three fibres were obtained and compared. PDMS-DVB fibre showed the best repeatability values followed by CW-DVB. PA fibre was not suitable for diethylhexylphthalate extraction and showed poor repeatability for the heavier phthalates, and was therefore discarded. Finally, the performance of CW-DVB and PDMS-DVB fibres was checked for red, white and rosé wines. PMID:17644103

  14. Stir frit microextraction: an approach for the determination of volatile compounds in water by headspace-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Roldán-Pijuán, M; Alcudia-León, M C; Lucena, R; Cárdenas, S; Valcárcel, M

    2012-08-17

    In this article, a novel extraction approach, called stir frit microextraction (SFME), is presented. The new approach combines the extractive capability of a commercial polyethylene frit (20 μm of pore size) with the stirring in the same device. The proposed extraction procedure allows the determination of benzene, toluene, ethylbenzene, xylene isomers and styrene (BTEX-S) in water samples. The analytes are extracted on the frit, previously conditioned with methanol, under continuous magnetic stirring. Once the extraction is performed, the frit is transferred to a headspace vial where the volatile compounds are desorbed from the frit (90 °C, 30 min) in a headspace module and analyzed by gas chromatography/mass spectrometry. Headspace conditions (time and temperature) as well as extraction conditions (ionic strength, type of stirring, extraction time, stirring rate and sample volume) have been systematically evaluated. The method was characterized on the basis of its linearity, sensitivity and precision. Limits of detection were in the range from 18 ng/L (o-xylene) to 65 ng/L (benzene). The repeatability of the proposed method, expressed as relative standard deviation (RSD) varied between 3.8% (toluene) and 8.2% (m- and p-xylene). The recovery study carried out in different water samples provided an average recovery of 94%, which demonstrated the applicability of the stir frit microextraction for the analytical problem selected in this article. PMID:22771255

  15. An in situ derivatization - dispersive liquid-liquid microextraction combined with gas-chromatography - mass spectrometry for determining biogenic amines in home-made fermented alcoholic drinks.

    Science.gov (United States)

    Płotka-Wasylka, Justyna; Simeonov, Vasil; Namieśnik, Jacek

    2016-07-01

    A novel dispersive liquid-liquid microextraction (DLLME) gas chromatography mass-spectrometry (GC-MS) method was developed for the determination of 13 biogenic amines in home-made wine samples. The method allows to simultaneous extraction and derivatization of the amines providing a simple and fast mode of extract enrichment. During the study, two different procedures were examined. Statistical analysis was performed to choose better procedure, as well as the conditions of derivatization reaction. At least, a mixture of methanol (dispersive solvent; 215μL), chloroform (extractive solvent; 400μL), and isobutyl choloroformate (derivatizing reagent; 90μL) was used as extractive/derivatizing reagent, added to 5mL of sample. The addition of mixture of pyridine and HCl was necessary to eliminate the by-products. The proposed method showed good linearity (correlation coefficients >0.9961), good recoveries (from 77 to 105%), and good intra-day precision (below 13%) and inter-day precision (below 10%). Moreover, detection limits were never over 4.1μg/L. The developed method was successfully applied to the analysis of 17 home-made wine samples not regulated by law. All of the biogenic amines analyzed were found in most of the wines. PMID:27237593

  16. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ruan, E D; Aalhus, J L; Summerfelt, S T; Davidson, J; Swift, B; Juárez, M

    2013-12-20

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry (SBSE-TD-GCMS). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

  17. Headspace solid-phase microextraction with on-fiber derivatization for the determination of aldehydes in algae by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ma, Jiping; Xiao, Ronghui; Li, Jinhua; Li, Jie; Shi, Benzhang; Liang, Yanjuan; Lu, Wenhui; Chen, Lingxin

    2011-06-01

    A simple, fast, sensitive and cost-effective method based on headspace solid-phase microextraction (HS-SPME) with on-fiber derivatization coupled with gas chromatography-mass spectrometry was developed for the determination of six typical aldehydes, 2E-hexenal, heptanal, 2E-heptenal, 2E,4E-heptadienal, 2E-decenal and 2E,4E-decadienal in laboratory algae cultures. As derivatization reagent, O-2,3,4,5,6-(pentafluorobenzyl) hydroxylamine hydrochloride, was loaded onto the poly(dimethylsiloxane)/divinylbenzene fiber for aldehydes on-fiber derivatization prior to HS-SPME. Various influence factors of extraction efficiency were systematically investigated. Under optimized extraction conditions, excellent method performances for all the six aldehydes were attained, such as satisfactory extraction recoveries ranging from 67.1 to 117%, with the precision (relative standard deviation) within 5.3-11.1%, and low detection limits in the range of 0.026-0.044 μg/L. The validated method was successfully applied for the analysis of the aldehydes in two diatoms (Skeletonema costatum and Chaetoceros muelleri), two pyrrophytas (Prorocentrum micans and Scrippsiella trochoidea) and Calanus sinicus eggs (feeding on the two diatoms above). PMID:21567947

  18. Rapid determination of caffeine in one drop of beverages and foods using drop-to-drop solvent microextraction with gas chromatography/mass spectrometry.

    Science.gov (United States)

    Shrivas, Kamlesh; Wu, Hui-Fen

    2007-11-01

    A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis. PMID:17904565

  19. Development and validation of a gas chromatography-mass spectrometry method for the determination of phenazopyridine in rat plasma: application to the pharmacokinetic study.

    Science.gov (United States)

    Chen, Qinhua; Li, Kaijun; Zhang, Zhuo; Li, Peng; Liu, Jia; Li, Qiang

    2007-11-01

    Phenazopyridine hydrochloride is a strong analgesic used in the treatment of urinary tract infections. The aim of the present study was to develop a procedure based on gas chromatography-mass spectrometry (GC-MS) for the analysis of phenazopyridine in rat plasma. The method was set up and adapted for the analysis of small biological samples taken from rats. Biological samples were extracted by liquid-liquid extraction. The extraction agent was ethyl acetate. The samples were separated by GC on a DB-5MS analytical column and determined by a quadrupole mass spectrometer detector operated under selected ion monitoring mode. Excellent linearity was found between 0.01 and 1.00 microg/ml (r = 0.9991, n = 9) for plasma samples. The limit of detection (LOD) was 0.3 ng/ml. Within-day and between-day precisions expressed as the relative standard deviation (RSD) for the method were 1.83-4.91% and 2.12-4.76%, respectively. The recoveries for all samples were >90%. The main pharmacokinetic parameters obtained were T(max) = (0.35+/-0.01) h, C(max) = (0.396+/-0.079) microg/ml, AUC = (0.373+/-0.065) h microg/ml and CL = (94.2+/-5.9) ml/g/h. The results presented here clearly indicate that this proposed method could be applicable to investigate the pharmacokinetic of phenazopyridine in rats after administration. (c) PMID:17847064

  20. In-syringe dispersive micro-solid phase extraction using carbon fibres for the determination of chlorophenols in human urine by gas chromatography/mass spectrometry.

    Science.gov (United States)

    García-Valverde, M T; Lucena, R; Cárdenas, S; Valcárcel, M

    2016-09-16

    In this article, carbon fibres (CFs) are presented as sorbent material for the dispersive micro-solid phase extraction of twelve chlorophenols from urine samples. CFs are synthesized by a reagentless and green procedure consisting of heating raw cotton, a natural precursor, at high temperature (400°C) in an inert atmosphere (Ar) during 2h. The resulting fibres, which present good water dispersibility, are finally loaded on an in-syringe device. This device, which integrates the extraction and final elution of the analytes, is disposable and it is adapted to process low sample volumes. Working at the optimum conditions, the extraction procedure in combination with gas chromatography/mass spectrometry allows the determination of the analytes in urine at the low μg/L range. In fact, the limits of quantification (LOQs) of the analytes were in the interval from 1μg/L to 2.5μg/L with precision values, expressed as relative standard deviations (RSD), better than 13%. Relative recovery values, ranging from 74.5% to 113%, demonstrate the applicability of the proposed method. PMID:27558356

  1. 质谱法测定柴油中多环芳烃%Determination of Polycyclic Aromatic Hydrocarbons in Diesel with Gas Chromatography- Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘文; 张小军

    2015-01-01

    The Gas Chromatography- Mass Spectrometry on determination of Polycyclic Aromatic Hydrocarbons in diesel was used, and the factors affecting solid phase extraction pretreatment of sample and the GC/MS data processing optimum experimental conditions were studied. Through the repeatability and accuracy testing of different samples, and with other laboratory data comparison, the repeatability of the method was illustrated with high accuracy.%采用气相色谱-质谱联用法测定柴油中多环芳烃,研究了固相萃取预处理样品影响因素和GC/MS气质联用数据处理最佳实验条件。通过对不同样品的重复性准确性试验,并与其它实验室进行数据比对,说明该方法的重复性好,准确度高。

  2. Determination of coumarin, vanillin, and ethyl vanillin in vanilla extract products: liquid chromatography mass spectrometry method development and validation studies.

    Science.gov (United States)

    de Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2007-03-23

    A LC-MS method was developed for the determination of coumarin, vanillin, and ethyl vanillin in vanilla products. Samples were analyzed using LC-electrospray ionization (ESI)-MS in the positive ionization mode. Limits of detection for the method ranged from 0.051 to 0.073 microg mL(-1). Using the optimized method, 24 vanilla products were analyzed. All samples tested negative for coumarin. Concentrations ranged from 0.38 to 8.59 mg mL(-1) (x =3.73) for vanillin and 0.33 to 2.27 mg mL(-1) (x =1.03) for ethyl vanillin. The measured concentrations are compared to values calculated using UV monitoring and to results reported in a similar survey in 1988. Analytical results, method precision, and accuracy data are presented.

  3. Validation of analytical conditions for determination of polycyclic aromatic hydrocarbons in roasted coffee by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Guatemala-Morales, Guadalupe María; Beltrán-Medina, Elisa Alejandra; Murillo-Tovar, Mario Alfonso; Ruiz-Palomino, Priscilla; Corona-González, Rosa Isela; Arriola-Guevara, Enrique

    2016-04-15

    Polycyclic aromatic hydrocarbons (PAHs) are of significant interest due to their genotoxicity in humans. PAHs quantification in coffee is complex since some of its compounds interfere in the chromatographic analysis, which hinders the reliable determination of the PAHs. Analytical conditions for the ultrasound extraction, purification and quantification of 16 PAHs in roasted coffee were studied. The better extraction efficiency of benzo[a]pyrene (68%) from ground-roasted coffee was achieved with a solvent ratio of Hex:MC (9:1 v/v) and three extraction periods of 20 min, followed by alkaline saponification and purification of the extracts. The detection limits were 0.85-39.32 ng mL(-1), and the quantification limits from 2.84 to 131.05 ng mL(-1), obtained for fluoranthene and chrysene, respectively. The extraction was effective for most of the analytes, with recoveries of 39.8% dibenzo[ah]anthracene and 69.0% benzo[b]fluoranthene. For coffee roasted in a spouted bed reactor, the summation of the 16 PAHs ranged from 3.5 to 16.4 μg kg(-1).

  4. Validation of analytical conditions for determination of polycyclic aromatic hydrocarbons in roasted coffee by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Guatemala-Morales, Guadalupe María; Beltrán-Medina, Elisa Alejandra; Murillo-Tovar, Mario Alfonso; Ruiz-Palomino, Priscilla; Corona-González, Rosa Isela; Arriola-Guevara, Enrique

    2016-04-15

    Polycyclic aromatic hydrocarbons (PAHs) are of significant interest due to their genotoxicity in humans. PAHs quantification in coffee is complex since some of its compounds interfere in the chromatographic analysis, which hinders the reliable determination of the PAHs. Analytical conditions for the ultrasound extraction, purification and quantification of 16 PAHs in roasted coffee were studied. The better extraction efficiency of benzo[a]pyrene (68%) from ground-roasted coffee was achieved with a solvent ratio of Hex:MC (9:1 v/v) and three extraction periods of 20 min, followed by alkaline saponification and purification of the extracts. The detection limits were 0.85-39.32 ng mL(-1), and the quantification limits from 2.84 to 131.05 ng mL(-1), obtained for fluoranthene and chrysene, respectively. The extraction was effective for most of the analytes, with recoveries of 39.8% dibenzo[ah]anthracene and 69.0% benzo[b]fluoranthene. For coffee roasted in a spouted bed reactor, the summation of the 16 PAHs ranged from 3.5 to 16.4 μg kg(-1). PMID:26617012

  5. Novel multiresidue method for determination of pesticides in red wine using gas chromatography-mass spectrometry and solid phase extraction.

    Science.gov (United States)

    Pelajić, Maja; Peček, Gorana; Mutavdžić Pavlović, Dragana; Vitali Čepo, Dubravka

    2016-06-01

    A new multiresidue method was developed for determination of 25 pesticide residues in red wine by gas chromatography coupled to mass spectrometry with a single run of 23.63 min. Samples were extracted from wine with solid phase extraction using Oasis HLB. Mixture of methanol and water was used for rinsing, while acetonitrile and n-hexane were used as elution solvents. Method was validated according to SANCO/12571/2013 criteria in wide linearity range (limit of quantification - 400 μg L(-1)). Limits of quantification (LOQ) were well below 10 μg L(-1) for most pesticides and recoveries at 2×LOQ and 10×LOQ concentration levels were in range 70-120%. Precision, expressed as a relative standard deviation, was always under 14%. The method was applied to 32 red wine samples from Croatia. Pesticides were detected in 30 samples with a total of 15 pesticides found, 7 of which were at a high concentration.

  6. Rapid determination of organochlorine pesticides in fish using selective pressurized liquid extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Choi, Minkyu; Lee, In-Seok; Jung, Rae-Hong

    2016-08-15

    A rapid automated extraction and cleanup method using selective pressurized liquid extraction was developed and validated for 14 organochlorine pesticides in fish. The lipid-removal efficiencies achieved by adding alumina, Florisil, acid-treated silica gel, and silica gel to the extraction cell were determined and optimized. In the optimized method, fish (2-3g) was placed above alumina (30 g) in the extraction cell, then the sample was extracted using a 7:3 mixture of hexane and dichloromethane. The method was validated using certified reference materials (NIST SRM 1946 and 1974c), spiked fish, and four lipid-rich fish samples. The mean low- and high-concentration spike recoveries were 91% and 93% with RSD<20%, respectively. Measured concentrations of target OCPs showed good agreement with the certified concentrations in certified reference materials. It suggests the good accuracy and precision of the SPLE method. The proposed method met the most important requirements of an extraction and cleanup procedure, including having a short preparation (cleanup and concentration) time and minimal sample contamination and being able to be automated. PMID:27006206

  7. Terbuthylazine and deethylterbuthylazine in rain and surface water - Determination by enzyme immunoassay and gas chromatography/mass spectrometry

    Science.gov (United States)

    Dankwardt, A.; Thurman, E.M.; Hock, B.

    1997-01-01

    Rain and surface water samples from Southern Germany were investigated from 1991 to 1995 for terbuthylazine and one of its major metabolites, deethylterbuthylazine. The concentrations observed were compared to the concentrations found for atrazine and deethylatrazine in the same water samples. Concentrations ranged from parent compound concentrations were calculated for deethylterbuthylazine to terbuthylazine (DTR) and deethylatrazine to atrazine (DAR). In rain water, DTR of 0.8...3.0 and DAR of 0.3...1.9 were determined with mean values of 0.9...1.7 for DTR and 0.6...0.9 for DAR in the different years. The ratios increased during summer periods. The highest ratios were observed in samples from forest stands, showing that degradation of the herbicide has occurred during transport between the source and the sampling site. The DTR in rain water were about 50...100% higher than the DAR. This indicates a higher degradation rate of terbuthylazine during atmospheric transport. In surface water, DTR of 0.3...1.2 with mean values of 0.5...0.8 and DAR of 0.2...2.2 with mean values of 0.2...1.3 were observed. The ratios increased from June to September.

  8. Simultaneous quantitative determination of alpha-ketoglutaric acid and 5-hydroxymethylfurfural in human plasma by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Wagner, Bernhard M; Donnarumma, Fabrizio; Wintersteiger, Reinhold; Windischhofer, Werner; Leis, Hans J

    2010-04-01

    Alpha-ketoglutaric acid (alpha-KG) and 5-hydroxymethylfurfural (5-HMF) are currently under investigation as promising cancer cell damaging agents. A method for the simultaneous quantitative determination of alpha-KG and 5-HMF in human plasma was established for screening these compounds in human plasma. Plasma samples were directly treated with O-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride to form the corresponding oximes, thus facilitating subsequent liquid-liquid extraction. After formation of the trimethylsilyl ethers, samples were analyzed by gas chromatography with electron ionization mass spectrometry. Stable isotope labeled standards were used, the preparation of (13)C(6)-5-HMF is described. Limits of quantitation were set to 0.938 microg/mL for alpha-KG and 0.156 microg/mL for 5-HMF. Inter-day accuracy was < or = 93.7% (alpha-KG) and < or = 92.8% (5-HMF). Inter-day precision was < or = 6.0% (alpha-KG) and < or = 4.6% (5-HMF). The method has been successfully applied to pharmacokinetic profiling of the compounds after intravenous application. PMID:20155414

  9. Enzyme-assisted extraction and liquid chromatography mass spectrometry for the determination of arsenic species in chicken meat.

    Science.gov (United States)

    Liu, Qingqing; Peng, Hanyong; Lu, Xiufen; Le, X Chris

    2015-08-12

    Chicken is the most consumed meat in North America. Concentrations of arsenic in chicken range from μg kg(-1) to mg kg(-1). However, little is known about the speciation of arsenic in chicken meat. The objective of this research was to develop a method enabling determination of arsenic species in chicken breast muscle. We report here enzyme-enhanced extraction of arsenic species from chicken meat, separation using anion exchange chromatography (HPLC), and simultaneous detection with both inductively coupled plasma mass spectrometry (ICPMS) and electrospray ionization tandem mass spectrometry (ESIMS). We compared the extraction of arsenic species using several proteolytic enzymes: bromelain, papain, pepsin, proteinase K, and trypsin. With the use of papain-assisted extraction, 10 arsenic species were extracted and detected, as compared to 8 detectable arsenic species in the water/methanol extract. The overall extraction efficiency was also improved using a combination of ultrasonication and papain digestion, as compared to the conventional water/methanol extraction. Detection limits were in the range of 1.0-1.8 μg arsenic per kg chicken breast meat (dry weight) for seven arsenic species: arsenobetaine (AsB), inorganic arsenite (As(III)), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), inorganic arsenate (As(V)), 3-nitro-4-hydroxyphenylarsonic acid (Roxarsone), and N-acetyl-4-hydroxy-m-arsanilic acid (NAHAA). Analysis of breast meat samples from six chickens receiving feed containing Roxarsone showed the presence of (mean±standard deviation μg kg(-1)) AsB (107±4), As(III) (113±7), As(V) (7±2), MMA (51±5), DMA (64±6), Roxarsone (18±1), and four unidentified arsenic species (approximate concentration 1-10 μg kg(-1)).

  10. Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather.

    Science.gov (United States)

    de Souza Silveira, Cristine D; Martendal, Edmar; Soldi, Valdir; Carasek, Eduardo

    2012-02-01

    This paper proposes a new analytical procedure based on the headspace solid-phase microextraction (HS-SPME) technique and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS-SPME were obtained through two experimental designs - a two-level fractional factorial design followed by a central composite design - using the commercial SPME fiber polyacrylate 85 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/g (2-phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.

  11. Enzyme-assisted extraction and liquid chromatography mass spectrometry for the determination of arsenic species in chicken meat.

    Science.gov (United States)

    Liu, Qingqing; Peng, Hanyong; Lu, Xiufen; Le, X Chris

    2015-08-12

    Chicken is the most consumed meat in North America. Concentrations of arsenic in chicken range from μg kg(-1) to mg kg(-1). However, little is known about the speciation of arsenic in chicken meat. The objective of this research was to develop a method enabling determination of arsenic species in chicken breast muscle. We report here enzyme-enhanced extraction of arsenic species from chicken meat, separation using anion exchange chromatography (HPLC), and simultaneous detection with both inductively coupled plasma mass spectrometry (ICPMS) and electrospray ionization tandem mass spectrometry (ESIMS). We compared the extraction of arsenic species using several proteolytic enzymes: bromelain, papain, pepsin, proteinase K, and trypsin. With the use of papain-assisted extraction, 10 arsenic species were extracted and detected, as compared to 8 detectable arsenic species in the water/methanol extract. The overall extraction efficiency was also improved using a combination of ultrasonication and papain digestion, as compared to the conventional water/methanol extraction. Detection limits were in the range of 1.0-1.8 μg arsenic per kg chicken breast meat (dry weight) for seven arsenic species: arsenobetaine (AsB), inorganic arsenite (As(III)), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), inorganic arsenate (As(V)), 3-nitro-4-hydroxyphenylarsonic acid (Roxarsone), and N-acetyl-4-hydroxy-m-arsanilic acid (NAHAA). Analysis of breast meat samples from six chickens receiving feed containing Roxarsone showed the presence of (mean±standard deviation μg kg(-1)) AsB (107±4), As(III) (113±7), As(V) (7±2), MMA (51±5), DMA (64±6), Roxarsone (18±1), and four unidentified arsenic species (approximate concentration 1-10 μg kg(-1)). PMID:26320952

  12. Methods of Analysis - Determination of Pyrethroid Insecticides in Water and Sediment Using Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Hladik, Michelle L.; Smalling, Kelly L.; Kuivila, Kathryn M.

    2009-01-01

    A method for the determination of 14 pyrethroid insecticides in environmental water and sediment samples is described. The method was developed by the U.S. Geological Survey in response to increasing concern over the effects of pyrethroids on aquatic organisms. The pyrethroids included in this method are ones that are applied to many agricultural and urban areas. Filtered water samples are extracted for pyrethroids using solid-phase extraction (SPE) with no additional cleanup steps. Sediment and soil samples are extracted using a microwave-assisted extraction system, and the pyrethroids of interest are separated from co-extracted matrix interferences by passing the extracts through stacked graphitized carbon and alumina SPE cartridges, along with the use of high-performance liquid chromatography and gel-permeation chromatography (HPLC/GPC). Quantification of the pyrethroids from the extracted water and sediment samples is done using gas chromatography with mass spectrometry (GC/MS) or gas chromatography with tandem mass spectrometry (GC/MS/MS). Recoveries in test water samples fortified at 10 ng/L ranged from 83 to 107 percent, and recoveries in test sediment samples fortified at 10 ug/kg ranged from 82 to 101 percent; relative standard deviations ranged from 5 to 9 percent in the water samples and 3 to 9 percent in the sediment samples. Method detection limits (MDLs), calculated using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), in water ranged from 2.0 to 6.0 ng/L using GC/MS and 0.5 to 1.0 ng/L using GC/MS/MS. For sediment, the MDLs ranged from 1.0 to 2.6 ug/kg dry weight using GC/MS and 0.2 to 0.5 ug/kg dry weight using GC/MS/MS. The matrix-spike recoveries for each compound, when averaged for 12 environmental water samples, ranged from 84 to 96 percent, and when averaged for 27 environmental sediment samples, ranged from 88 to 100 percent.

  13. Evaluation of magnetic nanoparticles to serve as solid-phase extraction sorbents for the determination of endocrine disruptors in milk samples by gas chromatography mass spectrometry.

    Science.gov (United States)

    Synaridou, Maria-Evangelia S; Sakkas, Vasilios A; Stalikas, Constantine D; Albanis, Triantafyllos A

    2014-06-27

    A rapid magnetic solid-phase extraction (MSPE) is proposed based on C18-functionalized magnetic silica nanoparticles as sorbents, for the determination of endocrine disruptors - 20 organochlorine pesticides and 6 polychlorinated biphenyls - in milk samples. Magnetic nanoparticles are characterized by several techniques, such as Scanning Electron Microscopy, X-Ray diffraction, Brunauer-Emmett-Teller and Fourier transform-infrared. The MSPE is performed by dispersion of the Fe3O4@SiO2@C18 nanoparticles in milk samples with sonication, after protein precipitation. Then, the sorbent is collected by applying an external magnetic field and the analytes are desorbed by n-hexane. Several parameters affecting the extraction efficiency of target analytes by the magnetic nanoparticles are investigated, including washing and elution solvents, amount of sorbents, time of extraction and elution, sample and elution solvent volume. The proposed method is optimized by means of experimental design and response surface methodology. When coupled with gas chromatography-mass spectrometry detection and under optimum extraction conditions, average recoveries of target analytes are found to be in the range of 79% to 116%. The proposed MSPE-GC-MS analytical method has a linear calibration curve for all target analytes with coefficients of determination to range from 0.9950 to 0.9999. The limits of quantification are found to be between 0.2 and 1μg/L ensuring compliance with the maximum residue limits established by European Commission and Codex Alimentarius, for OCPs and PCBs residues in milk. The proposed method is applied to the determination of target analytes in milk samples from local markets. PMID:24837417

  14. Micro-solid phase extraction followed by thermal extraction coupled with gas chromatography-mass selective detector for the determination of polybrominated diphenyl ethers in water.

    Science.gov (United States)

    Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

    2016-08-01

    A method of analyzing environmental contaminants in water based on micro-solid phase extraction (μ-SPE) followed by thermal extraction (TE) and a cold-trapping step, coupled with gas chromatography-mass selective detection (GC-MSD) was developed and validated. μ-SPE-TE- GC-MSD was employed in the determination of five polybrominated diphenyl ethers. The μ-SPE sorbent was chitosan-graphene oxide (CS-GO) composite, which was prepared by mixing CS and GO by means of ultrasonication. The CS in the composite was cross-linked with glutaraldehyde. After μ-SPE, the analytes in the extract were extracted thermally in a thermal desorption unit tube combined with a cooled injection system, coupled to GC-MSD. The extraction conditions were optimized for the detection of the target compounds in water. This method provided linearity ranges of between 0.1 and 20μgL(-1) (depending on the analytes), with coefficients of determination, r(2), ≥0.9982. The calculated relative recoveries were between 71.52 and 96.15% whereas precision (based on % relative standard deviations) was between 3.54 and 11.36%. The method showed limit of detection and limit of quantification ranges of between 0.007 and 0.016μgL(-1), and between 0.023 and 0.054μgL(-1), for the two groups of analytes, respectively. The method was applied to the determination of the target analytes in water. PMID:27373376

  15. [Determination of trichlorobenzenes in water-based cutting fluids and wastewater of machining using dispersive liquid-liquid microextraction-gas chromatography/mass spectrometry].

    Science.gov (United States)

    Shen, Haoyu; Zhao, Yonggang; Huai, Mingmin; Jiang, Hailiang

    2009-01-01

    The determination of trichlorobenzenes (TCBs) in water-based cutting fluids and wastewater of machining has been carried out. A gas chromatography/mass spectrometry (GC/ MS) method with selected ion monitoring (SIM) mode was employed. The target analyte was extracted from the matrix using dispersive liquid-liquid microextraction. Comparing with gas chromatography/electronic capture detection (GC/ECD) coupled with traditional sample preparation procedures, e.g. head-space extraction, liquid-liquid extraction and solid-phase extraction, the present method was accurate with broader linear range, better enrichment property, better replicability, easier to be operated and less interference. Overall recoveries were 94.7% - 104.3% with the relative standard deviations (RSDs) of at 2.3% - 7.8%. The detective limits for 1,3,5-, 1,2,4- and 1,2,3-trichlorobenzene were 2.0, 6.0 and 3.0 microg/L, respectively. The parameters, such as the nature and volume of extraction solvent, dispersive solvent, extraction time and salt effect, were studied and optimized. Some important factors, e.g., the concentration of common used additives in water-based cutting fluids, which may affect the recoveries and replicabilities for the determination of trichlorobenzenes, have been investigated. The result showed that no significant effects have been observed when the concentrations of NaNO2 and polyethylene glycol (PEG) were up to 1.0%. The present method has been applied for the determination of the trichlorobenzenes in 4 real samples. The result showed that two of them were found to contain these trichlorobenzenes. The TCBs in the samples were 0.15 - 1.67 mg/L.

  16. Evaluation of magnetic nanoparticles to serve as solid-phase extraction sorbents for the determination of endocrine disruptors in milk samples by gas chromatography mass spectrometry.

    Science.gov (United States)

    Synaridou, Maria-Evangelia S; Sakkas, Vasilios A; Stalikas, Constantine D; Albanis, Triantafyllos A

    2014-06-27

    A rapid magnetic solid-phase extraction (MSPE) is proposed based on C18-functionalized magnetic silica nanoparticles as sorbents, for the determination of endocrine disruptors - 20 organochlorine pesticides and 6 polychlorinated biphenyls - in milk samples. Magnetic nanoparticles are characterized by several techniques, such as Scanning Electron Microscopy, X-Ray diffraction, Brunauer-Emmett-Teller and Fourier transform-infrared. The MSPE is performed by dispersion of the Fe3O4@SiO2@C18 nanoparticles in milk samples with sonication, after protein precipitation. Then, the sorbent is collected by applying an external magnetic field and the analytes are desorbed by n-hexane. Several parameters affecting the extraction efficiency of target analytes by the magnetic nanoparticles are investigated, including washing and elution solvents, amount of sorbents, time of extraction and elution, sample and elution solvent volume. The proposed method is optimized by means of experimental design and response surface methodology. When coupled with gas chromatography-mass spectrometry detection and under optimum extraction conditions, average recoveries of target analytes are found to be in the range of 79% to 116%. The proposed MSPE-GC-MS analytical method has a linear calibration curve for all target analytes with coefficients of determination to range from 0.9950 to 0.9999. The limits of quantification are found to be between 0.2 and 1μg/L ensuring compliance with the maximum residue limits established by European Commission and Codex Alimentarius, for OCPs and PCBs residues in milk. The proposed method is applied to the determination of target analytes in milk samples from local markets.

  17. Salt-assisted dispersive liquid-liquid microextraction coupled with programmed temperature vaporization gas chromatography-mass spectrometry for the determination of haloacetonitriles in drinking water.

    Science.gov (United States)

    Ma, Huilian; Li, Yun; Zhang, Haijun; Shah, Syed Mazhar; Chen, Jiping

    2014-09-01

    We report here a new analytical method for the simultaneous determination of seven haloacetonitriles (HANs) in drinking water by coupling salt-assisted dispersive liquid-liquid microextraction (SADLLME) with programmed temperature vaporizer-gas chromatography-mass spectrometry (PTV-GC-MS). The newly developed method involves the dispersion of the extractant in aqueous sample by addition of a few grams of salt and no dispersion liquid was required as compared to the traditional DLLME methods. The extractant (CH2Cl2, 50μL) and the salt (Na2SO4, 2.4g) were successively added to water (8mL) in a conical centrifuge tube that was shaken for 1min and centrifuged (3500rpm, 3min). The aliquot of sedimented phase (4μL) was then directly injected into the PTV-GC-MS system. The limits of detection and quantification for the HANs were 0.4-13.2ngL(-1) and 1.2-43.9ngL(-1), respectively. The calibration curves showed good linearity (r(2)≥0.9904) over 3 orders of magnitude. The repeatability of the method was investigated by evaluating the intra- and inter-day precisions. The relative standard deviations (RSDs) obtained were lower than 10.2% and 7.8% at low and high concentration levels. The relative recoveries ranged from 79.3% to 105.1%. The developed methodology was applied for the analysis of seven HANs in several drinking water samples in coastal and inland cities of China. It was demonstrated to be a simple, sensible, reproducible and environment friendly method for the determination of trace HANs in drinking water samples.

  18. Study of different HILIC, mixed-mode, and other aqueous normal-phase approaches for the liquid chromatography/mass spectrometry-based determination of challenging polar pesticides.

    Science.gov (United States)

    Vass, Andrea; Robles-Molina, José; Pérez-Ortega, Patricia; Gilbert-López, Bienvenida; Dernovics, Mihaly; Molina-Díaz, Antonio; García-Reyes, Juan F

    2016-07-01

    The aim of the study was to evaluate the performance of different chromatographic approaches for the liquid chromatography/mass spectrometry (LC-MS(/MS)) determination of 24 highly polar pesticides. The studied compounds, which are in most cases unsuitable for conventional LC-MS(/MS) multiresidue methods were tested with nine different chromatographic conditions, including two different hydrophilic interaction liquid chromatography (HILIC) columns, two zwitterionic-type mixed-mode columns, three normal-phase columns operated in HILIC-mode (bare silica and two silica-based chemically bonded columns (cyano and amino)), and two standard reversed-phase C18 columns. Different sets of chromatographic parameters in positive (for 17 analytes) and negative ionization modes (for nine analytes) were examined. In order to compare the different approaches, a semi-quantitative classification was proposed, calculated as the percentage of an empirical performance value, which consisted of three main features: (i) capacity factor (k) to characterize analyte separation from the void, (ii) relative response factor, and (iii) peak shape based on analytes' peak width. While no single method was able to provide appropriate detection of all the 24 studied species in a single run, the best suited approach for the compounds ionized in positive mode was based on a UHPLC HILIC column with 1.8 μm particle size, providing appropriate results for 22 out of the 24 species tested. In contrast, the detection of glyphosate and aminomethylphosphonic acid could only be achieved with a zwitterionic-type mixed-mode column, which proved to be suitable only for the pesticides detected in negative ion mode. Finally, the selected approach (UHPLC HILIC) was found to be useful for the determination of multiple pesticides in oranges using HILIC-ESI-MS/MS, with limits of quantitation in the low microgram per kilogram in most cases. Graphical Abstract HILIC improves separation of multiclass polar pesticides

  19. [Determination of tris (2-chloroethyl) phosphate in leather by gas chromatography-mass spectrometry coupled with mixed-mode sorbent solid phase extraction].

    Science.gov (United States)

    Zhang, Weiya; Zhu, Yuling; Wang, Chengyun; Li, Lixia; Zhang, Junqing; Xing, Jun

    2014-10-01

    Leather is one of the important exporting products to European Union (EU), and tris(2-chloroethyl) phosphate (TCEP) is a commonly used flame retardant in leather and leather products. Recently, TCEP has been classified as a kind of substance of very high concern (SVHC) by EU for its carcinogenicity and reproductive toxicity. But to date, there is not a recognized method for the determination of TCEP in leather and leather products due to the serious matrix interferences and relatively low recovery of TCEP. In this work, a home-made mixed-mode sorbent (Silica-WCX) with carboxyl and alkyl groups was tested as the sorbent of solid phase extraction (SPE) to extract TECP from leather. The results demonstrated that, making the carboxyl groups protonized under acidic condition, Silica-WCX exhibited better extraction performance towards TCEP over some frequently used commercial sorbents tested. After the optimization of the SPE conditions based on Silica-WCX, a method of gas chromatography/mass spectrometry (GC-MS) was established for the determination of TCEP in leather samples. The linear range for TCEP ranged from 0.10 to 100.0 μg/L and the limit of quantification (LOQ, S/N = 10) was 44.46 ng/kg. The recoveries of TCEP spiked in samples at varied levels were in the range of 91.45%-99.98% with the relative standard deviations (RSDs) of 4.33%-5.97%. The method is simple, sensitive and reliable for the analysis of TCEP in leather and leather products.

  20. Determination of five booster biocides in seawater by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Giráldez, I; Chaguaceda, E; Bujalance, M; Morales, E

    2013-01-01

    Stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) have been optimized for the determination of five organic booster biocides (Chlorothalonil, Dichlofluanid, Sea-Nine 211, Irgarol 1051 and TCMTB) in seawater samples. The parameters affecting the desorption and absorption steps were investigated using 10 mL seawater samples. The optimised conditions consisted of an addition of 0.2 g mL(-1) KCl to the sample, which was extracted with 10mm length, 0.5mm film thickness stir bars coated with polydimethylsiloxane (PDMS), and stirred at 900 rpm for 90 min at room temperature (25 °C) in a vial. Desorption was carried out at 280 °C for 5 min under 50 mL min(-1) of helium flow in the splitless mode while maintaining a cryotrapping temperature of 20 °C in the programmed-temperature vaporization (PTV) injector of the GC-MS system. Finally, the PTV injector was ramped to a temperature of 280 °C and the analytes were separated in the GC and detected by MS using the selected-ion monitoring (SIM) mode. The detection limits of booster biocides were found to be in the range of 0.005-0.9 μg L(-1). The regression coefficients were higher than 0.999 for all analytes. The average recovery was higher than 72% (R.S.D.: 7-15%). All these figures of merit were established running samples in triplicate. This simple, accurate, sensitive and selective analytical method may be used for the determination of trace amounts of booster biocides in water samples from marinas. PMID:23246091

  1. Study of different HILIC, mixed-mode, and other aqueous normal-phase approaches for the liquid chromatography/mass spectrometry-based determination of challenging polar pesticides.

    Science.gov (United States)

    Vass, Andrea; Robles-Molina, José; Pérez-Ortega, Patricia; Gilbert-López, Bienvenida; Dernovics, Mihaly; Molina-Díaz, Antonio; García-Reyes, Juan F

    2016-07-01

    The aim of the study was to evaluate the performance of different chromatographic approaches for the liquid chromatography/mass spectrometry (LC-MS(/MS)) determination of 24 highly polar pesticides. The studied compounds, which are in most cases unsuitable for conventional LC-MS(/MS) multiresidue methods were tested with nine different chromatographic conditions, including two different hydrophilic interaction liquid chromatography (HILIC) columns, two zwitterionic-type mixed-mode columns, three normal-phase columns operated in HILIC-mode (bare silica and two silica-based chemically bonded columns (cyano and amino)), and two standard reversed-phase C18 columns. Different sets of chromatographic parameters in positive (for 17 analytes) and negative ionization modes (for nine analytes) were examined. In order to compare the different approaches, a semi-quantitative classification was proposed, calculated as the percentage of an empirical performance value, which consisted of three main features: (i) capacity factor (k) to characterize analyte separation from the void, (ii) relative response factor, and (iii) peak shape based on analytes' peak width. While no single method was able to provide appropriate detection of all the 24 studied species in a single run, the best suited approach for the compounds ionized in positive mode was based on a UHPLC HILIC column with 1.8 μm particle size, providing appropriate results for 22 out of the 24 species tested. In contrast, the detection of glyphosate and aminomethylphosphonic acid could only be achieved with a zwitterionic-type mixed-mode column, which proved to be suitable only for the pesticides detected in negative ion mode. Finally, the selected approach (UHPLC HILIC) was found to be useful for the determination of multiple pesticides in oranges using HILIC-ESI-MS/MS, with limits of quantitation in the low microgram per kilogram in most cases. Graphical Abstract HILIC improves separation of multiclass polar pesticides.

  2. Determination of chlorobutanol in cosmetics by gas chromatography-mass spectrometry%气相色谱-质谱法测定化妆品中的三氯叔丁醇

    Institute of Scientific and Technical Information of China (English)

    刘茜; 马强; 席海为; 王烨; 白桦; 王超

    2011-01-01

    建立了测定化妆品中三氯叔丁醇的气相色谱-质谱分析方法.膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品加入50%甲醇-无水乙醇或无水乙醇超声提取后,样品提取液高速离心处理,取上清液经无水硫酸钠脱水,进行气相色谱-质谱定性及定量分析.选用DB-1701(30 m×0.25 mm×0.25μm)石英毛细管柱,程序升温,流速1.0 mL/min,采用电子轰击电离源,选择监测离子(m/z 53、59、125,其中59为定量离子),外标法定量.方法的平均回收率为83.4%~107.6%,相时标准偏差(RSD)为1.0% ~5.3%,膏霜、水剂、散粉、香波、唇膏等不同类型化妆品中二氯叔丁醇的检出限均为0.8 mg/kg.%A gas chromatography-mass spectrometric method was developed for the determination of chlorobutanol in cosmetic samples. Hie cream, lotion, powder, shampoo and lipstick samples were ultrasonically extracted with 50% methanol-ethanol or ethanol, and then centrifuged. The eluent was further dehydrated and then analyzed with a capillary column ( DB-1701, 30 m × 0.25 mm × 0.25 jjun) under electron ionization conditions at a flow rate of 1. 0 mL/min. The quantitation was performed by the external standard method under selected ion monitoring mode (SIM) using monitoring ions of m/z 53, 59, 125. The recoveries were 83. 4% ~ 107.6% , with the relative standard deviations (RSDs) of 1.0% ~5. 3%. All the detection limit of cream, lotion, powder, shampoo and lipstick samples was 0. 8 mg/kg. This method was proved to be simple, accurate, and stable by testing experiments, which was suitable for the detection of chlorobutanol in cosmetics.

  3. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.)

  4. Photometric and emission-spectrometric determination of boron in steels

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  5. In-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction and silylation prior gas chromatography-mass spectrometry for ultraviolet filters determination in environmental water samples.

    Science.gov (United States)

    Clavijo, Sabrina; Avivar, Jessica; Suárez, Ruth; Cerdà, Víctor

    2016-04-22

    A novel online approach involving in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction and derivatization coupled to gas chromatography-mass spectrometry has been developed for the determination of seven UV filters extensively used in cosmetic products in environmental water samples. The effect of parameters such as the type and volume of extraction solvent, dispersive solvent and derivatization agent, pH, ionic strength and stirring time, was studied using multivariate experimental design. Extraction, derivatization and preconcentration were simultaneously performed using acetone as dispersive solvent, N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) as derivatization agent and trichloroethylene as extraction solvent. After stirring during 160s, the sedimented phase was transferred to a rotary micro-volume injection valve (3 μL) and introduced by an air stream into the injector of the GC through a stainless-steel tube used as interface. The detection limits were in the range of 0.023-0.16 μg L(-1) and good linearity was observed up to 500 μg L(-1) of the studied UV filters, with R(2) ranging between 0.9829 and 0.9963. The inter-day precision expressed as relative standard deviation (n=5) varied between 5.5 and 16.8%. Finally, the developed method was satisfactorily applied to assess the occurrence of the studied UV filters in seawater and pool water samples. Some of the studied UV filters were found in these samples and an add-recovery test was also successfully performed with recoveries between 82 and 111%.

  6. Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of synthetic musk fragrances in aqueous matrices by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Homem, Vera; Alves, Alice; Alves, Arminda; Santos, Lúcia

    2016-01-01

    A rapid and simple method for the simultaneous determination of twelve synthetic musks in water samples, using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was successfully developed. The influence of seven factors (volume of the extraction solvent and disperser solvent, sample volume, extraction time, ionic strength, type of extraction and disperser solvent) affecting the UA-DLLME extraction efficiency was investigated using a screening design. The significant factors were selected and optimised employing a central composite design: 80 μL of chloroform, 880 μL of acetonitrile, 6 mL of sample volume, 3.5% (wt) of NaCl and 2 min of extraction time. Under the optimised conditions, this methodology was successfully validated for the analysis of 12 synthetic musk compounds in different aqueous samples (tap, sea and river water, effluent and influent wastewater). The proposed method showed enrichment factors between 101 and 115 depending on the analyte, limits of detection in the range of 0.004-54 ng L(-1) and good repeatability (most relative standard deviation values below 10%). No significant matrix effects were found, since recoveries ranged between 71% and 118%. Finally, the method was satisfactorily applied to the analysis of five different aqueous samples. Results demonstrated the existence of a larger amount of synthetic musks in wastewaters than in other water samples (average concentrations of 2800 ng L(-1) in influent and 850 ng L(-1) in effluent). Galaxolide, tonalide and exaltolide were the compounds most detected.

  7. Development of a method for the determination of cocaine, cocaethylene and norcocaine in human breast milk using liquid phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Silveira, Gabriela de Oliveira; Belitsky, Íris Tikkanen; Loddi, Silvana; Rodrigues de Oliveira, Carolina Dizioli; Zucoloto, Alexandre Dias; Fruchtengarten, Ligia Veras Gimenez; Yonamine, Mauricio

    2016-08-01

    Most licit and illicit substances consumed by the nursing mother might be excreted in breast milk, which may cause potential short and long term harmful effects for the breastfed infant. The extraction of substances from this matrix represents an analytical challenge due to its high protein and fat content as well as the fact that its composition changes during postpartum period. The aim of the present study was to develop a liquid phase microextraction (LPME) method for detection of the active substances: cocaine (COC), cocaethylene (CE) and norcocaine (NCOC) in human breast milk using gas chromatography-mass spectrometry (GC-MS). Validation was performed working on spiked human breast milk samples. The limits of detection (LOD) and quantification (LOQ) were of 6 and 12ng/mL, respectively, for all analytes. Calibration curves were linear over a concentration range of 12.0ng/mL-1000ng/mL (r(2)=0.99). No interferences were noticed at the retention times of interest. Within-run and between-run precision was always less or equal to 15 as % relative standard deviation, and bias ranged from 3 to 18%. Forty six milk samples were analyzed. Only one sample was confirmed to be COC positive (138ng/mL) and another one presented COC concentration near the LOD (6ng/mL). This method has shown to be a reliable alternative for the determination of cocaine, cocaethylene and norcocaine in human breast milk in the fields of clinical and forensic toxicology. LPME extraction procedure demonstrated to be a rather promising, low cost and environmental-friendly technique for the purpose of this study.

  8. Determination and kinetics of enrofloxacin and ciprofloxacin in Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a liquid chromatography/mass spectrometry method.

    Science.gov (United States)

    Danyi, S; Widart, J; Douny, C; Dang, P K; Baiwir, D; Wang, N; Tu, H T; Tung, V T; Phuong, N-T; Kestemont, P; Scippo, M-L

    2011-04-01

    Determination and kinetics of enrofloxacin and ciprofloxacin in Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a liquid chromatography/mass spectrometry method. J. vet. Pharmacol. Therap. 34, 142-152. The fluoroquinolones enrofloxacin (EF) and ciprofloxacin (CF) residues were investigated in the edible tissues of two important Asian aquacultured species such as Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry method. Fish and prawn were treated with medicated feed with multiple doses of EF, in field conditions. A validation study of the analytical method was realized in terms of linearity, specificity, precision (repeatability and within-laboratory reproducibility), recovery and decision limit (CCα). The time needed before the antibiotic disappears from animal tissues or reach the maximum residue limit (MRL, 100μg/kg) was assessed. The concentration values of EF detected in Tra catfish tissue were between the MRL and 2×MRL concentrations, according to the fish density, 7days following the end of the enrofloxacin treatment (20mg/kg body weight per day, for seven consecutive days). The concentration value of ER in prawn tissue was lower than the MRL and the limit of quantification (LOQ, 14μg/kg) 5 and 7days after the stop of the EF treatment (50mg/kg body weight per day, for five consecutive days), respectively. The mean detected levels of CF was much lower in comparison with that of EF, indicating that only a small part of EF is metabolized into CF (<5%) in both Tra catfish and prawn.

  9. Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of synthetic musk fragrances in aqueous matrices by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Homem, Vera; Alves, Alice; Alves, Arminda; Santos, Lúcia

    2016-02-01

    A rapid and simple method for the simultaneous determination of twelve synthetic musks in water samples, using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was successfully developed. The influence of seven factors (volume of the extraction solvent and disperser solvent, sample volume, extraction time, ionic strength, type of extraction and disperser solvent) affecting the UA-DLLME extraction efficiency was investigated using a screening design. The significant factors were selected and optimised employing a central composite design: 80 μL of chloroform, 880 μL of acetonitrile, 6 mL of sample volume, 3.5% (wt) of NaCl and 2 min of extraction time. Under the optimised conditions, this methodology was successfully validated for the analysis of 12 synthetic musk compounds in different aqueous samples (tap, sea and river water, effluent and influent wastewater). The proposed method showed enrichment factors between 101 and 115 depending on the analyte, limits of detection in the range of 0.004-54 ng L(-1) and good repeatability (most relative standard deviation values below 10%). No significant matrix effects were found, since recoveries ranged between 71% and 118%. Finally, the method was satisfactorily applied to the analysis of five different aqueous samples. Results demonstrated the existence of a larger amount of synthetic musks in wastewaters than in other water samples (average concentrations of 2800 ng L(-1) in influent and 850 ng L(-1) in effluent). Galaxolide, tonalide and exaltolide were the compounds most detected. PMID:26653427

  10. Evaluation of dispersive liquid-liquid microextraction for the simultaneous determination of chlorophenols and haloanisoles in wines and cork stoppers using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Campillo, Natalia; Viñas, Pilar; Cacho, Juan I; Peñalver, Rosa; Hernández-Córdoba, Manuel

    2010-11-19

    Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was evaluated for the simultaneous determination of five chlorophenols and seven haloanisoles in wines and cork stoppers. Parameters, such as the nature and volume of the extracting and disperser solvents, extraction time, salt addition, centrifugation time and sample volume or mass, affecting the DLLME were carefully optimized to extract and preconcentrate chlorophenols, in the form of their acetylated derivatives, and haloanisoles. In this extraction method, 1mL of acetone (disperser solvent) containing 30μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5mL of sample solution containing 200μL of acetic anhydride (derivatizing reagent) and 0.5mL of phosphate buffer solution, thereby forming a cloudy solution. After extraction, phase separation was performed by centrifugation, and a volume of 4μL of the sedimented phase was analyzed by GC-MS. The wine samples were directly used for the DLLME extraction (red wines required a 1:1 dilution with water). For cork samples, the target analytes were first extracted with pentane, the solvent was evaporated and the residue reconstituted with acetone before DLLME. The use of an internal standard (2,4-dibromoanisole) notably improved the repeatability of the procedure. Under the optimized conditions, detection limits ranged from 0.004 to 0.108ngmL(-1) in wine samples (24-220pgg(-1) in corks), depending on the compound and the sample analyzed. The enrichment factors for haloanisoles were in the 380-700-fold range. PMID:20956005

  11. Xylem sap collection and extraction methodologies to determine in vivo concentrations of ABA and its bound forms by gas chromatography-mass spectrometry (GC-MS

    Directory of Open Access Journals (Sweden)

    Netting Andrew G

    2012-03-01

    Full Text Available Abstract Background Accurate quantification of xylem sap ABA concentrations is important to underpin models of root-to-shoot ABA signalling to predict the physiological effects of soil drying. Growing tomato plants in a whole plant pressure chamber allowed sequential xylem sap collection from a detached leaf, the petiole stub of an otherwise intact plant and finally the de-topped root system of the same plant, to determine the impact of xylem sap sampling methodology on xylem ABA concentration. Since xylem sap can contain bound forms of ABA, a novel gas chromatography-mass spectrometry (GC-MS procedure was developed to chemically separate free ABA from two in planta bound ABA forms known as Adducts I and II and ABA-glucose-ester (ABA-GE. Results Xylem sap ABA concentrations were highly dependent on the sampling methodology used: the highest concentrations were detected in sap collected by applying an overpressure to detached leaves following the measurement of leaf water potential. Irrespective of xylem sap source, the wild-type cultivars Ailsa Craig and Rheinlands Ruhm had higher free ABA concentrations than a range of ABA-deficient mutants (notabilis, flacca and sitiens. However, in the mutants, concentrations of bound forms of ABA were similar to wild-type plants, and similar to free ABA concentrations. Conclusions Although xylem concentrations of these bound ABA forms and ABA-GE suggest they have a limited physiological impact on ABA homeostasis in tomato, the methods developed here will allow a more complete understanding of ABA biochemistry and root-to-shoot signalling in species known to have higher concentrations of these compounds.

  12. Fully automated determination of parabens, triclosan and methyl triclosan in wastewater by microextraction by packed sorbents and gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Marino, Iria, E-mail: iria.gonzalez@usc.es [Department of Analytical Chemistry, Nutrition and Food Sciences, Institute for Food Analysis and Research-IIAA, University of Santiago de Compostela, 15782 Santiago de Compostela (Spain); Benito Quintana, Jose; Rodriguez, Isaac [Department of Analytical Chemistry, Nutrition and Food Sciences, Institute for Food Analysis and Research-IIAA, University of Santiago de Compostela, 15782 Santiago de Compostela (Spain); Schrader, Steffi; Moeder, Monika [Department of Analytical Chemistry, Helmholtz Centre for Environmental Research-UFZ, Permoserstrasse 15, D-04318 Leipzig (Germany)

    2011-01-17

    A fully automated method for the determination of triclosan (TCS), its derivative methyl triclosan (MeTCS) and six parabens (esters of 4-hydroxybenzoic acid) including branched and linear isomers of propyl (i-PrP and n-PrP) and butyl paraben (i-BuP and n-BuP) in sewage water samples is presented. The procedure includes analytes enrichment by microextraction by packed sorbent (MEPS) coupled at-line to large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS). Under optimised conditions, compounds were extracted from 2 mL samples, adjusted at pH 3, using a C18 MEPS-sorbent. Adsorbed analytes were eluted directly into the Programmable Temperature Vaporizer (PTV) injector of the chromatograph with 2 x 25 {mu}L of ethyl acetate. They were quantified using standard solutions in ultrapure water submitted to the same sample enrichment process as real sewage water samples. After signal normalisation using isotopic labelled species as internal surrogates, no differences were noticed among the extraction efficiency for sewage and ultrapure water; moreover, the proposed method reported lineal calibration curves from 0.1 to 10 ng mL{sup -1}, relative standard deviations (%RSD) between 2 and 7.1% and limits of detection (LODs) varying from 0.001 to 0.015 ng mL{sup -1} in ultrapure water and from 0.02 to 0.59 ng mL{sup -1} in the most complex sample (raw wastewater).

  13. Development of a method for the determination of cocaine, cocaethylene and norcocaine in human breast milk using liquid phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Silveira, Gabriela de Oliveira; Belitsky, Íris Tikkanen; Loddi, Silvana; Rodrigues de Oliveira, Carolina Dizioli; Zucoloto, Alexandre Dias; Fruchtengarten, Ligia Veras Gimenez; Yonamine, Mauricio

    2016-08-01

    Most licit and illicit substances consumed by the nursing mother might be excreted in breast milk, which may cause potential short and long term harmful effects for the breastfed infant. The extraction of substances from this matrix represents an analytical challenge due to its high protein and fat content as well as the fact that its composition changes during postpartum period. The aim of the present study was to develop a liquid phase microextraction (LPME) method for detection of the active substances: cocaine (COC), cocaethylene (CE) and norcocaine (NCOC) in human breast milk using gas chromatography-mass spectrometry (GC-MS). Validation was performed working on spiked human breast milk samples. The limits of detection (LOD) and quantification (LOQ) were of 6 and 12ng/mL, respectively, for all analytes. Calibration curves were linear over a concentration range of 12.0ng/mL-1000ng/mL (r(2)=0.99). No interferences were noticed at the retention times of interest. Within-run and between-run precision was always less or equal to 15 as % relative standard deviation, and bias ranged from 3 to 18%. Forty six milk samples were analyzed. Only one sample was confirmed to be COC positive (138ng/mL) and another one presented COC concentration near the LOD (6ng/mL). This method has shown to be a reliable alternative for the determination of cocaine, cocaethylene and norcocaine in human breast milk in the fields of clinical and forensic toxicology. LPME extraction procedure demonstrated to be a rather promising, low cost and environmental-friendly technique for the purpose of this study. PMID:26826849

  14. Determination of alkylphenols and phthalate esters in vegetables and migration studies from their packages by means of stir bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2012-06-01

    This paper describes a method for the determination of three alkylphenols (APs), 4-tert-octylphenol (tOP), 4-n-octylphenol (OP) and 4-nonylphenol (NP), and six phthalate esters (PEs), dimethylphthalate (DMP), diethylphthalate (DEP), di-n-butylphthalate (DBP), n-butylbenzylphthalate (BBP), di-2-ethylhexylphthalate (DEHP) and di-n-octylphthalate (DOP), in vegetables using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Ultrasonic radiation was used to extract the analytes from the solid food matrix, and the extract obtained was preconcentrated by SBSE. The different parameters affecting both stages were carefully optimized. The method was applied to analyze commercial vegetables, in the form of plastic packed salads and canned greens, as well as the corresponding filling liquids of the canned food. Quantification of the samples was carried out against aqueous standards using an internal standard (anthracene). The analysis of a 2 g vegetable sample provided detection limits between 12.7 and 105.8 pg g⁻¹ for OP and DEHP, respectively. Migration studies from the plastic packages of the vegetables samples analyzed were carried out. DEP, DBP and DEHP were found to have migrated from the bags to the simulant and the same compounds were quantified in lettuce, corn salad, arugula, parsley and chard, at concentration levels in the 8-51 ng g⁻¹ range. However, OP and NP were found in only two vegetable samples and one filling liquid, but neither was detected in any package. The proposed method provided recoveries of 83-118%.

  15. Chemometric-based determination of polycyclic aromatic hydrocarbons in aqueous samples using ultrasound-assisted emulsification microextraction combined to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ahmadvand, Mohammad; Sereshti, Hassan; Parastar, Hadi

    2015-09-25

    In the present research, ultrasonic-assisted emulsification-microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS) has been proposed for analysis of thirteen environmental protection agency (EPA) polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Tetrachloroethylene was selected as extraction solvent. The main parameters of USAEME affecting the efficiency of the method were modeled and optimized using a central composite design (CCD). Under the optimum conditions (9μL for extraction solvent, 1.15% (w/v) NaCl (salt concentration) and 10min for ultrasonication time), preconcentration factor (PF) of the PAHs was in the range of 500-950. In order to have a comprehensive analysis, multivariate curve resolution-alternating least squares (MCR-ALS) as a second-order calibration algorithm was used for resolution, identification and quantification of the target PAHs in the presence of uncalibrated interferences. The regression coefficients and relative errors (REs, %) of calibration curves of the PAHs were in the satisfactory range of 0.9971-0.9999 and 1.17-6.59%, respectively. Furthermore, analytical figures of merit (AFOM) for univariate and second-order calibrations were obtained and compared. As an instance, the limit of detections (LODs) of target PAHs were in the range of 1.87-18.9 and 0.89-6.49ngmL(-1) for univariate and second-order calibration, respectively. Finally, the proposed strategy was used for determination of target PAHs in real water samples (tap and hookah waters). The relative recoveries (RR) and the relative standard deviations (RSDs) were 68.4-109.80% and 2.15-6.93%, respectively. It was concluded that combination of multivariate chemometric methods with USAEME-GC-MS can be considered as a new insight for the analysis of target analytes in complex sample matrices. PMID:26319375

  16. Determination of anabolic esters in oily formulations and plasma in husbandry using high-performance liquid chromatography and gas chromatography-mass selective detection.

    Science.gov (United States)

    Hooijerink, D; Schilt, R; van Bennekom, E; Brouwer, B

    1994-12-01

    Two different analytical methods are described for the analysis of anabolic steroid esters in oily formulations for veterinary use and animal plasma samples, respectively. For the determination of anabolic steroid esters in oily formulations (at mg kg-1 levels) a reversed-phase high-performance liquid chromatographic method with gradient elution is described. Gradient elution is performed owing to the relatively large variations in polarity of the investigated anabolic steroid esters. For the analysis of anabolic steroid esters in plasma (at ng ml-1 levels) two different strategies are applied. After solid-phase extraction, the plasma samples are introduced into the high-performance liquid chromatography (HPLC) system where the obtained fractions are then analysed by using gas chromatography-mass selective detection (GC-MSD). An alternative method is direct analysis of plasma samples after solid-phase extraction by using GC-MSD without any further clean-up procedure. Prior to GC-MSD the samples are derivatized to corresponding trifluoroacyl (TFA) derivatives. The calibration graph for HPLC is rectilinear over the range 25-150 ng ml-1 plasma and the analytical recoveries for medroxyprogesterone acetate (MPA) and testosterone propionate (TP) are more than 95%. The detection limits for both analytes in GC-MS are 2.5 ng ml-1 plasma for MPA and 0.5 ng ml-1 plasma for TP with an acceptable signal-to-noise ratio (calculated for the derivatized relative molecular mass). In the analysis of plasma obtained from animal experiments concentrations of 6.5 ng ml-1 are found for MPA by using GC-MSD and 5.0 ng ml-1 are found for nortestosterone laurate (NL) by using HPLC. PMID:7879863

  17. Graphitic carbon nitrides modified hollow fiber solid phase microextraction for extraction and determination of uric acid in urine and serum coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sun, Ying-pei; Chen, Juan; Qi, Huan-yang; Shi, Yan-ping

    2015-11-01

    An elevated uric acid (UA) in urine or serum can affect renal function and blood pressure, which is an indicator of gout, cardiovascular and renal diseases, hypertension, etc. In this work, a new type of mixed matrix membrane (MMM), based on graphitic carbon nitrides (g-CNs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine UA in urine and serum followed by gas chromatography-mass spectrometry (GC/MS). The porous g-CNs were dispersed in ammonia, and then the exfoliated g-CNs nanosheets were held in the pores of HF by capillary forces and sonification. The prepared g-CNs modified HF (g-CNs-HF) was immersed in biofluid directly to extract UA with SPME mode and the solvent-free mode is convenient for further derivatization and analysis. To achieve the highest extraction efficiency (EF), main extraction and derivatization parameters, such as g-CNs-HF immobilizing time, sonification power and time of extraction, derivatization and desorption time, were optimized. Under the optimum extraction conditions, a favorable linearity of UA was obtained in the range 0.1-200μgmL(-1) with correlation coefficients higher than 0.9990, and the average recoveries at three spiked levels of UA in urine and serum ranged from 80.7% to 121.6%, from 84.7% to 101.1%, respectively. The obtained results demonstrated the developed g-CNs-HF-SPME is a simple, rapid, cost-effective, solvent-free method for the analysis of UA in biofluid.

  18. Simultaneous determination of pesticide residues in food safety risk monitoring in 2011 by gas chromatography-mass spectrometry%GC-MS法同时测定食品风险监测样品中的农残

    Institute of Scientific and Technical Information of China (English)

    沈平; 彭进; 谢朝梅; 谢燕湘; 谢敏

    2011-01-01

    Objective: To establish a gas chromatography - mass spectrometric method for simultaneous determination of pesticide residues in food safety risk monitoring samples. The pesticides include 9 kinds of organophosphorus, 1 kind of organochlorine pesticides, 3 kinds of carbamates and 4 kinds of pyrethroids. Methods: Samples were extracted using acetonitrile and then rotary evaporated to nearly dryness, the concentrated extract was dissolved with acetone and methylene chloride mixture and dehydrated with anhydrous Na2SO4 and finally purified with Carb/NH2 column and silicon magnesium column, the purified solution was concentrated before analyzed by GC. MS. Results: The results showed that the detection limit was 0.01 mg/L ~0.05 mg/L for organophosphorus ,0.005 mg/L for organochlorines ,0.03 mg/I, for carbomates and 0.005 mg/L ~ 0.01 mg/L for pyrethroids. The linear coefficient was ≥0.995 with recoveries of 67.6% -108.3% ,and the RSD was 2.5% ~8.3%. Conclusion: This method is able to determine all pesticide residues in food safety risk monitoring samples in 2011 at the same chromatographic and mass spectrometric conditions,and the method is sensitive and reproducible with high accuracy and precision, which can be used in the actual testing analysis.%目的:建立同时检测食品安全风险监测样品中的农残的GC-MS法,农残包括有机磷类9种、有机氯类1种、氨基甲酸酯类3种、拟除虫菊酯类4种.方法:样品中所含农药残留用乙腈一并提取,浓缩至近干,经丙酮和二氯甲烷混合液溶解,无水Na2SO4脱水,过Carb/NH2柱、硅镁柱净化,浓缩后用GC-MS法测定.结果:有机磷农药最低检出浓度为0.01 mg/L-0.05 mg/L,有机氯为0.005 mg/L,氨基甲酸酯类为0.03 mg/L,拟除虫菊酯为0.005 mg/L -0.01 mg/L,标准曲线r值均≥0.995,加标回收率为67.6%-108.3%,RSD为2.5%-8.3%.结论:该法能将2011年食品安全风险监测所有的农残类项目在同一色谱及质谱条件下检测,能实现良好的

  19. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  20. Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

    Science.gov (United States)

    Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

    1998-01-01

    Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected

  1. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Directory of Open Access Journals (Sweden)

    Hesham Salem

    2005-01-01

    Full Text Available Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate. The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed native fluorescence at 450 nm when excitation was at 290 nm. The calibration graph was rectilinear from 0.3-1.4 μg mL-1 (method I. Cobalt sulphate was used for precipitation of the ion associates formed from the reaction with the cited drugs. The formation and solubility of the solid complexes at the optimum conditions of pH and ionic strength values have been studied. The method depends on direct determination of the ions in the precipitate or indirect determination of the ions in the filtrate by atomic absorption spectroscopy. The optimum conditions for precipitation were carefully studied. Rectilinear calibration graphs were obtained in the range of 3-30 μg mL-1 for each of the investigated drugs. The molar ratios of the formed chelats were determined by Job's method and their association constants were also calculated (method II. Ammonium vanadate was used for the spectrophotometric determination of the selected fluoroquinolones by oxidation in sulphuric acid medium resulting in the development of a greenish blue colour measured at 766 nm which was attributed to the vanadium (IV produced by reduction of vanadium (V by the selected drugs. The optimum conditions for heating time, reagent concentration and sulphuric acid concentration were carefully studied. The accuracy and precision of the proposed method was confirmed by estimating five or six replicates within Beer's law limits were obtained in the range 10-40 μg mL-1 for each of the investigated drugs

  2. Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry

    OpenAIRE

    Cortada Cortés, Carolina; Costa dos Reis, Luciana; Vidal Martínez, Lorena; Llorca, Julio; Canals Hernández, Antonio

    2013-01-01

    A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) procedure has been developed to preconcentrate eight cyclic and linear siloxanes from wastewater samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selecting the significant factors involved in the USA-DLLME procedure, which was la...

  3. Determination of free and total phthalates in commercial whole milk products in different packaging materials by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lin, Jialu; Chen, Wanxin; Zhu, Hangcui; Wang, Chengjun

    2015-12-01

    We developed a method for extraction and determination of free and total phthalate esters in commercial whole milk products. The free phthalates in milk samples were extracted with ethyl acetate after general pretreatment procedures including protein precipitation, centrifugation, and filtration. The bound phthalates in samples were first desorbed with the aid of ultrasound irradiation before extraction of total phthalates. The separation and determination of phthalates in extracts was performed by gas chromatography coupled with mass spectrometric detection. The detection limits were in the range of 0.09 to 0.36ng/g and the average recovery between 79.1 and 110.3%. The developed methods were applied to extract and determine phthalates in commercial whole milk products with different packaging materials, including plastic, glass, and metal. All samples contained several phthalates, including diethyl, diisobutyl, and bis(2-ethylhexyl) phthalates at concentrations between 2.60 and 156.4ng/g. The identified phthalates occurred in both free and bound forms. The amounts of phthalates in milk samples packaged in glass and metal containers were much lower than those in plastic containers. Plastic packaging materials are a possible source of phthalate contamination in commercial whole milk products, and a considerable portion of bleached phthalates from packaging can be adsorbed on proteins and other solid components of milk.

  4. Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

    2009-05-15

    A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were Aflatoxins were detected at <10 ng/g in several commercial food samples. PMID:19328492

  5. [Determination of 2-methylisoborneol and geosmin in drinking water using headspace solid phase micro-extraction coupled with gas chromatography-mass-spectrometry].

    Science.gov (United States)

    Cheng, Jianguo; Liu, Kaiying; Bai, Mindong; Cheng, Chao; Yu, Yixuan; Zhou, Xinying

    2015-12-01

    The odorous compounds of 2-methylisoborneol (2-MIB) and geosmin (GSM) heavily produced and released in water source are one of the most important factors leading to off-flavor emergencies and resident water consumption panic in drinking water. A headspace solid phase micro-extraction ( HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of these two trace earthy and musty compounds in reservoir water, reservoir soil and tap water. The conditions of HS-SPME, such as salt amount, extraction time and extraction temperature, were optimized based on orthogonal analysis. The qualitative and quantitative analyses of 2-MIB and GSM were carried out in the electron impact (EI) -selective ion scanning mode. The results showed that the linear relationship between peak area and concentration of 2-MIB and GSM was good enough (r2 0.998) from 5 to 1 000 ng/L, the limits of detection were 0.72 ng/L for 2-MIB, 0.34 ng/L for GSM and the limits of quantification were 2.40 ng/L for 2-MIB, 1.13 ng/L for GSM. When the target samples spiked in the range of 10-600 ng/L, the average recoveries of the target compounds were 93.6% - 107.7% ( RSD ≤ 6.1%, n = 6). Based on the above method, the target compounds in reservoir water, reservoir soil and tap water in a certain region of Liaoning Province were analyzed. The results showed that the two target odors in reservoir water were 3.0 -3.6 ng/L. As for the extract of the soil around the reservoir, 2-MIB was 8.1 ng/L and GSM was 17.8 ng/L. The odorous substances were not detected in the tap water. This method is simple, accurate, reliable, highly sensitive and no need of organic solvents. And it is suitable for the detection of 2-MIB and GSM in drinking water.

  6. [Determination of 2-methylisoborneol and geosmin in drinking water using headspace solid phase micro-extraction coupled with gas chromatography-mass-spectrometry].

    Science.gov (United States)

    Cheng, Jianguo; Liu, Kaiying; Bai, Mindong; Cheng, Chao; Yu, Yixuan; Zhou, Xinying

    2015-12-01

    The odorous compounds of 2-methylisoborneol (2-MIB) and geosmin (GSM) heavily produced and released in water source are one of the most important factors leading to off-flavor emergencies and resident water consumption panic in drinking water. A headspace solid phase micro-extraction ( HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of these two trace earthy and musty compounds in reservoir water, reservoir soil and tap water. The conditions of HS-SPME, such as salt amount, extraction time and extraction temperature, were optimized based on orthogonal analysis. The qualitative and quantitative analyses of 2-MIB and GSM were carried out in the electron impact (EI) -selective ion scanning mode. The results showed that the linear relationship between peak area and concentration of 2-MIB and GSM was good enough (r2 0.998) from 5 to 1 000 ng/L, the limits of detection were 0.72 ng/L for 2-MIB, 0.34 ng/L for GSM and the limits of quantification were 2.40 ng/L for 2-MIB, 1.13 ng/L for GSM. When the target samples spiked in the range of 10-600 ng/L, the average recoveries of the target compounds were 93.6% - 107.7% ( RSD ≤ 6.1%, n = 6). Based on the above method, the target compounds in reservoir water, reservoir soil and tap water in a certain region of Liaoning Province were analyzed. The results showed that the two target odors in reservoir water were 3.0 -3.6 ng/L. As for the extract of the soil around the reservoir, 2-MIB was 8.1 ng/L and GSM was 17.8 ng/L. The odorous substances were not detected in the tap water. This method is simple, accurate, reliable, highly sensitive and no need of organic solvents. And it is suitable for the detection of 2-MIB and GSM in drinking water. PMID:27097462

  7. Gas chromatography-mass spectrometric analysis of volatile components in capsicum powder from different cultivars%不同品种辣椒粉挥发性成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    熊学斌; 夏延斌; 张晓; 邓后勤

    2012-01-01

    Volatile components from bell pepper,chili hot pepper,vietnam capsicum frutescens var and capsicum frutescens var were extracted by solid phase microextraction(SPME) and analyzed by gas chromatography- mass spectrometry(GC-MS). A total of 94 votatile components,which were mainly made up of esters and alkenes(especially terpene),with bell pepper 24,chili hot pepper 30,vietnam capsicum frutescens var 43,and capsicum frutescens var 58,including 10 common components were identified. The relative contents of esters which were mainly made up of hexyl hexanoate,hexyl 2-methylbutanoate and hexyl 3-methylbutanoate in capsicum frutescens vat and alkenes which were mainly made up of aromadendrene, (4aS-cis)-2,4a, 5,6,7,8,9,9a-octahydro-3,5,5-trimethyl-9-methylene- 1H-benzocycloheptene and cis- ( - ) -2,4a, 5,6,9a- hexahydro-3,5,5,9-tetramethyl (1H) benzocycloheptene in chili hot pepper were the highest. The relative contents of hexanal and 2-pentylfuran in bell pepper and vietnam capsicum frutescens var were high.%以灯笼椒、红干椒、越野椒、野山椒4个辣椒品种为材料,采用顶空固相微萃取和气相色谱-质谱联用技术,分析不同辣椒品种的香气特征。结果表明,4种辣椒粉共检出94种挥发性成分,其中灯笼椒、红干椒、越野椒、野山椒分别为24种、30种、43种、58种,10种物质为4种辣椒粉共有。辣椒香气主要由酯类和萜烯类组成。野山椒中主要香气成分为酯类,主要酯类物质有己酸己酯、2-甲基丁酸己酯,3-甲基丁酸己酯,红干椒中主要香气成分为萜烯类,主要萜烯类物质有香橙烯、(4aS-顺)-2,4a,5,6,7,8,9,9a-八氢-3,5,5-三甲基-9-亚甲基-1H-苯并环庚烯、顺-(-)-2,4a,5,6,9a-六氢-3,5,5,9-四甲基-1H-苯并环庚烯,灯笼椒和越野椒中己醛、2-戊基呋喃相对含量较高。

  8. Determination of the phytoalexin resveratrol (3,5,4'-trihydroxystilbene) in peanuts and pistachios by high-performance liquid chromatographic diode array (HPLC-DAD) and gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Tokuşoglu, Ozlem; Unal, Mustafa Kemal; Yemiş, Fadim

    2005-06-15

    The phytoalexin resveratrol (3,5,4'-trihydroxystilbene) in edible peanut (Arachis hypogaea L.) and pistachio (Pistacia vera L.) varieties grown in Turkey was analyzed by high-performance liquid chromatographic diode array and gas chromatography-mass spectrometric detection. trans-Resveratrol in six peanut varieties, five pistachio varieties, and four market samples ranged between 0.03 and 1.92 microg/g. The Cerezlik 5025 peanut (1.92 +/- 0.01 microg/g) and Ohadi pistachio genotype (1.67 +/- 0.01 microg/g) had significantly higher trans-resveratrol contents. Peanuts contained 0.03-1.92 microg/g (av = 0.84 microg/g) of trans-resveratrol, whereas pistachio contained 0.09-1.67 microg/g (av = 1.15 microg/g). With exposure to UV light for 1 min, trans-resveratrol concentrations of samples ranged from 0.02 to 1.47 microg/g and those of cis-resveratrol from 0.008 to 0.32 microg/g. The occurrence of resveratrol in peanut and pistachio was confirmed by total ion chromatograms (TIC) of bis[trimethylsilyl]trifluoroacetamide derivatives of resveratrol isomers and comparison of the mass spectral fragmentation data with those of a resveratrol standard. Formation of the cis-isomer in pistachios was higher than in peanuts. PMID:15941348

  9. 吹扫捕集-气相色谱/质谱法测定水中二甲氧基甲烷%Determination of Dimethoxymethane in Water by Purge-and-Trap Gas Chromatography/Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    陈国征; 林怡; 徐伟; 钱洪智

    2013-01-01

    [ Objective ] To establish a method for the determination of dimethoxymethane in water by purge-and-trap gas chromatography/mass spectrometry (GC/MS). [ Methods ] The dimethoxymethane in water were purged and trapped, then desorbed and analyzed by gas chromatography/mass spectrometry. The external standard method applied characteristic ions for quantification. [ Results ] The linearity of the method was good under the experimental condition of dimethoxymethane (r=0.999 5). The detection limit was 0.03 μg/L. The recovery rates were 95.2%-99.3%, and the relative standard deviations (RSD) were 2.18%-3.87%. [ Conclusion ] The purge-and-trap gas chromatography/mass spectrometry is a sensitive and accurate method for determination of dimethoxymethane in water.%[目的]建立吹扫捕集-气相色谱/质谱检测水中二甲氧基甲烷的方法. [方法]利用吹扫捕集富集水中二甲氧基甲烷,解吸后用气相色谱/质谱法测定,选用特征离子外标法定量. [结果]方法在试验浓度范围内线性良好(r=0.9995),检出限为0.03 μg/L,回收率为95.2%~99.3%,相对标准偏差为2.18%~3.87%. [结论]该方法准确性好、灵敏度高,适合于水中二甲氧基甲烷的检测.

  10. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  11. Simultaneous Determination of 13 Priority Polycyclic Aromatic Hydrocarbons in Tehran's Tap Water and Water for Injection Samples Using Dispersive Liquid-Liquid Micro Extraction Method and Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Sadeghi, Ramezan; Kobarfard, Farzad; Yazdanpanah, Hassan; Eslamizad, Samira; Bayate, Mitra

    2016-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are classified as persistent and carcinogenic organic pollutants. PAHs contamination has been reported in water. Many of relevant regulatory bodies such as EU and EPA have regulated the limit levels for PAHs in drinking water. In this study, 13 priority polycyclic aromatic hydrocarbons (PAHs) were determined in tap water samples of Tehran and water for injection. Dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry was used for the extraction and determination of PAHs in the samples. Under the optimized conditions, the range of extraction recoveries and relative standard deviations (RSDs) of PAHs in water using internal standard (anthracene-d10) were in the range of 71-90% and 4-16%, respectively. Limit of detection for different PAHs were between 0.03 and 0.1 ngmL(-1). The concentration of PAHs in all tap water as well as water for injection samples were lower than the limit of quantification of PAHs. This is the first study addressing the occurrence of PAHs in water for injection samples in Iran using dispersive liquid-liquid micro extraction procedure combined with gas chromatography-mass spectrometry.

  12. Simultaneous Determination of 13 Priority Polycyclic Aromatic Hydrocarbons in Tehran's Tap Water and Water for Injection Samples Using Dispersive Liquid-Liquid Micro Extraction Method and Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Sadeghi, Ramezan; Kobarfard, Farzad; Yazdanpanah, Hassan; Eslamizad, Samira; Bayate, Mitra

    2016-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are classified as persistent and carcinogenic organic pollutants. PAHs contamination has been reported in water. Many of relevant regulatory bodies such as EU and EPA have regulated the limit levels for PAHs in drinking water. In this study, 13 priority polycyclic aromatic hydrocarbons (PAHs) were determined in tap water samples of Tehran and water for injection. Dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry was used for the extraction and determination of PAHs in the samples. Under the optimized conditions, the range of extraction recoveries and relative standard deviations (RSDs) of PAHs in water using internal standard (anthracene-d10) were in the range of 71-90% and 4-16%, respectively. Limit of detection for different PAHs were between 0.03 and 0.1 ngmL(-1). The concentration of PAHs in all tap water as well as water for injection samples were lower than the limit of quantification of PAHs. This is the first study addressing the occurrence of PAHs in water for injection samples in Iran using dispersive liquid-liquid micro extraction procedure combined with gas chromatography-mass spectrometry. PMID:27642318

  13. Method of double tracer addition for determining uranium in geological samples by mass spectrometric isotope dilution

    International Nuclear Information System (INIS)

    The present work shows the experimental details on the uranium determination in materials by mass spectrometric isotope dilution technique with double tracer (233U + 235U). The mass discrimination phenomenon effect is studied. The uranium concentration values obtained by mass spectrometric isotope dilution technique with double tracer are compared with other techniques. The influence of the sampling in the accurate determination of uranium in the rock sample is discussed. (author)

  14. Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection.

    Science.gov (United States)

    Wang, Ke-Deng; Chen, Pai-Shan; Huang, Shang-Da

    2014-03-01

    A new up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME) for extraction and derivatization of five chlorophenols (4-chlorophenol, 4-chloro-2-methylphenol, 2,4-dichlorophenol, 2,4,6-trichloro-phenol, and pentachlorophenol) has been developed. The method requires minimal solvent usage. The relatively polar, water-soluble, and low-toxicity solvent 1-heptanol (12 μL) was selected as the extraction solvent and acetic anhydride (50 μL) as the derivatization reagent. With the use of an up-and-down shaker, the emulsification of aqueous samples was formed homogeneously and quickly. The derivatization and extraction of chlorophenols were completed simultaneously in 1 min. The common requirement of disperser solvent in DLLME could be avoided. After optimization, the linear range covered over two orders of magnitude, and the coefficient of determination (r (2)) was greater than 0.9981. The detection limit was from 0.05 to 0.2 μg L(-1), and the relative standard deviation was from 4.6 to 10.8 %. Real samples of river water and lake water had relative recoveries from 90.3 to 117.3 %. Other emulsification methods such as vortex-assisted, ultrasound-assisted, and manual shaking-enhanced ultrasound-assisted methods were also compared with the proposed UDSA-DLLME. The results revealed that UDSA-DLLME performed with higher extraction efficiency and precision compared with the other methods. PMID:23727731

  15. Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cortada, Carol; dos Reis, Luciana Costa; Vidal, Lorena; Llorca, Julio; Canals, Antonio

    2014-03-01

    A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) procedure has been developed to preconcentrate eight cyclic and linear siloxanes from wastewater samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selecting the significant factors involved in the USA-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were: extractant solvent volume, 13 µL; solvent type, chlorobenzene; sample volume, 13 mL; centrifugation speed, 2300 rpm; centrifugation time, 5 min; and sonication time, 2 min. Under the optimized experimental conditions the method gave levels of repeatability with coefficients of variation between 10 and 24% (n=7). Limits of detection were between 0.002 and 1.4 µg L(-1). Calculated calibration curves gave high levels of linearity with correlation coefficient values between 0.991 and 0.9997. Finally, the proposed method was applied for the analysis of wastewater samples. Relative recovery values ranged between 71 and 116% showing that the matrix had a negligible effect upon extraction. To our knowledge, this is the first time that combines LLME and GC-MS for the analysis of methylsiloxanes in wastewater samples. PMID:24468359

  16. Determination of volatile organic compounds in the dried leaves of Salvia species by solid-phase microextraction coupled to gas chromatography mass spectrometry.

    Science.gov (United States)

    Cozzolino, Rosaria; Ramezani, Sadrollah; Martignetti, Antonella; Mari, Angela; Piacente, Sonia; De Giulio, Beatrice

    2016-01-01

    Salvia spp. are used throughout the world both for food and pharmaceutical purposes. In this study, a method involving headspace solid-phase microextraction combined with gas chromatography-mass spectrometry was developed, to establish the volatiles profile of dried leaves of four Iranian Salvia spp.: Salvia officinalis L., Salvia leriifolia Benth, Salvia macrosiphon Boiss. and two ecotypes of Salvia reuterana Boiss. A total of 95 volatiles were identified from the dried leaves of the five selected samples. Specifically, α-thujone was the main component of S. officinalis L. and S. macrosiphon Boiss. (34.40 and 17.84%, respectively) dried leaves, S. leriifolia Benth was dominated by β-pinene (27.03%), whereas α-terpinene was the major constituent of the two ecotypes of S. reuterana Boiss. (21.67 and 13.84%, respectively). These results suggested that the proposed method can be considered as a reliable technique for isolating volatiles from aromatic plants, and for plant differentiation based on the volatile metabolomic profile.

  17. Determination of the alkylpyrazine composition of coffee using stable isotope dilution-gas chromatography-mass spectrometry (SIDA-GC-MS).

    Science.gov (United States)

    Pickard, Stephanie; Becker, Irina; Merz, Karl-Heinz; Richling, Elke

    2013-07-01

    A stable isotope dilution analysis based on gas chromatography-mass spectrometry analysis (SIDA-GC-MS) was developed for the quantitative analysis of 12 alkylpyrazines found in commercially available coffee samples. These compounds contribute to coffee flavor. The accuracy of this method was tested by analyzing model mixtures of alkylpyrazines. Comparisons of alkylpyrazine-concentrations suggested that water as extraction solvent was superior to dichloromethane. The distribution patterns of alkylpyrazines in different roasted coffees were quite similar. The most abundant alkylpyrazine in each coffee sample was 2-methylpyrazine, followed by 2,6-dimethylpyrazine, 2,5-dimethylpyrazine, 2-ethylpyrazine, 2-ethyl-6-methylpyrazine, 2-ethyl-5-methylpyrazine, and 2,3,5-trimethylpyrazine, respectively. Among the alkylpyrazines tested, 2,3-dimethylpyrazine, 2-ethyl-3-methylpyrazine, 2-ethyl-3,6-dimethylpyrazine, and 2-ethyl-3,5-dimethylpyrazine revealed the lowest concentrations in roasted coffee. By the use of isotope dilution analysis, the total concentrations of alkylpyrazines in commercially available ground coffee ranged between 82.1 and 211.6 mg/kg, respectively. Decaffeinated coffee samples were found to contain lower amounts of alkylpyrazines than regular coffee samples by a factor of 0.3-0.7, which might be a result of the decaffeination procedure.

  18. Agarose film liquid phase microextraction combined with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in water.

    Science.gov (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Aini; Hasan, Mohamed Noor

    2012-11-01

    Agarose film liquid phase microextraction (AF-LPME) procedure for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAHs) in water has been investigated. Agarose film was used for the first time as an interface between donor and acceptor phases in liquid phase microextraction which allowed for selective extraction of the analytes prior to gas chromatography-mass spectrometry. Using 1-octanol as acceptor phase, high enrichment factors in the range of 57-106 for the targeted analytes (fluorene, phenanthrene, fluoranthene and pyrene) were achieved. Under the optimum extraction conditions, the method showed good linearity in the range of 0.1-200 μgL(-1), good correlation coefficients in the range of 0.9963-0.9999, acceptable reproducibility (RSD 6.1-9.2%, n=3), low limits of detection (0.01-0.04 μgL(-1)) and satisfactory relative recoveries (92.9-104.7%). As the AF-LPME device was non-expensive, reuse or recycle of the film was not required, thus eliminating the possibility of analytes carry-over between runs. The AF-LPME technique is environment-friendly and compatible with the green chemistry concept as agarose is biodegradable polysaccharide extracted from seaweed and the procedure requires small volume of organic solvent and generates little waste. The validated method was successfully applied to the analysis of the four analytes in river water samples.

  19. Measurement of breakthrough volumes of volatile chemical warfare agents on a poly(2,6-diphenylphenylene oxide)-based adsorbent and application to thermal desorption-gas chromatography/mass spectrometric analysis.

    Science.gov (United States)

    Kanamori-Kataoka, Mieko; Seto, Yasuo

    2015-09-01

    To establish adequate on-site solvent trapping of volatile chemical warfare agents (CWAs) from air samples, we measured the breakthrough volumes of CWAs on three adsorbent resins by an elution technique using direct electron ionization mass spectrometry. The trapping characteristics of Tenax(®) TA were better than those of Tenax(®) GR and Carboxen(®) 1016. The latter two adsorbents showed non-reproducible breakthrough behavior and low VX recovery. The specific breakthrough values were more than 44 (sarin) L/g Tenax(®) TA resin at 20°C. Logarithmic values of specific breakthrough volume for four nerve agents (sarin, soman, tabun, and VX) showed a nearly linear correlation with the reciprocals of their boiling points, but the data point of sulfur mustard deviated from this linear curve. Next, we developed a method to determine volatile CWAs in ambient air by thermal desorption-gas chromatography (TD-GC/MS). CWA solutions that were spiked into the Tenax TA(®) adsorbent tubes were analyzed by a two-stage TD-GC/MS using a Tenax(®) TA-packed cold trap tube. Linear calibration curves for CWAs retained in the resin tubes were obtained in the range between 0.2pL and 100pL for sarin, soman, tabun, cyclohexylsarin, and sulfur mustard; and between 2pL and 100pL for VX and Russian VX. We also examined the stability of CWAs in Tenax(®) TA tubes purged with either dry or 50% relative humidity air under storage conditions at room temperature or 4°C. More than 80% sarin, soman, tabun, cyclohexylsarin, and sulfur mustard were recovered from the tubes within 2 weeks. In contrast, the recoveries of VX and Russian VX drastically reduced with storage time at room temperature, resulting in a drop to 10-30% after 2 weeks. Moreover, we examined the trapping efficiency of Tenax TA(®) adsorbent tubes for vaporized CWA samples (100mL) prepared in a 500mL gas sampling cylinder. In the concentration range of 0.2-2.5mg/m(3), >50% of sarin, soman, tabun, cyclohexylsarin, and HD were

  20. Measurement of breakthrough volumes of volatile chemical warfare agents on a poly(2,6-diphenylphenylene oxide)-based adsorbent and application to thermal desorption-gas chromatography/mass spectrometric analysis.

    Science.gov (United States)

    Kanamori-Kataoka, Mieko; Seto, Yasuo

    2015-09-01

    To establish adequate on-site solvent trapping of volatile chemical warfare agents (CWAs) from air samples, we measured the breakthrough volumes of CWAs on three adsorbent resins by an elution technique using direct electron ionization mass spectrometry. The trapping characteristics of Tenax(®) TA were better than those of Tenax(®) GR and Carboxen(®) 1016. The latter two adsorbents showed non-reproducible breakthrough behavior and low VX recovery. The specific breakthrough values were more than 44 (sarin) L/g Tenax(®) TA resin at 20°C. Logarithmic values of specific breakthrough volume for four nerve agents (sarin, soman, tabun, and VX) showed a nearly linear correlation with the reciprocals of their boiling points, but the data point of sulfur mustard deviated from this linear curve. Next, we developed a method to determine volatile CWAs in ambient air by thermal desorption-gas chromatography (TD-GC/MS). CWA solutions that were spiked into the Tenax TA(®) adsorbent tubes were analyzed by a two-stage TD-GC/MS using a Tenax(®) TA-packed cold trap tube. Linear calibration curves for CWAs retained in the resin tubes were obtained in the range between 0.2pL and 100pL for sarin, soman, tabun, cyclohexylsarin, and sulfur mustard; and between 2pL and 100pL for VX and Russian VX. We also examined the stability of CWAs in Tenax(®) TA tubes purged with either dry or 50% relative humidity air under storage conditions at room temperature or 4°C. More than 80% sarin, soman, tabun, cyclohexylsarin, and sulfur mustard were recovered from the tubes within 2 weeks. In contrast, the recoveries of VX and Russian VX drastically reduced with storage time at room temperature, resulting in a drop to 10-30% after 2 weeks. Moreover, we examined the trapping efficiency of Tenax TA(®) adsorbent tubes for vaporized CWA samples (100mL) prepared in a 500mL gas sampling cylinder. In the concentration range of 0.2-2.5mg/m(3), >50% of sarin, soman, tabun, cyclohexylsarin, and HD were

  1. Determination of 2-ethylhexyl 4-(dimethylamino) benzoate using membrane-assisted liquid-liquid extraction and gas chromatography-mass spectrometric detection.

    Science.gov (United States)

    March, J G; Genestar, C; Simonet, B M

    2009-06-01

    A flow-cell for micro-porous membrane liquid-liquid extraction with a sheet membrane was used to extract 2-ethylhexyl 4-(dimethylamino) benzoate (EDB) from urine of solar-cream users and spiked wine samples. The cell enabled the target analyte to be extracted from 7.9 mL of donor solution into 200 microL of acceptor solution (decane). After extraction, the acceptor solution was transferred to a micro-vial for GC-MS analysis without derivation. In this work, variables affecting the enrichment factor were also studied, such as organic solvent, extraction time, recirculation flow of the donor solution through the donor chamber, presence of potassium chloride and ethanol in the donor solution and pH. The method has been evaluated in terms of linearity, sensitivity, precision, limits of detection and quantification and extraction efficiency. Limits of quantification were 1 and 3 microg L(-1) EDB for urine and wine, respectively. Quantitative analysis has been carried out by applying the method of standard additions. Within- and between-day relative standard deviations were lower than 12% and 20%, respectively. EDB was found in the urine of users of cream containing EDB in the concentration interval 1.2-7.2 microg L(-1). Therefore, this provides evidence of EDB dermal absorption and subsequent excretion through the urinary tract. EDB was not found in the analysed wine samples. PMID:19347661

  2. Analysis of Marine Biotoxins by Liquid Chromatography Mass Spectrometric Detection

    NARCIS (Netherlands)

    Gerssen, A.

    2014-01-01

    The last few years have brought about many changes in the field of marine and freshwater toxins, with advances in analytical technology and the realization that these toxins are a global issue. Offering a complete reference guide, Seafood and Freshwater Toxins: Pharmacology, Physiology, and Detectio

  3. Determination of capsaicin, dihydrocapsaicin, and nonivamide in self-defense weapons by liquid chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Reilly, C A; Crouc, D J; Yost, G S; Fatah, A A

    2001-04-01

    Sensitive and selective liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS) methods for the analysis of capsaicin, dihydrocapsaicin, and nonivamide in pepper spray products have been developed. Chromatographic separation of the capsaicinoid analogues was achieved using a reversed-phase HPLC column and a stepwise gradient of methanol and distilled water containing 0.1% (v/v) formic acid. Identification and quantification of the capsaicinoids was achieved by electrospray ionization single-stage mass spectrometry monitoring the protonated molecules of the internal standard (m/z 280), capsaicin (m/z 306), dihydrocapsaicin (m/z 308), and nonivamide (m/z 294) or by tandem mass spectrometry monitoring the appropriate precursor-to-product-ion transitions. The plot of concentration versus peak area ratio was linear over the range of 10-750 ng/ml using LC-MS and 10-500 ng/ml using LC-MS-MS. However, to accurately quantify the capsaicinoids in the pepper spray products calibration curves between 10 and 1000 ng were constructed and fit using a weighted quadratic equation. Using the quadratic curve, the accuracy of the assay ranged from 91 to 102% for all analytes. The intra-assay precision (RSD) for capsaicin was 2% at 25 ng/ml, 10% at 500 ng/ml, and 3% at 800 ng/ml. The inter-assay precision (RSD) for capsaicin was 6% at 25 ng/ml, 6% at 500 ng/ml, and 9% at 800 ng/ml. Similar values for inter- and intra-assay precision were experimentally obtained for both dihydrocapsaicin and nonivamide. The analysis of selected pepper spray products demonstrated that the capsaicinoid concentration in the products ranged from 0.7 to 40.5 microg/microl. PMID:11330795

  4. Determination of geosmin and 2-methylisoborneol in water and wine samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cortada, Carol; Vidal, Lorena; Canals, Antonio

    2011-01-01

    A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USADLLME) procedure has been developed to preconcentrate geosmin and 2-methylisoborneol (MIB) from water and wine samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach was developed by means of a Plackett-Burman design for screening and selecting the significant variables involved in the USADLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were: solvent volume, 8μL; solvent type: tetrachloroethylene; sample volume, 12 mL; centrifugation speed, 2300 rpm; extraction temperature 20 °C; extraction time, 3 min; and centrifugation time, 3 min. Under the optimized experimental conditions the method gave good levels of repeatability with coefficient of variation under 11% (n=10). Limits of detection were 2 and 9 ng L⁻¹ for geosmin and MIB, respectively. Calculated calibration curves gave high levels of linearity with correlation coefficient values of 0.9988 and 0.9994 for geosmin and MIB, respectively. Finally, the proposed method was applied to the analysis of two water (reservoir and tap) samples and three wine (red, rose and white) samples. The samples were previously analyzed and confirmed free of target analytes. Recovery values ranged between 70 and 113% at two spiking levels (0.25 μg L⁻¹ and 30 ng L⁻¹) showing that the matrix had a negligible effect upon extraction. Only red wine showed a noticeable matrix effect (70-72% recovery). Similar conclusions have been obtained from an uncertainty budget evaluation study.

  5. Efficacy of head space solid-phase microextraction coupled to gas chromatography-mass spectrometry method for determination of the trace extracellular hydrocarbons of cyanobacteria.

    Science.gov (United States)

    Guan, Wenna; Zhu, Tao; Wang, Yuejie; Zhang, Zhongyi; Jin, Zhao; Wang, Cong; Bai, Fali

    2016-09-01

    Hydrocarbons are widespread in cyanobacteria, and the biochemical synthetic pathways were recently identified. Intracellular fatty alka(e)nes of cyanobacteria have been detected by liquid-liquid extraction (LLE) coupled to gas chromatography-mass spectrometry (GC/MS). However, whether fatty alka(e)nes can be released to cyanobacterial culture media remains to be clarified. This work develops a sensitive method for analyzing the trace level of extracellular hydrocarbons in cyanobacterial culture media by head space solid-phase microextraction (HS-SPME) coupled to GC/MS. Headspace (HS) extraction mode using polydimethylsiloxane fiber to extract for 30min at 50°C was employed as the optimal extraction conditions. Five cyanobacterial fatty alka(e)nes analogs including pentadecene (C15:1), pentadecane (C15:0), heptadecene (C17:1), heptadecane (C17:0), nonadecane (C19:0) were analyzed, and the data obtained from HS-SPME-GC/MS method were quantified using internal standard peak area comparisons. Limits of detection (LOD), limits of quantitation (LOQ), linear dynamic range, precisions (RSD) and recovery for the analysis of extracellular fatty alka(e)nes of cyanobacteria by HS-SPME-GC/MS were evaluated. The LODs limits of detection (S/N = 3) varied from 10 to 21 ng L-1. The correlation coefficients (r) of the calibration curves ranged from 0.9873 to 0.9977 with a linearity from 0.1 to 50 μg L-1. The RSD values were ranging from 7.8 to 14.0% and from 4.0 to 8.8% at 1.0 μg L-1 and 10.0 μg L-1 standard solutions, respectively. Comparative analysis of extracellular fatty alka(e)nes in the culture media of model cyanobacteria Synechocystis sp. PCC 6803 demonstrated that sensitivity of HS-SPME-GC/MS method was significantly higher than LLE method. Finally, we found that heptadecane can be released into the culture media of Synechocystis sp. PCC 6803 at the later growth period. PMID:27428454

  6. Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas Pesticides residue determination in cattle plasma by gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Daniele Fernanda Maffei

    2009-01-01

    Full Text Available An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..

  7. Development of a thermal desorption gas chromatography-mass spectrometry method for quantitative determination of haloanisoles and halophenols in wineries' ambient air.

    Science.gov (United States)

    Camino-Sánchez, F J; Ruiz-García, J; Zafra-Gómez, A

    2013-08-30

    An analytical method for the detection and quantification of haloanisoles and their corresponding halophenols in wineries' ambient air was developed. The target analytes were haloanisoles and halophenols, reported by previous scientific literature as responsible for wine taint. A calibrated pump and active tubes filled with Tenax GR™ were used for sampling. These tubes were thermally desorbed and analyzed using gas chromatography-triple quadrupole mass spectrometry in the selected reaction monitoring mode. The adsorption efficiencies of five commercial sampling tubes filled with different materials were evaluated. The efficiencies of the selected adsorbent were close to 100% for all sampled compounds. Desorption, chromatographic and mass spectrometric conditions were accurately optimized allowing very low limits of quantification and wide linear ranges. The limits of quantification in ambient air ranged from 0.8pgtube(-1) for 2,4,6-trichlorophenol, to 28pgtube(-1) for pentachlorophenol. These results are of great importance because human sensory threshold for haloanisoles is very low. The chromatographic method was also validated and the instrumental precision and trueness were established, a maximum RSD of 9% and a mean recovery of 91-106% were obtained. The proposed method involves an easy and sensitive technique for the early detection of haloanisoles and their precursor halophenols in ambient air avoiding contamination of wine or winery facilities. PMID:23891369

  8. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

    1995-01-01

    A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

  9. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  10. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  11. 固相萃取-气质联用仪检测尿液中多种内源性类固醇%Solid phase extraction and determination of endogenous anabolic steroids in urine by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘慧燕

    2015-01-01

    目的:为监控运动员食品药品安全问题,利用气质联用仪(gas chromatography-mass spectrometry, GC-MS)建立正常运动员尿液中多种内源性类固醇的分析方法。方法尿液冷冻处理解冻后离心,取上清液经固相萃取,β-葡萄糖醛酸甙酶水解后再次萃取干燥衍生化后,采用选择离子监控SIM模式进行检测。结果方法的最低检出限为0.2~0.5 ng/mL,平均提取回收率为93.64%~116.74%,相对标准偏差(relative standard deviation, RSD)低于6.59%。结论该方法可以用于内源性类固醇兴奋剂的检测。%Objective To develop a method of gas chromatography-mass spectrometry (GC-MS) for the simultaneous identification and quantification of endogenous anabolic steroids in urine of athletes,for assurance of their food and drug safety. Methods The thawed iced urine sample was centrifuged, and the liquid supernatant was extracted using reverse phase C18 column. The methanol eluant was collected, hydrolized by β-glucuronidase, derivatized with a derivatization reagent and detected using GC-MS in SIM mode. Results The limits of detection for endogenous anabolic steroids were in the range of 0.2~0.5 ng/mL, the average recoveries were 93.64%~116.74% with relative standard deviation (RSD) less than 6.59%. Conclusion The method can be used for the determination of endogenous anabolic steroids in urine for doping control.

  12. Mass spectrometric determination of early and advanced glycation in biology.

    Science.gov (United States)

    Rabbani, Naila; Ashour, Amal; Thornalley, Paul J

    2016-08-01

    Protein glycation in biological systems occurs predominantly on lysine, arginine and N-terminal residues of proteins. Major quantitative glycation adducts are found at mean extents of modification of 1-5 mol percent of proteins. These are glucose-derived fructosamine on lysine and N-terminal residues of proteins, methylglyoxal-derived hydroimidazolone on arginine residues and N(ε)-carboxymethyl-lysine residues mainly formed by the oxidative degradation of fructosamine. Total glycation adducts of different types are quantified by stable isotopic dilution analysis liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring mode. Metabolism of glycated proteins is followed by LC-MS/MS of glycation free adducts as minor components of the amino acid metabolome. Glycated proteins and sites of modification within them - amino acid residues modified by the glycating agent moiety - are identified and quantified by label-free and stable isotope labelling with amino acids in cell culture (SILAC) high resolution mass spectrometry. Sites of glycation by glucose and methylglyoxal in selected proteins are listed. Key issues in applying proteomics techniques to analysis of glycated proteins are: (i) avoiding compromise of analysis by formation, loss and relocation of glycation adducts in pre-analytic processing; (ii) specificity of immunoaffinity enrichment procedures, (iii) maximizing protein sequence coverage in mass spectrometric analysis for detection of glycation sites, and (iv) development of bioinformatics tools for prediction of protein glycation sites. Protein glycation studies have important applications in biology, ageing and translational medicine - particularly on studies of obesity, diabetes, cardiovascular disease, renal failure, neurological disorders and cancer. Mass spectrometric analysis of glycated proteins has yet to find widespread use clinically. Future use in health screening, disease diagnosis and therapeutic monitoring, and

  13. X-ray spectrometric determination of thorium in bone and other biological materials

    International Nuclear Information System (INIS)

    An x-ray spectrometric method has been developed for the determination of thorium in bone and other biological materials. The limit of detection at the 95% confidence level is 20 ng. This corresponds to a concentration of 2 ppb in a 10-g sample of bone ash

  14. Fast automated dual-syringe based dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    Science.gov (United States)

    Guo, Liang; Tan, Shufang; Li, Xiao; Lee, Hian Kee

    2016-03-18

    An automated procedure, combining low density solvent based solvent demulsification dispersive liquid-liquid microextraction (DLLME) with gas chromatography-mass spectrometry analysis, was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Capitalizing on a two-rail commercial autosampler, fast solvent transfer using a large volume syringe dedicated to the DLLME process, and convenient extract collection using a small volume microsyringe for better GC performance were enabled. Extraction parameters including the type and volume of extraction solvent, the type and volume of dispersive solvent and demulsification solvent, extraction and demulsification time, and the speed of solvent injection were investigated and optimized. Under the optimized conditions, the linearity ranged from 0.1 to 50 μg/L, 0.2 to 50 μg/L, and 0.5 to 50 μg/L, depending on the analytes. Limits of detection were determined to be between 0.023 and 0.058 μg/L. The method was applied to determine PAHs in environmental water samples.

  15. Method Development and Validation for Determining 1,3-Butadiene in Human Blood by Gas Chromatography-Mass Spectrometry and Head-Space Gas Chromatography%Method Development and Validation for Determining1,3-Butadiene in Human Blood by Gas Chromatography-Mass Spectrometry and Head-Space Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    ZHANG Su-jing; SHEN Bao-hua; ZHUO Xian-yi

    2013-01-01

    To develop a simple,validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC).BD was identified by GC-MS and HS-GC,and quantified by HS-GC.The method showed that BD had a good linearity from 50 to 500 μg/mL (r>0.99).The limits of detection and quantification were 10 μg/mL and 50 μg/mL,respectively.Both the intra-day precision and inter-day precision were <6.08%,and the accuracy was 96.98%-103.81%.The method was applied to an actual case,and the concentration of BD in the case was 242 μg/mL in human blood.This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

  16. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group?Determination of acetamide herbicides and their degradation products in water using online solid-phase extraction and liquid chromatography/mass spectrometry

    Science.gov (United States)

    Lee, E.A.; Strahan, A.P.

    2003-01-01

    An analytical method for the determination of 6 acetamide herbicides (acetochlor, alachlor, dimethenamid, flufenacet, metolachlor, and propachlor) and 16 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is described in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using octadecylsilane as the solid-phase extraction media on online automated equipment followed by liquid chromatography/mass spectrometry. The method uses only 10 milliliters of sample per injection. Three different water-sample matrices, a reagent-water, a ground-water, and a surface-water sample spiked at 0.10 and 1.0 microgram per liter, were analyzed to determine method performance. Method detection limits ranged from 0.004 to 0.051 microgram per liter for the parent acetamide herbicides and their degradation products. Mean recoveries for the acetamide compounds in the ground- and surface-water samples ranged from 62.3 to 117.4 percent. The secondary amide of acetochlor/metolachlor ethanesulfonic acid (ESA) was recovered at an average rate of 43.5 percent. The mean recoveries for propachlor and propachlor oxanilic acid (OXA) were next lowest, ranging from 62.3 to 95.5 percent. Mean recoveries from reagent-water samples ranged from 90.3 to 118.3 percent for all compounds. Overall the mean of the mean recoveries of all compounds in the three matrices spiked at 0.10 and 1.0 microgram per liter ranged from 89.9 to 100.7 percent, including the secondary amide of acetochlor/metolachlor ESA and the propachlor compounds. The acetamide herbicides and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter. The upper concentration limit is 2.0 micrograms per liter for all compounds without dilution. With the exception of the secondary amide of

  17. Rapid determination of benzimidazole pesticide in orange juice by liquid chromatography -mass spectrometry%LC-MS快速检测橙汁中苯并咪唑类农药

    Institute of Scientific and Technical Information of China (English)

    姚艳玲; 倪炜华; 顾益

    2013-01-01

    Objective: A method was established to rapidly determine carbendazim, thiophanate, thiophanate -methyl, 2 - aminobenzimidazole and triabendazole in orange juice by liquid chromatography - mass spectrometry. Methods; The orange juice was diluted with water, and then subjected to solid phase extraction using HLB 3cc cartridge. Then the extract was analyzed by liquid chromatography - mass spectrometry with a mobile phase of water and methanol at a flow rate of 0.20 ml/min. Results: The method showed good linearity in the range of 0.01 mg/L ~ 0. 10 mg/L, the average recoveries of the 5 benzimidazole pesticide in orange juice ranged from 75.0% to 97. 5% , the relative standard deviations ranged from 1. 0% ~ 8. 6% , the limit of detection was from 0. 0046 μg/kg ~ 0.0116 μg/kg. Conclusion; The method was applied to determine carbendazim, thiophanate, thiophanate - methyl, 2 - aminobenzimidazole and triabendazole in orange juice with satisfactory results.%目的:建立液相色谱质谱法快速检测橙汁中多菌灵、硫菌灵、甲基硫菌灵、2-氨基苯并咪唑和噻菌灵5种苯并咪唑类农药的试验方法.方法:样品直接用水稀释后,经HLB 3cc固相萃取柱净化,采用液相色谱质谱仪进行定性、定量分析,以水和甲醇为流动相,在0.20 ml/min下梯度洗脱.结果:该方法在0.01 mg/L~0.10 mg/L范围内呈良好的线性关系,平均回收率为75.0% ~ 97.5%,相对标准偏差为1.0% ~8.6%,检出限为0.0046 μg/kg ~0.0116 μg/kg.结论:该方法适用于橙汁中多菌灵、硫菌灵、甲基硫菌灵、2-氨基苯并咪唑和噻菌灵的检测.

  18. Coupling of size-exclusion chromatography to liquid chromatography/mass spectrometry for determination of trace levels of thifensulfuron-methyl and tribenuron-methyl in cottonseed and cotton gin trash.

    Science.gov (United States)

    Stry, J J; Amoo, J S; George, S W; Hamilton-Johnson, T; Stetser, E

    2000-01-01

    Size-exclusion chromatography (SEC) was coupled to reversed-phase liquid chromatography/mass spectrometry for the determination of thifensulfuron-methyl and tribenuron-methyl in cottonseed and cotton gin trash. The limit of quantitation was 20 parts per billion (ppb), and the limit of detection was 6 ppb. The analytes were extracted by homogenization in a buffer solution. The extracts underwent a solvent exchange into methanol and were injected onto an SEC column. As the analytes eluted from the SEC column, the eluate was diverted onto a reversed-phase column for additional separation of the analytes and their detection via mass spectrometry. This method is unique because the samples are not cleaned up before analysis, the analytes are injected in methanol, and the entire analysis is completed in 30 min. Average recoveries and standard deviations for thifensulfuronmethyl and tribenuron-methyl in cotton gin trash were 91 +/- 6% and 88 +/- 5%, respectively. Average recoveries and standard deviations for thifensulfuron-methyl and tribenuron-methyl in cottonseed were 91 +/- 11% and 99 +/- 12%, respectively. This is an effective method for the detection and determination of thifensulfuron-methyl and tribenuron-methyl in cotton. PMID:10868588

  19. 加速溶剂提取气-质联用分析土壤中的多环芳烃%Determination of Polycyclic Aromatic Hydrocarbons in Soils Using Accelerated Solvent Extraction and Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王新成; 赵金; 赵汝松; 程传格

    2014-01-01

    Based on accelerated solvent extraction, gel permeation chromatography and gas chromatography-mass spectrometry, a novel method was developed for the simultaneous determination of 16 polycyclic aromatic hydrocarbons in soil samples. The limits of detection and the limits of quantitation were 1. 1-12 μg/kg and 3. 7-40 μg/kg for 16 polycyclic aromatic hydrocarbons, respectively. The average recoveries of all the compounds were 76. 6%-96. 8%, and relative standard deviations were 2. 9%-9. 5%. This method was fast, simple and easy to operate. The method has been used to determine 16 polycyclic aromatic hydrocarbons in real soil samples with satisfactory results. It can be applied in routine soil analysis.%建立了加速溶剂提取-凝胶渗透色谱净化和气相色谱-质谱联用快速分析土壤中16种多环芳烃的新方法。方法的检出限、定量限分别为1.1~12μg/kg、3.7~40μg/kg。16种 PAHs 的回收率为76.6%~96.8%,相对标准偏差为2.9%~9.5%。应用于多个环境样品的分析测试,结果满意。

  20. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of triazine and phenylurea herbicides and their degradation products in water using solid-phase extraction and liquid chromatography/mass spectrometry

    Science.gov (United States)

    Lee, Edward Alan; Strahan, Alex P.; Thurman, Earl Michael

    2002-01-01

    An analytical method for the determination of 7 triazine and phenylurea herbicides and 12 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is presented in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using 0.5 gram graphitized carbon as the solid-phase extraction media followed by liquid chromatography/mass spectrometry. Three different water-sample matrices?ground-water, surface-water, and reagent-water samples?spiked at 0.2 and 2.0 micrograms per liter were analyzed. Method detection limits ranged from 0.013 to 0.168 microgram per liter for the parent triazine herbicides and the triazine degradation products. Method detection limits ranged from 0.042 to 0.141 microgram per liter for the parent phenylurea herbicides and their degradation products. Mean recoveries for the triazine compounds in the ground- and surface-water samples generally ranged from 72.6 to 117.5 percent, but deethyl-cyanazine amide was recovered at 140.5 percent. Mean recoveries from the ground- and surface-water samples for the phenylurea compounds spiked at the 2.0-micrograms-per-liter level ranged from 82.1 to 114.4 percent. The mean recoveries for the phenylureas spiked at 0.2-microgram per liter were less consistent, ranging from 87.0 to 136.0 percent. Mean recoveries from reagent-water samples ranged from 87.0 to 109.5 percent for all compounds. The triazine compounds and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter, with the exception of deethylcyanazine and deethylcyanazine amide which are reported at 0.20 to 2.0 micrograms per liter. The phenylurea compounds and their degradation products are reported in concentrations ranging from 0.20 to 2.0 micrograms per liter. The upper concentration limit was 2

  1. Chemical Composition of Latent Fingerprints by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Hartzell-Baguley, Brittany; Hipp, Rachael E.; Morgan, Neal R.; Morgan, Stephen L.

    2007-01-01

    An experiment in which gas chromatography-mass spectrometry (GC-MS) is used for latent fingerprint extraction and analysis on glass beads or glass slides is conducted. The results determine that the fingerprint residues are gender dependent.

  2. Xylem sap collection and extraction methodologies to determine in vivo concentrations of ABA and its bound forms by gas chromatography-mass spectrometry (GC-MS)

    OpenAIRE

    Netting Andrew G; Theobald Julian C; Dodd Ian C

    2012-01-01

    Abstract Background Accurate quantification of xylem sap ABA concentrations is important to underpin models of root-to-shoot ABA signalling to predict the physiological effects of soil drying. Growing tomato plants in a whole plant pressure chamber allowed sequential xylem sap collection from a detached leaf, the petiole stub of an otherwise intact plant and finally the de-topped root system of the same plant, to determine the impact of xylem sap sampling methodology on xylem ABA concentratio...

  3. Determination of methyl tert-butyl ether (MTBE) in Chinese fuels by gas chromatography/mass spectrometry and gas chromatography/flame ionization detector

    Institute of Scientific and Technical Information of China (English)

    LIU Jie-min; CHENG Wei; WEN Mei-juan; JIANG Gui-bin

    2004-01-01

    A method was developed to determine the concentration of methyl tert-butyl ether(MTBE) in gasoline,diesel and heating oil by gas chromatography(GC) with mass spectrometry(GC-MS) or flame ionization detection (FID). The diluted gasoline was directly injected into the GC, and the complete separation of MTBE from co-eluting hydrocarbons was not required. GC/MS or GC/FID method can be used to analyze MTBE in different concentration range and have good consistency.

  4. Hollow fiber based liquid phase microextraction for the determination of organochlorine pesticides in ecological textiles by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cai, Jin'an; Chen, Guosheng; Qiu, Junlang; Jiang, Ruifen; Zeng, Feng; Zhu, Fang; Ouyang, Gangfeng

    2016-01-01

    In this study, the hollow fiber-liquid phase microextraction (HF-LPME) coupled gas chromatograph/mass spectrometry (GC/MS) was firstly developed to determine 10 organochlorine pesticides (OCPs) in ecological textiles. The present method can offer high separation efficiencies with minimal sample and solvent consumption. The extraction conditions were optimized, including the types of hollow fiber and organic solvent, the extraction time, the stirring and the salinity. Under the optimized conditions, the linear ranges of OCPs in cotton, terylene and fur samples were 5-1000 ng/g, 10-1000 ng/g and 10-800 ng/g, respectively, and the detection limit of the three samples were 0.07-2.30 ng/g, 0.89-1.66 ng/g and 0.06-1.04 ng/g, respectively. The optimized method was then successfully used to determine the OCPs in 3 kinds of spiked real samples, including cotton, terylene and fur. The good recoveries and RSDs of the quantification in real textile samples were obtained and the results were confirmed by the traditional liquid extraction method (GB/T 18412-2006). This study proved that the HF-LPME method, which was simple, low-cost and virtually solvent-free, was reliable for the qualitative and quantitative analysis of the harmful OCP residues in ecological textiles.

  5. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R.; Garcia-Lopez, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I., E-mail: isaac.rodriguez@usc.es [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2010-07-12

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL{sup -1} and linear responses for concentrations up to 2.5 {mu}g mL{sup -1}, referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL{sup -1}. Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  6. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    International Nuclear Information System (INIS)

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL-1 and linear responses for concentrations up to 2.5 μg mL-1, referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL-1. Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  7. Methods of analysis and quality-assurance practices of the U.S. Geological Survey organic laboratory, Sacramento, California; determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Crepeau, Kathryn L.; Domagalski, Joseph L.; Kuivila, Kathryn M.

    1994-01-01

    Analytical method and quality-assurance practices were developed for a study of the fate and transport of pesticides in the Sacramento-San Joaquin Delta and the Sacramento and San Joaquin River. Water samples were filtered to remove suspended parti- culate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide, and the pesticides were eluted with three 2-milliliter aliquots of hexane:diethyl ether (1:1). The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for analytes determined per 1,500-milliliter samples ranged from 0.006 to 0.047 microgram per liter. Recoveries ranged from 47 to 89 percent for 12 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.05 and 0.26 microgram per liter. The method was modified to improve the pesticide recovery by reducing the sample volume to 1,000 milliliters. Internal standards were added to improve quantitative precision and accuracy. The analysis also was expanded to include a total of 21 pesticides. The method detection limits for 1,000-milliliter samples ranged from 0.022 to 0.129 microgram per liter. Recoveries ranged from 38 to 128 percent for 21 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.10 and 0.75 microgram per liter.

  8. Determination of Plasticizer in Food by Gas Chromatography and Gas Chromatography Mass Spectrometry%气相色谱及气相色谱-质谱法检测食品中增塑剂

    Institute of Scientific and Technical Information of China (English)

    张薇

    2016-01-01

    Plasticizer is a kind of polymer additives, in environmental estrogen, which belongs to the phthalic acid esters, in the middle of the industry, a very wide range of applications. Plasticizing agent is not used to the food, if eating human will to the reproductive system, endocrine system caused a lot of damage. Based on this, this article uses the test method, mainly takes the ortho benzene two formic acid ester compound as the example, has carried on the analysis to the use of gas chromatography and gas chromatography-mass spectrometry determination of the plasticizer in food.%增塑剂是一种高分子材料助剂,在环境雌激素中,属于酞酸酯类物质,在工业当中,有着十分广泛的应用。增塑剂不可应用于食品当中,如果人类误食,将会对生殖系统、内分泌系统造成很大的伤害。基于此,本文采用试验的方法,主要以邻苯二甲酸酯类化合物为例,对利用气相色谱及气相色谱-质谱法检测食品中的增塑剂进行了分析。

  9. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group; determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

    Science.gov (United States)

    Zimmerman, L.R.; Hostetler, K.A.; Thurman, E.M.

    2000-01-01

    Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: acetochlor ethanesulfonic acid (ESA), acetochlor oxanilic acid (OXA), alachlor ESA, alachlor OXA, metolachlor ESA, and metolachlor OXA. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The mean HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.50, and 2.0 mg/L (micrograms per liter) ranged from 84 to 112 percent, with relative standard deviations of 18 percent or less. The mean HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.20, and 2.0 mg/L ranged from 81 to 125 percent, with relative standard deviations of 20 percent or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 mg/L, whereas the LOQ using the HPLC/MS method was 0.05 mg/L. These metabolite-determination methods are valuable for acquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water.

  10. Method of analysis and quality-assurance practices by the U.S. Geological Survey Organic Geochemistry Research Group; determination of geosmin and methylisoborneol in water using solid-phase microextraction and gas chromatography/mass spectrometry

    Science.gov (United States)

    Zimmerman, L.R.; Ziegler, A.C.; Thurman, E.M.

    2002-01-01

    A method for the determination of two common odor-causing compounds in water, geosmin and 2-methylisoborneol, was modified and verified by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas. The optimized method involves the extraction of odor-causing compounds from filtered water samples using a divinylbenzene-carboxen-polydimethylsiloxane cross-link coated solid-phase microextraction (SPME) fiber. Detection of the compounds is accomplished using capillary-column gas chromatography/mass spectrometry (GC/MS). Precision and accuracy were demonstrated using reagent-water, surface-water, and ground-water samples. The mean accuracies as percentages of the true compound concentrations from water samples spiked at 10 and 35 nanograms per liter ranged from 60 to 123 percent for geosmin and from 90 to 96 percent for 2-methylisoborneol. Method detection limits were 1.9 nanograms per liter for geosmin and 2.0 nanograms per liter for 2-methylisoborneol in 45-milliliter samples. Typically, concentrations of 30 and 10 nanograms per liter of geosmin and 2-methylisoborneol, respectively, can be detected by the general public. The calibration range for the method is equivalent to concentrations from 5 to 100 nanograms per liter without dilution. The method is valuable for acquiring information about the production and fate of these odor-causing compounds in water.

  11. 吹扫捕集气相色谱质谱法测定水中的三氯乙醛%Purge and Trap-Gas Chromatography Mass Spectrometry Determination of Chloral in Drinking water

    Institute of Scientific and Technical Information of China (English)

    王敏捷; 曹立峰; 袁润蕾; 来克冰

    2013-01-01

      本文采用吹扫捕集气相色谱质谱法对水中的三氯乙醛进行测定。研究了碱性条件下反应温度与反应时间对三氯乙醛转化速度的影响。标准曲线范围在 1~50μg/L 时,所得三氯乙醛的线性相关系数为 0.9999。回收率为 97.0%~99.8%,RSD 为 0.9%。该法回收率高、精密度好、准确度好,且操作简便、快速,适用于水中三氯乙醛的分析。%Established the purge and trap-gas chromatography mass spectrometry determination of chloral in water. Study on reaction temperature and reaction time under alkaline conditions on the transformation effect of chloral hydrate. The linear correlation coefficient was 0.9999 when the standard curve in the range of 1 ~50µ g/L, The recovery was 97% ~ 99.8% and RSD was 0.9%. The method has high recovery rate and good precision, good accuracy, simple operation, fast, suitable for actual analysis.

  12. The determination of BTEX and typical monomer hydrocarbon in gas oil by gas chromatography/mass spectrometer%汽油中BTEX及典型单体烃的GC/MS分析

    Institute of Scientific and Technical Information of China (English)

    郑永杰; 刘艳; 丁有毅

    2001-01-01

    对汽油中的BTEX组份及典型单体烃,采用HP-PLOT Al203大口径毛细管柱和程序升温方式,与EI离 子源四极杆质谱联用进行快速分析,对不同类型汽油进行了芳烃组份及典型单体烃组份的测定。用标准气体结合相对重量校正因子并采用面积归一化法进行了定量。%The rapid determination of BTEX and typical monomer hydrocarbon in gas oil by gas chromatography/Mass spectrometer combine with HP-PLOT Al2O3 wide inside diameter capillary column and EI ion source quadrupole mass spectrometer under a grade programming temperature. was setup.There are several different type of gas-oil wasdeterminated with a relative correction factor area normalization method.

  13. Determination of antioxidants in new and used lubricant oils by headspace-programmed temperature vaporization-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nogal Sanchez, Miguel del; Perez Pavon, Jose Luis; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Salamanca (Spain); Glanzer, Paul [University of Vienna, Department of Analytical Chemistry, Vienna (Austria)

    2010-12-15

    A sensitive method is presented to determine antioxidants (2-, 3-, and 4-tert-butylphenol, 2,6-di-tert-butylphenol, 3-tert-butyl-4-hydroxyanisol, 2,6-di-tert-butyl-4-methylphenol, 1-naphthol, and diphenylamine) in new and used lubricant oil samples. Research was carried out on a GC device equipped with a headspace sampler, a programmed temperature vaporizer, and an MS detector unit. The proposed method does not require sample treatment prior to analyses, hence eliminating possible errors occurring in this step. Sample preparation is reduced when placing the oil sample (2.0 g) in the vial and adding propyl acetate (20 {mu}L). Solvent vent injection mode permits a pre-concentration of the compounds of interest in the liner filled with Tenax-TA {sup registered}, while venting other species present in the headspace. Thereby, both the life of the liner and the capillary column is prolonged, and unnecessary contamination of the detector unit is avoided. Calibration was performed by adding different concentrations of analytes to a new oil which did not contain any of the studied compounds. Limits of detection as low as 0.57 {mu}g/L (2-tert-butylphenol) with a precision lower or equal to 5.3% were achieved. Prediction of the antioxidants in new oil samples of different viscosities (5W40, 10W40, and 15W40) was accomplished with the previous calibration, and the results were highly satisfactory. To determine antioxidants in used engine oils, standard addition method was used due to the matrix effect. (orig.)

  14. Aptamer-functionalized stir bar sorptive extraction coupled with gas chromatography-mass spectrometry for selective enrichment and determination of polychlorinated biphenyls in fish samples.

    Science.gov (United States)

    Lin, Saichai; Gan, Ning; Zhang, Jiabin; Qiao, Li; Chen, Yinji; Cao, Yuting

    2016-03-01

    In this paper, a novel aptamer-functionalized stir bar sorptive extraction (SBSE) was developed for selective enrichment of the low abundance polychlorinated biphenyls (PCBs) from fish samples. This approach was based on the immobilization of aptamer which could recognize 2,3',5,5'-tetrachlorobiphenyl (PCB72) and 2',3',4',5,5'-pentachlorobiphenyl (PCB106) on one kind of metal-organic frameworks (Zn4O(BDC)3, MOF-5). MOF-5 as a substrate was prepared by potential-controlled cathodic electrodeposition on stainless steel. This aptamer-functionalized stir bar sorptive extraction (Apt-MOF SBSE) fiber could be facile synthesized in one-step. PCB72 and PCB106 were employed as target analytes for selective extraction by the developed method. The adsorbed targets could be desorbed easily in pH 3.0 100mM glycine-HCl buffers and then extracted by the methylene chloride. Afterwards, the detection was carried out with gas chromatography-tandem mass spectrometry (GC-MS). The Apt-MOF SBSE pretreatment coupled with GC-MS exhibited high selectivity, good binding capacity, stability and reproducibility for the detection of PCBs. It provided a linear range of 0.02-250ngmL(-1) with a good coefficient of determination (R(2)=0.9991-0.9996) and the detection limit was 0.003-0.004ngmL(-1). More importantly, the method was successfully utilized for the determination of PCBs in fish samples with good enrichment factor (1930-2304). Therefore, this new SBSE coating opens up the possibility of selective enrichment of a given target PCBs from complex fish samples. PMID:26717840

  15. Development and application of a dispersive liquid-liquid microextraction method for the determination of tetracyclines in beef by liquid chromatography mass spectrometry.

    Science.gov (United States)

    Mookantsa, S O S; Dube, S; Nindi, M M

    2016-02-01

    A rapid, cost effective and environmentally friendly extraction method, based on dispersive liquid-liquid microextraction (DLLME) was developed for the determination of six tetracyclines in meat destined for human consumption. Meat extracts were analysed for tetracyclines using liquid chromatography tandem mass spectrometry (LC-MS/MS), a sensitive and selective analytical technique. Various factors influencing the pre-concentration of tetracyclines such as sample pH, type and volume of both disperser solvent and extraction solvent were optimized. Validation parameters such as calibration function, limit of detection (LOD), limit of quantification (LOQ), detection capability (CCα), decision limit (CCβ), accuracy and precision were established according to Commission Decision 2002/657/EC. Linearity in the range of 25-200 µg kg(-1) was obtained with regression coefficients ranging from 0.9991 to 0.9998. Recoveries of spiked blank muscle samples at three levels (50, 100 and 150 µg kg(-1)) ranged from 80% to 105% and reproducibility was between 2% and 7%. LODs and LOQs ranged from 2.2 to 3.6 µg kg(-1) and from 7.4 to 11.5 µg kg(-1) respectively while CCα ranged from 105 to 111 µg kg(-1) and CCβ ranged from 107 to 122 µg kg(-1). The proposed method compared well with the existing accepted dispersive solid phase extraction method and was successfully applied to the pre-concentration and determination of tetracyclines in meat samples. Eleven of the thirty bovine muscle samples obtained from local abattoirs and butcheries were found to contain residues of two tetracycline antibiotics (chlortetracycline and oxytetracycline), with oxytetracycline being the most detected. Concentration levels of the tetracycline residues detected in bovine muscle samples were lower (12.4 and 68.9 µg kg(-1)) than the stipulated European Union maximum residue level (MRL) of 100 µg kg(-1), hence the meat was fit for human consumption. From this work it can be concluded that the DLLME

  16. Optimization of derivatization procedure and gas chromatography-mass spectrometry method for determination of bensulfuron-methyl herbicide residues in water.

    Science.gov (United States)

    Zhang, Yan; Wang, Jian; Wang, Guoping; Gao, Chuanyu; Yan, Yan; Wen, Bolong

    2015-07-15

    A simple and efficient technique based on liquid phase extraction with CH2Cl2 solvent followed by derivatization with (C2H5)2O·BF3 solution and confirmation analysis with GC-MS analytical method was developed for detecting the bensulfuron-methyl (BSM) residues in water. Box-Behnken response surface methodology was employed for optimization of the derivatization efficiency. According to the optimization model, the derivatization time of 45min, derivatization temperature at 55°C and 0.2mL (C2H5)2O·BF3 solvent were selected as the optimal derivatization condition for obtaining the maximum desirability of response. Method validation was performed at 6 working standard levels (0.05, 0.1, 0.2, 0.5, 1.0, 5.0μg/mL) and the linearity of the calibration curve was linear well over the 6 fortification levels with the squared correlation coefficient of determination r(2)=0.998 and the LOD was found to be 0.1μg/L for BSM herbicide. The mean value of BSM was detected from 0.0414 to 4.7542μg/mL at levels from 0.05 to 5μg/mL with the recoveries remained at the acceptable level (42.8-95.0%) with the RSD values from 3.5% to 6.2%, which is more accptable and desirable than the results obtained by LC methods. Moreover, the method allowed the determination of BSM residue in real paddy field water samples at concentrations between 0.0902 and 3.4605μg/L. Average recovery rates of the BSM spiked at levels 0.1, 0.2, 0.5, 1.0μg/mL into thirty water samples ranged from 74.1% and 94.1% with the relative standard derivation (RSD) values from 1.9% to 6.7%. PMID:26021849

  17. Dispersive liquid-liquid microextraction for the determination of nitrophenols in soils by microvial insert large volume injection-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2016-07-22

    A rapid and sensitive procedure for the determination of six NPs in soils by gas chromatography and mass spectrometry (GC-MS) is proposed. Ultrasound assisted extraction (UAE) is used for NP extraction from soil matrices to an organic solvent, while the environmentally friendly technique dispersive liquid-liquid microextraction (DLLME) is used for the preconcentration of the resulting UAE extracts. NPs were derivatized by applying an "in-situ" acetylation procedure, before being injected into the GC-MS system using microvial insert large volume injection (LVI). Several parameters affecting UAE, DLLME, derivatization and injection steps were investigated. The optimized procedure provided recoveries of 86-111% from spiked samples. Precision values of the procedure (expressed as relative standard deviation, RSD) lower than 12%, and limits of quantification ranging from 1.3 to 2.6ngg(-1), depending on the compound, were obtained. Twenty soil samples, obtained from military, industrial and agricultural areas, were analyzed by the proposed method. Two of the analytes were quantified in two of the samples obtained from industrial areas, at concentrations in the 4.8-9.6ngg(-1) range.

  18. Simultaneous determination of acrylonitrile, carbon disulfide, methyl ethyl ketone, and isobutanol leachates by purge and trap- gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    According to the Mexican General Law of the Ecological Equilibrium and Environmental Protection, issued by the National Institute of Ecology, some chemicals such as acrylonitrile, methyl ethyl ketone, carbon disulfide, and isobutanol must be monitored in industrial residues because of their toxicity. This report describes an analytical method for the simultaneous determination of these four analytes in leachates. A purge and trap concentrator coupled to a computerized gas-chromatograph-mass selective detector was used to achieve the analysis. Quantitation measurements were based on the internal standardization method, using the area ratios of the molecular ions of the analytes and the internal standard obtained by deconvolution of the data. The scope of this method as well as the validation data is reported. The method is reliable in spite of the fact that, in some cases, the analytes or the standard coeluted with other compounds of the samples. Because the data acquisition is carried out in the scan mode it is possible to detect and identify other substances in the samples. (Author)

  19. Cork as a new (green) coating for solid-phase microextraction: determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

    2013-04-15

    A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80°C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L(-1), respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n=3). The linear range was 0.1-10 μg L(-1) with r≥0.96 and the fiber-to-fiber reproducibility showed RSD≤18.6% (n=5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME.

  20. Dispersive liquid-liquid microextraction for the determination of nitrophenols in soils by microvial insert large volume injection-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2016-07-22

    A rapid and sensitive procedure for the determination of six NPs in soils by gas chromatography and mass spectrometry (GC-MS) is proposed. Ultrasound assisted extraction (UAE) is used for NP extraction from soil matrices to an organic solvent, while the environmentally friendly technique dispersive liquid-liquid microextraction (DLLME) is used for the preconcentration of the resulting UAE extracts. NPs were derivatized by applying an "in-situ" acetylation procedure, before being injected into the GC-MS system using microvial insert large volume injection (LVI). Several parameters affecting UAE, DLLME, derivatization and injection steps were investigated. The optimized procedure provided recoveries of 86-111% from spiked samples. Precision values of the procedure (expressed as relative standard deviation, RSD) lower than 12%, and limits of quantification ranging from 1.3 to 2.6ngg(-1), depending on the compound, were obtained. Twenty soil samples, obtained from military, industrial and agricultural areas, were analyzed by the proposed method. Two of the analytes were quantified in two of the samples obtained from industrial areas, at concentrations in the 4.8-9.6ngg(-1) range. PMID:27317004

  1. Microwave-assisted on-spot derivatization for gas chromatography-mass spectrometry based determination of polar low molecular weight compounds in dried blood spots.

    Science.gov (United States)

    Sadones, Nele; Van Bever, Elien; Archer, John R H; Wood, David M; Dargan, Paul I; Van Bortel, Luc; Lambert, Willy E; Stove, Christophe P

    2016-09-23

    Dried blood spot (DBS) sampling and analysis is increasingly being applied in bioanalysis. Although the use of DBS has many advantages, it is also associated with some challenges. E.g. given the limited amount of available material, highly sensitive detection techniques are often required to attain sufficient sensitivity. In gas chromatography coupled to mass spectrometry (GC-MS), derivatization can be helpful to achieve adequate sensitivity. Because this additional sample preparation step is considered as time-consuming, we introduce a new derivatization procedure, i.e. "microwave-assisted on-spot derivatization", to minimize sample preparation of DBS. In this approach the derivatization reagents are directly applied onto the DBS and derivatization takes place in a microwave instead of via conventional heating. In this manuscript we evaluated the applicability of this new concept of derivatization for the determination of two polar low molecular weight molecules, gamma-hydroxybutyric acid (GHB) and gabapentin, in DBS using a standard GC-MS configuration. The method was successfully validated for both compounds, with imprecision and bias values within acceptance criteria (weight compounds of interest in clinical and/or forensic toxicology, including vigabatrin, beta-hydroxybutyric acid, propylene glycol, diethylene glycol, 1,4-butanediol and 1,2-butanediol, can also be detected using this method. PMID:27578413

  2. Simultaneous determination of praziquantel, pyrantel embonate, febantel and its active metabolites, oxfendazole and fenbendazole, in dog plasma by liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Klausz, Gabriella; Keller, Éva; Sára, Zoltán; Székely-Körmöczy, Péter; Laczay, Péter; Ary, Kornélia; Sótonyi, Péter; Róna, Kálmán

    2015-12-01

    A liquid chromatography-electrospray-mass spectrometry method (LC/MS) has been developed and validated for determination of praziquantel (PZQ), pyrantel (PYR), febantel (FBT), and the active metabolites fenbendazole (FEN) and oxfendazole (OXF), in dog plasma, using mebendazole as internal standard (IS). The method consists of solid-phase extractions on Strata-X polymeric cartridges. Chromatographic separation was carried out on a Phenomenex Gemini C6 -Phenyl column using binary gradient elution containing methanol and 50 mm ammonium-formate (pH 3). The method was linear (r(2)  ≥ 0.990) over concentration ranges of 3-250 ng/mL for PYR andFEB, 5-250 ng/mL for OXF and FEN, and 24-1000 ng/mL for PZQ. The mean precisions were 1.3-10.6% (within-run) and 2.5-9.1% (between-run), and mean accuracies were 90.7-109.4% (within-run) and 91.6-108.2% (between-run). The relative standard deviations (RSD) were <9.1%. The mean recoveries of five targeted compounds from dog plasma ranged from 77 to 94%.The new LC/MS method described herein was fully validated and successfully applied to the bioequivalence studies of different anthelmintic formulations such as tablets containing PZQ, PYR embonate and FBT in dogs after oral administration.

  3. Use of solid-phase microextraction followed by on-column silylation for determining chlorinated bisphenol A in human plasma by gas chromatography-mass spectrometry.

    Science.gov (United States)

    del Olmo, M; Zafra, A; Suárez, B; Gonzalez-Casado, A; Taoufiki, J; Vílchez, J L

    2005-03-25

    In this study, a solid-phase microextraction (SPME) method based on poly(acrylate)-coated fibres has been developed for detection and quantification of chlorinated bisphenol A in human plasma due to the need for an assessment of human exposure to them. After desorption of the analytes for 7 min at 300 degrees C, they were directly derivatized in the GC injector port by injection of 2 microL of diluted bis(trimethylsilyl)trifluoroacetamide (BSTFA). The formation of trimethylsilylate derivatives improves the selectivity, sensitivity and performance of the chromatographic properties obtained when the analytes are directly separated. Quantification was carried out using single-ion monitoring (SIM). The respective chloroderivative molecular ions appear at 406, 440, 474 and 508 m/z; whereas the base peaks corresponding to a loss of a methyl group in all cases appear at 391, 425, 459 and 493 m/z for mono-, di-, tri- and tetrabisphenol A, respectively. Deuterated bisphenol A (BPA-d16) was used as an internal standard. The method was applied to the determination of Cl-BPA, Cl2-BPA, Cl3-BPA and Cl4-BPA at very low concentration levels in plasma. Recovery efficiencies were close to 100% in all cases. PMID:15686981

  4. Formation of multiple trimethylsilyl derivatives in the derivatization of 17α-ethinylestradiol with BSTFA or MSTFA followed by gas chromatography-mass spectrometry determination

    Institute of Scientific and Technical Information of China (English)

    ZHOU Yi-qi; WANG Zi-jian; JIA Ning

    2007-01-01

    N,O-bis(trimethylsily)trifluoroacetamide (BSTFA) and N-methyl-N(trimethylsily) trifluoroacetamide (MSTFA) are common derivatization reagents used in the GC-MS analysis of estrogen steroids such as estrone (E1) and 17(-ethinylestradiol (EE2). In this study, three trimethylsilyl (TMS) steroid derivatives, mono-and di-trimethylsilyl EE2 and mono-trimethylsilyl E1, were observed during the derivatization of EE2 with BSTFA or MSTFA and/or GC separation. Factors influencing the production of multiple TMS derivatives and their relative abundance were examined. It was found that both methanol and bisphenol A competed with estrogenic esteroids when reacting with silylation reagents, and thus affected the formation of TMS derivatives and their relative abundance in the derivatization products. Methanol was found to be more reactive than bisphenol A with the BSTFA reagent. None of the three solvents tested in this study could prevent the generation of multiple TMS derivatives during the derivatization of EE2 with BSTFA, followed by GC analysis. A similar result was observed using MSTFA as the derivative reagent followed by GC analysis. Thus, the suitability of BSTFA or MSTFA as the derivatization reagent for the determination of E1 and EE2 by GC-MS, under the conditions reported here, is questionable. This problem can be solved by adding trimethylsilylimidaz (TMSI) in the BSTFA reagent as recommended, and the performance of the method has been proved in this study.

  5. A novel method for the determination of some pesticides in vegetable oils based on dissociation extraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zayats, Mikhail F; Leschev, Sergey M; Zayats, Marina A

    2016-08-01

    The distribution of 40 pesticides of basic nature in different extraction systems was studied at 20 ± 1°C. The distribution constants (P) and distribution ratios (D) between n-hexane and polar phases are calculated. It was found that the studied pesticides are most fully and selectively extracted from hexane and vegetable oils by solutions of perchloric acid in acetonitrile. In particular, the acidification of acetonitrile decreases the D-value of fenpropimorph by 29,000 times. This phenomenon was used for the development of an improved technique for the quantitative analysis of widely used pesticides of basic nature in rapeseed, linseed, sunflower and olive oils by GC-MS. The proposed approach allows obtaining much purer sample extracts, compared with the use of standard solvent extraction with further purification by the freezing-out technique. This approach expands the range of pesticides (flutriafol, fenpropidine, metazachlor, cyprodinil and others) that can be determined by GC-MS. The recovery values of the studied pesticides from vegetable oils were between 85% and 115% with RSD values below 10%. The obtained limits of detection ranged from 0.001 to 0.1 mg kg(-)(1), and are below or equal to the maximum residue levels (MRLs) set by the European Union for the corresponding pesticides. PMID:27382960

  6. Determination of organophosphorus pesticides in ginseng by carbon nanotube envelope-based solvent extraction combined with ultrahigh-performance liquid chromatography mass spectrometry.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wang, Xinghua; Yang, Hongmei; Shi, Xiaoyu; Liu, Shuying

    2016-06-01

    A miniature extraction envelope containing multiwall carbon nanotubes, diatomite, neutral alumina, and anhydrous magnesium sulfate was developed for the solvent extraction of organophosphorus pesticides in dried ginseng. After the powder of dried ginseng sample was introduced into the envelope, the envelope was heat sealed and sonicated in acetonitrile for the extraction and clean-up of analytes. The resulting extracts were analyzed by an ultrahigh-performance liquid chromatograph with an electrospray ion source and a quadrupole orbitrap mass spectrometer (UHPLC-ESI/Q-Orbitrap MS) under target-MS(2) mode, and the analytes were quantified by matrix-match calibration. Finally, the simultaneous identification and quantification of 19 pesticide residues were carried out by the present method. It is noteworthy that in this method the processes of extraction and clean-up for the analytes could be carried out and accomplished in one step. The recoveries and relative standard deviations (RSDs) of analytes were in the range of 82.6-110.8% and 1.0-10.6%, respectively. The limits of detection (LODs) and quantification (LOQs) for analytes were determined to be 0.08-0.29μgkg(-1) and 0.26-0.98μgkg(-1), respectively. Several pesticide residues investigated in this study were found in 4 real samples, with the concentrations lower than the maximum residue limit (0.050mgkg(-1)) established by European Union. PMID:27093495

  7. Microwave-assisted on-spot derivatization for gas chromatography-mass spectrometry based determination of polar low molecular weight compounds in dried blood spots.

    Science.gov (United States)

    Sadones, Nele; Van Bever, Elien; Archer, John R H; Wood, David M; Dargan, Paul I; Van Bortel, Luc; Lambert, Willy E; Stove, Christophe P

    2016-09-23

    Dried blood spot (DBS) sampling and analysis is increasingly being applied in bioanalysis. Although the use of DBS has many advantages, it is also associated with some challenges. E.g. given the limited amount of available material, highly sensitive detection techniques are often required to attain sufficient sensitivity. In gas chromatography coupled to mass spectrometry (GC-MS), derivatization can be helpful to achieve adequate sensitivity. Because this additional sample preparation step is considered as time-consuming, we introduce a new derivatization procedure, i.e. "microwave-assisted on-spot derivatization", to minimize sample preparation of DBS. In this approach the derivatization reagents are directly applied onto the DBS and derivatization takes place in a microwave instead of via conventional heating. In this manuscript we evaluated the applicability of this new concept of derivatization for the determination of two polar low molecular weight molecules, gamma-hydroxybutyric acid (GHB) and gabapentin, in DBS using a standard GC-MS configuration. The method was successfully validated for both compounds, with imprecision and bias values within acceptance criteria (<20% at LLOQ, <15% at 3 other QC levels). Calibration lines were linear over the 10-100μg/mL and 1-30μg/mL range for GHB and gabapentin, respectively. Stability studies revealed no significant decrease of gabapentin and GHB in DBS upon storage at room temperature for at least 84 days. Furthermore, DBS-specific parameters, including hematocrit and volume spotted, were evaluated. As demonstrated by the analysis of GHB and gabapentin positive samples, "microwave-assisted on-spot derivatization" proved to be reliable, fast and applicable in routine toxicology. Moreover, other polar low molecular weight compounds of interest in clinical and/or forensic toxicology, including vigabatrin, beta-hydroxybutyric acid, propylene glycol, diethylene glycol, 1,4-butanediol and 1,2-butanediol, can also be

  8. Online determination of levoglucosan in ambient aerosols with particle-into-liquid sampler - high-performance anion-exchange chromatography - mass spectrometry (PILS-HPAEC-MS)

    Science.gov (United States)

    Saarnio, K.; Teinilä, K.; Saarikoski, S.; Carbone, S.; Gilardoni, S.; Timonen, H.; Aurela, M.; Hillamo, R.

    2013-10-01

    Biomass burning, such as domestic heating, agricultural, and wild open-land fires, has a significant influence on the atmosphere at the global and, especially, at the local scale. Levoglucosan has been shown to be a good tracer for biomass burning emissions in atmospheric particulate matter, and several analytical techniques have been presented for the determination of levoglucosan from filter samples. In this paper, a novel combination of a particle-into-liquid sampler (PILS) to a high-performance anion-exchange chromatograph (HPAEC) with the detection by a mass spectrometer (MS) is presented for the online analysis of levoglucosan in ambient particles. The PILS-HPAEC-MS technique enables a fast online analysis of levoglucosan from the particulate samples. The method was tested at an urban background station in Helsinki, Finland, in winter 2011. A comparison with simultaneous levoglucosan measurements from filter samples by the HPAEC-MS was performed and it showed a good agreement between the online and offline methods. Additionally, the online levoglucosan data were compared with the biomass burning tracer fragments measured by a high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS). As there were no local biomass burning sources close to the measurement station, online levoglucosan measurements revealed that most of the particles from biomass burning were either regionally distributed or long-range transported in the urban background of Helsinki. The average levoglucosan concentrations were relatively low (average 0.083 μg m-3) during the measurement campaign. The highest concentration peak measured for levoglucosan (1.4 μg m-3) seemed to originate from biomass burning in the Baltic countries, likely in Estonia, that was transported to Helsinki.

  9. Development and optimization of ultra-high performance supercritical fluid chromatography mass spectrometry method for high-throughput determination of tocopherols and tocotrienols in human serum.

    Science.gov (United States)

    Pilařová, Veronika; Gottvald, Tomáš; Svoboda, Pavel; Novák, Ondřej; Benešová, Karolína; Běláková, Sylvie; Nováková, Lucie

    2016-08-31

    The goal of this study was to develop an effective supercritical fluid chromatography method using single quadrupole MS for analysis of all isomeric forms of vitamin E. Finally, two fast and effective methods, the high resolution one and the high speed one, for the determination of 8 vitamin E isomers in human serum were developed. Rapid high-throughput liquid-liquid extraction was selected as a sample preparation step. Sample pretreatment of 100 μL human serum was consisted of protein precipitation with 200 μL ethanol and liquid-liquid extraction by 400 μL hexane/dichloromethane (80/20, v/v). The separation was performed on BEH 2-EP (3.0 × 100 mm, 1.7 μm) stationary phase, using isocratic elution with carbon dioxide and 10 mM ammonium formate in methanol in the ratio 98:2 for high resolution method with run time 4.5 min and in the ratio 95:5 for high speed method, where the run time was 2.5 min. The method development included optimization of key parameters: the choice of the suitable stationary phase and the composition of mobile phase, where an influence of various modifiers, their ratio and additives were tested, and optimization of fine tunning parameters including BPR pressure, flow-rate and column temperature. Quantification of all isomeric forms was performed using SIM (single ion monitoring) experiments in ESI positive ion mode. Both high speed and high resolution chromatographic methods were validated in terms of precision, accuracy, range, linearity, LOD, LOQ and matrix effects using the same LLE procedure. The high resolution method provided more sensitive results (LOD: 0.017-0.083 μg mL(-1)) and better linearity (r(2) > 0.9930) than the high speed one (LOD: 0.083-0.25 μg mL(-1), r(2) > 0.9877) at the cost of double time of analysis. PMID:27506367

  10. Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.; Barber, Larry B.; Burkhardt, Mark R.

    2002-01-01

    A method for the determination of 67 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclicaromatic hydrocarbons, and high-use domestic pesticides. Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ? 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

  11. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  12. Determination of vitamins D2 and D3 in selected food matrices by online high-performance liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS).

    Science.gov (United States)

    Nestola, Marco; Thellmann, Andrea

    2015-01-01

    An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.

  13. Gas chromatography-mass spectrometry determination of pharmacologically active substances in urine and blood samples by use of a continuous solid-phase extraction system and microwave-assisted derivatization.

    Science.gov (United States)

    Azzouz, Abdelmonaim; Ballesteros, Evaristo

    2012-04-01

    A sensitive method based on gas chromatography-mass spectrometry was used to determine 22 pharmacologically active substances (frequently used in the treatment of human and animal's diseases) including analgesics, antibacterials, anti-epileptics, antiseptics, β-blockers, hormones, lipid regulators and non-steroidal anti-inflammatories in blood and urine samples. Samples were subjected to continuous solid-phase extraction in a sorbent column (Oasis HLB), and then the target analytes were eluted with ethyl acetate and derivatized in a household microwave oven at 350 W for 3 min. Finally, these products were determined in a gas chromatograph-mass spectrometer equipped with a DB-5 fused silica capillary column. The analyte detection limits thus obtained ranged from 0.2 to 1.3 ng L⁻¹ for urine samples and 0.8-5.6 ng L⁻¹ for blood samples. Recoveries from both blood and urine ranged from 85 to 102%, and within-day and between-day relative standard deviations were all less than 7.5%. The proposed method offers advantages in reduction of the exposure danger to toxic solvents used in conventional sample pretreatment, simplicity of the extraction processes, rapidity, and sensitivity enhancement. The method was successfully used to quantify pharmacologically active substances in human and animal (lamb, veal and pig) blood and urine. The hormones estrone and 17β-estradiol were detected in virtually all samples, and so were other analytes such as acetylsalicylic acid, ibuprofen, ketoprofen and triclosan in human samples, and florfenicol, pyrimethamine and phenylbutazone in animal samples. PMID:22391330

  14. 气相色谱/质谱联用检测唇用产品中二甘醇的残留%The Determination of Residual Diethylene Glycol in Lipstick by Gas Chromatography/Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    余雯静; 郑晨; 赵玉兰; 沈洁

    2011-01-01

    The method for determination of residual diethylene glycol in lipstick by gas chromatography/mass spectrometry (GC/MS) was established. After grinding by sea sand, removing moisture by anhydrous sodium sulfate, the sample was ultrasonic extracted with methanol, then it was detected directly. Using external standard method and selecting ion quantification,the diethylene glycol had good linear relationship within concentrations between 10. 0 to 1 000. 00 mg/kg. And the correlation coefficient (R2 ) was 0. 999 4. In 10 - 1 000 mg/kg, the average recovery of added level was 92. 5% - 106. 9% and the relative standard deviation (RSD) was 3.5% - 4. 6%. The results showed that the method is suitable for determination residual diethylene glycol in lipstick and other cosmetics.%建立了气相色谱/质谱联用(GC/MS)检测唇膏中二甘醇残留量的方法.样品经海砂研磨均匀、无水硫酸钠除水后,以甲醇超声提取,滤液直接检测.采用外标法,选择离子定量.二甘醇在10.0~1000.0 mg/kg浓度范围内线性关系良好,相关系数(R2)为0.9994.在10~1000mg/kg添加水平的平均回收率为92.5%~106.9%,相对标准偏差(RSD)为3.5%~4.6%.实验表明,该方法适用于唇膏等化妆品中二甘醇残留量的检测.

  15. Enhanced methods for conditioning, storage, and extraction of liquid and solid samples of manure for determination of steroid hormones by solid-phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Combalbert, Sarah; Pype, Marie-Laure; Bernet, Nicolas; Hernandez-Raquet, Guillermina

    2010-09-01

    Hormones are among the highest-impact endocrine disrupters affecting living organisms in aquatic environments. These molecules have been measured in both wastewater and sewage sludge. Analytical techniques for such matrices are well described in the literature. In contrast, there is little information about the analysis of hormones in animal waste. The objectives of this study were, first, to propose a method for conditioning swine manure samples (addition of formaldehyde, separation of the solid and liquid phases, and duration of storage) in order to determine hormones in the liquid fraction of manure by solid-phase extraction (SPE) coupled with gas chromatography-mass spectrometry (GC-MS). Our results showed that analysis of hormones was affected by matrix changes which occurred during freezing and thawing and after addition of formaldehyde, an additive frequently used to preserve environmental samples. Thus, our results argue for the conditioning of samples without formaldehyde and for separating the solid and liquid fractions of manure before freezing. Second, this study reports on the use of a liquid extraction method coupled with SPE and GC-MS analysis for determination of hormones in the solid fraction of manure. Under the conditions selected, hormone recoveries were between 80 and 100%. Finally, the optimized method was used to quantify hormones in both liquid and solid fractions of swine manure from different breeding units. High levels of estrone and α-estradiol were found in samples whereas β-estradiol was detected in smaller amounts. Estriol and progesterone were mainly found in manure from the gestating sow building whereas testosterone was detected in manure from male breeding buildings.

  16. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  17. Determination of thiamethoxam in fruit by high performance liquid chromatography-mass spectrometry/mass spectrometry%水果中噻虫嗪农药残留LC/MS/MS测定

    Institute of Scientific and Technical Information of China (English)

    聂鲲; 周相娟

    2015-01-01

    目的:建立一种简单、快速、灵敏的水果中噻虫嗪农药残留的液相色谱-串联质谱(liquid chromatography-mass spectrometry/mass spectrometry, LC-MS/MS)分析方法。方法称取水果样品5 g,加入乙腈20 mL在超声波振荡条件下提取,提取液使用20 mg石墨化炭黑(Carb)和60 mg N-丙基乙二胺(PSA)粉末进行分散固相萃取净化,经液相色谱质谱联用仪检测,外标法定量。结果噻虫嗪农药残留的色谱图分离效果良好,方法的检出限为0.3μg/kg,线性相关系数为0.9999,噻虫嗪在苹果、梨、桃中的添加水平为0.01、0.05、0.10 mg/kg,回收试验表明该方法平均回收率为88.9%~100.3%(n=6),相对标准偏差为1.98%~4.53%。结论该方法简单、快速、灵敏、净化效果好、回收率高,适合水果中噻虫嗪农药残留的检测和安全监控。%Objective To establish an easy, rapid and sensitive method to determine thiamethoxam pesticide residues in fruit by utilizing liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). Methods Fruit sample 5 g with 20 mL acetonitrile was extracted in the condition of ultrasonic oscillation , then the extract was purified by dispersive solid phase extraction using 20 mg carb and 60 mg PSA as purification sorbent and determined by LC/MS/MS. Results A good separation for thiamethoxam was achieved, with a correlation coefficients about 0.9999. The detection limit of the method was 0.3 μg/kg. The average recoveries of thiamethoxam ranged from 88.9%to 100.3%in the range of 0.01 mg/kg, 0.05 mg/kg and 0.10 mg/kg in apple, pear and peach, and the relative standard deviation (RSD) was between 1.98%and 4.53%, respectively. Conclusion The method is simple, rapid and sensitive, with a good purifying effect and a high recovery rate, which is suitable for the detection and security monitoring of the thiamethoxam in fruit.

  18. Determination of N-Acyl-homoserine Lactones Signal Molecules by Gas Chromatography- Mass Spectrometry%气相色谱-质谱法检测细菌中N-酰基高丝氨酸内酯类信号分子

    Institute of Scientific and Technical Information of China (English)

    郭秀春; 郑立; 张魁英; 徐鲁燕; 王小如

    2012-01-01

    建立了N-酰基高丝氨酸内酯类(N-acyl-homoserine lactones,AHLs)群体感应信号分子的气相色谱-质谱( GC - MS)检测方法,并优化了检测条件.在优化条件下,采用选择离子扫描模式(SIM)从细菌Pseudoalteromonas sp.NJ6 -3 -1培养液中检测到3种AHLs(N-己基高丝氨酸内酯(C6- HSL)、N-辛基高丝氨酸内酯(C8- HSL)和N-十四基高丝氨酸内酯(C14- HSL)).与传统的薄层层析-生物传感器(TLC - biosensor)和高效液相色谱法(HPLC)相比,该方法更加简单、高效,只需对培养液样品进行简单处理,即可定性检测样品中的AHLs分子.该方法为从复杂基质中检测和鉴定AHLs信号分子提供了有效手段.%A rapid and sensitive method for the determination of N-acyl-homoserine lactones( AHLs) , a kind of quorum sensing signal molecules in Gram-negative bacteria, was established based on gas chromatography - mass spectrometric technique. The GC - MS conditions for the detection of AHLs were optimized. Under the optimal conditions, three kinds of AHLs, e. g. N-hexanoyl-L-homoserine lactone(C6 -HSL) , N-octanoyl-L-homoserine lactone(C8 -HSL) and N-tetradecanoyl-L-homoserine lactone(C14 - HSL) , were detected in the cultured supernatants of bacteria Pseudoalteromonas sp. NJ6 -3-1 under selected ion monitoring(SIM) mode. Compared with the traditional TLC-biosensor and HPLC method, this method is rapid and simple. AHLs in the samples could be detected qualitatively only by a simple sample handling procedure. The study provides a useful method in the detection of AHLs from complicated mixtures.

  19. Comparison of hollow fiber liquid-phase microextraction and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of drugs of abuse in biological samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Meng, Liang; Zhang, Wenwen; Meng, Pinjia; Zhu, Binling; Zheng, Kefang

    2015-05-01

    Two microextraction techniques based on hollow fiber liquid-phase microextraction (HF-LPME) and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) had been applied for the determination of drugs of abuse (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, methcathinone, ketamine, meperidine, and methadone) in urine and blood samples by gas chromatography-mass spectrometry. Parameters affecting extraction efficiency have been investigated and optimized for both methods. Under the optimum conditions, linearities were observed for all analytes in the range 0.0030-10 μg/ml with the correlation coefficient (R) ranging from 0.9985 to 0.9995 for HF-LPME and in the range 0.0030-10 μg/ml with the R ranging from 0.9985 to 0.9994 for DLLME. The recovery of 79.3-98.6% with RSDs of 1.2-4.5% was obtained for HF-LPME, and the recovery of 79.3-103.4% with RSDs of 2.4-5.7% was obtained for DLLME. The LODs (S/N=3) were estimated to be in the range from 0.5 to 5 ng/ml and 0.5 to 4 ng/ml, respectively. Compared with HF-LPME, the UA-LDS-DLLME technique had the advantages of less extraction time, suitability for batches of sample pretreatment simultaneously, and higher extraction efficiency, while HF-LPME has excellent sample clean-up effect, and is a robust and suitable technique for various sample matrices with better repeatability. Both methods were successfully applied to the analysis of drugs of abuse in real human blood sample.

  20. Comparison of hollow fiber liquid-phase microextraction and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of drugs of abuse in biological samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Meng, Liang; Zhang, Wenwen; Meng, Pinjia; Zhu, Binling; Zheng, Kefang

    2015-05-01

    Two microextraction techniques based on hollow fiber liquid-phase microextraction (HF-LPME) and ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) had been applied for the determination of drugs of abuse (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, methcathinone, ketamine, meperidine, and methadone) in urine and blood samples by gas chromatography-mass spectrometry. Parameters affecting extraction efficiency have been investigated and optimized for both methods. Under the optimum conditions, linearities were observed for all analytes in the range 0.0030-10 μg/ml with the correlation coefficient (R) ranging from 0.9985 to 0.9995 for HF-LPME and in the range 0.0030-10 μg/ml with the R ranging from 0.9985 to 0.9994 for DLLME. The recovery of 79.3-98.6% with RSDs of 1.2-4.5% was obtained for HF-LPME, and the recovery of 79.3-103.4% with RSDs of 2.4-5.7% was obtained for DLLME. The LODs (S/N=3) were estimated to be in the range from 0.5 to 5 ng/ml and 0.5 to 4 ng/ml, respectively. Compared with HF-LPME, the UA-LDS-DLLME technique had the advantages of less extraction time, suitability for batches of sample pretreatment simultaneously, and higher extraction efficiency, while HF-LPME has excellent sample clean-up effect, and is a robust and suitable technique for various sample matrices with better repeatability. Both methods were successfully applied to the analysis of drugs of abuse in real human blood sample. PMID:25801996

  1. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of selected herbicides and their degradation products in water using solid-phase extraction and gas chromatography/mass spectrometry

    Science.gov (United States)

    Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

    2000-01-01

    A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

  2. 气相色谱-质谱法分析饮用水源水中甲基汞%Determination of Methyl Mercury in Drinking Water Using Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘浩; 甘志永; 邹塞; 王海棠

    2013-01-01

    Automatic solid phase extract equipment (SPE) and Gas Chromatography-Mass Spectrometry were used to analyze methyl mercury in drinking water.Large volume of water sample (SL) was extracted by Mercapto Cotton and then determinated by Selected Ion Monitoring (SIM).The results showed that better linearity was achieved compared to national standard method.The experiment operation was easy and fast with high sensitivity.The recovery of three different levels were over 71.0% 、74.4% 、76.0%,respectively.The 10ug/L sample was tested 6 times and the relative standard deviation(BSD) was 4.8%.The detection limit was 3 × 10-4 μg/L,which satisfied with methyl mercury standard of drinking water.%采用自动固相萃取-气质联用法分析饮用水源中的甲基汞,通过巯基棉小柱萃取大体积(5L)水样后,选择离子扫描方式(SIM)进行定量.实验对比国家标准方法具有更好的线性关系,实际操作简单快捷,灵敏度高.3个浓度水平进行加标回收实验,回收率分别大于71.0%、74.4%、76.0%.对10 μg/L浓度重复进样6次,相对标准偏差(RSD)为4.8%.该方法检出限可达到3×104μg/L,满足饮用水源水中甲基汞标准限值要求.

  3. Recent advances in thermal desorption-gas chromatography-mass spectrometery method to eliminate the matrix effect between air and water samples: application to the accurate determination of Henry's law constant.

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2014-05-16

    Accurate values for the Henry's law constants are essential to describe the environmental dynamics of a solute, but substantial errors are recognized in many reported data due to practical difficulties in measuring solubility and/or vapor pressure. Despite such awareness, validation of experimental approaches has scarcely been made. An experimental approach based on thermal desorption-gas chromatography-mass spectrometery (TD-GC-MS) method was developed to concurrently allow the accurate determination of target compounds from the headspace and aqueous samples in closed equilibrated system. The analysis of six aromatics and eight non-aromatic oxygenates was then carried out in a static headspace mode. An estimation of the potential bias and mass balance (i.e., sum of mass measured individually from gas and liquid phases vs. the mass initially added to the system) demonstrates compound-specific phase dependency so that the best results are obtained by aqueous (less soluble aromatics) and headspace analysis (more soluble non-aromatics). Accordingly, we were able to point to the possible sources of biases in previous studies and provide the best estimates for the Henry's constants (Matm(-1)): benzene (0.17), toluene (0.15), p-xylene (0.13), m-xylene (0.13), o-xylene (0.19), styrene (0.27); propionaldehyde (9.26), butyraldehyde (6.19), isovaleraldehyde (2.14), n-valeraldehyde (3.98), methyl ethyl ketone (10.5), methyl isobutyl ketone (3.93), n-butyl acetate (2.41), and isobutyl alcohol (22.2). PMID:24704185

  4. Simultaneous determination of perfluoroalkyl iodides, perfluoroalkane sulfonamides, fluorotelomer alcohols, fluorotelomer iodides and fluorotelomer acrylates and methacrylates in water and sediments using solid-phase microextraction-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bach, Cristina; Boiteux, Virginie; Hemard, Jessica; Colin, Adeline; Rosin, Christophe; Munoz, Jean-François; Dauchy, Xavier

    2016-05-27

    Here, we developed and validated a headspace-solid-phase microextraction-gas chromatography/mass spectrometry (HS-SPME-GC/MS) method for the determination of 14 volatile perfluorinated alkylated substances (PFASs) in water and sediment samples according to SANTE 11945/2015 guidelines. Three fluorotelomer alcohols (FTOHs), two perfluoroalkyl iodides (PFIs), three fluorotelomer iodides (FTIs), four fluorotelomer acrylates and methacrylates (FTACs and FTMACs) and two perfluoroalkyl sulfonamides (FASAs) were analysed simultaneously to assess the occurrence of these compounds from their emission sources to the outlets in water treatment plants. Several SPME parameters were optimised for both water and sediment to maximise responses and keep analysis time to a minimum. In tap water, the limits of quantification (LOQs) were found to be between 20ng/L and 100ng/L depending on the analyte, with mean recoveries ranging from 76 to 126%. For sediments, LOQs ranged from 1 to 3ng/g dry weight depending on the target compound, with mean recoveries ranging from 74 to 125%. SPME considerably reduced sample preparation time and its use provided a sensitive, fast and simple technique. We then used this HS-SPME-GC/MS method to investigate the presence of volatile PFASs in the vicinity of an industrial facility. Only 8:2 FTOH and 10:2 FTOH were detected in a few water and sediment samples at sub-ppb concentration levels. Moreover, several non-target fluorotelomers (12:2 FTOH, 14:2 FTOH and 10:2 FTI) were identified in raw effluent samples. These long-chain fluorotelomers have high bioaccumulative potential in the aquatic environment compared with short-chain fluorotelomers such as 6:2 FTOH and 6:2 FTI. PMID:27125188

  5. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection

    OpenAIRE

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-01-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer...

  6. Accuracy of X-ray fluorescence spectrometric determination of Rb and Sr concentrations in rock samples

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering for matrix correction in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide concentrations at a relative accuracy level of 1%. The empirical method applies to rock samples showing differences in mass absorption up to a factor of two. The accuracy of the method has been tested by analysis of 57 samples analysed for Rb and Sr by mass spectrometric isotope dilution. In addition a few of the U.S. Geological Survey reference rock powders, showing significantly different mass absorption, were analysed for Rb and Sr. It is demonstrated that the mica effect, if significant, is smaller than 1% relative. There is no advantage in the use of the LiF(220) analysing crystal as a substitute for the LiF(200). The method appears to be insensitive to the pellet thickness. (author)

  7. 气相色谱及气相色谱-质谱法检测食品中增塑剂%Determination of Phthalates in Foods by Gas Chromatography and Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    李一尘; 徐静; 董伟峰; 肖珊珊

    2012-01-01

    利用气相色谱及气相色谱-质谱联用技术,对食品中4种邻苯酸二甲酯类化合物进行检测。对于非油脂类食品,气相色谱法的检出限为1.5mg/kg,平均回收率为67.4%-92.9%,相对标准偏差为1.6%-4.7%;气相色谱-质谱联用的检出限为0.05mg/kg,平均回收率为66.3%-112.9%,相对标准偏差为2.9%-11.3%。对于油脂类食品,气相色谱法的检出限为30mg/kg,平均回收率为73.4%-96.1%,相对标准偏差为1.6%-2.8%;气相色谱-质谱联用的检出限为1.5mg/kg,平均回收率为64.1%-80.2%,相对标准偏差为1.6%-4.5%。用该分析方法对285批食品样品进行了分析检测,1批食品样品检出BBP,13批检出DBP,63批检出DEHP,总检出阳性样品68批,总阳性检出率23.9%,其检出质量分数为0.05-1.27mg/kg。该方法前处理简单,分离效果好,灵敏度高,能够满足食品中4种邻苯二甲酸酯检测的需要。%In this paper,4 phthalates(DBP,BBP,DEHP,DNOP) in the foods were determined by gas chromatography and gas chromatography-mass spectrometry.In the fat free foods with gas chromatography,the method detection limits was 1.5mg/kg,the recoveries ranged from 67.4%-92.9%,and the relative standard deviations were between 1.6% and 4.7%;with gas chromatography-mass spectrometry,the method detection limits was 0.05mg/kg,the recoveries ranged from 66.3%-112.9%,and the relative standard deviations were between 2.9% and 11.3%.In the greasy foods with gas chromatography,the method detection limits was 30mg/kg,the recoveries ranged from 73.4%-96.1%,and the relative standard deviations were between 1.6% and 2.8%;with gas chromatography-mass spectrometry,the method detection limits was 1.5mg/kg,the recoveries ranged from 64.1%-80.2%,and the relative standard deviations were between 1.6% and 4.5%.Altogether 285 pieces of food samples were detected by this method.The findings were as follows: 1 sample contained BBP,13 samples contained DBP,and 63 samples contained DEHP.The total 68 samples

  8. Extraction-mass spectrometric determination of platinum metals in materials of complex composition

    International Nuclear Information System (INIS)

    A method is developed for the extraction mass-spectrometric determination of platinum metals, including ruthenium. The loWer limit of detectable contents is 1.6x10-6 mass.% (a coefficient of concentration is 50). The relative standard deviation is 0.19-0.38. Relative sensitivity coefficients determined experimentally with the aid of reference samples for platinum metals enable the systematic errors of analysis results to be taken into account. The method is most advisably used for the simultaneous determination of platinum metals in complex objects (minerals, rocks, etc.)

  9. Determination of Epichlorohydrin in Water by Purge and Trap/Gas Chromatography-Mass Spectrometry%吹扫捕集/气相色谱-质谱联用法测定水中环氧氯丙烷

    Institute of Scientific and Technical Information of China (English)

    张芹; 陈科平; 王少青

    2015-01-01

    A method for determination of epichlorohydrin was established based on purge and trap / gas chromatography mass spectrometry. The purge temperature, purge time, desorption temperature and desorption time were adjusted ,the efficiency of purge and trap affected by purge and trap conditions was analyzed, and the best purge and trap condition were determined. Under the optimized conditions, the correlation coefficients of epichlorohydrin were 0.999 9, the average recoveries were 99.7%, and the relative standard deviations of method were 3.0%; the detection limits of method were 0.10 μg/L. Compared with the national standard method, this method takes advantages of easy to operation, the linear relations, accuracy and precision were well. The method can meet the requirements for the determination of epichlorohydrin in surface water and drinking water.%建立吹扫捕集/气相色谱-质谱法(GC-MS)测定水中环氧氯丙烷的方法。通过对吹扫捕集条件进行调整,讨论吹扫温度和吹扫时间、解吸温度和解吸时间对吹扫捕集效率的影响,确定最佳吹扫捕集条件。结果表明,在最佳条件下,环氧氯丙烷的线性相关系数为0.9999,平均加标回收率为99.7%,相对标准偏差为3.0%;方法检出限为0.10μg/L。该方法与国家标准方法相比,操作简便、检出限低、准确度和精密度高,适用于地表水和生活饮用水中环氧氯丙烷的分析测定。

  10. Quantitative Determination of Perfluorocarbon in Breath by Gas Chromatography-Mass Spectrometry%气相色谱-质谱法测定全氟丙烷血药浓度的方法学研究

    Institute of Scientific and Technical Information of China (English)

    李晓明; 胡蓓; 江骥

    2004-01-01

    A quantitative method has been developed for the detection of perfluorocarbon in breath gas by gas chromatography mass spectrometry(GC/MS) with the column of DB-5M (40m×0.25mm×0. 25μm). The quantization range of the assay for perfluorocarbon in collected expired gas is 0. 02 to 5mg/kg after bolus injection intravenously within 15min in normal subjects.

  11. Electrothermal atomization atomic absorption spectrometric determination of trace metals in uranium-plutomium fuel materials

    International Nuclear Information System (INIS)

    Atomic absorption spectrometric methods using the electrothermal mode of atomization developed for the determination of Ag, Be, Ca, Cd, Cr, Co, Cu, Fe, Li, Mn, Na, Ni, Sn and Zn in (U, Pu) solution with 4% plutonium have been described. The carbon rod atomizer has been adapted for glove box operation to enable handling of plutonium containing solution samples. Multielement solution standards with graded concentrations of the analytes and fixed concentration of the matrix are used in the standardization process. Nanogram to sub-nanogram quantities of the analytes have been determined with a precision of better than 9% RSD using 5 μl of the sample aliquots. (orig.)

  12. Analytical approach to determining human biogenic amines and their metabolites using eVol microextraction in packed syringe coupled to liquid chromatography mass spectrometry method with hydrophilic interaction chromatography column.

    Science.gov (United States)

    Konieczna, Lucyna; Roszkowska, Anna; Synakiewicz, Anna; Stachowicz-Stencel, Teresa; Adamkiewicz-Drożyńska, Elżbieta; Bączek, Tomasz

    2016-04-01

    Analysis of biogenic amines (BAs) in different human samples provides insight into the mechanisms of various biological processes, including pathological conditions, and thus may be very important in diagnosing and monitoring several neurological disorders and cancerous tumors. In this work, we developed a simple and fast procedure using a digitally controlled microextraction in packed syringe (MEPS) coupled to liquid chromatography mass spectrometry (LC-MS) method for simultaneous determination of biogenic amines, their precursors and metabolites in human plasma and urine samples. The separation of 12 low molecular weight and hydrophilic molecules with a wide range of polarities was achieved with hydrophilic interaction chromatography (HILIC) column without derivatization step in 12 min. MEPS was implemented using the APS sorbent in semi-automated analytical syringe (eVol(®)) and small volume of urine and plasma samples, 5 0µL and 100 μL, respectively. We evaluated important parameters influencing MEPS efficiency, including stationary phase selection, sample pH and volume, number of extraction cycles, and washing and elution volumes. In optimized MEPS conditions, the analytes were eluted by 3 × 50 μL of methanol with 0.1% formic acid. The chromatographic separation of analytes was performed on XBridge Amide™ BEH analytical column (3.0mm × 100 mm, 3.5 µm) using gradient elution with mobile phase consisting of phase A: 10mM ammonium formate buffer in water pH 3.0 and phase B: 10mM ammonium formate buffer in acetonitrile pH 3.0. The LC-HILIC-MS method was validated and, in optimum conditions, presented good linearity in concentration range within 10-2000 ng/mL for all the analytes with a determination coefficient (r(2)) higher than 0.999 for plasma and urine samples. Method recovery ranged within 87.6-104.3% for plasma samples and 84.2-98.6% for urine samples. The developed method utilizing polar APS sorbent along with polar HILIC column was applied for

  13. Determination of Aldrin and Dieldrin residue in food by gas chromatography-mass spectrometry%气相色谱-质谱法测定食品中残留的艾氏剂和狄氏剂

    Institute of Scientific and Technical Information of China (English)

    庞艳华; 胡晓静; 孙兴权; 李军; 李一尘

    2011-01-01

    建立了一种测定食品中艾氏剂和狄氏剂残留量的气相色谱-质谱方法.样品中的艾氏剂和狄氏剂经丙酮-正己烷混合溶剂均质提取,凝胶层析柱结合弗罗里硅土固相萃取小柱净化,气相色谱-质谱选择离子方法进行测定,外标法定量.实验结果表明:样品中加入5~200,μg/kg浓度水平的艾氏剂和狄氏剂,回收率在79.8%~106.2%之间,相对标准偏差小于7.17%(RSD,n=10).本方法线性响应良好,提取效率高,干扰少,可用于粮谷、蔬菜、水果等植物产品以及肉、鱼等动物产品中艾氏剂和狄氏剂残留量的测定.%A method was established for the determination of Aldrin and Dieldrin residue in foods by gas chromatography-mass spectrometry (GC-MS). The samples were extracted with acetone and hex-ane,and purified by gel permeation chromatograp and florisil solid phase extraction. The external standard method was adopted for the determination by GC-MS with selected ion m onitoring mode (SIM). Tests of recovery were made by addition of standard Aldrin and Dieldrin to food samples at the concentration levels in the range of 5 ~ 200 ptg/kg,and the results of recovery were between 79. 8% and 106. 2% with relative standard deviations less than 7.17% (n=10). The results indicate the method has the advantage of good linearity, high extraction efficiency and less interference, and can be applied to routine analysis and quality control in vegetable and animal ptoducts.

  14. Analytical approach to determining human biogenic amines and their metabolites using eVol microextraction in packed syringe coupled to liquid chromatography mass spectrometry method with hydrophilic interaction chromatography column.

    Science.gov (United States)

    Konieczna, Lucyna; Roszkowska, Anna; Synakiewicz, Anna; Stachowicz-Stencel, Teresa; Adamkiewicz-Drożyńska, Elżbieta; Bączek, Tomasz

    2016-04-01

    Analysis of biogenic amines (BAs) in different human samples provides insight into the mechanisms of various biological processes, including pathological conditions, and thus may be very important in diagnosing and monitoring several neurological disorders and cancerous tumors. In this work, we developed a simple and fast procedure using a digitally controlled microextraction in packed syringe (MEPS) coupled to liquid chromatography mass spectrometry (LC-MS) method for simultaneous determination of biogenic amines, their precursors and metabolites in human plasma and urine samples. The separation of 12 low molecular weight and hydrophilic molecules with a wide range of polarities was achieved with hydrophilic interaction chromatography (HILIC) column without derivatization step in 12 min. MEPS was implemented using the APS sorbent in semi-automated analytical syringe (eVol(®)) and small volume of urine and plasma samples, 5 0µL and 100 μL, respectively. We evaluated important parameters influencing MEPS efficiency, including stationary phase selection, sample pH and volume, number of extraction cycles, and washing and elution volumes. In optimized MEPS conditions, the analytes were eluted by 3 × 50 μL of methanol with 0.1% formic acid. The chromatographic separation of analytes was performed on XBridge Amide™ BEH analytical column (3.0mm × 100 mm, 3.5 µm) using gradient elution with mobile phase consisting of phase A: 10mM ammonium formate buffer in water pH 3.0 and phase B: 10mM ammonium formate buffer in acetonitrile pH 3.0. The LC-HILIC-MS method was validated and, in optimum conditions, presented good linearity in concentration range within 10-2000 ng/mL for all the analytes with a determination coefficient (r(2)) higher than 0.999 for plasma and urine samples. Method recovery ranged within 87.6-104.3% for plasma samples and 84.2-98.6% for urine samples. The developed method utilizing polar APS sorbent along with polar HILIC column was applied for

  15. 气相色谱-质谱法测定电子产品中的四溴双酚-A%Determination of tetrabromobisphenol-A in electronic products by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    肖进进; 富玉; 林舒; 张姝

    2011-01-01

    A method for the determination of tetrabromobisphenol-A ( TBBP-A ) in electronic products was developed by gas chromatography-mass spectrometry ( GC-MS ). The TBBP-A was extracted from electronic products by automatic digestion oven with acetone and concentrated by the evaporation of solvent. It was redissolved in methylene chloride , back-extracted by potassium carbonate solution and reacted with acetic anhydride. The derivative was extracted by hexane and determined by GC-MS. The linear calibration curve was obtained in the range of 0.25 - 5.0 mg/L with a correlation coefficient of 0.996. The detection limit of the method was 0.05 mg/kg. The recoveries were 87.3% - 104.1% and the relative standard deviations were 5.6% - 8.5%. The method is accurate and sensitive, and it is suitable for the analysis of tetrabromobisphenol-A in electronic products.%建立了电子产品中四溴双酚-A(TBBP-A)的气相色谱-质谱联用(GC-MS)检测方法.样品经丙酮提取后挥发至干,经二氯甲烷重新溶解后,用碳酸钾溶液反提取,反提取液与乙酸酐衍生化反应.衍生产物经正己烷提取后,采用GC-MS进行分析.结果表明,方法的线性范围为0.25~5.0 mg/L,相关系数为0.996;方法的检出限为0.05mg/kg;平均回收率为87.3%~104.1%,相对标准偏差为5.6%~8.5%.该方法准确、灵敏,可用于实际电子产品中四溴双酚-A的分析.

  16. 气相色谱-质谱法对食用油中17种邻苯二甲酸酯的测定%Determination of 17 Phthalates in Edible Oil by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王鹏功; 高明星; 程刚; 马绪丽; 刘润珠; 李璐

    2012-01-01

    采用乙腈液一液萃取法对邻苯二甲酸酯类物质进行提取,通过弗洛里硅土固相萃取柱去除样品杂质,经旋转蒸干后定容,选择气相色谱一质谱联用技术进行测试,建立食用油中17种邻苯二甲酸酯的检测方法。该方法操作简单、准确可靠、重现性良好,各种邻苯二甲酸酯化合物的方法检出限为20~60μg/L,加标回收率为83.20%102.09%,相对标准偏差为2.73%~5.77%,能够满足食用油中邻苯二甲酸酯类化合物含量的测定。%An analytical method to determine 17 phthalates in edible oil was presented using liquid-liquid extraction and gas chromatography-mass spectrometry (GC-MS). The sample pretreatment before GC-MS analysis was achieved by liquid-liquid extraction with acetonitrile, removal of unwanted impurities using a Florian silica solid phase column, rotary evaporation until dryness, re-dissolution. The presented method was simple, accurate, reliable and reproducible. The limits of detection of this method for 17 phthalates tested were in the range of 20 -- 60 μa g/L. The average spike recovery rates of these phthalates from blank edible oil samples varied from 83.20% to 102.09% with relative standard deviation of 2.73%-5.77%. This method could meet the requirements for the determination of phthalates in edible oil.

  17. Determination of 26 Kinds of Volatile Organic Compounds in Water with Purge and Trap/Gas Chromatography-Mass Spectrometry%吹扫捕集/GC-MS法测定水中26种挥发性有机物

    Institute of Scientific and Technical Information of China (English)

    张芹; 曾凡海; 王少青

    2013-01-01

    采用吹扫捕集/气相色谱-质谱(GC-MS)法测定水中26种挥发性有机物(VOCs),并对吹扫捕集条件进行优化,分析了吹扫温度和吹扫时间、解吸温度和解吸时间对吹扫捕集效率的影响.分析结果表明,在此条件下,挥发性有机物的线性相关系数为0.999 0~0.999 9,平均加标回收率为94.0%~108.3%,相对标准偏差为2.4%~6.1%,具有较好的线性关系,准确度和精密度;方法检出限为0.03~0.28 μg/L,远低于《地表水环境质量标准》(GB 3838-2002)中限值.%Purge and trap/gas chromatography-mass spectrometry was used to determine 26 volatile organic compounds (VOCs) in water, and the conditions of the method were optimized. The influences of purge temperature, purge time, desorption temperature and desorption time on the efficiency of purge and trap were analyzed. Under the optimized conditions, this method had good linear relations, accuracy and precision, with a linear correlation coefficient of VOCs of 0. 999 0~0. 999 9, an average recovery of 94. 0%~ 108. 3% , a relative standard deviation of 2. 4%~6. 1% and a detection limit of 0. 03~0. 28 μg/L, which is much lower than the mid-limited value stipulated in Environmental Quality Standards for Surface Water (GB 3838-2002).

  18. 气相色谱-质谱法同时测定氧化型染发剂中的17种染料%Simutaneous Determination of 17 Components in Oxidative Hair Dyes by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    赖莺; 陈和秀; 林睿; 王鸿辉; 董清木; 黄宗平

    2011-01-01

    建立了氧化型染发剂中17种染料中间体(包括苯二胺类、氨基酚类、苯二酚类、萘酚和氨基吡啶类等)的气相色谱-质谱检测方法.采用体积分数为50%的乙醇超声提取染发剂中的染料中间体,加入还原剂连二亚硫酸钠防止待测物变质,选择DB-WAX毛细管柱实现了在25 min内同时分离17种水溶性和醇溶性染料.结果表明,本方法对所测物质的检出限(LOD)为2~380 mg/kg,定量限(LOQ)为7.5~1267.5 mg/kg.在1,2,10,20或100倍LOQ 4个添加水平下的平均回收率在81.1%~103.7%之间,相对标准偏差(n=6)在0.67%~3.73%之间.%A reliable Gas Chromatography-Mass Spectrometry(GC-MS) method was developed for the simultaneous determination of 17 dye intermediates, including benzenediamines, aminophenols, benzenediols, naphthalenediol and diaminopyridine, in oxidative hair dyes. Samples were extracted with 50% ethanol by adding sodium dithionite to prevent oxidation. A DB-WAX capillary column was selected for the separation of both water soluble and alcohol soluble hair dye intermediates. The results showed that 17 dye intermediates were well separated within 25 min. The detection limits of these compounds were in the range of 2-380 mg/kg. The recoveries of the target compounds in hair dyes ranged from 81. 1% to 103. 7% with four addition levels. The method described was validated by 5 different laboratories and successfully applied to the analysis of commercial oxidative hair dyes.

  19. Determination of tetrabromobisphenol in a electronics by gas chromatography-mass spectrometry with ultrasonic extraction and derivatisation%气相色谱-质谱法测定电子产品中四溴双酚A

    Institute of Scientific and Technical Information of China (English)

    陈啟荣; 郎爽; 魏岩; 范筱京; 夏敏

    2011-01-01

    A method for the determination of tetrabromobisphenol A in electronics using ultrasonic extraction and derivatisation by Gas Chromatography-Mass spectrometry was established. Samples were extracted with hexane and acetone mixtures. A derivatisation step was carried out with BSTFA + TMCS as derivatisation reagents. Effect of experiment conditions, such as derivative volume, derivatisation time and temperature were investigated. Under the optimized conditions, the calibration curve showed good linearity between 0. 4 μg/mL and 4. 0 μg/mL. The results showed that the recoveries of samples were 61.2% ~ 93%. The relative standard deviation was less than 5%. The limit of detection was 1. 25 mg/kg, and the limit of quantity was 3.75 mg/kg.%建立了超声提取-硅烷化气相色谱-质谱测定电子产品中四溴双酚A的方法.样品用正己烷/丙酮作提取剂,浸泡后超声提取,经N,O-双三甲基硅烷三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)衍生化,利用气相色谱-质谱仪进行定性定量分析.讨论了浸泡时间对提取效率的影响,优化衍生温度和衍生时间.结果表明:标样衍生后在0.4~4.0 μg/mL范围内具有良好的线性.加标回收率范围在61%~93%之间,平行测定的相对标准偏差小于5%.方法的检出限为1.25 mg/kg,定量限为3.75 mg/kg.

  20. 气相色谱-质谱法测定化妆品中3种防腐剂%Determination of three preservatives in cosmetics by gas chromatography- mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    金红利; 林维宣; 郭桂媛; 徐伟

    2011-01-01

    建立了同时测定化妆品中2-氯-4-甲氧基苯酚、4-溴-2-甲氧基苯酚和三氯生3种防腐剂含量的气相色谱-质谱法.采用Agilent 6890N-5975气相色谱-质谱联用仪,配DB-5 MS色谱柱(30 m×0.25 mm×0.25μm),对3种型式的化妆品:口红(膏状)、香波(乳状)和化妆水(水状)的样品进行测试.结果表明,检测的相对标准偏差为0.86%~4.49%,平均回收率为92.2%~ 98.9%,对2-氯-4-甲氧基苯酚、4-溴-2-甲氧基苯酚和三氯生的检出限分别为0.1,0.5及0.1 mg/L.%Method for simultaneous determination of content of three preservatives, 2 - chloro - 4 -methoxyphenol ,4 - bromo - 2 - methoxyphenol and triclosan in cosmetics by gas chromatography - mass spectrometry (GC - MS) was established. Agilent 6890N - 5975 GC - MS with DB - 5MS GC column (30 m ×0. 25 mm x 0. 25 pun) was adopted as the main instrument. Samples of three forms of cosmetics, lipstick ( as gel form) , hair shampoo ( as emulsion form) and toilet water ( as aqueous solution form) were taken for testing. The results showed that the relative standard deviations lies between 0. 86% and 4. 49% ;the recoveries achieves between 92. 2% and 98. 9% ;while the limit of detection for 2 -chloro -4 -methoxyphenol, 4 - bromo - 2 - methoxyphenol and triclosan was identified as 0. 1,0. 5 and 0. 1 mg/L respectively.

  1. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U+ , UO+ and UO2+ ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  2. Determination of Human-Health Pharmaceuticals in Filtered Water by Chemically Modified Styrene-Divinylbenzene Resin-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Furlong, Edward T.; Werner, Stephen L.; Anderson, Bruce D.; Cahill, Jeffery D.

    2008-01-01

    In 1999, the Methods Research and Development Program of the U.S. Geological Survey National Water Quality Laboratory began the process of developing a method designed to identify and quantify human-health pharmaceuticals in four filtered water-sample types: reagent water, ground water, surface water minimally affected by human contributions, and surface water that contains a substantial fraction of treated wastewater. Compounds derived from human pharmaceutical and personal-care product use, which enter the environment through wastewater discharge, are a newly emerging area of concern; this method was intended to fulfill the need for a highly sensitive and highly selective means to identify and quantify 14 commonly used human pharmaceuticals in filtered-water samples. The concentrations of 12 pharmaceuticals are reported without qualification; the concentrations of two pharmaceuticals are reported as estimates because long-term reagent-spike sample recoveries fall below acceptance criteria for reporting concentrations without qualification. The method uses a chemically modified styrene-divinylbenzene resin-based solid-phase extraction (SPE) cartridge for analyte isolation and concentration. For analyte detection and quantitation, an instrumental method was developed that used a high-performance liquid chromatography/mass spectrometry (HPLC/MS) system to separate the pharmaceuticals of interest from each other and coextracted material. Immediately following separation, the pharmaceuticals are ionized by electrospray ionization operated in the positive mode, and the positive ions produced are detected, identified, and quantified using a quadrupole mass spectrometer. In this method, 1-liter water samples are first filtered, either in the field or in the laboratory, using a 0.7-micrometer (um) nominal pore size glass-fiber filter to remove suspended solids. The filtered samples then are passed through cleaned and conditioned SPE cartridges at a rate of about 15

  3. DETERMINATION OF SYNTHETIC MUSKS IN AQUATIC PRODUCTS BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY%气相色谱-质谱联用测定水产品中的合成麝香

    Institute of Scientific and Technical Information of China (English)

    车金水; 王利平; 宋启军; 虞锐鹏

    2011-01-01

    ynthetic musks,as the substitutes for natural musks,are widely distributed in the environment.They are considered toxic,bioaccumulative and resistent to biodegradation.In this paper,a new analytical method,based on accelerated solvent extraction(ASE),on-line sample clean-up and gas chromatography/mass spectrometry(GC/MS) detection was developed for the determination of synthetic musks in aquatic products.The experiment conditions were initially optimized and the highest extraction efficiency was obtained when n-hexane was used as the extraction solvent,the neutral aluminum oxide as the selective adsorbent and the temperature of extraction was set at 100 ℃.A limit of detection as low as 0.1—0.5 ng·g-1 with a linear range between 1—80 ng·g-1 was achieved for eight synthetic musks.The recoveries for spiked samples were in the range of 85.3%—94.6% with RSD between 2.3%—8.4%.Using this method,the contents of 8 synthetic musks in 20 aquatic products form the Taihu lake were determined,and the average contents of synthetic musks were 2.8,0.2,12.7,4.2,12.4,18.5 and 1.4 ng·g-1 respectively for ADBI,AHMI,HHCB ATII AHTN MX and MK.DPMI was below the limit of detection in all samples.%利用快速溶剂萃取(ASE)和在线吸附净化,气相色谱-质谱(GC/MS)联用测定水产品中8种合成麝香.以正己烷为萃取溶剂,中性氧化铝为吸附剂,在100℃的温度下对水产品进行萃取.实验结果表明,方法的检测限为0.1—0.5 ng·g-1;在浓度1—80 ng·g-1的范围内,峰面积与样品浓度呈良好线性关系;8种合成麝香的回收率为85.3%—94.6%,相对标准偏差为2.3%—8.4%.对20个太湖水产品样品中的8种合成麝香进行检测,发现水产品中广泛存在合成麝香,平均浓度(干重)分别为ADBI 2.8 ng·g

  4. 固相萃取-气相色谱-质谱法测定化妆品中的硝基甲烷%Determination of Nitromethane in Cosmetics by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘茜; 马强; 郭亚丽; 席海为; 王烨; 白桦; 王超

    2012-01-01

    A method of solid phase extraction-gas chromatography-mass spectrometry was developed for the determination of nitromethane in cosmetic samples. The cream, lotion,powder,shampoo and lipstick samples were ultrasonically extracted with methanol or ethanol.and centrifuged. Then the concentrated supernatant was purified with a Sep-Pak Silica solid phase extraction cartridge with 80% methanol-20% dichloromethane as eluent. The eluent was further dehydrated and then analyzed with a HP-INNOWax capillary column(30 m X 0. 25 mm X 0. 25μm) under electron ionization conditions at a flow rate of 1. 0 mL/min. The quantitation was performed by the external standard method under selected ion monitoring mode(SIM) by monitoring ions of m/z30,46,61. The recoveies were 83. 0%~96. 4%,with the relative standard deviations(RSD) of 1.0%~5. 3%. The detection limit was 0. 2 mg/kg. The proposed method was proved to be accurate and stable, which was applicable for the determination of nitromethane in cosmetics.%建立了测定化妆品中硝基甲烷的固相萃取-气相色谱-质谱分析方法.膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品加入甲醇或无水乙醇超声提取后,提取液高速离心处理,浓缩上清液,采用Sep-Pak Silica固相萃取柱净化,收集80%甲醇-20%二氯甲烷洗脱液,浓缩后经无水硫酸钠脱水,进行气相色谱-质谱定性及定量分析.选用HP-INNOWax石英毛细管柱(30m×0.25 mm×0.25 μm),程序升温,流速1.0mL/min;采用电子轰击电离源,选择监测离子(m/z30、46、61,其中61为定量离子),外标法定量.方法的平均回收率为83.0%~96.4%,相对标准偏差(RSD)为1.0%~5.3%,方法对硝基甲烷的检出限为0.2 mg/kg.该方法准确、灵敏度高,可用于化妆品中硝基甲烷的测定.

  5. Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

    1992-01-01

    A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

  6. Mass-spectrometric determination of trace elements in aqueous media without preconcentration

    Energy Technology Data Exchange (ETDEWEB)

    Foss, G. O.

    1981-10-01

    Feasibility of using a low pressure glow discharge as an ion source for the mass spectrometric determination of trace elements in aqueous media was investigated. A cryogenically cooled hollow cathode ion source was developed to analyze aqueous samples without external preconcentration. Aqueous solutions containing seventy elements were analyzed and the detection limits, sensitivity factors, and linear regression correlation coefficients were determined. A standard test solution of trace elements in water was analyzed and the concentrations of trace elements were calculated using the sensitivity factors determined previously. The results compared favorably within the error limits predicted by the semiquantitative survey methods used. Tap water and natural lake water samples were examined and minimal interference effects due to organic compounds and biological compounds were noted. A research ion optical system (RIOS) was developed as a flexible mass analyzer for the development of new ion sources. The RIOS is a double focussing mass analyzer designed utilizing the Mattauch-Herzog geometry with externally adjustable slit assemblies.

  7. Particle size independent spectrometric determination of wear metals in aircraft lubricating oils

    International Nuclear Information System (INIS)

    A method for the particle size independent determination of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti in synthetic ester lubricating oils by spectrometric analysis is presented. Partial dissolution of Cr, Si, Pb, and Ag also occurs. Used ester lubricating oils as well as samples prepared with -325 mesh (44 μm) or -200 mesh (74 μm) metal powders were reacted with a small amount of hydrofluoric acid and aqua regia at 650C for 45 min with ultrasonic agitation. The reacted mixture was then diluted with a methyl isobutyl ketone and isopropyl alcohol mixture and analyzed spectrometrically. The recoveries for metal powder suspensions of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti ranged from 97 to 103% and the relative standard deviation ranged from 4 to 10%. In addition to the metal powder suspensions, over 200 aircraft oil samples were analyzed. The method is much faster and more convenient than previously reported particle size independent methods using ashing techniques

  8. Determination of trans-fatty acid isomers in human milk fat by gas chromatography-mass spectrometry%气相色谱-质谱联用法检测母乳脂肪中反式脂肪酸

    Institute of Scientific and Technical Information of China (English)

    林麒; 李国波; 葛品; 许榕仙; 林国斌

    2016-01-01

    建立了母乳中反式脂肪酸( TFAs)的气相色谱-质谱( GC-MS)检测方法,并应用于母乳脂肪中 TFAs 的检测。母乳用氨水水解,乙醚和石油醚提取脂肪,提取的脂肪加入 C21:0内标,用三氟化硼甲醇溶液在80℃水浴中冷凝回流15 min进行甲酯化,正己烷提取,上清液用 GC-MS分析,内标法定量。在低、中、高加标水平上验证方法的准确度与精密度,结果显示该方法可用于母乳中18种 TFAs及其同分异构体的检测,其中12种 TFAs在母乳脂肪中的方法检出限为4.0~47.1 mg/kg,回收率为80%~113%,RSD为2.9%~14.5%( n=6)。TFAs在部分母乳脂样品中检出,含量为9.54~6.9 mg/kg。该方法定性、定量准确,可有效用于母乳中 TFAs的检测,但仍存在脂肪酸本底干扰等问题,可结合银离子固相萃取柱预分离技术进一步完善。%A method for the determination of trans-fatty acid isomers in human milk fat was developed by gas chromatography-mass spectrometry( GC-MS),and applied to analyze TFAs in human milk fat. The fat was extracted with diethylether and petroleum ether after ammonia hydrolysis of human milk. C21:0 internal standard and boron trifluoride methanol solution were added to the extract for fat esterification. The solution then was refluxed in 80 ℃ water bath for 15 min. Finally the trans-fatty acid methyl ester isomers were extracted with hexane,and ana-lyzed by GC-MS. GC conditions were as follows:an HP-88 column(100 m×0. 25 mm×0. 2 μm) with inlet temperature of 260 ℃,at a split ratio of 10:1,and a He flow rate of 1 mL/min. The initial column temperature was 140 ℃( held for 5 min),then raised up to 240 ℃ at a rate of 4℃/min( held for 15 min). The electronic ionization( EI)source energy was 70 eV,with auxil-iary( AUX)temperature of 280 ℃,ion source temperature of 230 ℃,quadrupole temperature of 150 ℃ in selected ion monitoring( SIM)mode. This method can

  9. 气相色谱-质谱法测定化妆品中13种硝基苯类化合物%Simultaneous Determination of Thirteen Nitrobenzenes in Cosmetics by Gas Chromatography-Mass Spec-trometry

    Institute of Scientific and Technical Information of China (English)

    何东

    2014-01-01

    建立了水剂、粉剂、膏霜类、唇膏唇彩类化妆品中13种硝基苯类化合物的气相色谱-质谱(GC-MS)测定方法。水剂和粉剂类化妆品采用溶剂提取,浓缩后测定;膏霜类和唇膏唇彩类化妆品采用溶剂提取,佛罗里硅土固相萃取柱净化后测定。样液经 OV-225(30 m×0.25 mm×0.25μm)毛细管色谱柱分离,GC-MS 的选择离子监测(SIM)模式检测,以保留时间和特征离子比值定性,内标法定量。结果显示,13种硝基苯类化合物在0.1~5.0 mg/L 浓度范围内线性关系良好,方法检出限(S/N=3)在0.02~0.85 mg/kg 之间,3个添加水平的平均回收率在81.2%~113%之间,相对标准偏差(RSD,n=6)为4.5%~12.1%。%A method to determine 13 nitrobenzens in cosmetics by gas chromatography-mass spectrometry (GC-MS)was es-tablished.Different pre-treatment methods were optimized according to the specific properties of different types of cosmetics. For powder and aqueous samples,directly GC-MS test could be operated after solvent extraction.For cream and lipstick,sam-ples were extracted by appropriate solvent,followed by purification using Florisil solid phase extracting column.All of the samples were separated by OV-225 (30 m×0.25 mm×0.25 μm)chromatography column,and detected with selected ion mo-nitoring (SIM)mode by GC-MS.The target analytes were qualitative confirmed by retention time and abundance ratio of char-acteristic ions,and quantified by internal standard method.Results showed that 13 nitrobenzens presented favorable linearity in a certain range of concentrations of 0.1 mg/L to 5.0 mg/L,the method detection limits ranged from 0.02 to 0.85 mg/kg (S/N=3),the average recoveries ranged from 81 .2% to 113% at three spiked levels,and the relative standard deviations (RSDs,n=6)were in the range of 4.5% to 12.1 %.

  10. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    OpenAIRE

    Hou, Xiaolin; Roos, Per

    2008-01-01

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for rad...

  11. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.;

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro......-prophyrin permethylester were all found to have the same molecular ion sensitivities as their metal-free porphyrin ester. The relative metalloporphyrin ester content in a sample of porphyrin ester was thus obtained directly as the integrated ion current ratios of the normalized molecular ions. The preparation of...

  12. Study on Determination of 21 Phthalate Acid Esters and Their Distributions in Different Types of Foods by Gas Chromatography-Mass Spectrometry%不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱测定及其分布情况研究

    Institute of Scientific and Technical Information of China (English)

    吴惠勤; 朱志鑫; 黄晓兰; 林晓珊; 黄芳; 马叶芬; 罗辉泰; 邓欣; 潘亮君

    2011-01-01

    A sensitive method for the simultaneous determination of 21 phthalale acid esters( PARs) in foods by gas chromatography - mass Bpeclrome.-try{ GC - MS) was firstly proposed. Different separation and purification methods were selected according lo the types spectrometric fragmentation rule of PAEs was also discussed in detail. The. Calibration curves of 21 compounds were linear in the range of 0.1 -100 mg/L with correlation coefficients not less than 0.999 2. The quantitative limits (LOQs, S/N = 10) ranged torn 0. 05 mg/kg to 0. 5 mg/kg. The average spiked recoveries were in the range of 83% -106% at spiked levels of 0. 10 -10 mg/kg with relative standard deviations (RS-Ds, n =6)of 2.9% -5. 5% . The method was successfully applied in the investigation of the PAEs distribution in foods and food packaging material of South China area, and the source of PAEs was also discussed in detail.%首次建立了同时测定不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱(GC-MS)分析方法.对各种类别的食品采取不同的分离、净化方法;优化了成分复杂的香精或植物提取物等样品的色谱测定条件,通过提取特征离子进行检测和确证,消除了基质干扰,避免产生假阳性结果;探讨了邻苯二甲酸酯类的质谱碎裂机理.21种邻苯二甲酸酯的质量浓度在0.1-100 mg/L范围内呈良好线性,相关系数(r)不低于0.9992,方法的定量下限(S/N=10)为0.05-0.5 mg/kg.在0.10-10 mg/kg加标水平下的回收率为83%-106%,相对标准偏差(RSD,n = 6 )为2.9%-5.5%.采用该方法研究了华南地区不同食品及包装材料中邻苯二甲酸酯含量的分布情况,并对其来源进行了探讨.

  13. GC-MS同时检测食品中多种常见毒物的方法研究%Determination of various poisons in common in food by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    沈平; 彭进; 谢朝梅; 谢燕湘; 谢敏

    2011-01-01

    Objective:To establish a method with Gas Chromatography - Mass Spectrometry also detection of various common poisons in food in same conditions, including 18 kinds of organophosphorus,8 kinds of organochlorine pesticides, killing rat poisons fluoroacetamide and tetramine, and optimize the sample pretreatment of extraction and purification conditions.Methords:Extracted samples were classified pesticide category, containing fat fewer extracted using acetonitrile sample after nearly dry, concentrated extract by acetone and methylene chloride mixture dissolve, over Na2SO4 dehydration without water, had Carb/NH2 column and silicon magnesium column purification, concentrated to determine; Containing fat more samples, first with petroleum ether extract the fat content, using mixture of acetonitrile and petroleum ether liquid - liquid allocation methods will adipose the pesticide residue separation, over Na2SO4 dehydration without water, with different volume percentage of methylene chloride, acetonitrile and are hexane as eluent, over florisil column and Carb/NH2 column, samples to determination after purification and concentration.Containing killed of rat poison samples by ethyl acetate extracted, over Na2SO4 dehydration without water, with ethyl acetate as eluent, had silicon magnesium column purification then concentrated determination.Results: The results showed that 18 kinds of organophosphorus detection of limiting was 0.01 mg/L ~ 0.05 mg/L, 8 kinds of organochlorines in the 0.001 mg/L ~0.01 mg/L, tetramine was 0.03 mg/L, Fluoroacetamide was 0.05 mg/l, the method recoveries were 67.7% ~ 83.2%, 68.6% ~85.3% ,89.6% ~ 92.7% ,81.5% ~ 83.6% ,and the RSD were 1.3% ~ 7.9%, 1.8% ~ 3.7%, 4.5% ,2.5 %.Conclusion:This method is able to determinate various poisons in food for good separation and determination, accurate qualitative and quantitative, experimental results show that the method is sensitive and reproducibility, and high

  14. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  15. Characterization of Pentachlorophenol in Soil by Liquid Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    JIN Mi-cong; WANG Biao

    2004-01-01

    A simple, accurate and sensitive method for characterization of pentachlorophenol in soil was presented. The method included Soxhlet extraction using extracting agent of methanol/water/triethylamine (80∶20∶2), decontamination using solid-phase extraction (SPE) column and characterization by liquid chromatography-mass spectrometry (LCMS). The developed analytical method was successfully used to the determination of pentachlorophenol in soil samples.

  16. Clinical applications of gas chromatography and gas chromatography-mass spectrometry of steroids

    NARCIS (Netherlands)

    Wolthers, BG; Kraan, GPB

    1999-01-01

    This review article underlines the importance of gas chromatography-mass spectrometry (GC-MS) for determination of steroids in man. The use of steroids labelled with stable isotopes as internal standard and subsequent analysis by GC-MS yields up to now the only reliable measurement of steroids in se

  17. Development of gamma spectrometric method for the determination of thorium in phosphoric acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Mirashi, N.N.; Chaudhury, S.; Aggarwal, S.K. [Fuel Chemistry Div., Bhabha Atomic Research Centre, Mumbai (India)

    2010-07-01

    Gamma spectrometric determination of thorium in sintered thoria dissolved in strong phosphoric acid was studied using a high purity germanium (HPGe) detector. {sup 232}Th was determined using the highly abundant (27%) gamma ray (911.4 keV) emitted by its daughter {sup 228}Ac. The count rates in peak regions were plotted against the amount of thorium present in thorium nitrate working standard solution to obtain a calibration curve and the extent of thoria dissolved in 88% phosphoric acid was determined. Further studies on determination of thorium were carried out using thorium phosphate solutions, instead of using thorium nitrate working standard solutions. The solution of thorium phosphate obtained after quantitative dissolution of thoria in 88% phosphoric acid was also found to give a linear calibration curve at 911.4 keV. Using the calibration curves, expected count rates for thorium in sintered thoria dissolved in 88% phosphoric acid were calculated and were in good agreement ({+-}3%) with the observed count rates. (orig.)

  18. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    Science.gov (United States)

    Musshoff, F; Daldrup, T

    1997-08-01

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

  19. 热脱附-气相色谱质谱分析热环境下汽车沙发释放的挥发性有机物%Thermal Desorption-Gas Chromatography/Mass Spectrometric Analysis of Volatile Organic Compounds Emitted from Automobile Chair in Thermal Condition

    Institute of Scientific and Technical Information of China (English)

    谢成屏; 李勇; 蓝敏剑

    2011-01-01

    There are many volatile organic compounds emissions from car chair in thermal condition to pollute environment and affect the health of the people. A method for the detection of volatile organic compounds from emissions of automobile chair parts in the thermal condition by TD-GC/MS was developed. The automobile Chair sample was put into a special plastic bag of 2 m3, the volatile organic compounds were emitted in the thermal condition, then were collected with a Tenax adsorption tube, and were tested by thermal desorption-gas chromatography-mass spectrometry. The total numbers of identified components were 49 VOCs emitted from the automobile chair in the thermal condition, including alkenes(11, 7.46%), aromatic compounds(13, 6.02%), alcohols(5, 10.33%),ketones(5, 3.56%), esters (7, 29. 51%), aldehydes (2, 0. 50%), N-containing compounds (2,29.36%) and siloxane (4, 5.51%). If the content of VOC emissions was converted into the concentrations in the automobile air, the total volatile organic compounds(TVOC)is 7. 361 mg/m3 , which was 12 times over the tolerable concentrations prescribed in the standard.%汽车沙发部件在热环境中,会释放出许多挥发性有机物(VOC),污染环境,危害人体健康.本研究将汽车沙发放置在2 m3特制塑料采样袋中,在热环境下释放挥发性有机物,然后以Tenax管富集有机物,用热脱附-气相色谱质谱进行分析.结果表明:汽车沙发在热环境状态下,挥发出大量有机物,共定性检测出49种挥发性有机物(VOC),包括11种烷烃(7.46%)、13种芳香类化合物(6.02%)、5种醇醚类化合物(10.33%)、5种酮类化合物(3.56%)、7种酯类化合物(29.51%)、2种醛类化合物(0.50%)、2种含氮类化合物(29.36%)及4种硅氧烷类化合物(5.51%).通过将释放的挥发性有机物量换算成车内空气污染浓度可见,一个副驾驶位沙发释放的挥发性有机物对车内空气污染贡献浓度达7.36mg/m3,是国家室内限值标准的12倍,污染十分严重.

  20. Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Sergio L.C. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil)]. E-mail: slcf@ufba.br; Andrade, Jailson B. de [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Korn, Maria das Gracas A. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Pereira, Madson de G. [Departamento de Ciencias Exatas e da Terra Campus 1-Cabula, Universidade do Estado da Bahia, Salvador, Bahia 41195-001 (Brazil); Lemos, Valfredo A. [Laboratorio de Quimica Analitica, Campus de Jequie, Universidade Estadual do Sudoeste da Bahia, Jequie, Bahia 45200-190 (Brazil); Santos, Walter N.L. dos [Departamento de Ciencias Exatas e da Terra Campus 1-Cabula, Universidade do Estado da Bahia, Salvador, Bahia 41195-001 (Brazil); Rodrigues, Frederico de Medeiros [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Empresa Baiana de Desenvolvimento Agricola S.A., Avenida Dorival Caymmi 15649, Itapoan, Salvador, Bahia 41635-150 (Brazil); Souza, Anderson S. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Instituto Multidisciplinar em Saude, Campus AnisioTeixeira, Universidade Federal da Bahia, Vitoria da Conquista, Bahia 45055-090 (Brazil); Ferreira, Hadla S. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Silva, Erik G.P. da [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil)

    2007-07-16

    Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques.

  1. Determination of U and Th content in the zirconium purification process using alpha spectrometric method

    International Nuclear Information System (INIS)

    It has been performed determination of U and Th and decay daughter in the zirconium purification process using alpha spectrometric method. U and Th analysis applications as well as decay daughter of zirconium purification process done, from Na2ZrO3 dissolved stage, Na2ZrO3 dissolved with 4 M HCl, dissolving Chloride Zircon Oxide (ZOC) with 6M H2SO4 at 105°C the heating. The purpose of this study is to determine the concentration of U and Th and decay daughter of Na2ZrO3 dissolved process, Na2ZrO3 dissolved with 4 M HCl, dissolving Chlorid Zircon oxide (ZOC) with 6M H2SO4 at 105° C the heating. From the experiments it can be concluded that the Na2ZrO3 solution and ZrOCI2, there is no U and Th nuclides, where as in solution Zr5O8(SO4)2 there are U and Th content. (author)

  2. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group-Update and Additions to the Determination of Chloroacetanilide Herbicide Degradation Compounds in Water Using High-Performance Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Lee, E.A.; Kish, J.L.; Zimmerman, L.R.; Thurman, E.

    2001-01-01

    An analytical method using high-performance liquid chromatography/mass spectrometry (HPLC/MS) was developed by the U.S. Geological Survey in 1999 for the analysis of selected chloroacetanilide herbicide degradation compounds in water. These compounds were acetochlor ethane sulfonic acid (ESA), acetochlor oxanilic acid (OXA), alachlor ESA, alachlor OXA, metolachlor ESA, and metolachlor OXA. The HPLC/MS method was updated in 2000, and the method detection limits were modified accordingly. Four other degradation compounds also were added to the list of compounds that can be analyzed using HPLC/MS; these compounds were dimethenamid ESA, dimethenamid OXA, flufenacet ESA, and flufenacet OXA. Except for flufenacet OXA, good precision and accuracy were demonstrated for the updated HPLC/MS method in buffered reagent water, surface water, and ground water. The mean HPLC/MS recoveries of the degradation compounds from water samples spiked at 0.20 and 1.0 ?g/L (microgram per liter) ranged from 75 to 114 percent, with relative standard deviations of 15.8 percent or less for all compounds except flufenacet OXA, which had relative standard deviations ranging from 11.3 to 48.9 percent. Method detection levels (MDL's) using the updated HPLC/MS method varied from 0.009 to 0.045 ?g/L, with the flufenacet OXA MDL at 0.072 ?g/L. The updated HPLC/MS method is valuable for acquiring information about the fate and transport of the parent chloroacetanilide herbicides in water.

  3. Mass spectrometric methods for studying nutrient mineral and trace element absorption and metabolism in humans using stable isotopes: a review

    International Nuclear Information System (INIS)

    Mass spectrometric methods for determining stable isotopes of nutrient minerals and trace elements in human metabolic studies are described and discussed. The advantages and disadvantages of the techniques of electron ionization, fast atom bombardment, thermal ionization, and inductively coupled plasma and gas chromatography mass spectrometry are evaluated with reference to their accuracy, precision, sensitivity, and convenience, and the demands of human nutrition research. Examples of specific applications are described and the significance of current developments in mass spectrometry are discussed with reference to present and probable future research needs. (Author)

  4. Radioisotope spectrometric method to determine diffusion coefficients in metals and alloys

    International Nuclear Information System (INIS)

    A brief description of the spectrometric installation to study diffusion in metals using #betta#-decay radio-isotopes is presented. Diffusion coefficients of nickel in 70% Co-5% Fe-15% Si-10% B amorphous alloy are determined according to #betta#-radiation absorption in diffusion zone. Plate samples of 10x10 mm size and about 300 μm in thickness are used. Diffusion annealing is conducted during 100 hrs. The calculation of the diffusion coefficients has been carried out by the formula I/I0= esup(μsup(2)Dtau)erfc μ √ Dtau, where I0, I is an initial and a final radiation intensity; μ- an absorption coefficient of 63Ni #betta#-ray in the given material (at calculation μ=1.3x106 m-1 was taken); tau- duration of diffusion annealing; D- diffusion coefficient at the designed temperature. The value of the diffusion coefficient of nickel in 70% Co-5% Fe-15% S-10% B amorphous alloy at the temperature of 200 deg C is turned out to be equal to 4x10-21 m2/s. It should be noted that the self-diffusion coefficient of cobalt in Co-Fe alloy, found by extrapolation from high-temperature region, is equal to 10-35 m2/s, i.e. in 14 orders lower than that of the same basis in amorphous alloy

  5. Separation of trace antimony and arsenic prior to hydride generation atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    A separation method utilizing a synthetic zeolite (mordenite) was developed in order to eliminate the gas phase interference of Sb(III) on As(III) during quartz furnace hydride generation atomic absorption spectrometric (HGAAS) determination. The efficiency of the proposed separation method in the reduction of suppression effects of transition metal ions on As(III) signal was also investigated. Among the volatile hydride-forming elements and their different oxidation states tested (Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), and Te(VI)), only Sb(III) was found to have a signal depression effect even at low (μg l-1) concentrations under the experimental conditions employed. It has been shown that mordenite adsorbs Sb(III) quantitatively, even at a concentration of 1000 μg l-1, at pHs greater than two, and also, it reduces the initial concentrations of the transition metal ions to lower levels which can be tolerated in many studies. The adsorption of Sb(III) on mordenite follows the Freundlich isotherm and is endothermic in nature

  6. Validated method for the simultaneous determination of Delta9-THC and Delta9-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography-mass spectrometry with electrospray ionization.

    Science.gov (United States)

    Teixeira, Helena; Verstraete, Alain; Proença, Paula; Corte-Real, Francisco; Monsanto, Paula; Vieira, Duarte Nuno

    2007-08-01

    A fully validated, sensitive and specific method for the extraction and quantification of Delta(9)-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-Delta(9)-THC (THC-COOH) and for the detection of 11-hydroxy-Delta(9)-THC (11-OH THC) in oral fluid, urine and whole blood is presented. Solid-phase extraction and liquid chromatography-mass spectrometry (LC-MS) technique were used, with electrospray ionization. Three ions were monitored for THC and THC-COOH and two for 11-OH THC. The compounds were quantified by selected ion recording of m/z 315.31, 329.18 and 343.16 for THC, 11-OH THC and THC-COOH, respectively, and m/z 318.27 and 346.26 for the deuterated internal standards, THC-d(3) and THC-COOH-d(3), respectively. The method proved to be precise for THC and THC-COOH both in terms of intra-day and inter-day analysis, with intra-day coefficients of variation (CV) less than 6.3, 6.6 and 6.5% for THC in saliva, urine and blood, respectively, and 6.8 and 7.7% for THC-COOH in urine and blood, respectively. Day-to-day CVs were less than 3.5, 4.9 and 11.3% for THC in saliva, urine and blood, respectively, and 6.2 and 6.4% for THC-COOH in urine and blood, respectively. Limits of detection (LOD) were 2 ng/mL for THC in oral fluid and 0.5 ng/mL for THC and THC-COOH and 20 ng/mL for 11-OH THC, in urine and blood. Calibration curves showed a linear relationship for THC and THC-COOH in all samples (r(2)>0.999) within the range investigated. The procedure presented here has high specificity, selectivity and sensitivity. It can be regarded as an alternative method to GC-MS for the confirmation of positive immunoassay test results, and can be used as a suitable analytical tool for the quantification of THC and THC-COOH in oral fluid, urine and/or blood samples.

  7. Determination of 26 kinds of residual solvent in cigarette paper by headspace gas chromatography mass spectrometry%顶空-气相色谱质谱联用法分析烟用纸张中26种溶剂残留物

    Institute of Scientific and Technical Information of China (English)

    杜显生; 张颖明; 侯鑫

    2016-01-01

    建立了烟用纸张中26种溶剂残留物的顶空—气相色谱质谱联用(HS-GCMS)研究方法。以三醋酸甘油酯作为溶剂,使用静态顶空仪对烟用纸张进行前处理,溶剂残留混合组分导入气相色谱仪中逐一分离,进入质谱检测器进行定性定量分析。结果表明:方法的回收率在87.1%~107.8%之间,检出限在0.001~0.204m g/m2之间,相对标准偏差(R S D)小于5%。该方法可同时检测烟用纸张中26种溶剂残留物。%A determination method of 26 kinds of solvent residual in cigarette paper by headspace gas chromatography mass spectrometry (HS-GCMS) was established. Cigarette paper sample was pretreated with static headspace sampling used glyceryl triacetate as dissolvent. The mixed solvent residues were separated speciifcally by gas chromatography mass spectrometry and were qualitatively and quantitatively analyzed in MS Detector. The results showed that this method has good relative standard deviation (RSD<5%). Recovery rate is 87.1% to 107.8% and the detection limit is 0.001 to 0.204mg/m2. So this testing method can be applied to determine 26 kinds residual solvent in cigarette paper simultaneously.

  8. Radiogas chromatography mass spectrometry in the selected ion monitoring mode

    International Nuclear Information System (INIS)

    The value of selected ion monitoring in analyzing biological radio isotope incorporation experiments by radiogas chromatography mass spectrometry is illustrated with reference to the biosynthesis of the mycotoxin mycophenolic acid in Penicillium brevicompactum and the mode of action of the anticholesterolemic drug 20,25-diazacholesterol. Both examples used 1-[14C]acetate precursors. It is shown that the increased sensitivity and specificity of the selected ion monitoring mode detector permits straightforward detection and identification of the relatively small cellular pools associated with metabolic intermediates. The computer program RADSIM is described. Problems that still exist in using radiogas gas chromatography mass spectrometry technology to analyse isotope incorporation experiments are discussed. (author)

  9. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge;

    1982-01-01

    , was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions...

  10. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    International Nuclear Information System (INIS)

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l-1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l-1. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l-1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l-1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l-1 for As(III) and 0.3 μg l-1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l-1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

  11. Specialized Gas Chromatography--Mass Spectrometry Systems for Clinical Chemistry.

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

    A discussion of the basic design and characteristics of gas chromatography-mass spectrometry systems used in clinical chemistry. A comparison of three specific systems: the Vitek Olfax IIA, Hewlett-Packard HP5992, and Du Pont DP-102 are included. (BB)

  12. Application Of Dexamethasone Analysis Procedure In Pharmaceutical Product And Food Samples By Using The Liquid Chromatography Mass Spectrometry (LC-MS)

    International Nuclear Information System (INIS)

    The high pressure liquid chromatography mass spectrometry method for determination of dexamethasone has been studied. The authors have some results in found the optimal conditions in high pressure liquid chromatography mass spectrometry system for applications analysis of dexamethasone such as flow rate 0.5 ml/minute, the rate of mobile phase ACN: 0.1% HCOOH (80:20), injection volume was 20 μl. Besides, the authors analyzed a number of experimental samples with recovery range 84-96%. These initial results give the high pressure liquid chromatography mass spectrometry in operation. (author)

  13. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  14. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  15. Chromatographic separation and inductively coupled plasma atomic emission spectrometric determination of the rare earth metals contained in terbium

    International Nuclear Information System (INIS)

    The chromatographic separation of rare earth elements (REEs), prior to inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements, using a column packed with 2-ethylexyl hydrogen 2-ethyl-hexylphosphonate (PC-88A)-loaded polymer resin in order to exclude spectral interferences was examined. A favourable separation of trace amounts of metals (La, Nd and Sm) from a large amount of terbium was achieved simply by elution with dilute hydrochloric acid. Trace lanthanum and neodymium in metallic terbium were determined by separation of the analyte ions from the matrix element followed by ICP-AES analysis. (author). 16 refs.; 5 figs.; 2 tabs

  16. 程序升温大体积进样和解卷积气相色谱-质谱法测定蔬菜水果中32种农药残留量%Combination of programmable temperature vaporizer-large volume injection gas chromatography-mass spectrometry and automated mass spectral deconvolution and identification system for the determination of 32 pesticides in fruits and vegetables

    Institute of Scientific and Technical Information of China (English)

    曹赵云; 牟仁祥; 吴俐; 林晓燕; 朱智伟; 陈铭学

    2014-01-01

    建立了蔬菜、水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯等32种农药的气相色谱-质谱( GC-MS)检测方法。样品经乙腈提取,石墨碳黑串联丙氨基固相萃取柱净化,采用程序升温大体积进样,GC-MS 全扫描模式采集,结合解卷积技术定性分析,内标法定量。分别对程序升温和大体积进样等条件进行了研究,并考察了方法选择性和耐用性。在最优条件下,32种农药的响应值与浓度呈良好的线性关系( r>0.995),各农药的方法检出限为2.0~5.0μg/kg,以菠菜、四季豆和黄瓜为代表基质,进行3个水平(0.010~0.50 mg/kg)的加标回收试验( n=6),回收率为65.2%~120.3%,相对标准偏差( RSD)为4.1%~22.3%。该方法快速、灵敏、可靠、耐用,能满足蔬菜、水果中多类多残留痕量分析的要求。%An analytical method was developed for the simultaneous determination of 32 pesti-cides including organophosphorus, organochlorine, pyrethroid and carbamate pesticides in fruits and vegetables using gas chromatography-mass spectrometry( GC-MS). The sample was extracted with acetonitrile,and the organic layer was cleaned up with ENVI-Carb and LC-NH 2 cartridges. A large volume of 20 μL purified solution was injected into the GC system using pro-grammable temperature vaporizer( PTV). The mass spectrometric detection was operated with full scan mode. The automated mass spectral deconvolution and identfication system( AMDIS) and an isotopic internal standard were used for the qualitative and quantitative determination of the 32 pesticides,respectively. The conditions for PTV-large volume injection were studied. Furthermore,the selectivity and durability of the method were also assessed. Under the opti-mized conditions,the experimental results showed that all the linearities were good within their test ranges,with correlation coefficients more than 0. 995,and the method detection

  17. Quantitative analysis of trace levels ofβ-ionone in water by liquid-liquid- phase extraction-gas chromatography-mass spectrometry (LLE-GC-MS)

    Institute of Scientific and Technical Information of China (English)

    高梦鸿; 高乃云; 谢茴茴; 安娜; 邓扬; 戎文磊

    2015-01-01

    A simple and rapid technique based on liquid−liquid extraction coupled to gas chromatography-mass spectrometric detection (LLE-GC-MS) was developed for analysis of taste and odour compoundβ-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and pH on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without NaCl addition at pH=9. Good linearity (R2=0.9997) was obtained when the linear range was 10−500μg/L. The recoveries ofβ-ionone in ultrapure water and tap water samples were 88%−95% and 110%−114%, respectively. The relative standard deviations (RSD) were less than 10%. The method detection limit (MDL) and rejection quality level (RQL) were achieved at 1.98μg/L and 6.53μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.

  18. Direct analysis of intact glycidyl fatty acid esters in edible oils using gas chromatography-mass spectrometry

    NARCIS (Netherlands)

    H. van Steenbergen; K. Hrnčiřík; A. Ermacora; S. de Koning; H.-G. Janssen

    2013-01-01

    Glycidyl esters (GE), fatty acid esters of glycidol, are process contaminants formed during edible oil processing. A novel direct method for the determination of intact GE in oils and fats based on gas chromatography-mass spectrometry (GC-MS) is presented. The method consists of a simple extraction

  19. Determination of Ethylene Oxide and Methyloxirane in Clean Cosmetics by Headspace Sampling-Gas Chromatography-Mass Spectrometry%顶空进样-气相色谱-质谱法检测清洁类化妆品中环氧乙烷和环氧丙烷残留量

    Institute of Scientific and Technical Information of China (English)

    张敬轩; 李挥; 蔡立鹏; 范斌; 张岩

    2013-01-01

    A method based on headspace sampling-gas chromatography-mass spectrometry (HS-GCMS) was developed for the qualitative and quantitative detection of ethylene oxide and methyloxirane in clean cosmetics.About 1.0 g of sodium chloride and 5.0 mL of deionized water was added to the sample.After vortex mixed,the mixture above was placed in a headspace sampler,and then qualitative and quantitative analysis was carried out by HS-GCMS with SIM model.The calibration curve was linear in the range of 1.0-100.0 μg (ethylene oxide) and 0.5-50.0 μg (methyloxirane) with R>0.995.The detection limits were 0.02 μg (ethylene oxide) and 0.01 μg (methyloxirane),and the quantitative limit were 0.07 μg (ethylene oxide) and 0.03 μg (methyloxirane).By determination to 15 batches cleanser,15 batches shampoo and 20 batches bath foam bought in the supermarket,we found that this method was suitable for the determination of ethylene oxide and propylene oxidein.

  20. Determination of 6 Pesticide Residues in Peanut Using Gel Permeation Chromatography and Gas Chromatography-Mass Spectrometry%凝胶渗透色谱-气相色谱质谱法测定花生中6种除草剂农药残留

    Institute of Scientific and Technical Information of China (English)

    马金凤; 刘雪; 赵志强; 吴成; 许志强; 王明林

    2012-01-01

    A method was developed for the determination of 6 pesticides (trifluralin, clomazone, alachlor, pendimethalin, oxyfluorfen, quizalofop) in peanuts by gel permeation chromatography and gas chromatography-mass spectrometry(GPC-GCMS), The herbicide pesticide residues were extracted by acetonitrile. The extract was cleaned up with NH2 solid-phase extractor and gel permeation chromatography(GPC), then analyzed by gas chromatography-mass spectrometry(GC / MS) under selected ion monitoring(SIM) mode. The pesticide residues were calculated by external standard method. Good linear relation was obtained in the range of 0.02 -LOO mg / L with the correlation coefficient of 0.994 9-0.999 8. The average recoveries of six pesticides were 77.8%-101.6% with RSD of 4.4%-11.4%(n=5), The detection limit was 0.1-1.3 μg/kg.%建立了凝胶渗透色谱-气相色谱质谱( GPC-GC-MS)法测定花生中6种除草剂(氟乐灵、异恶草酮、甲草胺、二甲戊乐灵、乙氧氟草醚、喹禾灵)农药残留的方法.样品经乙腈提取,氨基固相萃取柱和凝胶渗透色谱净化,在选择离子扫描(SIM)模式下进行气相色谱质谱法测定,外标法定量.6种除草剂浓度在0.02~1.00 mg/L范围内与色谱峰面积呈良好的线性,线性相关系数为0.9949~0.9998,添加回收率为77.8%~ 101.6%,测定结果的相对标准偏差为4.4%~11.4%(n=5),方法的检出限为0.1~1.3 μg/kg.

  1. Determination of Ten Glucocorticoids in Traditional Chinese Medicine Preparations by High Performance Liquid Chromatography-Mass/Mass%液相色谱-串联质谱法同时检测中药制剂非法添加的10种糖皮质激素

    Institute of Scientific and Technical Information of China (English)

    姜春来; 曹红; 陈玉敏; 水彩红; 邢俊波; 乌宁奇

    2011-01-01

    目的 建立准确、灵敏的液相色谱-串联质谱方法,检查中药制剂中非法添加的10种糖皮质激素.方法 采用液相色谱-串联质谱分析法,以SHIMADZU Shim-pack VP-ODS C1s(4.6 mm×150 mm,5μm)为色谱柱;流动相:乙腈-10 mmol/L乙酸铵溶液(30:70);流速:0.3 ml/min;柱温:30℃;质谱条件:以正离子模式进行质谱数据采集.结果 10种糖皮质激素高效液相色谱图谱分离度良好,质谱分辨率符合要求.结论 此方法简便、快速,灵敏度高,专属性强,可作为检测中药制剂中非法添加10种糖皮质激素的有效手段.%Objective To establish an high performance liquid chromatography-mass/mass spectrometry method for the identification of ten glucocorticoids which may be illegally adulterated in Traditional Chinese Medicine preparations. Methods The determination was carried out by liquid chromatography-mass/mass spectrometry in the positive mode using a VP-ODS C18(4.6 mm xl50 mm,5 μm) column and acetonitrile/10 mmol/L ammonium acetate (30:70) as the eluting solvent. The flow rate was 0.3 ml/min and the column temperature was 30℃. Results A good resolution of the ten kinds of glucocorticoids was reached in the high performance liquid chromatogra-phy-mass analysis. Conclusion The method is simple, rapid, sensitive and specific and can be used to detect the ten glucocorticoids illegally added in in Traditional Chinese Medicine preparations.

  2. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples.

    Science.gov (United States)

    Hou, Xiaolin; Roos, Per

    2008-02-11

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry, resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer application in the environmental and biological researches, these radionuclides include (3)H, (14)C, (36)Cl, (41)Ca, (59,63)Ni, (89,90)Sr, (99)Tc, (129)I, (135,137)Cs, (210)Pb, (226,228)Ra, (237)Np, (241)Am, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection/sequential injection) for separation of radionuclides and automated determination of radionuclides is also discussed.

  3. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples.

    Science.gov (United States)

    Hou, Xiaolin; Roos, Per

    2008-02-11

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry, resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer application in the environmental and biological researches, these radionuclides include (3)H, (14)C, (36)Cl, (41)Ca, (59,63)Ni, (89,90)Sr, (99)Tc, (129)I, (135,137)Cs, (210)Pb, (226,228)Ra, (237)Np, (241)Am, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection/sequential injection) for separation of radionuclides and automated determination of radionuclides is also discussed. PMID:18215644

  4. Determination of squalene in pumpkin seed oil by gas chromatography-mass spectrometry%气相色谱-质谱联用测定南瓜籽油中角鲨烯的含量

    Institute of Scientific and Technical Information of China (English)

    石金娥; 于海玲; 王岩; 尚淑霞; 王庆峰; 吕航

    2014-01-01

    A simple and rapid method for the determination of squalene in pumpkin seed oil by gas chro-matography-mass spectrometry( GC-MS) was developed based on the national standard GB/T 22110—2008 . The optimal determination conditions were obtained through studying the effects of dosage of methyl esterification reagent on the extraction result of squalene and different polarity columns on the separation degree of squalene. The results showed that after pumpkin seed oil (0. 2 g) was methyl esterified by 1 mL 0. 5 mol/L potassium hydroxide-methanol solution and then extracted by n-hexane, the product was separated by HP-FFAP column,now the squalene could be determined quantitatively by GC-MS in selective ion monitoring mode. The linear range, correlation coefficient, the limit of detection, recovery rate of standard addition and average relative standard deviation of the method were 10 -500 mg/L, 0. 999 9,0. 12 mg/kg, 79. 33% -91. 33% and 3. 99%, respectively. The average content of squalene of 14 kinds of commercial pumpkin seed oils determined by the method was 1. 44 g/kg.%基于GB/T 22110—2008方法,建立一种简单、快速测定南瓜籽油中角鲨烯含量的气相色谱-质谱联用( GC-MS)方法,考察了甲酯化试剂浓度对角鲨烯提取效果及不同极性色谱柱对角鲨烯分离程度的影响,确定南瓜籽油中角鲨烯含量测定的最佳条件。结果表明,0.2 g南瓜籽油经1 mL 0.5 mol/L的氢氧化钾-甲醇溶液进行甲酯化反应,正己烷提取后经极性色谱柱HP-FFAP分离,用GC-MS选择离子监测模式对角鲨烯可以进行定量测定。该方法在10~500 mg/L范围内线性关系良好,相关系数r=0.9999;检出限为0.12 mg/kg,加标回收率为79.33%~91.33%,平均相对标准偏差为3.99%。采用该方法测定的14种市售南瓜籽油中角鲨烯平均含量为1.44 g/kg。

  5. Ultrasound-assisted dispersive liquid-liquid microextraction combined with gas chromatography-mass spectrometry in negative chemical ionization mode for the determination of polybrominated diphenyl ethers in water.

    Science.gov (United States)

    Zhang, Qian; Liang, Tao; Guan, Lili

    2013-04-01

    A simple and economical method for the determination of eight polybrominated diphenyl ethers (BDE-28, 47, 99, 100,153,154,183, and 209) in water was developed. This method involves the use of ultrasound-assisted dispersive liquid-liquid microextraction combined with GC-MS in negative chemical ionization mode. Various parameters affecting the extraction efficiency, including the type and volume of extraction and dispersive solvents, salt concentration, extraction time, and ultrasonic time, were investigated. A volume of 1.0 mL of acetone (dispersive solvent) containing 10 μL tetrachloroethylene (extraction solvent) was injected into 5.0 mL of water samples and then emulsified by ultrasound for 2.0 min to produce the cloudy solution. Under the optimal condition, the enrichment factors for the eight PBDEs were varied from 845- to 1050-folds. Good linearity was observed in the range of 1.0-200 ng L(-1) for BDE-28, 47, 99, and 100; 5.0-200 ng L(-1) for BDE-153, 154, and 183; and 5.0-500 ng L(-1) for BDE-209. The RSD values were in the range of 2.5-8.4% (n = 5) and the LODs ranged from 0.40 to 2.15 ng L(-1) (S/N = 3). The developed method was applied for the determination of eight BPDEs in the river and lake water samples, and the mean recoveries at spiking levels of 5.0 and 50.0 ng L(-1) were in the range of 70.6-105.1%. PMID:23483741

  6. GC-MS检测杏鲍菇中的有机氯农药残留%Determination of Organochlorine Pesticide in Pleurotus Eryngii by Gas Chromatography-Mass Spectrography

    Institute of Scientific and Technical Information of China (English)

    孟晓萌; 宋烨; 潘少香; 郑晓冬; 闫新焕; 刘雪梅

    2014-01-01

    本实验建立了一种农残测定的气相色谱-质谱联用法(GC-MS),实现了对杏鲍菇中16种有机氯农药的快速定量定性检测。试样以乙酸乙酯为溶剂,经乙腈均质提取,采用气相色谱-质谱仪进行分析。16种农药的检出限为0.65~19.34g/kg,平均回收率为93.8%~108.9%,相对标准偏差RSD为0.5%~4.7%,符合国家检测标准。该方法操作简单、结果准确、灵敏度高,可适用于多种蔬菜中有机氯农药残留的定量检测。%In our work, 16 kinds of organochlorine pesticides in Pleurotus Eryngii were determined by GC-MS. Ethyl acetate was used as solvent in the experiment, and the sample of pleurotus eryngtu was extracted with acetonitrile. The limits of detection for 16 organochlorine pesticides were in the range of 0.65~19.34g/kg, and the average recoveries were in the range of 93.8%~108.9%. Meanwhile, the relative standard deviations (RSD) were obtained from 0.5% to 4.7%. The results showed that this method has simple operation, good sensitivity, reproducibility and high efficiency, which could be applied to the quantitative determination for pesticide residue in vegetables.

  7. GC—MS法测定芜菁子中油脂组成研究%Determination of oil Compositions in Brassica rapa L. seed by Gas Chromatography--Mass

    Institute of Scientific and Technical Information of China (English)

    马和木提; 米丽班·霍加; 拜合提努尔

    2012-01-01

    目的:分析测定芜菁子中油脂的组成。方法:采用索氏提取法提取芜菁子中的油脂,甲酯化后,气相色谱-质谱法分析其油脂中脂肪酸的成分。结果:芜菁子中含有油酸,亚油酸,亚麻酸,硬脂酸,软脂酸,芥酸6种脂肪酸,其含量分别为12.5%、19.6%、8.9%、7.4%、5.8%、18.2%。结论:该法操作简便,灵敏度高,准确可靠,可用于芜菁子油中脂肪酸的组成及含量测定。%Objective: To determine the oil compositions and contents in Brassica rapa L. seed. Meth- ods: the oil of Brassica rapa L. seed was extracted by Soxhlet extraction method, and its component were analyzed by GC--MS, Results: there were six kinds of fatty acid in Brassica rapa L. seed. Its contents were oleic acid(12.5%),linoleic acid(19.6%),linolenic acid(8.9%) ,stearic acid(7.4%),palmitic acid(5. 8%) ,erucic acid (18.2%). Conclusions: The method was simple, sensitive, the results was accurate and reliable and can be used in the composition of fatty acids and determination in Brassica rapa L. seed.

  8. Determination of malachite green in sediment by ultra performance liquid chromatography-mass spectrometry%超高效液相色谱串联质谱法测定环境底泥中的孔雀石绿

    Institute of Scientific and Technical Information of China (English)

    梅光明; 郭远明; 张小军; 严忠雍; 李佩佩; 尤炬炬; 丁跃平

    2014-01-01

    Summary Malachite green(MG)is a kind of triphenylmethanedyes,which had ever been widely used around the world as fungicide,ectoparasiticide and antiseptic in the aquaculture.Current datas suggest that both MG and its metabolite leucomalachite green(LMG)may be carcinogenic and mutagenic.For those reasons MG has been banned in aquaculture industry in European Commission and U.S.A,and is also not approved in China.However,owing to low cost and marked effect,MG may still be used illegally.Additionally,the environment has been polluted because of MG's wide use before.Much of the pollutants have been transferred to sediment.In order to guarantee the safety of aquaculture,a sensitive and selective analytical method is needed for the determination of MG in aquaculture sediment.The current researches mainly focus on the determination of MG in aquatic products,rarely in sediment. Due to the matrix complex of sediment,sample pretreatment technology is the key technology.As a new type of functional material,muti-walled nanotubes(MWCNTs)have extensive prospect in the field of analytical chemistry. Now several articles have illustrated that MWCNTs have been used in the pretreatment of heavy metals and organic pollutants.Few literatures available were involved in determination of MG in sediment.During the past research, much more expensive materials such as cation exchange columns or alumina columns were mostly applied as solid-phase extraction adsorbents to determine MG in aquatic products and water.However,with advantages of lower price and good chemical properties,MWCNTs still have not been well used in analysis of MG. Now,a method for the determination of MG in sediment was established by using MWCNTs as solid-phase extraction adsorbents combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The sediment sample was extracted by acetonitrile and cleaned up on MWCNTs solid phase extraction (SPE) cartridges.The effects of experimental

  9. Application of wall-stabilized plasma arc for the spectrometric determination of impurity elements in uranium yellow cake

    International Nuclear Information System (INIS)

    The application of a seeded wall-stabilized argon plasma arc as an excitation source for the emission spectrometric determination of some impurity elements in a sample of uranium yellow cake has been investigated. The sample was dissolved in nitric acid. Uranium was extracted from the sample solution using tributyl phosphate (TBP), and the aqueous solution was injected into the arc. The elements determined were Al, Ca, Fe, Mg, Mn, Mo, Sr and Zr. Limits of detection and precision of the technique are presented. The study of the influence of residual uranium in the nebulized solution on the intensity of spectral lines revealed that uranium concentrations up to 100 μg mL-1 have no significant interfering effect

  10. 气相色谱-质谱法同时测定乳酸和7种糖的研究%Simultaneous Determination of Lactate and Seven Sugars by Gas Chromatography-mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    徐正华; 李晓宁; 易伦朝; 谭斌斌; 梁逸曾; 曾茂茂; 何君

    2011-01-01

    建立了气相色谱-质谱(GC-MS)法同时测定乳酸和葡萄糖、葡萄糖-6-磷酸、果糖、半乳糖、乳糖、1,5-脱水山梨醇、山梨醇7种糖的方法.选择核糖醇为内标,进样前先进行肟化反应再进行硅烷化反应.采用DB-5熔融石英毛细管柱,升温程序为初始温度70℃,保持4 min,以8℃/min的速率升至300℃,保持3 min.在优化测定条件下各对照品得到良好分离,且在测定范围内具有良好线性关系(r2>0.9983),平均加标回收率为74.5%~104.2%,日间相对标准偏差(RSD)与日内RSD小于9.2%.该方法简便、灵敏度高,已成功应用于2型糖尿病大鼠和健康大鼠血清中乳酸和糖类物质的定性定量分析.%A method was developed for simultaneous determination of lactate, glucose, glucose-6-phosphate, fructose, galactose, lactose, 1, 5-anhydro-sorbitol and sorbitol. Adonitol was used as an internal standard. The oximation and silylation of samples were carried out before chromatographic analysis. A DB-5 fused silica capillary column was used for chromatographic separation. The column temperature was maintained at 70℃ for 1 min and then programmed from 70 to 300℃ at the rate of 8℃, then hold 3 min at 300℃. All compounds were baseline separated under the conditions, and all the compounds had good linearity (r2>0. 9925) in the concentration range of detection. The added sample recovery was in the range of 74. 5 % ~ 104. 2%,and the inter-day relative standard deviation(RSD) and intra-day RSD were less than 9.2 %. The method is simple, sensitive and has been successfully applied to the determination of lactate and sugars in the serum of type 2 diabetic rats and health controls.

  11. Determination of Volatile Oil of Hedychium yunnanense Gagnep.by Gas Chromatography-Mass Spectrography%气相色谱质谱联用法分析滇姜花挥发油化学成分

    Institute of Scientific and Technical Information of China (English)

    谢小燕; 史小波; 徐俊驹; 何承刚; 杨生超

    2012-01-01

    To study chemical constituents from the flowers of Hedychium yunnanense Gagnep. , the essential oil were obtained by steam distillation. The chemical constituents in essential oil were separated and identified by GC - MS and HPMSD Chemstation analysis, and their relative contents were determined by the method of area normalization. As a result, twenty-nine compounds together with their contents were determined. Among them, (2E, 6E) -3, 7, 11-trimethyl-9- (phenylsulfonyl) -2, 6, 10-dodecatrien-l-ol, (1R) - ( +) -a-pinene, camphene, sabenene, 1, 7, 7-trimethyl-bicyclo [2. 2. 1 ] heptan-2-ol-2-acetate, a-caryophyllen, (E) -|3-farnesene and borneol were the major components. The contents of them were 20. 636% , 5. 913% , 4. 128% , 3. 964% , 2. 046% , 1. 786% , 1. 737% , 1. 568% , respectively. These compounds with relatively higher content might be the mainly characteristic aroma components of H. yunnanense.%为了研究滇姜花挥发油的化学成分,本试验采用水蒸气蒸馏法从滇姜花的花中提取挥发油,用气相色谱-质谱联用仪对其进行分离测定,通过HPMSD化学工作站检索,对分离的化合物进行结构鉴定,应用色谱峰面积归一化法测定各成分的相对百分含量,鉴定出了29个化学成分.其中主要成分为(2E,6E) -3,7,11-三甲基-9-苯磺酰-2,6,10-十二烷基三烯-1-醇、(1R) -(+)-α-蒎烯、莰烯、桧烯、乙酸1,7,7-三甲基二环[2.2.1]-2-庚酯、α-石竹烯、 (E)-β-金合欢烯、2-茨醇,其含量分别为20.636%,5.913%,4.128%,3.964%,2046%,1.786%,1.737%,1.568%.这些成分可能是滇姜花的主要释香成分.

  12. Determination of 16 phthalates in oil by solid-phase extraction and chromatography/mass spectrometry%SPE-GC/MS法测定植物油中16种邻苯二甲酸酯类化合物

    Institute of Scientific and Technical Information of China (English)

    张征; 王峰; 王宛; 徐春祥; 覃素姿

    2012-01-01

    Objective:To establish a quick and accurate method used for determination of 16 phthalates(PAEs) in vegetable oil.Methods:Glass hardware solid-phase cartridges without PAEs(SPE) were introduced to prepare sample.Qualitative and quantitative evaluation were performed by GC-MS.The method appeared to simple,accurate,and have good repeatability,purification effect.Compared with normal solid-phase cartridges and GPC method,this method avoided the higher blank value and long treating time.%目的:建立快速准确地测定植物油中16种邻苯二甲酸酯的检测方法。方法:采用不含邻苯二甲酸酯的CleanertPAE玻璃固相萃取小柱(SPE法)进行前处理,通过气相色谱-质谱法(GC-MS)法进行定性和定量测定。实验结果表明,该方法净化效果较好,处理方法快速、准确、重复性好,克服了普通固相萃取柱处理样品空白值高,凝胶渗透色谱(GPC)法处理样品时间长、空白值较高等不足。

  13. Sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as a new dispersive solid-phase extraction material for acrylamide determination in food with direct gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Omar, Mei Musa Ali; Wan Ibrahim, Wan Aini; Elbashir, Abdalla Ahmed

    2014-09-01

    A sol-gel hybrid sorbent, methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was successfully used as new dispersive solid phase extraction (dSPE) sorbent material in the determination of acrylamide in several Sudanese foods and analysis using GC-MS. Several important dSPE parameters were optimised. Under the optimised conditions, excellent linearity (r(2)>0.9998) was achieved using matrix matched standard calibration in the concentration range 50-1000 μg kg(-1). The limits of detection (LOD) and limit of quantification ranged from 9.1 to 12.8 μg/kg and 27.8-38.9 μg/kg, respectively. The precision (RSD%) of the method was ⩽6.6% and recoveries of acrylamide obtained were in the range of 88-103%, (n=3). The LOD obtained is comparable with the LODs of primary secondary amine dSPE. The proposed MTMOS-TEOS dSPE method is direct and safe for acrylamide analysis, showed reliable method validation performances and good cleanup effects. It was successfully applied to the analysis of acrylamide in real food samples.

  14. Determination of Gaseous and Particulate Trifluoroacetic Acid in Atmosphere Environmental Samples by Gas Chromatography-Mass Spectrometry%大气中气相和颗粒相三氟乙酸浓度测定

    Institute of Scientific and Technical Information of China (English)

    胡瑕; 吴婧; 翟紫含; 张博雅; 张剑波

    2013-01-01

    建立了我国大气中气相和颗粒相三氟乙酸(Trifluoroacetic acid,TFA)的采集和分析方法.采用环形扩散管-滤膜联用装置分离气相和颗粒相,利用环形扩散管的碱性涂层吸附气相TFA,石英滤膜吸附颗粒相物质.对气相和颗粒相样品分别处理,以2,4-二氟苯胺作为衍生剂,与TFA反应生成TFA的苯胺产物,采用GC/MS进行分析.本方法在0.31 ~4.91μg/L浓度范围内呈线性关系(R2=0.9991),检出限为66 ng/L.采样装置回收率为(101±3)%,当采样量为48 m3,TFA大气浓度检出限为31 pg/m3.于2012年4 ~10月在北京大学采样点采集大气,测得其中TFA总浓度在501 ~ 7447 pg/m3范围,TFA在气相中的浓度大于在颗粒相中的浓度,气固分配系数Kp随温度变化.%Trifluoroacetic acid (TFA) concentration was measured in air samples by a sampling device composed of annular denuders coupled with a quartz filter,which was efficient for collection and separation of gaseous and particulate TFA.Gaseous TFA was performed by means of annular denuders coated with alkaline solution,while particulate TFA was absorbed by quartz filters.TFA can be determined by gas chromatographymass spectrometry after derivation with 2,4-difluoroaniline.Calibration curves were linear with a correlation coefficient of 0.9991.Detection limit of TFA was 66 ng/L,which was 31 pg/m3 when sampling volume was 48 m3.Recoveries of the TFA sampling device ranged between 98% and 105% with relative standard deviation (RSD) ≤ 3%.The developed method was applied for the determination of TFA in atmosphere samples collected in Peking University in Beijing in 2012.Total TFA concentrations ranged between 501 and 7447 pg/m3.Concentrations of gaseous TFA were significantly higher than those of particulate,and the gasparticle partition coefficient of TFA decreased as air temperature rose.

  15. 气质联用法分析赤霞珠干红葡萄酒中脂肪酸%Determination of the Fatty Acids in Cabernet Sauvignon Wines by Gas Chromatography Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘河疆; 冯婷; 王成; 安冉; 孙婷

    2016-01-01

    采用气质联用法(GC/MS法)分析赤霞珠干红葡萄酒中脂肪酸组成,样品用正己烷提取,氢氧化钾-甲醇法甲酯化,归一化法计算含量。结果显示,干红葡萄酒中主要含有己酸、辛酸、十一烷酸、月桂酸、肉豆蔻酸、肉豆蔻烯酸、十五烷酸、棕榈酸、棕榈油酸、十七烷酸、十七碳烯酸、硬脂酸、油酸、反油酸、亚油酸、亚麻酸、花生酸、花生一烯酸、山嵛酸、顺-13,16-二十二碳二烯酸、二十二碳五烯酸、神经酸、木焦油酸等23种脂肪酸。%The chemical composition and contents of fatty acid in cabernet sauvignon wines was determined by GC/MS. The GC/MS detection showed containing 23 kinds of fatty acid, such as:hexanoic acid,caprylic acid, undecanoic acid,lauric acid,myristic acid,myristoleic acid,pentadecanoic acid,palmitic acid,palmitoleic acid,heptadecanoic acid,heptadecenoic acid,stearic acid,oleic acid,elaidic acid,linoleic acid,linolenic acid, arachidic acid,eicosatrienoic acid,behenic acid,docosadienoic acid,DPA,nervonic acid,lignoceric acid.

  16. Simultaneous determination of two kinds of rat poison and five pesticide residues by gas chromatography - mass spectrography%气质法同时测定两种鼠药和五种农药残留

    Institute of Scientific and Technical Information of China (English)

    张丹

    2011-01-01

    Objective:To establish GC -MS method for simultaneous determination of Fluoroacetamide, tetramine, methami-dophos, methyl parathion, triadimefon, chlorpyrifos and dicofol. Methods: Samples were extracted, concentrated and measured by the use of GC - MS. Results: The linear ranges of fluoroacetamide and tetramine were 5 μg/ml ~40 μg/ml and 0. 5 fμg/ml ~ 20. 0 μg/ml respectively. The linear ranges of five pesticides were 0. 05 μg/ml ~ 10 μg/ml. The recovery rate was 77% to 112%. Conclusion; This method is rapid, sensitive and accurate.%目的:建立用GC - MS能同时测定氟乙酰胺、毒鼠强、甲胺磷、甲基对硫磷、三唑酮、毒死蜱、三氯杀螨醇的测定方法.方法:样品经提取、净化、浓缩后运用气质联用仪(GC - MS)进行测定.结果:氟乙酰胺及毒鼠强的线性范围分别为5 μg/ml~ 40 μg/ml和0.5μg/ml ~ 20.0 μg/ml,五种农药的线性范围0.05 μg/ml~ 10 μg/ml,回收率为77%~112%.结论:该法快速、灵敏、准确,可用于实际检测分析.

  17. Simultaneous determination of five major compounds in the traditional medicine Pyeongwee-San by high performance liquid chromatography-diode array detection and liquid chromatography-mass spectrometry/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Bohyoung Lee

    2014-01-01

    Full Text Available Background: Pyeongwee-San (PWS has been widely used for treating acute gastritis, chronic, and gastritis. Objective: In this paper, simultaneous determination of five compounds (naringin, hesperidin, glycyrrhizin, atractylenolide III, and magnolol from traditional medicine PWS using the high performance liquid chromatography (HPLC was established for quality control. Materials and Methods: Optimum separations were obtained with a SHISEIDO C18 reverse-phase column by gradient elution with 0.1% Trifluoroacetic acid (TFA water-acetonitrile as the mobile phase. The flow rate was 1 mL/min and detection wavelength was set at 205 nm and 250 nm. Validation of the analytical method was evaluated by linearity, precision, and accuracy test. Results: The calibration curves were linear over the established range with R 2 > 0.9978. The limit of detection (LOD and limit of quantification (LOQ ranged from 0.09 to 0.43 and 0.27 to 1.29 μg/mL. The method exhibited intra-day and inter-day precision range between 0.01-1.86% and 0.04-0.35% respectively. The recoveries of five compounds in PWS were in the range between 93.18-106.40%, and 0.20-1.51%. The application of this method was identified through the successful analysis of five compounds in 12 batches of PWS. In addition, identification of five compounds was confirmed by a liquid chromatography method and mass spectrometry. Conclusion: The HPLC method was could be accomplished to the quality control and stable experiment for the preparations consisted of five major compounds.

  18. 安非他明类毒品的手性对映体气相色谱-质谱分析%Enantiomer Separation and Determination of Amphetamines with Chiral Derivatization by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    孟品佳

    2001-01-01

    采用手性衍生化试剂:(S)(-)N-三氟乙酰-1-脯胺酰氯(TPC)和(R)(+)-α-甲氯基-α-三氟甲基苯乙酸(MTPA)与安非他明类对映体反应生成非对映体衍生化产物,通过常规的GC/MS方法将其分离。本文较系统地考察了这两种手性试剂衍生化反应中溶剂、手性试剂用量、加热温度、反应时间等因素对安非他明类对映体衍生化结果的影响。实现了Am、MAm、MDA、MDMA、MDEA、MBDB等几种毒品对映体间的良好分离。%Most drugs of amphetamines contain chiral centers, which form different optical isomers, or enantiomers. Because different enantiomers have different pharmcological effect and have different machnism of metabolism. Besides, the ratio of the two eanatiomers could reflect the route and method used in the synthesis of the drugs. So the separation and determination of these eanantiomers for seizured samples or for biological samples became very important in the sence of forensic science.The paper used two chiral reagents: N-trifluroacetylprolyl chloride (TPC) and ( R )-( + )-α-methoxy-α-(trifluormethyl)phenylacetic acid (MTPA) to reach the purpose. They reacted with amphetamine enantiomers to form diasteromeric pairs, which possess some diffeences in physical and chemical natures and could be separated by GC/MS. The paper examined in detail some fectors such as the solvents, chiral reagent amounts, reaction time,temperature,etc. on the effect of chiral derivatization. Some enantiomers of amphetamine (Am),N-methylamphetamine(MAm),3,4-methylenedioxyamphetamin (MDA), 3,4-methylenedioxy-N-methylamphetamine (MDMA), 3, 4-methylenedioxy-N-ethylamphetamine ( MDEA ) and N-methyl-1-( 3, 4-methylenedioxy )-2-butanamine (MBDB) were well separated each other.

  19. 高效液相色谱法和气相色谱质谱联用法测定炼油碱性污水中酚类物质的含量%Determination of Phenols in Alkaline Wastewater from Oil Refinery by High-performance Liquid Chromatography and Gas Chromatography-mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    胡江涌; 闻环; 徐玲

    2013-01-01

      建立了高效液相色谱法和气相色谱质谱联用法测定炼油碱性污水中的酚类物质含量的两种方法。对同一样品,用高效液相色谱分析其含量,其中苯酚含量为18.49%,对甲酚含量为8.12%,邻甲酚含量为1.80%,用气质联用法测得苯酚含量为18.40%,对、间甲酚含量为9.09%,邻甲酚含量为1.91%。两种方法对三种主要的酚类物质的测定结果相近,都有很好的精密度和准确度。%A high-performance liquid chromatography method and a gas chromatography -mass spectrometry method is developed for the determination of phenols in alkaline wastewater from oil refinery. For the same sample, the content of phenol, p-cresol and 0-cresol was 18.49 %, 8.12 % and 1.80 % determined by HPLC, and the content of phenol, p,m-cresol and 0-cresol was 18.40 %, 9.09 % and 1.91 % determined by GC-MS. The results show that the method is precise and accurate. The method is simple and rapid and can be used for the determination of phenols in alkaline wastewater from oil refinery.

  20. Determination of Phenols in Alkaline Wastewater from Oil Refinery by High-performance Liquid Chromatography and Gas Chromatography-mass Spectrometry%高效液相色谱法和气相色谱质谱联用法测定炼油碱性污水中酚类物质的含量

    Institute of Scientific and Technical Information of China (English)

    胡江涌; 闻环; 徐玲

    2013-01-01

    A high-performance liquid chromatography method and a gas chromatography -mass spectrometry method is developed for the determination of phenols in alkaline wastewater from oil refinery. For the same sample, the content of phenol, p-cresol and 0-cresol was 18.49 %, 8.12 % and 1.80 % determined by HPLC, and the content of phenol, p,m-cresol and 0-cresol was 18.40 %, 9.09 % and 1.91 % determined by GC-MS. The results show that the method is precise and accurate. The method is simple and rapid and can be used for the determination of phenols in alkaline wastewater from oil refinery.%  建立了高效液相色谱法和气相色谱质谱联用法测定炼油碱性污水中的酚类物质含量的两种方法。对同一样品,用高效液相色谱分析其含量,其中苯酚含量为18.49%,对甲酚含量为8.12%,邻甲酚含量为1.80%,用气质联用法测得苯酚含量为18.40%,对、间甲酚含量为9.09%,邻甲酚含量为1.91%。两种方法对三种主要的酚类物质的测定结果相近,都有很好的精密度和准确度。

  1. Determination of Residual Twenty Kinds of Organophosphorus Pesticide in Edible Packaging Materials by QuEChERS Gas Chromatography-Mass Spectrometry%QuEChERS法气相色谱-质谱法同时测定可食性食品包装材料中20种有机磷农药

    Institute of Scientific and Technical Information of China (English)

    刘俊; 谢秀秀; 刘建

    2014-01-01

    采用一个萃取柱柱体,使用一种石墨化炭黑和伯仲胺叠加在一起的双层固相萃取法提取、过滤,气相色谱-质谱法同时测定可食性包装材料中20种有机磷农药含量。选择离子监测模式,外标法定量。平均回收率为84%-108%,相对标准偏差为0.3%-2.7%。结果表明,该方法简便、快速、灵敏、准确、检出限低,适合可食性包装材料中20种有机磷农药含量的测定。%Studies twenty kinds of organophosphorus pesticide in edible packaging materials have been carried out. A extraction column cylinder was presented in this paper, using a graphitized carbon black (GCB) and close amine (PSA) added together double (GCB)/PSA solid-phase extraction (SPE) extraction andfi ltering, then the determination of 20 organophosphorus pesticides in edible packing material were performed using a gas chromatography mass spectrometry (GC/MS). The external standards calibration curves were used for quantitative determination. The average recoveries were 84%-108% and relative standard deviations were 0.3%-2.7%. The method was simple, rapid, sensitive, accurate. The limits of detection were low. It was suitable for the determination of organophosphorus pesticides in edible packaging materials.

  2. 超声提取-气相色谱质谱法测定大气PM2.5中正构烷烃%Determination of N-alkanes in Atmospheric Fine Particulate Matter by Gas Chromatography Mass Spectrometry with Ultrasonic Extraction

    Institute of Scientific and Technical Information of China (English)

    刘保献; 王小菊; 常淼; 沈秀娥; 赵红帅; 张大伟

    2015-01-01

    建立了超声提取-气相色谱质谱法测定大气PM2.5中32种正构烷烃方法,经离子温度优化、前处理比较、空白滤膜考察等获得了最佳的实验条件。研究发现,高、中、低3种浓度标准曲线的相关系数均在0.995以上,3种浓度的空白样品加标回收率分别为72.2%~117.8%、73.5%~104.4%、73.8%~109.5%,精密度均小于10%,实际样品加标回收率为75.7%~108.9%。当采样体积为24 m3时,各目标化合物的方法检出限为0.046~2.6 ng/m3;经正构烷烃浓度范围为0.17~64.3 ng/m3的1月及浓度范围为0.53~7.67 ng/m3的6月的实际样品验证,该方法的检出限和测量范围也可较好的满足实际样品的测定。%A method of Gas Chromatography Mass Spectrometry with Ultrasonic Extraction determination of 32 N-alkanes in PM2. 5 has been established. In order to acquire the best conditions, various parameters were studied, like as the effect of different ion source temperature, the pretreatment of the method, the selection of blank quartz filter, and investigating the adaptability of this method by detecting the actual samples. Results showed that the correlation coefficient of 32 N-alkanes in PM2. 5 detected by Gas Chromatography Mass Spectrometry with Ultrasonic Extraction were all above 0. 995, it has high accuracy and precision. In addition the recovery of 32 N-alkanes of different concentration in blank quartz filters were in the range of 72. 2%-117. 8%, 73. 5%-104. 4%,73. 8%-109. 5%, precision is less than 10%, and the recovery of actual sample was in the range of 75. 7%-108. 9%. Otherwise, When the sampling volume was 24 m3 ,the limit detection of 32 N-alkanes was 0. 046-2. 6 ng/m3 . We detected actual samples in in January and June, the concentration of N-alkanes ranged from 0. 53-7. 67 ng/m3 and 0. 17-64. 3 ng/m3 separately, With this result we can see this method has low detection limit, can completely suitable for determination of N-alkanes in PM2. 5 .

  3. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    Science.gov (United States)

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection.

  4. Determination of 2 Methylisoborneol and Geosmin in Water by Purge and Trap Technology with Gas Chromatography/Mass Spectrometry(GC/MS)%吹扫捕集气相色谱-质谱联用测定水中二甲基异莰醇和土臭素

    Institute of Scientific and Technical Information of China (English)

    乐洋; 孙坚伟

    2015-01-01

    该文介绍了吹扫捕集气相色谱—质谱联用测定地表水/饮用水中痕量嗅味物质二甲基异莰醇和土臭素。采用吹扫捕集装置对样品中目标分析物进行富集,再用盐化和红外加热提高吹扫效果[1];用VF 624 ms的毛细管色谱柱进行分离,质谱检测定量。结果表明线性相关系数均大于0.99,RSD小于10%,加标回收率为90%~110%,最低检出限满足GB 5749—2006中的检测要求[2]。%Determination of 2 methylisoborneol and geosmin in drinking water and surface water by purge and trap capillary column gas chromatography/mass spectrometry was introduced in this paper.Samples of 2 methylisoborneol and geosmin in the water were enriched by purge and trap with Na2 SO4 and infrared heating.The samples were separated by the capillary column VF 624 ms, and detected by mass spectrometry.The results show the linear coefficients of all the calibration curves are more than 0.99 and RSD of all are less than 10%.The recovery rates are 90%~110%.The detection limit meets the requirement of GB 5749—2006.

  5. Dispersive liquid-liquid microextraction with situ derivatation combined with gas chromatography-mass spectrometry for the determination of tetrabromobisphenol-A in water samples%原位衍生分散液相微萃取-气相色谱-质谱快速测定水中的四溴双酚A

    Institute of Scientific and Technical Information of China (English)

    李锋丽; 崔兆杰; 王怀利

    2011-01-01

    A method that is"dispersive liquid-liquid microextraction with situ derivatation combined with gas chromatography-mass spectrometry for the determination of tetrabromobisphenol-A in water samples" has been developed through studying the influence of type and volume of extraction solvents and disperser solvent,amount of potassium hydrogen and acetic anhydride,extraction time on the extraction efficiency. The linear range was 0. 5 - 100μg/L and limit of detection was 0. Lμg/L. The relative standard deviations (RSD) was 5. 4% (n =5). The recoveries and RSD of TBBPA from real water samples were 53. 5%-89. 4% and 3. 8% ~ 7. 6% ,respectively.%通过研究萃取剂、分散剂的种类和体积,KHCO3用量,衍生剂乙酸酐的用量和萃取时间对萃取效率的影响,建立了原位衍生分散液相微萃取-气相色谱质谱联用测定水中四溴双酚A的方法.方法线性范围:0.5~ 100 μg/L,检出限:0.1μg/L;RSD:5.4% (n =5).将该方法用于环境水样的测定,加标回收率:53.5% ~89.4%,RSD:3.8 ~7.6%.

  6. Determination of 16 kinds of phthalates in drinking water by gas chromatography-mass spectrometry%气相色谱-质谱法测定饮用水中16种邻苯二甲酸酯类化合物

    Institute of Scientific and Technical Information of China (English)

    李伟

    2011-01-01

    To explore the kinds and levels of phthalates pollutants in drinking water, a liquid-liquid extraction gas chromatography mass spectrometry method was developed and validated for the determination phthalates in drinking water. Phthalates in drinking water were extracted with hexane and transferred to capillary column for gas chromatographic separation and mass spectrometic detection in selective ion monitoring mode (SIM).Sixteen phthalates can be separated by this method. The limits of detection were less than O.2μg/L. The recoveries were 85.5%~110.2% ,and the relative standard deviations were 0.35%~1.94%.%为了解我国饮用水中邻苯二甲酸酯类化合物污染状况,采用液液萃取气相色谱-质谱法测定三个小瓶水、两个大桶水、五个自来水中邻苯二甲酸酯类化合物的含量;采用正己烷提取后,气相色谱-质谱分析,选择离子扫描(SIM).该方法能有效分离16种邻苯二甲酸酯类化合物,检出限均<0.2μg/L,加标回收率在85.5%~110.2%,相对标准偏差0.35%~1.94%.

  7. Determination of Polycyclic Aromatic Hydrocarbons(PAHS)in Infant Cereal Samples by Gel Permeation Chromatography Purification-Gas Chromatography- Mass Spectrometry%凝胶净化-气质联用法测定婴幼儿米粉中的多环芳烃

    Institute of Scientific and Technical Information of China (English)

    张萌萌; 丁云; 应晓虹; 陈剑伟; 孙军; 王韩英

    2014-01-01

    A new analytical method was developed for the determination of polycyclic-aromatic- hydrocarbons (PAHs)in rice samples by gas chromatography-mass spectrometry(GC-MS)based on isotope internal standard method and gel permeation chromatography purification(GPC).The target analytes in samples were extracted with the solution of acetonitrile(ACN),purified using GPC to eliminate most of the coextracts,detected by GC-MS,and then quantified by internal standard method. The method recovery percentages and relative standard deviations(RSD)were 62.8%~93.7%and 8.2%~21.0%.The method detection limit(MDL)was 0.3μg/kg~2.4μg/kg.%采用同位素内标法并结合凝胶净化技术,建立了婴幼儿米粉中多环芳烃残留的气相色谱一质谱(GC-MS)检测方法。样品中的多环芳烃经乙腈提取,凝胶渗透色谱柱去除杂质后,进行GC-MS测定,内标法定量。方法的样品加标回收率和相对标准偏差分别为62.8%~93.7%、8.2%~21.0%。多环芳烃的方法检测限为0.3μg/kg~2.4μg/kg。

  8. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection.

    Science.gov (United States)

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-06-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The analytes were separated in gradient elution mode on C(18) column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification, trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r(2) ≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio of 3) were below 0.25 μg mL(-1) (μg g(-1)), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL(-1) (μg g(-1)). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the range of 84.2 ÷ 106.7%, with relative standard deviations sweeteners in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine quality control analysis of foodstuffs. PMID:21465096

  9. Development of a Gas Chromatography-Mass Spectrometry Method for the Quantification of Glucaric Acid Derivatives in Beverage Substrates

    OpenAIRE

    Ana Paula Craig; Fields, Christine C.; Simpson, John V.

    2014-01-01

    A gas chromatography-mass spectrometry (GC-MS) method using the standard addition methodology was developed for the determination of glucuronolactone (GL) and glucuronic acid (DGuA) in four beverages categorized as detoxification, recovery, or energy drinks. The method features a precolumn derivatization step with a combination of BSTFA (N,O-bis(trimethylsilyl)trifluoroacetamide) and TMCS (trimethylchlorosilane) to silylate the analytes. The sample pretreatment required no extraction, filtrat...

  10. 衍生化气相色谱-质谱法测定玩具和食品接触材料中双酚A%Determination of bisphenol A from toys and food contact materials by derivatization and gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    高永刚; 张艳艳; 高建国; 张慧玲; 郑丽莎; 陈静

    2012-01-01

    建立了玩具和与食品接触的材料中双酚A的衍生化气相色谱-质谱( GC-MS)检测方法.通过索氏萃取富集样品中的双酚A,与乙酸酐反应,终产物用 GC-MS进行测定.优化了衍生化时间、衍生化试剂用量等衍生化条件.在最佳条件下,双酚A衍生物稳定且峰形良好,在0.05~ 50mg/L范围内,相关系数(r2)在0.999以上.在0.05、1.00、10.00 mg/kg 3个添加水平下,双酚A的加标回收率为80%~ 93%,相对标准偏差(RSD)均小于3.7%;检出限(以信噪比(S/N)=3计)为10 μg/kg.该方法精密度好、回收率高,可用于玩具和食品接触材料中双酚A的定量检测.%A method was developed for the determination of bisphenol A (BPA) in toys and food contact materials. The BPA was extracted with Soxhlet extraction method from the sample and reacted with acetic anhydride. The final product was determined by gas chromatography-mass spectrometry ( GC-MS). To achieve the optimum derivatization performance, the derivatization time and dosage of derivatization reagent etc. were investigated. Under the optimized experimental conditions, the final product was stable and the peak shape was good. The linearity of the derivative was good in the range of 0. 05 to 50 mg/L with the correlation coefficient (r2) above 0. 999. The recoveries ranged from 80% to 93% at the spiked levels of 0. 05 , 1.00, 10.00 mg/kg with the relative standard deviations (RSDs) less than 3.7%. The limit of detection (S/N - 3) was 10μg/kg. The method is accurate and has high recovery. The method is suitable for the inspection of bisphenol A in toys and food contact materials.

  11. Determination of 3-Monochloropropane-l,2-diol in Soy Sauce and Oyster Sauce by Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry%固相萃取与气相色谱-质谱联用分析调味料中3-氯-1,2-丙二醇

    Institute of Scientific and Technical Information of China (English)

    熊珺; 龚亮; 赖毅东

    2011-01-01

    A simple and sensitive method for determination of 3-monochloropropane-1,2-diol (3-MCPD) in sauce samples by solid phase extraction (SPE) coupled with with gas chromatography-mass spectrometry (GC-MS) is described. In this work, elution solvent type and amount and sample loading amount were investigated to optimize SPE conditions. The optimal sample preparation procedure for treating 5.0 g of samples involved homogenization with 5 mol/L sodium chloride solution, clean-up on SPE column and derivitization prior to GC-MS analysis. The limit of detection of the method for 3-MCPD was 0.15 μg/kg, and the linear range 0.51 -- 6144μ g/kg, with a correlation coefficient of 0.9998 and a relative standard deviation of 8.8% (RSD, n = 5). The method was applied to determine soy sauce and oyster sauce samples and spiked recoveries of 87.2%- 109.4% with RSDs (n = 3) of 5.6% - 10.2% were obtained.%建立固相萃取与气相色谱一质谱联用(solid phase extraction with gas chromatography—mass spectrometry,SPE.GC—MS)测定调味料中3-氯-1,2-丙二醇的新方法。对影响分析物SPE萃取效率的诸因素如洗脱溶剂、洗脱溶剂的体积和上样体积等进行详细考察和优化。最佳萃取条件为5.0g样品与5mol/L氯化钠溶液混匀,经SPE萃取净化、衍生后,以GC—MS进行测定,该方法对3-氯-1,2-丙二醇的检出限为0.15μg/kg,线性范围为0.51-614

  12. Determination of Benzophenone and 4-methylbenzophenone Photoinitia-tors in Printing Inks for Food Packaging Material by Gas Chromatography-mass Spectrometry%GC-MS法测定食品包装材料印刷油墨中光引发剂二苯甲酮和4-甲基二苯甲酮

    Institute of Scientific and Technical Information of China (English)

    文韵漫; 张亚宁; 杨坚

    2012-01-01

    建立了气相色谱-质谱(GC-MS)检测食品包装材料表面印刷油墨中光引发剂二苯甲酮(BP)和4-甲基二苯甲酮(MBP)迁移量的方法。样品以正己烷为提取溶剂进行振荡提取和超声波辅助萃取,提取液用GC-MS分析检测。结果表明:该方法线性范围为0.02~0.1mg/mL,检测限为0.004~0.005mg/mL,在0.01,0.02,0.10mg/mL 3个添加水平下,2种光引发剂的平均回收率为88.2%~114.5%,相对标准偏差(n=6)为5.13%~7.95%。该方法简单快速,适用于食品包装材料的日常检测需要。%An analytical method based on gas chromatography-mass spectrometry (GC-MS) tech-niques was developed for determination of benzophenone and 4-methylbenzophenone photoini-tiators in printing inks used for food packaging materials. The test samples were extracted from selected food packaging materials using oscillating extraction and ultrasonic assisted extraction with n-Hexane as the extraction solvent, and the extracts was analyzed by GC-MS. The results showed that the linearity range of the method is 0.02-0. 1 mg/mL and the limits of detection for benzophenone and 4-methylbenzophenone are 0. 004 mg/mL and 0. 005 mg/mL; the average re-coveries of the three adding levels(0.01, 0.02, 0.10 mg/mL) are 88.2 % - 114.5 %, with the relative standard deviations(n=6)of 5.13-7.95%. It was concluded that the method is simple and rapid, which is applicable for routine determination of food packaging materials.

  13. Determination of Bisphenol A in polycarbonate resin and its products by Gas chromatography mass spectrography%气相色谱-质谱法测定聚碳酸酯树脂及其成型品中的双酚A

    Institute of Scientific and Technical Information of China (English)

    王立宛; 陈秋平; 魏强; 卢陈平; 满晓琴

    2011-01-01

    建立了聚碳酸酯树脂及其成型品中双酚A(BPA)的气相色谱-质谱联用(GC—MS)检测方法。样品经丙酮提取后挥发至干,用碳酸钾溶液溶解,再与乙酸酐衍生反应。衍生产物经正已烷提取后,采用GC—MS进行分析。结果表明,方法的线性范围为0.05—1.0mg/L,相关系数为0.9989,线性范围为1.0—10.0mg/L,相关系数为0.9999;方法的检出限为0.05mg/kg;平均回收率为93.0%-100.5%;相对标准偏差为4.2%-7.2%。该方法准确、灵敏,可用于实际聚碳酸酯树脂及其成型品中双酚A的分析。%The method for the determination of bisphenol A (BPA) in polycarbonate resin and its products was developed by gas chromatography -mass spectrometry( GC -MS).The BPA was extracted from polycarbonate resin and its products with acetone and concentrated by the evaporation of solvent. It was redissolved by potassium carbonate solution and reacted with acetic anhydride. The derivative was extracted by hexane and determined by GC - MS. The linear calibration curve was obtained in the range of 0.05 ~ 1.0mg/L with a correlation coefficient of 0. 9989 ,the linear calbration curve was obtained in the range of 1.0 - 10, 0mg/L with a correlation coefficient of 0.9999 ;The detection limit of the method was 0.05 mg/kg; The recoveries were 93.0% - 100.5% ,and the relative standard deviations were 4.2% - 7.2% ;The method is accurate and sensitve, and it is suitable for the analysis of bisphenol A in polycabonate resin and its products.

  14. 超高压液相色谱-串联质谱法快速测定酒类中的4种甜味剂%Rapid determination of four sweeteners content in liquor by ultra pressure liquid chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    马作江; 柏雪; 蔡学; 黄波; 谢义梅; 单长海; 刘必英

    2013-01-01

      目的建立酒类中安赛蜜、糖精钠、甜蜜素和三氯蔗糖4种甜味剂的超高压液相色谱-串联质谱联用(UPLC-MS/MS)快速测定方法。方法采用Agilent ZORBAX SB-C18色谱柱(50 mm×2.1 mm,1.8μm)分离,以0.1%甲酸水溶液-甲醇作为流动相梯度洗脱,在电喷雾离子源 ESI负离子模式下多重反应监测(MRM)定性、定量测定甜味剂。结果4种甜味剂在10~500μg/L的范围内与峰面积有良好的线性关系,相关系数大于0.99,检出限为0.5~2.4μg/L,加标回收率在89.4%~104.6%之间, RSD小于4%。结论该方法简便灵敏,准确快速,可用于酒类食品中低剂量、复合甜味剂的测定。%Objective To establish a rapid determination method of four sweeteners (acesulfame, saccha-rin sodium, sodium cyclamate and suralose) in liquors by ultra pressure liquid chromatography-mass spectro-metry (UPLC-MS/MS). Methods The samples were separated by Agilent ZORBAX SB-C18 column (50 mm×2.1 mm, 1.8μm) using 0.1%formic acid water-methanol as mobile phase and analyzed by electrospray ioni-zation (ESI) in the negative ion and multiple reaction monitoring mode (MRM). Results The method showed a good linearity over the range of 10∼500μg/L. The average recoveries were 89.4%∼104.6% with RSD less than 4%. The quantitative limits of four sweeteners were 0.5∼2.4μg/L. Conclusion This method is accurate, rapid, and highly sensitive, and suitable for the determination of low concentration sweeteners in liquors.

  15. 分散固相萃取-气相色谱-质谱法测定鸡肉香精中17种邻苯二甲酸酯%Determination of 17 kinds of phthalate esters in chicken flavor by dispersive solid phase extraction coupled with gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    朱莉萍; 朱涛; 马运平; 李修平; 倪永付

    2014-01-01

    目的:建立同时测定鸡肉香精中17种邻苯二甲酸酯的分析方法。方法经水预处理后的鸡肉香精样品,用乙腈饱和的正己烷提取,并用正己烷饱和的乙腈反提取除去提取液中残留的大部分油脂,用分散固相萃取进行净化,最后用气相色谱-质谱(GC-MS)进行分析。结果17种邻苯二甲酸酯在0.05~10 mg/L 之间线性关系良好,检出限为0.05 mg/kg。17种邻苯二甲酸酯回收率在72.8%~94.7%之间, RSD为1.0%~16.3%。结论本方法简单、试剂用量少,具有绿色环保的优势。在最优实验条件下,此方法有效地降低了检测限,提高了灵敏度,具有良好的回收率。%Objective A rapid method has been developed for the determination of phthalate esters (PAEs) residues in chicken flavor. Methods PAEs in chicken flavor were extracted by n-hexane after water pre-treatment, and re-extracted by acetonitrile treated by n-hexane in order to remove fat. Then sample was pu-rified with dispersive solid phase, and detected by gas chromatography-mass spectrometry. Results The me-thod showed a good linearity over the range of 0.05~10 mg/L for 17 kinds of phthalate esters. The detection limits(S/N≥10) of milk were 0.05 mg/kg. The recoveries were 72.8%~94.7%with relative standard deviation of 1.0%~16.3%. Conclusion The method is simple, and has the less use of the detecting organic reagent. It is environment friendly. By the optimization, the method can low the detection limit, and has a high sensitivity for determination of phthalate esters in chicken flavor.

  16. Determination of 11 Triazole Pesticides Residues in Fruits and Vegetables byGas Chromatography- Mass Spectrometry%气相色谱-质谱法测定蔬菜与水果中11种三唑类农药残留

    Institute of Scientific and Technical Information of China (English)

    葛娜; 刘晓茂; 李学民; 黄学者; 吴艳萍; 李金; 刘永明

    2011-01-01

    A method was developed for the determination of 11 triazole pesticides residues in fruits and vegetables using gas chromatography - mass spectrometry ( GC - MS ) . The samples were homogeneous extracted with acetonitrile and then cleaned up by a solid phase extraction ( Sep - Pak Car-bonNH2 ) cartridge, eluted with acetonitrile - toluene (3 : 1 ) . The elution solvent was concentrated, solvent exchanged to constant volume, then determined by GC - MSD/SIM with the internal standard method. The calibration curves of 11 triazole pesticides were linear in the range of 0. 05 - 5 ng with correlation coefficients of 0. 996 - 1. 000. The spiked recoveries of 11 triazole pesticides from five matrices(e. G. Cabbage, tomato, apple, orange, spinach) at three spiked levels of 0. 01 , 0.05, 0. 10 mg/kg were in the range of 80% -97% with relative standard deviations ( RSDs, n = 10) of 2. 5% -8. 4% . The limits of detection were 0. 01 mg/kg for 11 triazole pesticides. The method is simple, sensitive, accurate and reliable.%建立了蔬菜和水果中11种三唑类农药残留的气相色谱-质谱(GC - MS)测定方法.样品用乙腈均质提取,经石墨化炭黑/氨基复合柱净化,乙腈-甲苯(3:1)洗脱.洗脱液经浓缩、溶剂交换后定容,采用气相色谱-质谱的选择离子监测方式( GC - MSD/SIM)进行测定,内标法定量.方法的线性范围为0.05~5 ng,相关系数为0.996~1.000,对甘蓝、番茄、苹果、柑橘、菠菜5种空白基质分别进行0.01、0.05、0.10 mg/kg 3个水平加标,平均回收率为80%~ 97%,相对标准偏差(RSD,n=10)为2.5% ~ 8.4%.11种农药的检出限均为0.01 mg/kg.该方法操作简单,灵敏度高,结果准确可靠.

  17. Characterization of volatile organic compounds by thermal desorption/gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Carbonaceous triple sorbent traps (TSTs) have been widely used to collect and concentrate volatile organic compounds (VOCs) in vapor phase samples for subsequent GC/MS analysis. Recently, this laboratory has been involved in sampling and analyzing VOCs collected from various emission sources, including headspace samples from underground storage tanks at the Department of Energy's Hanford site, in Richland, Washington. In order to evaluate the sampling adequacy and to assess any health-related impact based on the analysis results, a validated method must be employed. Therefore, the main objective of this study was to develop a methology for thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) determination of VOCs in the vapor phase samples collected on Carbotrap C/Carbotrap/Carbosieve S III triple sorbent traps. Techniques used in method validation included VOC standard generation, thermal desorption efficiency, reproducibility of spiking on and recovery from TST, use of internal standards, detection limits determination, linearity and reproducibility of calibration

  18. Partial vapor-phase hydrolysis of peptide bonds: A method for mass spectrometric determination of O-glycosylated sites in glycopeptides

    DEFF Research Database (Denmark)

    Mirgorodskaya, E; Hassan, H; Wandall, H H;

    1999-01-01

    In this study we present a method for determination of O-glycosylation sites in glycopeptides, based on partial vapor-phase acid hydrolysis in combination with mass spectrometric analysis. Pentafluoropropionic acid and hydrochloric acid were used for the hydrolysis of glycosylated peptides. The r...... of the reaction products without further purification both by matrix-assisted laser desorption/ionization and electrospray ionization mass spectrometry....

  19. Determination of 15 phthalic acid esters in infant formula milk powder and raw material by gas chromatography-mass spectrometry%气相色谱-质谱法测定婴幼儿配方乳粉及原料中15种邻苯二甲酸酯

    Institute of Scientific and Technical Information of China (English)

    杨国良; 孔福奎; 张开翔; 赖世云; 任一平

    2013-01-01

      Objective To establish a method for determination of phthalic acid esters in infant formula milk powder and raw materials by gas chromatography-mass spectrometry (GC-MS). Methods Samples were extracted with acetonitrile, and then detected by GC-MS. The external standard method was conducted for the quantitative analysis. Results The linear range of 15 phthalic acid esters were 0.001~1 mg/L, except that the linear range of phthalate isononyl ester was 0.01~1 mg/L with R>0.99. LOD (S/N=3) and LOQ(S/N=10) were 0.006~0.2 mg/kg and 0.02~0.7 mg/kg, respectively. The recoveries were 88.6%~117.2% at three spiked level with relative standard deviation of 1.0%~9.3%. Conclusion This method is simple, accurate, fast, cheap and stable, and it is suitable for the detection of phthalic acid esters in milk powder.%  目的建立婴幼儿配方乳粉及原料中15种邻苯二甲酸酯的气相色谱-质谱检测方法。方法样品经乙腈提取后,用GC-MS检测。采用外标法进行定量分析。结果15种邻苯二甲酸酯的线性范围除了邻苯二甲酸二异壬酯为0.01~1 mg/L,其余均为0.001~1 mg/L,相关系数大于0.99。方法检出限(S/N=3)为0.006~0.2 mg/kg,定量限(S/N=10)为0.02~0.7 mg/kg。在奶粉基质中3个加标水平下邻苯二甲酸酯的平均回收率在88.6%~117.2%,相对标准偏差为1.0%~9.3%。结论本方法操作简单、精确、快速、廉价、稳定,适用于奶粉中邻苯二甲酸酯类化合物的检测分析。

  20. 顶空液相微萃取/气相色谱-质谱检测葡萄酒中的氨基甲酸乙酯%Applied the method of headspace liquid-phase micro-extraction coupled with gas chromatography-mass spectro metry to the determination of ethyl carbamate in wines

    Institute of Scientific and Technical Information of China (English)

    姜自军; 阎雪; 单纪平; 徐刚; 慈慧

    2013-01-01

    建立了顶空液相微萃取/气相色谱仪-质谱联用测定葡萄酒中的氨基甲酸乙酯的方法。对影响萃取效率的实验条件进行了优化。采用Rtx-Wax毛细管柱进行检测,以癸烷为萃取溶剂,在60℃、搅拌速度为200r/min条件下对1mL葡萄酒样品萃取30min。该方法对氨基甲酸乙酯的富集倍数为62;在100~1600µg/L的范围内线性关系良好。相关系数为0.9999;氨基甲酸乙酯的检出限为1µg/L(S/N=3)。实际酒样的加标回收率为81.0%~103.1%。%Headspace liquid-phase micro-extraction (HS-LPEM) coupled with gas chromatography-mass spectrometry (GC-MS) was used to determine the ethyl carbamate of wines. Some main experimental parameters that affect the extraction efficiency were optimized. Decane was selected as extraction solvent. The extraction was carried out at 60℃in a 2mL vial filled with 1mL of sample solution at a stirring rate of 500r/min for 30min. The enrichment factors for the ethyl carbamate was 62. The linear range for the quantification of the ethyl carbamate was 100~1600 µg/L(R2=0.9999) . The limit of detection was 1µg/L(S/N=3)for the ethyl carbamate. Recovery was 81.0%~103.1%.

  1. Determination of 2-Methylisoborneol and Geosmin in Water by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry%固相微萃取-气相色谱-质谱联用测定水中痕量2-甲基异冰片和土臭素

    Institute of Scientific and Technical Information of China (English)

    寇立娟; 梁春实; 魏树龙; 臧金海; 蔡柳燕

    2011-01-01

    A method for the determination of 2-methylisoborneol (MIB) and geosmin (GSM) in water was developed by solid phase microextraction (SPME) coupled with gas chromatography-mass spectrometry(GC-MS). The best extraction conditions were as follows: water bath heating (The level of water surface in bath was set at the same level of sample) , extraction temperature of 65 ℃ and extraction time of 30 min. The method was highly sensitive, better precisive and accuracy based on GC-MS results. The correlative coefficients for MIB and GSM were both over 0. 999; detection limits and RSD were 0. 2 ng/L, 0. 3 ng/L and 5. 8%, 3. 2% respectively! Recoveries of spiked respectively were 102. 0% and 101. 7%. The method can be used to detect MIB and GSM in water.%1 引 言2-甲基异冰片(2-Methylisobomeol,M1B)和土臭素(Geosmin,GSM)主要由放线菌、真菌和蓝绿藻代谢产生,这两种物质是目前造成饮用水具有霉昧和土味的主要原因,尽管其在样品中的含量极低,但人的嗅觉对其极为敏感,微量的这些物质便能感觉,有研究表明,人类对2-甲基异冰片和土臭素的嗅阈值分别为10和30 ng/L[1].目前,吹扫捕集(PT)和固相微萃取(SPME)技术结合气相色谱质谱法(GC-MS)是测定这两种异味物质较普遍的方法[2~4],但PT技术相比SPME技术需昂贵的仪器设备,操作也相对复杂.SPME技术多采用磁力加热方式萃取挥发性化合物[5~7],但这种加热方式需配备专门的仪器没备,升温相对较慢,而水浴加热方式鲜见报道.本研究采用水浴加热,建立了水中2-甲基异冰片和土臭素的SPME-GC-MS测定方法,为水中异味物质分析提供了参考.

  2. 固相微萃取-气相色谱-质谱法测定饮用水中土嗅素和2-甲基异茨醇%Determination Geosmin and 2-Methylisoborneol in Drinking Water by Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    沈斐; 李睿; 苏晓燕; 朱培育

    2013-01-01

    采用固相微萃取法富集,气相色谱-质谱联用法定性和定量测定饮用水中致嗅物质土嗅素和2-甲基异茨醇.研究并讨论优化了纤维头的类型、盐的种类和浓度、温度、萃取时间等因素对异味化合物萃取量的影响.土嗅素和2-甲基异茨醇的检出限分别为1.02、2.13 ng/L,相对标准偏差分别为4.96%、7.74%.2种异味化合物在5~1000 ng/L的范围内线性关系良好,相关系数均大于0.985.因此,用该方法能够很好地分析水中痕量的异味化合物.%Determination of musty odorants,geosmin (GSM) and 2-methylisoborneol (2-MIB),in drink water was developed by solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry.The operating conditions of SPME,such as fibre type,salt concentration,water temperature and absorption time were studied and discussed.The limits of detection for geosmin and 2-MIB in water were 1.02,2.13 ng/L,and the relative standard deviations for them were 4.96%,7.74%,respectively.There were good linear correlation (the calibration coefficients were all above 0.985) for the two odorous compounds in the range of 5-1000 ng/L.This method was successfully applied to the analysis trace of the odor compounds in drink water samples.

  3. Simultaneous Determination of 22 Phthalate Acid Esters in Edible Oils by Gas Chromatography/Mass Spectrometry Coupled with Gel Permeation Chromatography%凝胶渗透色谱-气相色谱/质谱法同时测定食用油中22种邻苯二甲酸酯

    Institute of Scientific and Technical Information of China (English)

    黄永辉

    2012-01-01

    建立了凝胶渗透色谱-气相色谱/质谱法同时测定食用油中22种邻苯二甲酸酯的方法.方法具有良好线性,相关系数R均大于0.999,检测限在0.09~11.83 mg/kg之间,平均回收率在81.45%~113.90%范围内,相对标准偏差为1.55%~9.41%.采用该方法对国内食用油中邻苯二甲酸酯增塑剂进行检测,实际样品中检出邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯和邻苯二甲酸二(2-乙基)己酯,可满足目前食用油中邻苯二甲酸酯的检测要求.%A method for the simultaneous determination of 22 phthalate acid esters in edible oils by gas chromatography-mass spectrometry coupled with gel permeation chromatography was developed. The correlation coefficients(i?) of 22 phthalate acid esters were over 0. 999 with detection limits from 0. 09~ 11. 83 mg/kg. The average recoveries of 22 phthalate acid esters in edible oils were ranged from 81. 45% ~113. 90%. In addition,the relative standard deviations(RSDs) were in the range of 1. 55%6~9.41%. The level of phthalate acid esters plasticizers in edible oils was investigated by this method .and di-iso-butyl phthalate, dibutyl phthalate, bis (2-ethylhexy1) phthalate were found in some real samples. The simplicity,sensitivity and precision of the method made it be well suitable for the analysis of phthalate acid esters in edible oils.

  4. Atomic-spectrometric determination of lithium, sodium, potassium and strontium in high-pure scandium

    International Nuclear Information System (INIS)

    Determination of lithium, sodium and potassium in strontium by flame photometry with atomic-absorption spectrophotometer is described. Scandium effect on value of Li, K. Na analytical signal in flame is studied. It is shown, that the base understates analytical signals. Determination of strontium by flame photometry is impossible. Determination of strontium (1x10-13 kg/ml) by atomic-absorption method with electrothermal atomization is possible

  5. Spectrometric Methods Used to Determine Heavy Metals and Total Cyanides in Accidental Polluted Soils

    OpenAIRE

    A. Mihaly-Cozmuta; L. M. Cozmuta; V. Viman; Gh. Vatca; Varga, C.

    2005-01-01

    The study presents the level of soil pollution in the area adjacent to three sedimentation ponds as a result of an environmental accident. Soil samples from various sites have been collected and analyzed to determine the concentration of heavy metals (Cu, Pb, Zn) and total cyanides. The analysis methods used were ICP-AES for heavy metals and the colorimetric for total cyanides. The accuracy of both methods is determined subject to the reproducibility of the results. The values of determined c...

  6. Comparison of accelerator mass spectrometric measurement with liquid scintillation counting measurement for the determination of {sup 14}C in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Yasuike, Kaeko, E-mail: k-yasuike@hokuriku-u.ac.j [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Yamada, Yoshimune [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Amano, Hikaru [AMS Management Section, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan)

    2010-04-15

    The concentrations of organically-bound {sup 14}C in tree-ring cellulose of a Japanese Black Pine grown in Shika-machi (37.0 deg. N, 136.8 deg. E) and those of a Japanese Cedar grown in Kanazawa (36.5 deg. N, 136.7 deg. E), Japan, were analyzed for the ring-years from 1989 to 1998 by the accelerator mass spectrometric measurement. The results were compared with those of the same samples analyzed by the liquid scintillation counting measurement to determine the reliability of liquid scintillation counting measurement. An important result of this study is that the sensitivity and reproducibility of accelerator mass spectrometric measurement was almost equal to that of liquid scintillation counting measurement.

  7. Simultaneous Determination of Nicotine and Metabolite Cotinine in Urine, Hair and Saliva by Gas Chromatography- Mass Spectrometry%尿液和头发及唾液中尼古丁及其代谢物可替宁的气相色谱-质谱同时测定法

    Institute of Scientific and Technical Information of China (English)

    何怡; 徐东群

    2011-01-01

    To establish a assay method for simultaneous determination of nicotine and its metabolite cotinine in urine, hair and saliva by gas chromatography-mass spectrometry. Methods The sample (urine, hair and saliva) was alkalized by NaOH, diphenylamine as an internal standard, and nicotine and cotinine were extracted simultaneously with chloroform, and then were determined by gas chromatography-mass spectrometry, the concentration of nicotine and cotinine in urine would be corrected by creatinine. Results The limits of detection of the method were 6.5 ng/ml and 14.5 ng/ml for nicotine and cotinine respectively.The limits of quantification were 22 ng/ml and 48 ng/ml respectively. The line ranges of the method were 0.022-4 μg/ml and 0.048-4 μg/ml for nicotine and cotinine respectively. The precisions of the method were 1.98%-2.69% and 4.70%-6.65% for nicotine and cotinine in urine, 0.87%-2.89% for nicotine in hair, 4.89%-4.54% for cotinine in saliva respectively. The recoveries of the spiked samples were 82.40%-106.48% and 81.80%-99.55% for nicotine and cotinine respectively in urine, 85.37%103.91% for nicotine in hair, 80.50%-93.00% for cotinine in saliva. Conclusion The method is simple, rapid and accurate, and it is satisfying to evaluate the human tobacco exposure.%目的 建立利用气相色谱-质谱(GC-MS)法同时测定人体尿液、头发、唾液中尼古丁及其代谢物可替宁的方法.方法 将样品(消解完全的头发、尿液、唾液)经NaOH碱化后用三氯甲烷萃取,气相色谱分离,质谱检测采用选择离子扫描,并以二苯胺作为内标物进行定量.尿液中尼古丁和可替宁的浓度用尿肌酐校正.结果 该方法的尼古丁和可替宁的检出限为分别为6.5、14.5 ng/ml,测定下限分别为22、48 ng/ml;尼古丁和可替宁的线性范围分别为0.022~4μg/ml、0.048~4μg/ml.尿液中尼古丁和可替宁的精密度分别为2.02%~2.62%、5.27%~7.24%;头发

  8. Quantitative Analysis and Fingerprint Profiles for Quality Control of Fructus Schisandrae by Gas Chromatography: Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Yong-Gang Xia

    2014-01-01

    Full Text Available This paper describes a simple, rapid, and effective quality assessment method for Fructus Schisandrae by gas chromatography-mass spectrum (GC-MS. The method was established by using specific lignan fingerprint profiles and quantitation of characteristic compounds in this herbal medicine. The GC-MS fingerprints of 15 batches of Schisandra samples from different regions of China showed similar lignan profiles. Five peaks were selected as characteristic peaks, and all of these were identified by using GC-MS techniques. The relative retention times of these characteristic peaks in the GC-MS fingerprint were established as an important parameter for identification of Schisandra samples. Meanwhile, relative peak areas may be a feasible approach to discriminate the S. chinensis and S. sphenanthera. Finally, these pharmacologically active constituents in the titled plant, schisandrins A–C and schizandrols A and B, were quantitatively determined using a validated GC-MS method.

  9. Electrothermal atomic absorption spectrometric determination of total and hexavalent chromium in atmospheric aerosols

    International Nuclear Information System (INIS)

    A method was developed which allow separate determination of Cr(VI) and total Cr from the same minute sample of atmospheric aerosols. Cr(VI) was leached was with 0.1 M Na2CO3 and the total Cr concentrations were determined after acid digestion. The method was validated by the analysis of certified reference materials, CRM 545, Mess-3 and Pacs-2 with good agreement between certified and found values. Cr concentrations in air samples taken around the chromium smelter show concentrations that exceed the maximum allowed levels in 8 h with higher values closer to the smelter. The limit of detection (LOD) of the method for Cr(VI) determination in air samples was found to be 0.2 ng m-3, i.e. lower than offered by the commonly preferred spectrophotometric and colorimetric techniques

  10. 'Age' determination of irradiated materials utilizing inductively coupled plasma mass spectrometric (ICP-MS) detection

    International Nuclear Information System (INIS)

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The GPEC system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. A commercially available Sr-ResinTM was used to perform the separation for the above mentioned analytes. A 1% acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic uncertainties of the experiments. (author)

  11. Determination of 10 sedative-hypnotics in human plasma using pulse splitless injection technique and gas chromatography-mass spectrometry%脉冲不分流进样气相色谱-质谱法分析血浆中的10种镇静催眠药

    Institute of Scientific and Technical Information of China (English)

    常青; 马虹英; 王方杰; 欧红莲; 邹明

    2011-01-01

    A simple, precise and sensitive gas chromatography-mass spectrometry ( GC-MS ) method coupled with pulse splitless injection technique was developed for the determination of 10 sedative-hypnotics ( barbital, amobarbital, phenobarbital, oxazepam, diazepam, nitraze-pam, clonazepam, estazolam, alprazolam, triazolam ) in human plasma. The drugs spiked in plasma were extracted with ethyl acetate after alkalization with 0. 1 mol/L NaOH solution. The organic solvent was evaporated under nitrogen stream, and the residues were redissolved by ethyl acetate. The separation was performed on an HP-5MS column ( 30 m × 250 μm × 0. 25 μm ). The analytes were determined and identified using selected ion monitoring ( SIM ) mode and scan mode, respectively. The internal standard method was used for the determination. The target analytes were well separated from each other on their SIM chromatograms and also on the total ion current ( TIC ) chromatograms. The blank extract from human plasma gave no peaks that interfered with all the analytes on the chromatogram. The calibration curves for 10 sedative-hypnotics showed excellent linearity. The correlation coefficients of all the drugs were higher than 0. 995 4. The recoveries of the drugs spiked in human plasma ranged from 92. 28% to 111. 7%, and the relative standard deviations ( RSDs ) of intra-day and inter-day determina-tions were from 4. 09% to 14. 26%. The detection limits ranged from 2 to 20 μg/L. The method is simple, reliable, rapid and sensitive for the determination and the quantification of 10 seda-tive-hypnotics in human plasma and seems to be useful in the practice of clinical toxicological cases.%采用脉冲不分流进样技术建立了血浆中10种镇静催眠药(巴比妥、异戊巴比妥、苯巴比妥、奥沙西泮、地西泮、硝西泮、氯硝西泮、艾司唑仑、阿普唑仑、三唑仑)的气相色谱-质谱(GC-MS)快速定性定量分析方法.血浆样品经0.1 mol/L 氢氧化钠溶液碱化后,

  12. Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

    Science.gov (United States)

    Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.

  13. Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aqueous Solution

    Institute of Scientific and Technical Information of China (English)

    ZHANG,Xiao-Ling(张小玲); YAN,Hong-Tao(阎宏涛)

    2002-01-01

    A selective and sensitive method for determination of platinum and palladium(Ⅱ) in an aqueous solntion simultaneously by laser thermal lens spectrometry, based on the complex reaction of 2- (3,5-dichloropyridylazo)-5- dimethylaminoamiline (3,5-diCl-PADMA) with platinum and palladium, has been developed. It is shown that the palladium complex can be formed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath. By using this difference of reaction temperature and the characteristic of the complexes mentioned above, the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation. The results show that the dynamic linear ranges of determination for platinum and pallladium are 0.005-0.04 μg/mL and 0.005-0.25 μg/mL respectively, and that the detection limits are both 0.002 μg/mL. The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.

  14. Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aquesous Solution

    Institute of Scientific and Technical Information of China (English)

    张小玲; 阎宏涛

    2002-01-01

    A selective and sensitive method for determination of platinum and palladium(Ⅱ)in an aqueous solution simultaneously by laser thermal lens spectrometry,based on the complex reaction of 2-(3,5-dichloropyridylazo)-5-dimethylaminoamiline(3,5-diCl-PADMA) with platinum and palladium,has been developed.It is shown that the palladium complex can be fromed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath.By using this difference of reaction temperature and the characteristic of the complexes mentioned above,the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation.The results show that the dynamic linear ranges of determination for platinum and palladium are 0.005-0.04μg/mL and 0.005-0.25μg/mL respectively,and that the detection limits are both 0.002/μg/mL.The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.

  15. Determination of γ-spectrometric parameters for some chloride salt solutions

    International Nuclear Information System (INIS)

    The mass attenuation coefficients, atomic cross-sections and effective atomic numbers are determined for LiCl, NaCl and KCl solutions with contents up to 0.2 g cm-3.The energies used are 0.511, 0.662 and 1.274 keV. The combined results were employed to determine the mass attenuation coefficients and atomic cross-sections of the salts and water in the solutions. The results are compared with the calculated values from elemental data. It was found that the mass attenuation coefficients and corresponding total cross-sections are, in general, less from measurement than from tabulated data, either for water or for the chloride salts

  16. Atomic absorbtion spectrometric determination of platinum, palladium and rhodium in catalysts for automotive exhaust

    International Nuclear Information System (INIS)

    Analytical parameters of the electrothermal atomic absorption spectrometry method have been optimized for determination of platinum, palladium and rhodium in ceramic-supported catalysts for automobile exhaust gas treatment. Two chemical sample preparation methods have been proposed. In order to simplify the sample preparation procedure and to prevent the possible losses of platinum group metals the treatment of the previously ground sample with a mixture of mineral acids is recommended. (authors)

  17. Atomic-absorption spectrometric determination of trace metals in zirconium and zircaloy by discrete sample nebulization

    International Nuclear Information System (INIS)

    A discrete sample nebulization technique was employed to determine trace metals in nuclear grade zirconium and Zircaloy by flame atomic-absorption spectrometry. With 10% (w/v) sample solutions, detection limits for Cd, Cu, Mn, Ni and Pb were 0.6, 2, 1, 3, and 10 μg/g. Micro standard-addition procedures and background correction were employed to minimize matrix interferences produced by the high salt content of the aspirated solutions. (author)

  18. Determination of rhenium in molybdenite by X-ray fluorescence: A combined chemical-spectrometric technique.

    Science.gov (United States)

    Solt, M W; Wahlberg, J S; Myers, A T

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 microg of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. PMID:18960464

  19. Microwave plasma atomic emission spectrometric determination of Ca, K and Mg in various cheese varieties.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

    Microwave plasma-atomic emission spectrometry (MP-AES) was used to determine calcium, magnesium and potassium in various Turkish cheese samples. Cheese samples were dried at 100 °C for 2 days and then digested in a mixture of nitric acid/hydrogen peroxide (3:1). Good linearities (R(2) > 0.999) were obtained up to 10 μg mL(-1) of Ca, Mg and K at 445.478 nm, 285.213 nm and 766.491 nm, respectively. The analytes in a certified reference milk powder sample were determined within the uncertainty limits. Moreover, the analytes added to the cheese samples were recovered quantitatively (>90%). All determinations were performed using aqueous standards for calibration. The LOD values for Ca, Mg and K were 0.036 μg mL(-1), 0.012 μg mL(-1) and 0.190 μg mL(-1), respectively. Concentrations of Ca, K and Mg in various types of cheese samples produced in different regions of Turkey were found between 1.03-3.70, 0.242-0.784 and 0.081-0.303 g kg(-1), respectively. PMID:26304350

  20. Simultaneous Determination of Five Alcohols in E-cigarette Emissions by Gas Chromatography-Mass Spectrometry%GC/MS法同时测定电子烟烟气释放物中的5种醇类化合物

    Institute of Scientific and Technical Information of China (English)

    段沅杏; 吴亿勤; 杨威; 杨继; 韩敬美; 田永峰; 赵伟; 杨柳; 陈永宽

    2015-01-01

    In order to accurately determine the contents of alcohols in e-cigarette emissions, a gas chromatography-mass spectrometry (GC/MS) method was developed for simultaneously determining 1, 2-propylene glycol, 1,3-butanediol, glycerol, diethylene glycol and triethylene glycol, wherein 1, 4-butanediol was used as an internal standard. Sixteen samples of e-cigarette were tested by the developed method. The results showed that: 1) The limit of detection and limit of quantitation were 0.08-0.32 and 0.27-1.07 μg/puff, respectively; the recoveries were 90.0%-99.5% with the relative standard deviations (RSD) ranged from 1.20% to 4.93%. 2) 1,2-Propylene glycol and glycerin were detectable, while diethylene glycol and triethylene glycol were undetectable in all samples; and 1,3-butanediol was detectable in four samples. 3) This method was suitable for the qualitative and quantitative determination of 1,2-propylene glycol, 1,3-butanediol, glycerol, diethylene glycol, triethylene glycol in e-cigarette emissions.%为了准确测定电子烟烟气释放物中醇类化合物的量,以1,4-丁二醇为内标建立了同时检测电子烟烟气释放物中1,2-丙二醇、1,3-丁二醇、丙三醇、二甘醇和三甘醇的气相色谱/质谱(GC/MS)方法,采用该法测定了16种电子烟样品.结果表明:①该法的检出限和定量限范围在0.08~0.32 μg/口和0.27~1.07 μg/口之间;回收率在90.0%~99.5%之间,相对标准偏差(RSD)为1.20%~4.93%.②所测样品中均检出1,2-丙二醇、丙三醇,均未检出二甘醇和三甘醇;4个样品中检测出1,3-丁二醇.该法灵敏度高、定性准确,适合电子烟样品烟气释放物中1,2-丙二醇、1,3-丁二醇、丙三醇、二甘醇和三甘醇的定性定量分析.

  1. HS-SPME/GC/MS法测定水中土臭素和2-甲基异崁醇的条件优化%Determination of GSM and 2-MIB in natural water by headspace solid-phase micro-extraction coupled with gas chromatography/mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    彭世富; 丁震; 夏卫文; 郑浩; 夏玉婷; 陈晓东

    2013-01-01

    目的:探索顶空固相微萃取-气相色谱/质谱法(HS-SPME/GC/MS)测定水中嗅味物质土臭素(GSM)和2-甲基异嵌醇(2-MIB)的最佳实验条件.方法:应用L32(49)正交表安排顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质时的萃取温度、萃取时间、搅拌子转速、盐浓度、解吸时间和解吸温度并进行实验,优化各项操作参数.结果:顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质的优化后实验条件是:萃取温度和解吸温度分别为65℃和260℃,萃取时间和解吸时间分别是40 min和7 min,搅拌子转速是600 r/min,盐浓度为30%(W/V).分别测定高低加标样,回收率为91%~107%,检出限(S/N=3)为0.04 ng/L,回收率为91%~104%,检出限(S/N=3)为0.13 ng/L.结论:通过正交实验设计优化实验条件,所建立的分析方法准确、简便、可靠,符合水中嗅味物质的测定要求.%Objective:To optimize the conditions for determination of the earthy and musty odors geosmin,2-methylisoborneol (2-MIB) in natural water by hcadspace solid-phase micro-extraction (SPME) coupled with gas chromatography/mass spectrometry and to establish a proposed method for determining the typical odor compounds in water.Methods:By applying the orthogonal experiment design L32(49) to arrange the determination conditions,several parameters of the extraction and desorption were studied and optimized (such as extraction temperature,desorption temperature,extraction time,ionic strength and rotate-speed),and some other parameters (such as correlation coefficient,limits of detection,RSD and recovery) were applied to evaluate effect of this method.Results:The optimum temperature of extraction and desorption were 65℃ and 260℃,respectively;time of extraction and desorption were 40 min and 7 min,respectively ;ionic strength,30% (W/V) ; rotate-speed,600 rpm.Under the optimized experimental conditions,limits of detection (S/N=3) were 0.04 and 0.42 ng/L for

  2. 外标-气相色谱-质谱法准确测定猪肉中的14种脂肪酸%Accurate determination of fourteen fatty acids in pork by external standard-gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    喻文娟; 侯静文; 朱邦尚

    2012-01-01

    采用外标-气相色谱-质谱法准确测定了猪肉中14种脂肪酸的含量和百分含量,并与峰面积归-化法的结果进行了比较,两种方法都测出猪肉中8种主要的脂肪酸:肉豆蔻酸、棕榈酸、棕榈油酸、硬脂酸、反油酸、油酸、亚麻酸、亚油酸.峰面积归-化法测定高含量脂肪酸结果较为准确,测定低含量脂肪酸则误差较大.同时对相关国标中的前处理方法进行了改进,脂肪提取用溶剂浸提法代替索氏提取法,脂肪酸甲酯化用碱常温催化酯交换法代替先皂化、再甲酯化的方法.方法学试验结果表明:14种脂肪酸甲酯的线性回归相关指数R2皆大于0.992、加标回收率皆大于75%、而样品平行测定3次的相对标准偏差RSD皆小于5%.该方法简便、环保、准确性好、精密度高,完全满足猪肉中脂肪酸的分析需要,可广泛应用于猪肉等肉类样品中脂肪酸的日常检测工作.%The contents and percent contents of fourteen fatty acids in pork has been accurately determined by external standard-gas chromatography-mass spectrometry and compared with the percent contents determined using peak area normalization method. Both methods have shown that the eight primary components in pork are myristic acid, palmitic acid, palmitoleic acid, stearic acid, elaidic acid, oleic acid, linolenic acid and linoleic acid. As for nomalisation method, the results of high-content fatty acids were more accurate, while those of low-content fatty acids produced some errors. Meanwhile, the sample preparation procedures in relevant Chinese Standards have been improved. Soxhlet extraction was replaced by solvent extraction to obtain fats the two-step method of saponification before methyl esterification was replaced by the one-step method of ester exchanging reaction catalyzed by base at room temperature to obtain fatty acid methyl ester (FAME). The methodological study showed that for all the fourteen fatty acids, Rz of

  3. Determination of six phthalate plasticizers in coatings on toys by gas chromatography-mass spectrometry%气相色谱-质谱法测定玩具涂层中6种邻苯二甲酸酯增塑剂

    Institute of Scientific and Technical Information of China (English)

    陈梅; 沈培康; 蒋小良

    2015-01-01

    A method for determining six kinds of phthalate plasticizers including dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), bis(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-iso-nonyl phthalate (DINP), and di-iso-decyl phthalate (DIDP) in coatings on toys by gas chromatography-mass spectrometry (GC-MS) was established. The conditions of microwave assisted extraction were optimized as follows:dichloromethane as extractant, extraction temperature 60 °C, and extraction time 25 min. Under the selected experimental conditions, six phthalate plasticizers in coatings on toys were determined by the method, and the linear regression between peak area and mass concentration of individual plasticizer was made. The linear range is 0.5-50 mg/L, correlation coefficient higher than 0.999, detection limit 0.5-1.0 mg/L, recovery of standard addition 83.5%-105.6%, and relative standard deviation less than 5.8%. The method is easy and rapid to operate with good accuracy and sensitivity, suitable for simultaneous determination of the concentrations of six phthalate plasticizers in coatings on toys.%建立了气相色谱–质谱法测定玩具涂层中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2−乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)等6种邻苯二甲酸酯类增塑剂的分析方法,确定了适宜的微波辅助萃取条件为:以二氯甲烷为萃取剂,萃取温度60°C,萃取时间25 min。在试验选定的条件下,以该方法测定玩具涂层中6种邻苯二甲酸酯类增塑剂,以峰面积对质量浓度线性回归,线性范围在0.5~50 mg/L,则相关系数大于0.999,最低检出限为0.5~1.0 mg/L,加标回收率在83.5%~105.6%之间,相对标准偏差小于5.8%。该方法操作简便快速,准确度和灵敏度高,适合于玩具涂层中6种邻苯二甲酸酯类增塑剂含量的同时测定。

  4. Flame atomic absorption spectrometric determinations of some trace metals after coprecipitation with gold-APDC

    International Nuclear Information System (INIS)

    Complete text of publication follows. For the determination of trace metals in various samples, preconcentration is an inevitable step to overcome interferences. Among various techniques for the separation of trace metals proposed until now, coprecipitation is one of the most useful ones. Many different coprecipitation procedures including use of organic and inorganic collectors have been developed. So far, in the literature, it is reported that APDC, NaDDTC, PAN, TAR, Oxine, etc. as chelating agent for metal-chelate collector have been extensively used for coprecipitation of trace metals. However, metal chelates, especially dithocarbamates, as collectors are ideal for their sensitivities, simplicities and tolerances to interferences.Therefore, in the present work, fundamental studies on the coprecipitation with gold/APDC chelate have been carried out for determination of trace metals in environmental samples by FAAS with microinjection. According to our literature survey, gold/APDC is not used for the coprecipitation of heavy metal ions, until now. In this work, the coprecipitation was carried out in a centrifuge tube. Firstly, the main factors, such as amount of coprecipitant reagent and carrier element, pH of the solution, standing time, sample volume and diverse ions, affecting the coprecipitation of some trace metals were evaluated. Under optimized conditions, the recoveries of Cu, Ni, Pb and Cd were ≥ 95 %. R.S.D. values for ten replicates were lower than 5.0 %. Preconcentration factors were found to be 20. The coprecipitation was applied to various water samples and non-alcoholic beverage.

  5. An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    MAHMOUD MOHAMED ISSA

    2008-05-01

    Full Text Available A highly sensitive indirect atomic absorption spectrophotometric (AAS method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III. The excess of iron(III was extracted into diethyl ether and then the iron(II in the aqueous layer was aspirated into an air–acetylene flame and determined by AAS. The linear concentration ranges were 25–400, 50–500 and 60–600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

  6. Determination of total body water by a simple and rapid mass spectrometric method.

    Science.gov (United States)

    Van Kreel, B K; Van der Vegt, F; Meers, M; Wagenmakers, T; Westerterp, K; Coward, A

    1996-01-01

    A rapid and inexpensive method was developed to determine deuterium enrichment in body fluids. This is achieved by converting water into acetylene. To vacutainer tubes a small amount of calcium carbide is added. The tubes are evacuated and 25 microliters of sample are injected through the stopper. The reaction takes place spontaneously at room temperature in a few seconds. Enrichment at mass 27 compared with mass 26 can be determined by continuous flow isotope ratio mass spectrometry without any interference from the carrier gas helium. A series of D2O samples diluted with increasing amounts of H2O is prepared at the time of measurement of the biological samples and the measured ratios are used to calculate the isotope dilution of the unknown. The relative error of the method is 1.6% when a dose of 25 ml kg-1 is administered to the patient. The method was compared with two different methods in use in other laboratories, by a published method The means of the differences were -0.1 and 0.08 1, respectively, with standard deviations of 0.63 and 3.0.

  7. Experimental determination of the self-absorption factor for MTR plates by passive gamma spectrometric measurement

    Science.gov (United States)

    Berndt, R.; Mortreau, P.

    2011-07-01

    The measurement of the absolute activity or the mass of radioactive substances by gamma spectrometry needs to include a correction for the radiation absorption inside the source volume, the so-called self-absorption factor. It depends on geometry and material composition of the source, the detector geometry and on the geometrical arrangement of source and gamma radiation detector; it can be calculated if full information about all that is available. This article however describes how to determine the self-absorption factor from measurements if the radiation sources are plates of uranium fuel with typical parameters of nuclear fuel for MTR reactors and without using detail information on the source geometry, thus allowing easy inspection without relying on - potentially falsified - declarations on the internal properties of the fuel objects and without calculation.

  8. Experimental determination of the self-absorption factor for MTR plates by passive gamma spectrometric measurement

    Energy Technology Data Exchange (ETDEWEB)

    Berndt, R., E-mail: Reinhard.Berndt@jrc.ec.europa.eu [European Commission, Joint Research Centre, Institute for Transuranium Elements, TP 800, Via Fermi, Ispra (Italy); Mortreau, P. [European Commission, Joint Research Centre, Institute for Transuranium Elements, TP 800, Via Fermi, Ispra (Italy)

    2011-07-11

    The measurement of the absolute activity or the mass of radioactive substances by gamma spectrometry needs to include a correction for the radiation absorption inside the source volume, the so-called self-absorption factor. It depends on geometry and material composition of the source, the detector geometry and on the geometrical arrangement of source and gamma radiation detector; it can be calculated if full information about all that is available. This article however describes how to determine the self-absorption factor from measurements if the radiation sources are plates of uranium fuel with typical parameters of nuclear fuel for MTR reactors and without using detail information on the source geometry, thus allowing easy inspection without relying on - potentially falsified - declarations on the internal properties of the fuel objects and without calculation.

  9. Gamma-ray spectrometric enrichment determination of a low enriched UF6 sample

    International Nuclear Information System (INIS)

    Non-destructive gamma-ray spectroscopic measurements have been done on a solid 80-gram UF6 sample in the framework of an interlaboratory measurement evaluation programme for isotopic abundance measurements on low enriched UF6. In the ECN measurements the photopeak areas of the 185.72 keV gamma-rays of 23'5U have been determined with different peak evaluation methods. In spite of the rather large spread in un-certainty values between the different methods, no statistically significant differences in the 235U atomic abundance values have been obtained. The average measured 235U atomic abundance in uranium is 3.480% with a relative uncertainty of 0.2% (2 σ confidence level). The certified value is 3.5001% with a relative uncertainty of 0.03% (2 σ). An explanation for this discrepancy has not been found. (author). 8 refs.; 7 figs.; 20 tabs

  10. Determination of long-lived radionuclides at ultratrace level using advanced mass spectrometric techniques

    International Nuclear Information System (INIS)

    Determination of long-lived radionuclides at sub-fg concentration level is a challenging task in analytical chemistry. Inductively coupled plasma mass spectrometry (ICP-MS) with its ability to provide the sensitive and fast multielemental analysis is one of the most suitable method for the measurements of long lived radionuclides in the trace and ultra trace concentration range. In present the Ph.D. study a variety of procedures have been developed permitting the sub fg ml-1 determination of long-lived radionuclides (e.g. U, Th, Pu) as well as 226Ra (T1/2 = 1600 y) and 90Sr (T1/2= 28.1 y) in different samples. In order to avoid isobaric interferences, to increase the sensitivity, precision and accuracy of the methods the application of different techniques: pre-concentration of the sample, off-line separation on the crown resin, measurements under cold plasma conditions, using microconcentric nebulizers (e.g DIHEN, DS-5) or the application of LA-ICP-MS for sample introduction have been studied. The limits of detection for different radionuclides was significantly improved in comparison to the ones reported in the literature, and, depending on the method applied, was varied from 10-15 to 10-18 g ml-1 concentration range. In addition to the analysis of long lived radionuclides, some other elements, that can present potential interest to the analyzed sample, were measured within the framework of the present study. Laser ablation inductively coupled plasma mass spectrometry (LAICP- MS) was used to produce images of element distribution in 20μm m thin sections of human brain tissue. The sample surface was scanned (raster area ∝80 mm2) with a focused laser beam (wavelength 213 nm, diameter of laser crater 50μm, and laser power density 3x109 W cm-2) in a cooled laser ablation chamber developed for these measurements. Cross sections of human brain samples - hippocampus as well as brain tissues infected and non-infected with Glioblastoma Multiforme (tumor cells) were

  11. 单壁碳纳米管固相萃取-气相色谱-质谱联用法测定茶油中6种邻苯二甲酸酯%Determination of six phthalate acid esters in camellia oil by gas chromatography-mass spectrometry coupled with solid-phase extraction using single-walled carbon nanotubes as adsorbent

    Institute of Scientific and Technical Information of China (English)

    张帆; 李忠海; 张莹; 黄志强; 王小淞

    2014-01-01

    建立了单壁碳纳米管( SWCNTs)为吸附剂的固相萃取净化-气相色谱-质谱检测茶油中6种邻苯二甲酸酯(PAEs)的分析方法。样品经正己烷稀释,玻璃 SWCNTs SPE小柱净化,GC-MS选择离子监测(SIM)模式测定,外标法定量。对正己烷的稀释体积、吸附材料的类型、SWCNTs 用量、淋洗液用量、洗脱溶剂类型和体积等影响萃取效率的条件进行了优化,得到的最优萃取条件为:正己烷稀释体积为5 mL,SWCNTs 用量为0.6 g,淋洗液为20 mL正己烷,洗脱溶剂为5 mL 甲苯。6种 PAEs 在0.05~1.0 mg/L 范围内线性关系良好,相关系数( r)均大于0.9999;在0.05~1.0 mg/kg添加范围内,6种目标物的平均回收率为86.4%~111.7%,相对标准偏差为4.2%~10.4%。该方法准确、快速,可满足茶油中6种邻苯二甲酸酯的检测需要。%An analytical method based on solid-phase extraction with single-walled carbon nanotubes( SWCNTs ) as adsorbent was developed for the simultaneous determination of six phthalate acid esters( PAEs)in camellia oil by gas chromatography-mass spectrometry( GC-MS). The samples were diluted by hexane and then cleaned up with a glass SWCNTs solid phase extraction( SPE)column. The PAEs were measured by GC-MS in selected ion monito-ring( SIM)mode,using external standard method for quantitative analysis. The important fac-tors affecting extraction efficiency,such as the dilution volume of hexane,the type of adsor-bent material,the dosage of SWCNTs,the volume of wash solution,the type and volume of elution solution were optimized. The optimal conditions were as follows:the dilution volume of hexane was 5 mL,the dosage of SWCNTs was 0. 6 g,the wash solution was 20 mL hexane,and the elution solution was 5 mL toluene. The six PAEs had a good linear range from 0. 05 mg/L to 1. 0 mg/L,with the correlation coefficients( r)all above 0. 999 9. The average recoveries of the six targets in spiked

  12. 气相色谱-质谱法测定聚氯乙烯包装材料和食品模拟物中的46种增塑剂%Determination of 46 plasticizers in food contact polyvinyl chloride packaging materials and their migration into food simulants by gas chromatography- mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    郭春海; 薄海波; 段文仲; 贾海涛; 陈瑞春; 马育松; 艾连峰

    2011-01-01

    建立了46种增塑剂在聚氯乙烯(PVC)食品包装材料中的含量及其在水、3%乙酸、10%乙醇和橄榄油4种食品模拟物中迁移量的气相色谱-质谱(GC-MS)测定方法.食品包装材料、水质模拟物和橄榄油中增塑剂分别采用溶解-沉淀法、正己烷液-液萃取和凝胶渗透色谱(GPC)法提取.采用GC-MS法,在选择离子监测模式(SIM)下对46种增塑剂进行定性,采用外标法进行定量测定.各种增塑剂在0.1~2.0 mg/L 质量浓度范围内呈线性,相关系数为 0.9910~0.9999,各组分检出限均在0.005~0.05 mg/kg 之间.在2种食品模拟物中,3个浓度添加水平下46种增塑剂的加标回收率在69.51% ~107.21%之间,精密度(RSD, n=6)为3.53% ~18.95% .该方法可满足PVC食品接触制品及4种不同性质的食品模拟物中多种类增塑剂的快速筛查和准确定性、定量测定要求.%A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 46 plasticizers in food contact polyvinyl chloride (PVC) packaging materials and their migration into food simulants, i.e. water, 3% acetic acid, 10% ethanol and olive oil.Plasticizers in the PVC packaging materials, aqueous food simulants and olive oil food simulants were extracted by the dissolution-precipitation, liquid-liquid extraction and gel permeation chromatography (GPC) approaches, respectively. The extracts were analyzed by GC-MS in selective ion monitoring (SIM) mode and quantified using the external standard method. The calibration curves were linear in the ranges of 0.1 - 2.0 mg/L with the correlation coefficients of 0. 991 0 -0. 999 9. The limits of detection were from 0.005 mg/kg to 0.05 mg/kg ( S/N = 5 ).The recoveries at 3 spiked levels were 69.51% - 107.21% and the relative standard deviations ( RSDs, n =6) ranged from 3.53% to 18.95%. These results show that this method is fast, sensitive and accurate for the qualitative and quantitative determination

  13. Simultaneous Determination of Toxic Alkaloids and Rat Poisons in Toxic Samples by Dispersive Liquid-liquid Micro-extraction Combined with Gas Chromatography-Mass Spectrometry%分散液-液微萃取-气相色谱-质谱法同时测定中毒样品中有毒生物碱和鼠药

    Institute of Scientific and Technical Information of China (English)

    麦沛明; 余胜兵; 吴西梅; 苏广宁; 钟秀华; 朱炳辉

    2015-01-01

    建立了分散液-液微萃取( Dispersive liquid-liquid micro-extraction, DLLME)与气相色谱-质谱( GC-MS)联用同时测定中毒样品中3种鼠药(毒鼠强、溴鼠灵、溴敌隆)和5种有毒生物碱(莨菪碱、东莨菪碱碱、钩吻碱、士的宁、马钱子碱)的方法。100μL萃取剂氯仿与600μL分散剂甲醇混合后,迅速注入样品,萃取过程在乳化体系中完成;以8000 r/min离心5 min,使两相分层,取下层有机相进行GC-MS分析。考察了萃取剂、分散剂的种类和体积、萃取时间、pH值及盐浓度对萃取效率的影响。在优化条件下,各目标物在水样、尿样、黄酒样的检出限为0.003~1.0μg/L,在米饭样品检出限为0.002~0.2μg/kg;各目标物低、中、高加标回收率为81.0%~110%,精密度均小于7%。本方法灵敏度高,快捷高效,适用于中毒样品中有毒生物碱和鼠药的同时测定。%A novel method for simultaneous determination of 3 rat poisons ( tetramine, bromadiolone, brodifacoum) and 5 toxic alkaloids ( hyoscyamine, scopolamine, gelsemine, strychnine, brucine ) in toxic samples by dispersive liquid-liquid micro-extraction ( DLLME ) coupled with gas chromatography-mass spectrometry was established. A mixture extractant containing 100 μL trichloromethane and 600 μL methanol was injected into the prepared sample to form an emulsion and the extraction process was accomplished. After centrifuged at 8000 r/min for 5 min, the settled drop of trichloromethane solvent was transferred to a conical insert within a GC autosampler vessel, and analyzed by GC-MS. Factors affecting extraction efficiency such as the type and volume of extractant, dispersive agent, extraction time, pH value and salt concentration of extraction system were studied. The limits of detection(LODs) were from 0. 003 to 1 μg/L in water sample, urine sample and rice wine sample. LODs were from 0. 002 to 0. 2 μg/kg in rice sample. The recoveries of toxic samples were in the range of 81

  14. 稳定同位素稀释气相色谱-质谱联用测定化妆品中5种磷酸三酯类化合物%Determination of Organophosphate Esters in Cosmetics by Stable Isotope Dilution-Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    韩婉清; 罗海英; 陈立伟; 吴玉銮; 冼燕萍; 王斌

    2014-01-01

    根据不同化妆品的基质特性探讨优化不同的提取净化方法,建立了稳定同位素稀释气相色谱-质谱联用测定化妆品中5种磷酸三酯类化合物( OPEs)的方法。膏霜乳液类和蜡基类化妆品经溶剂提取后,采用ENVI-Carb固相萃取柱净化;粉剂类和水剂类化妆品经溶剂提取、浓缩后直接检测。样液经DB-5MS(30 m×0.25 mm×0.25μm)色谱柱分离,GC-MS的选择离子监测( SIM)模式检测,以保留时间和特征离子丰度比定性,稳定同位素稀释内标法定量。在优化的实验条件下,5种磷酸三酯类化合物在各自的线性范围内相关系数大于0.9995,方法检出限为1.0~30μg/kg,平均回收率为89.5%~105%,相对标准偏差(n=6)为2.9%~9.1%。本方法净化效果好,可有效消除基质效应,且有较好的回收率,可用于不同类型的化妆品基质中磷酸三酯类化合物的测定。%A method based on stable isotope dilution gas chromatography-mass spectrometry ( GC-MS ) was established to determine five kinds of organophosphate esters ( OPEs ) in different kinds of cosmetics. For cream and wax-based cosmetics, samples were extracted by appropriate solvent, and then purified by ENVI-Carb solid phase extracting column. For powder and aqueous samples, GC-MS test could be operated directly after solvent extraction and concentration. All of the samples were separated by DB-5MS (30 m×0. 25 mm× 0. 25 μm) chromatographic column, and detected by selected ion monitoring ( SIM ) mode. The target analytes were qualitatively confirmed by retention time and abundance ratio of characteristic ions, and quantified by stable isotope diluted internal standard method. Under the optimized conditions, the linear coefficients of the OPEs were larger than 0. 9995, the detection limits were 1. 0-30 μg/kg, the average recoveries ( n=6 ) ranged from 89 . 5% to 105%, and the RSDs were in the range of 2 . 9%-9 . 1%. The developed method, which was characteristic by

  15. 气相色谱/质谱联用法测定烟用水基型乳胶中的邻苯二甲酸酯%Determination of Phthalates in Water-based Emulsion Adhesives for Tobacco with Gas Chromatography/Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    杨斌; 陈超英; 吴达; 林华清; 陈星洁; 戴云辉

    2011-01-01

    为测定烟用水基型乳胶中的邻苯二甲酸酯,用加有内标物质的正己烷溶液对乳胶样品进行了超声萃取,并采用气相色谱/质谱/选择离子监测法(GC/MS/SIM)测定了144个样品中的7种邻苯二甲酸酯:邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己)酯(DEHP)、邻苯二甲酸二辛酯(DOP)和邻苯二甲酸丁基苄基酯(BBP).结果表明:①样品中加入2 mL水,超声30 min萃取效果较好;②在标准溶液浓度范围内,7种邻苯二甲酸酯的线性均较好,相关系数达到0.996以上;③低、中、高3种浓度的加标回收率在85% ~ 111%之间,相对标准偏差(RSD)均小于5%;④当前国内烟用水基胶中使用的邻苯二甲酸酯类增塑剂主要集中在D1BP,DBP两种.%In order to determine the phthalates in water-based emulsion adhesives for tobacco, the adhesives were extracted with rc-hexane containing internal standard by ultrasonic instruments. Seven phthalates in 144 water-based emulsion adhesive samples, including dimethyl phthalate ( DMP) , diethyl phthalate ( DEP ) , diisobutyl phthalate (DIBP) ,dibutyl phthalate ( DBP) , di-(2-ethylhexyl) phthalate ( DEHP) , dioctyl phthalate (DOP) and benzyl butyl phthalate ( BBP) , were determined by gas chromatography/mass spectrometry. The results showed that;l) 30 minutes were preferable duration for extraction by adding 2 mL water into the sample ;2) the regression coefficients of the 7 phthalates were over 0. 996 within the range of their calibration ;3) the recoveries (the standard spiked at low,middle and high concentration levels) ranged from 85% to 111% ,and the relative standard deviation (USD) of the method was below 5% ;4) DIBP and DBP are the two phthalate plasticizers among the water-based adhesives most commonly used in the cigarette industry.

  16. Determination of 23 phthalate esters in food by solid-phase extraction coupled with gas chromatography-mass spectrometry%固相萃取-气相色谱-质谱法测定食品中23种邻苯二甲酸酯

    Institute of Scientific and Technical Information of China (English)

    郑向华; 林立毅; 方恩华; 黄永辉; 周爽; 周昱; 郑小严; 徐敦明

    2012-01-01

    建立了同时检测食品中23种邻苯二甲酸酯类化合物的固相萃取-气相色谱-质谱(GC-MS)分析方法.样品经正己烷或乙腈提取、玻璃ProElut PSA固相萃取柱净化,GC-MS选择离子监测模式(SIM)测定.考察了不同种类食品的提取、净化方法.23种邻苯二甲酸酯的线性范围除邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二异癸酯(DIDP)为0.5~5 mg/L外,其余均为0.05 ~5 mg/L,相关系数(r)除DIDP外均大于0.99.方法的检出限(信噪比为3)为0.005~0.05 mg/kg,定量限(信噪比为10)为0.02 ~0.2 mg/kg.在10种食品基质中3个加标水平的平均回收率为77%~112%,相对标准偏差(RSD,n=6)为4.1%~12.5%.该方法稳定、可靠,操作简单,适用于食品中邻苯二甲酸酯类化合物的检测与确证.%A method for the simultaneous determination of 23 phthalate esters in food samples by solid-phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was developed and evaluated. The samples were extracted with hexane or acetonitrile, and cleaned up with a glass ProElut PSA SPE column. The identification and quantification were performed by GC-MS in selected ion monitoring (SIM) mode. The extraction processes of different foods were investigated. The calibration curves of phthalate esters showed good linearity in the range of 0. 05 - 5 mg/L (0. 5 - 5 mg/L for diisononyl phthalate ( DINP), diisodecyl-phthalate (DIDP)) with the correlation coefficients (r) between 0.984 8 and 0. 999 6. The limits of detection of phthalate esters in food samples ranged from 0. 005 to 0. 05 mg/kg (S/N = 3) and the limits of quantification ranged from 0. 02 to 0. 2 mg/kg (S/N = 10). The average recoveries of 23 analytes spiked in 10 kinds of food matrices ranged from 77% to 112% with the relative standard deviations (RSDs, n =6) of 4. 1% - 12. 5%. The method is suitable for the determination of 23 phthalate esters simultaneously in foodstuffs with easy operation, high

  17. Simultaneous determination of neutral sugars and uronic acid constituents in a novel bacterial polysaccharide using gas chromatography-mass spectrometry%气相色谱-质谱联用同时分析新型细菌多糖中的单糖和糖醛酸

    Institute of Scientific and Technical Information of China (English)

    王凤芹; 杨航仙; 汪以真

    2013-01-01

    对纯化的新型细菌多糖进行酸水解,用乙硫醇-三氟乙酸和醋酐-吡啶体系先后对酸水解物进行衍生,与之前报道不同的是糖醛酸得到有效衍生化.以木糖为内标,采用气相色谱-质谱联用(GC-MS)定量分析该多糖酸水解物中单糖和糖醛酸衍生物发现,该多糖的糖链由岩藻糖、葡萄糖、葡萄糖醛酸和半乳糖组成,其相对物质的量比为1.50∶1.0∶0.79∶2.06;中性糖比例与糖醇乙酸酯化分析岩藻糖、葡萄糖和半乳糖的相对物质的量比(1.76∶1.0∶1.98)接近;糖醛酸咔唑法与该方法分析葡萄糖醛酸的含量分别为16.19%和14.85%.以上结果表明所建立的衍生化方法及GC-MS同时定量分析多糖酸水解物中单糖和糖醛酸的方法可行.此外还对葡萄糖醛酸的质谱裂解机理进行了阐述.%The purified novel bacterial polysaccharide was acid-hydrolyzed, followed by the subsequent derivatization using ethanethiol-trifluoroacetic acid and acetic anhydride-pyridine systems sequentially. Our findings differ from the previous reports in that the glucuronic acid was obtained through effective derivatization. The neutral sugars and glucuronic acid were analyzed using gas chromatography-mass spectrometry (GC-MS) with xylose as an internal standard. The polysaccharide was found to be composed of fucose, glucose, glucuronic acid and galactose, with the relative molar ratio of 1. 50: 1. 0: 0. 79= 2. 06. The neutral sugars ratio was similar to the relative molar ratio for fucose, glucose and galactose of 1. 76: l. 0: 1. 98 through alditol acetates determined by GC. The percentages of glucuronic acid analyzed using either the carbazole and sulfuric acid method or the above method were 16. 19% and 14. 85%, respectively. These results indicate that it is practicable to use the derivatization method and GC-MS to quantitatively analyze neutral sugars and glucuronic acid simultaneously in polysaccharide. For GC-MS analysis, the

  18. 固相萃取-气相色谱-质谱法测定食用油中7种邻苯二甲酸酯类塑化剂%Determination of seven kinds of phthalate acid esters in edible oil by solid-phase extraction-gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    张明明; 刘玉兰; 马宇翔; 张东东

    2015-01-01

    建立了SPE-GC-MS联用法测定食用油中7种邻苯二甲酸酯的方法。该方法在0.01~5.0 mg/L范围内具有良好的线性,相关系数R2均在0.9987以上,仪器检出限(S/N=3)在0.06~0.5μg/L之间,平均回收率在72.4%~103 .0%之间。采用本方法对不同种类、不同包装的27个食用油样中7种邻苯二甲酸酯类塑化剂( DMP、DEP、DBP、DPP、BBP、DEHP、DnOP )的含量进行测定。结果表明:食用油中都不同程度地检出塑化剂;27个油样都检测出DEHP,含量范围为0.007~4.752 mg/kg;25个油样检测出DBP,含量范围为0.007~21.290 mg/kg;DEP仅在铁盒装的稻米油样中检出,BBP在2个玻璃瓶装的橄榄油样中检出,所有油样中没有检测出DnOP。在27个受检食用油样中,有9个油样的DBP含量超出国家标准限量(≤0.3 mg/kg),超标率为33.3%;有2个油样的DEHP含量超出国家标准限量(≤1.5 mg/kg),超标率为7.4%。%A method for determining seven kinds of phthalate acid esters( PAEs) in edible oil by solid-phase extraction-gas chromatography-mass spectrometry ( SPE-GC-MS) was established. The meth-od had good linearship in the range of 0. 01-5. 0 mg/L with correlation coefficient R2 more than 0. 998 7;the instrumental limit of detection ( S/N=3 ) of the method ranged from 0 . 06 to 0 . 5 μg/L;the average recovery was 72. 4% - 103. 0%. The contents of seven kinds of PAEs ( DMP,DEP,DBP,DPP,BBP, DEHP,DnOP) in 27 edible oils samples of different kinds and packaging materials were determined by SPE-GC-MS. The results showed that PAEs were all detected in the 27 edible oils in different degrees;DEHP was detected in all of the 27 edible oils samples, and its content ranged from 0. 007 to 4. 752 mg/kg;DBP was detected in 25 edible oils samples, and its content was in the range of 0. 007-21. 290 mg/kg;DEP was only detected in rice bran oil sample packaged in iron box, BBP was detected in two ol-ive oils samples packaged in glass bottle and DnOP was detected in none

  19. Quantitative gas chromatographic mass spectrometric determination of pinaverium-bromide in human serum.

    Science.gov (United States)

    de Weerdt, G A; Beke, R P; Verdievel, H G; Barbier, F; Jonckheere, J A; de Leenheer, A P

    1983-03-01

    A method has been developed for quantitative determination of pinaverium-bromide, a quaternary ammonium derivative with papaverine-like activity, in human serum. The method involves a chloroform extraction of serum spiked with N-(6,6-dimethyl bicyclo[3.1.1]2-heptenyl-ethoxyethyl) perhydro-1,4-oxazine as internal standard. After evaporation of the solvent, and reduction of the residue with Raney-Nickel, the internal standard and the reduced pinaverium-bromide are re-extracted from the reaction mixture with toluene and analysed isothermally on a fused silica column coated with OV-101. Although chemical ionization with methane revealed intense protonated molecular ions for both pinaverium-bromide and the internal standard, selectivity and sensitivity were significantly lower in comparison with electron impact ionization at 70 e V. Therefore, quantification was performed in the electron impact mode by single ion monitoring of the common fragment ion at m/z 100.2. A linear detector response was observed up to 160 ng ml-1. A within-run assay precision better than 2% CV (n = 5) was found, and a detection limit of 1 ng pinaverium-bromide ml-1 of serum was attained. PMID:6850068

  20. Development of a gas chromatographic/mass spectrometric method for determination of phthalates in oily foods.

    Science.gov (United States)

    Sannino, Anna

    2010-01-01

    A GC/MS method was developed for simultaneous determination of 12 phthalates and four other plasticizers--acetyl tributyl citrate, di(2-ethylhexyl) adipate, dibutyl sebacate, di-isononyl cyclohexane 1,2-dicarboxylate (DINCH)--in vegetable oil, pesto, and tomato sauce. Samples were extracted with acetonitrile and cleaned on a Florisil column. The final extract was analyzed by GC in combination with ion trap MS. The phthalates and di-isononyl cyclohexane 1,2-dicarboxylate were detected by MS/MS, while the other three plasticizers were monitored in the same GC run using full scan mode. The analytical process was validated in each matrix by the analysis of blank samples. Performance characteristics, such as linearity, LOQ, precision, and recoveries were studied. Studies at fortification levels of 0.25-200 mg/kg gave mean recoveries ranging from 71 to 106% and RSD values between 7 and 12% for all compounds. LOQs were 0.050-0.10 mg/kg for all the target compounds except di-isononyl phthalate, di-isodecyl phthalate, and DINCH (2.0 mg/kg).

  1. Honeybee Venom Proteome Profile of Queens and Winter Bees as Determined by a Mass Spectrometric Approach

    Directory of Open Access Journals (Sweden)

    Ellen L. Danneels

    2015-10-01

    Full Text Available Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS. Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings.

  2. Honeybee venom proteome profile of queens and winter bees as determined by a mass spectrometric approach.

    Science.gov (United States)

    Danneels, Ellen L; Van Vaerenbergh, Matthias; Debyser, Griet; Devreese, Bart; de Graaf, Dirk C

    2015-11-01

    Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS). Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings. PMID:26529016

  3. Liquid Chromatography-Tandem Mass Spectrometric Assay for Determination of Stavudine in Human Plasma

    Directory of Open Access Journals (Sweden)

    Fengdan Jin

    2014-01-01

    Full Text Available A LC-MS/MS method for determination of stavudine in human plasma was established and validated, and it was applied to the pharmaceutical formulations bioequivalence study. 0.5 mL plasma sample was extracted by liquid-liquid extraction. Stavudine was detected by a LC-MS/MS system. The pharmacokinetic parameters of stavudine in different formulations were calculated by noncompartment model statistics. The method was linear over the concentration ranges 5.00–1000 ng/mL in plasma. The intra- and interassay relative standard deviation (RSD was <10%. The average accuracies for the assay at three concentrations (5.00, 80.0, and 900 ng/mL were from 100.2% to 102.5%. Pharmacokinetic parameters of stavudine reference formulation were obtained as follows: Tmax was 0.6±0.2 h, Cmax was 480.7±150.9 g/L, t1/2 was 1.7±0.4 h, and AUC0-t was 872.8±227.8 g·h/L, and pharmacokinetic parameters of stavudine test formulation were obtained as follows: Tmax was 0.5±0.2 h, Cmax was 537.5±178.5 g/L, t1/2 was 1.7±0.3 h, and AUC0-t was (914.1±284.5 g·h/L. Calculated with AUC0-t, the bioavailability of two formulations was 105.0%.

  4. Determination of N-Methylformanilide, N-Methylaniline and Formanilide in Waste Water by Gas Chromatography-Mass Spectrometry Using Liquid-Liquid Extraction%液液萃取-气相色谱-质谱联用技术测定废水中N-甲基甲酰苯胺、N-甲基苯胺和甲酰苯胺

    Institute of Scientific and Technical Information of China (English)

    周永生; 王文昌; 顾浩

    2014-01-01

    建立了液液萃取-气相色谱-质谱(GC-MS)联用测定废水中N-甲基甲酰苯胺(NMF)、N-甲基苯胺(NMA)和甲酰苯胺(FA)的分析方法.考察了萃取溶剂、盐加入量和pH等影响萃取效果的参数.结果表明,当以二氯甲烷为萃取剂,将pH调至11.85,15%NaCl溶液加入量为1%(体积比)条件下,NMF、NMA和FA的萃取效果最佳.以N,N-二乙基苯胺(DEA)为内标,在GC-MS选择离子模式下测定NMF、NMA和FA,该方法对三种目标物的平均回收率为97.5%~101.0%,相对标准偏差为4.3%~6.3%(n=6),检测限(S/N=3)为0.0018~0.0023 μg/L,测得某废水样品中NMF、NMA和FA的含量依次为0.94±0.08、0.14±0.02和0.12±0.02 g/L.%A liquid-liquid extraction and gas chromatography-mass spectrometry(GC-MS) method for the determination of N-methyl formanilide(NMF),N-methyl aniline(NMA) and formanilide (FA) in waste water was developed.The parameters affecting the extraction process such as the type of extracting agent,salt addition and pH value of waste water were investigated.A good extraction efficiency for NMF,NMA and FA was obtained when dichloromethane was used as the extraction agent,the pH value of waste water was adjusted to 11.85 and the addition of 15% NaCl solution(mass concentration) was 1% (by volume).GC-MS was employed to detect NMF,NMA and FA under the mode of selected-ion-monitoring(SIM) and N,N-diethyl aniline(DEA) was used as an internal standard.The average recoveries of the target compounds ranged from 97.5% to 101.0% with the relative standard deviations of 4.3%-6.3% (n=6),and the limits of detection estimated for the individual target compound(three times of the standard deviation of baseline) were in the range of 0.0018-0.0023 μg/L.The contents of NMF,NMA and FA in actual sample were 0.94±0.08,0.14±0.02 and 0.12±0.02 g/L,respectively.

  5. Simultaneous determination of 4 kinds of illicit drugs in health-care foodstuffs by ultra performance liquid chromatography-mass spectrometry%液相色谱-串联质谱法同时测定保健食品中四种违禁药物含量

    Institute of Scientific and Technical Information of China (English)

    陈吉汉; 侯彩云; 路勇; 姜洁; 冯楠

    2014-01-01

    目的:建立超高效液相色谱-串联质谱法测定保健食品中西地那非、他达那非、伐地那非以及红地那非四种违禁药物含量的方法。方法采用ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以甲醇和添加0.1%甲酸5 mmol乙酸铵为流动相,梯度洗脱程序,进样分析20 min,在电喷雾正离子模式下以多反应监测(MRM)方式检测,外标法定量。结果四种那非类违禁药物的检出限(LOD, S/N=3)和定量限(LOD, S/N=10)分别0.1~0.5μg/kg 和0.3~2.0μg/kg 在0.1~100μg/kg 浓度范围内线性关系良好(r>0.99),加标回收率为73.6%~90.4%,相对标准偏差为1.0%~8.9%。结论该方法操作简单,重现性好,背景噪音低,具有较高的灵敏度和选择性。%Objective To develop a method for the simultaneous determination of sildenafil, tadalafil, vardenafil and acetildenafil in health-care foodstuffs by ultra performance liquid chromatography-mass spec-trometry. Methods The elution was separated on an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7μm) using the methanol-5 mmol ammonium acetate containing 0.1% formic acid as the mobile phase and a gradient elution program with a cycle time of 20 min, detected by electrospray ionization mass spectrometry in positive mode with multiple reaction monitoring, quantified by external standard method. Results The limits of detection(LOD, S/N=3)and quantification(LOQ, S/N=10) of 4 compounds were 0.1~0.5 μg/kg and 0.3~2.0μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0.99 in the ranges of 0.1~100μg/kg. Average fortified recoveries were 73.6%~90.4%, and the relative standard deviations were in the ranges of 1.0%~8.9%. Conclusion This method has the advantages of simple operation, good reproduci-bility, low background noise, higher sensitivity and selectivity.

  6. Determination of three synthetic sweeteners in fruits by ultra pressure liquid chromatography-mass spectrometry%超高压液相色谱-质谱法测定水果中添加的3种人工合成甜味剂

    Institute of Scientific and Technical Information of China (English)

    曾绍东; 杜海群; 郭宏斌; 王明月; 查玉兵

    2013-01-01

    Objective To establish a method for the determination of three synthetic sweeteners(sodium cyclamate, saccharin sodium, and acesulfame) in fruits by ultra-high pressure liquid chromatography-mass spectrometry (UPLC-MS/MS). Methods The synthetic sweeteners were extracted with water, separated on a reversed phase C18 column using acetonitrile-0.02mol/L ammonium acetate as mobile phase, and then detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode. Results The method showed a good linearity for all the analysts over the range of 10~600μg/L with r≥0.995. The detection limits of sodium cy-clamate, saccharin sodium and acesulfame were 0.8、5.0 μg/kg and 1.0 μg/kg, respectively. The recoveries ranged from 74.9% to 111.2% at two spiked concentrations with the relative standard deviations lower than 8%.Conclusion This established method has the advantages of easy to operate, fast to perform, with high sensitivity and accuracy, and it is suitable for detection of sodium cyclamate, saccharin sodium and acesulfame in fruits.%  目的建立水果中3种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱(UPLC-MS/MS)检测方法.方法以反相C18柱为色谱柱,乙腈−0.02 mol/L乙酸铵溶液为流动相,样品经纯水提取后用色谱柱进行分离,串联质谱负离子多反应监测(MRM)模式测定.结果3种人工合成甜味剂在10~600μg/L范围内响应峰面积和样品质量浓度之间有良好的线性关系(相关系数r≥0.995);甜蜜素、糖精钠和安赛蜜的最低检出限分别为0.8、5.0、1.0μg/kg;在2种添加水平下,样品平均回收率为74.9%~111.2%,相对标准偏差<8%.结论该方法前处理简单,分析时间短,具有良好的灵敏度和准确性,可用于水果中甜蜜素、糖精钠、安赛蜜的同时检测.

  7. Simultaneous Determination of 34 Pesticide Residues in Vegetable Oil by QuEChERS-on-line Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry%QuEChERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留

    Institute of Scientific and Technical Information of China (English)

    阮华; 荣维广; 宋宁慧; 吉文亮; 刘华良; 马永建

    2014-01-01

    A method for the simultaneous determination of 34 pesticides in sunflower oil, soybean oil and corn oil was developed. The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry ( GPC-GC-MS ) . The linear range was from 0 . 01 to 0 . 2 mg/L with a good correlation coefficients ( r≥0. 9913). The average recoveries of 31 pesticides (except p,p′-DDE, p,p′-DDD, p,p′-DDT. For detail, please reference to section 3 . 6 ) ranged from 70 . 3% to 115 . 4%, 69 . 5% to 112 . 6% and 70 . 2% to 116 . 1%spiked at 0. 05 μg/g and 0. 1 μg/g with the relative standard deviations (RSDs, n=6) less than 13. 3%, 13. 5% and 12. 1% in sunflower oil, soybean oil and corn oil samples, respectively. The LODs of this method ranged from 0. 0692 to 2. 28, 0. 0559 to 2. 01 and 0. 0584 to 2. 14μg/kg (S/N=3) in sunflower oil, soybean oil and corn oil samples respectively. The convenient operation and versatility of this method are suitable for the fast screening and detection of 34 pesticide residues in sunflower oil, soybean oil and corn oil.%建立了葵花油、大豆油和玉米油中34种中高毒农药的快速筛查方法。样品采用改进的QuEChERS方法进行提取净化,提取液采用在线GPC-GC-MS检测。结果表明,34种农药在0.01~0.2 mg/L范围内具有良好的线性关系,相关系数为0.9913~0.9997。除p,p′-DDE, p,p′-DDD, p,p′-DDT外的31种农药在葵花油、大豆油和玉米油中的检出限分别为0.0692~2.28μg/kg,0.0559~2.01μg/kg,0.0584~2.14μg/kg;在0.05和0.1μg/g添加水平的平均回收率分别为70.3%~115.4%,69.5%~112.6%,70.2%~116.1%;相对标准偏差(RSD, n=6)分别为2.9%~13.3%,3.9%~13.5%,4.2%~12.1%。本方法具有操作便捷、快速等特点,适用于葵花油、大豆油和玉米油中34种农药残留的快速筛查与检测。

  8. Determination of plasticizers included in balloon by solid phase microextraction and gas chromatography with mass spectrometric detection.

    Energy Technology Data Exchange (ETDEWEB)

    Park, H.M.; Kim, J.H.; Ryu, J.Ch.; Kim, Y.M.; Lee, K.B. [Korea Institute of Science and Technology, Seoul (Korea)

    2001-02-01

    Solid-phase microextraction (SPME) with 85 {mu}m polyacrylate fiber, coupled to gas chromatography-mass spectrometry was used to analyze the plasticizers contained in balloon samples. The balloons were identified to be made of polyisoprene by IR spectroscopy. The plasticizers extracted from the balloon samples soaked in acetone-added water solvent for an hour were quantified by external standard method using nine kinds of plasticizers. The quantification method was validated for standard plasticizers in the range of 0.25-25 {mu}g/g. The detection limits were 0.11-0.38 {mu}g/g for different plasticizers. The RSDs for the reproducibility of this quantitation method were 3.7-14.2%. A few of balloons included risky level of plasticizer concerned as an endocrine disrupter, and it is necessary to regulate these products. (author). 10 refs., 3 tabs., 4 figs.

  9. Instrumental modification intended to save time, and volumes of sample and reagent solutions, in the atomic fluorescence spectrometric determination of mercury.

    Science.gov (United States)

    Pérez-Sirvent, Carmen; Martínez-Sánchez, María J; García-Lorenzo, Mariluz; López-García, Ignacio; Hernández-Córdoba, Manuel

    2007-05-01

    Use of small membrane pumps, instead of peristaltic pumps, to introduce sample and reagent solutions into the spectrometer has several advantages in atomic fluorescence spectrometric determination of mercury. This simple modification results in a substantial saving in the time required for the measurements and so 90% of reagent solution volumes and 95% of sample solution volumes are saved, with a consequent decrease in the volume of waste generated. The sampling frequency is almost tripled, with no deterioration in sensitivity, which is similar to that obtained by use of peristaltic pumps. The relative standard deviation for ten consecutive measurements of a 1 microg L-1 mercury solution was approximately 2%. PMID:17351707

  10. Simultaneous Determination of 1,2-Propylene Glycol,Glycerol and Triethylene Glycol in Smokeless Tobacco Products by Gas Chromatography-Mass Spectrometry%GC/MS法同时检测无烟气烟草制品中的1,2-丙二醇、丙三醇和三甘醇

    Institute of Scientific and Technical Information of China (English)

    张杰; 李鹏; 孙世豪; 宋瑜冰; 谢剑平; 宗永立

    2011-01-01

    A gas chromatography-mass spectrometry (GC/MS) method under selected ion monitoring (SIM) mode was developed for the simultaneous determination of 1,2-propylene glycol, glycerol and triethylene glycol in smokeless tobacco products (STPs) by using 1 ,4-butanediol as an internal standard.Thirty STP samples were parallel tested by GC/MS/SIM and GC/FID, a CORESTA recommended method, and the results were compared.The results showed that; 1 ) The recoveries of 1,2-propylene glycol, glycerol and triethylene glycolranged from 89.3% to 100.3% with the limits of detection of 1.25 to 2.75 μg/g and RSDs of 1.16 % to 4.37%.2) The contents of 1 ,2-propylene glycol, glycerol, and triethylene glycol in the samples ranged from 0.011 to 40.817, 0.024 to 39.044, 0.012 to 0.099 mg/g, respectively.3) 1,2-propylene glycol in 13 samples and glycerol in 14 samples were detected, and their contents in 9 of the samples were accurately determinable, however, triethylene glycol was undetectable in all samples by GC/FID.4) 1 ,2-propylene glycol in 29 samples, glycerol in 28 samples and triethylene glycol in 21 samples were detected, their contents in 16, 25 and 11 of the samples could be accurately determined by GC/MS/SIM method, respectively.5) The Pearson correlation coefficients between the contents of 1,2-propylene glycol in 13 samples and glycerol in 9 samples determined by GC/FID and GC/MS/SIM were over 0.99 probable value less than significant level of 0.05 and paired test t value over significant level of 0.05.It was concluded that the target analytes in the samples determined by GC/MS/SIM agreed with those by GC/FID, however, GC/MS/SIM method was more sensitive and accurate.GC/MS/SIM method is more suitable for the qualitative and quantitative determination of 1 ,2-propylene glycol, glycerol, and triethylene glycol in smokeless tobacco products.%为了准确测定无烟气烟草制品中保润剂的含量,以1,4-丁二醇为内标建立了同时检测无烟气烟草制品中1

  11. Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all r...

  12. Determination of burnup balance for nuclear reactor fuel on the basis of γ-spectrometric determination of fission products

    International Nuclear Information System (INIS)

    Results are given of experimental investigations in one of the versions of the method for determination of the balance of nuclear fuel burnup process by means of the γ-spectrometry of fission products. In the version being considered a balance of the burnup process was determined on the base of 106Ru, 134Cs.Activity was measured by means of a γ-spectrometer with Ge counter. Investigations were done on the natural uranium metal fuel from the heavy-water moderated reactor of the first Czechoslovakian nuclear power plant A1 in Yaslovske Bohunice. Possibility was checked of determination of the fuel burnup depth as well as of the isotope ratio and content of plutonium. Results were compared with the control data which had been obtained on the base of the mass-spectrometry of U, Pu and Nd. The reasors for deviations were estimated in the cases when they were greater tan error in the control data

  13. Mass spectrometric analysis of isotope effects in bioconversion of benzene to cyclohexanone

    Science.gov (United States)

    Nam, In-Hyun; Murugesan, Kumarasamy; Kim, Young-Mo; Yang, In-Hee; Chang, Yoon-Seok

    2006-06-01

    Pseudomonas veronii strain PH-03 has been shown to convert benzene to cyclohexanone through phenol. Mass spectrometry results revealed that unusual isotopic effects have been occurred in the transformation product, cyclohexanone. The isotopic composition was strongly depends on the compound specific hydrogen or oxygen source. The exchange of labile deuterium atoms has been investigated through electrospray ionization liquid chromatography mass spectrometry. The mass spectrometric analysis of biotransformation products enabled the proposal of a corresponding bioconversion pathway.

  14. 加速溶剂萃取凝胶渗透色谱/固相萃取净化气相色谱质谱法测定咸鱼中有机磷农药残留%Determination of Organophosphate Pesticide Residues in Salt Fish Using Accelerated Solvent Extraction and Gel Permeation Chromatography/Solid Phase Extraction with Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王耀; 刘少彬; 谢翠美; 张汉霞; 卢伟华

    2011-01-01

    建立了咸鱼中有机磷农药残留的分析方法.乙腈为溶剂,样品经ASE萃取,提取液用凝胶渗透色谱除去脂类、蛋白质和大部分的色素,再经Carb/PSA小柱净化.采用GC-MS定性分析,GC-FPD定量分析.加标水平为0.05~0.20mg/kg时,农药的回收率为64.5%~98.6%,相对标准偏差2.7%~14.7%.方法的检出限为0.6~9.0μg/kg(以3倍性噪比计).本方法具有提取效率高,净化效果好,回收率高,准确灵敏等优点,适用于咸鱼中农药残留检测实际工作的需要.%A novel method for the determination organophosphrous pesticides residues in salt fish was established. The target anslytes were extracted by accelerated solvent extraction (ASE) using acetonitrile as the extraction solvent. The gel permeation chromatography was used to remove the grease,protein and pigment and then, the small molecule compounds in the extracted solution were purified by the Carb/PSA solid phase extraction. The qualitative analysis were performed by using mass spectrometric detection GC-MSD(SIM) and quantitative analysis by GC-flame photometry detector(FPD) method. The average recoveries of organophosphrous pesticides were 64.5%-98.6%, spiked at 0.05 -0.20mg/kg levels. The relative standard deviations for all the compounds were 2.7%-14. 7%.The detection limit of the method varied between 0. 0006-0. 0090 mg/kg. The method is rapid, precise, sensitive, high efficient. It can be applied to the routine analysis for organophosphrous pesicide resdues in salt fish.

  15. Analysis of endogenous aldehydes in human urine by static headspace gas chromatography-mass spectrometry.

    Science.gov (United States)

    Serrano, María; Gallego, Mercedes; Silva, Manuel

    2016-03-11

    Endogenous aldehydes (EAs) generated during oxidative stress and cell processes are associated with many pathogenic and toxicogenic processes. The aim of this research was to develop a solvent-free and automated analytical method for the determination of EAs in human urine using a static headspace generator sampler coupled with gas chromatography-mass spectrometry (HS-GC-MS). Twelve significant EAs used as markers of different biochemical and physiological processes, namely short- and medium-chain alkanals, α,β-unsaturated aldehydes and dicarbonyl aldehydes have been selected as target analytes. Human urine samples (no dilution is required) were derivatized with O-2,3,4,5,6-pentafluorobenzylhydroxylamine in alkaline medium (hydrogen carbonate-carbonate buffer, pH 10.3). The HS-GC-MS method developed renders an efficient tool for the sensitive and precise determination of EAs in human urine with limits of detection from 1 to 15ng/L and relative standard deviations, (RSDs) from 6.0 to 7.9%. Average recoveries by enriching urine samples ranged between 92 and 95%. Aldehydes were readily determined at 0.005-50μg/L levels in human urine from healthy subjects, smokers and diabetic adults.

  16. Determination of 10 Plant Growth Regulators in Bean Sprouts by Sequential Cleaning-Gas Chromatography-Mass Spectrometry%分级净化结合气相色谱-质谱联用法测定豆芽中10种植物生长调节剂

    Institute of Scientific and Technical Information of China (English)

    吴平谷; 王天娇; 谭莹; 张晶; 王立媛; 汤鋆; 姜维; 潘晓东; 马冰洁; 倪竹南

    2014-01-01

    建立了豆芽10种植物生长调节剂的分级净化体系,采用气相色谱质谱法(GC/ MS)对该体系的效果进行了评价。豆芽先用酸性乙腈提取,浓缩后用甲醇复溶,部分经 QuECHERS 试剂盒净化后用 GC/ MS 分析2,4-D-乙酯2,4-D-丁酯。另一部分经 MCS 固相萃取柱净化,先用5 mL 甲醇洗脱得组分1,再用5%氨化甲醇洗脱得组分2;组分1浓缩后用10%三氟化硼甲醇溶液甲酯化,提取后 GC/ MS 测定4-氯苯氧乙酸、α-萘乙酸、2,4-二氯苯氧乙酸、吲哚乙酸、吲哚丁酸,组分2浓缩后用 GC/ MS 测定多效唑、激动素、6-苄基腺嘌呤。采用此净化体系对可以对不同性质的植物生长调节剂进行有效净化。结果表明,本方法完全可以用于豆芽中10种植物生长调节剂残留的检测,在豆芽中的添加0.01~0.1 mg/ kg,10种植物生长调节剂平均回收率范围为70.5%~93.2%,RSD 为5.2%~12.3%,本方法对10种植物生长调节剂的定量限(S/ N≥10)为0.01~0.025 mg/ kg,检出限(S/ N≥3)为0.003~0.008 mg/ kg。此净化体系简便、快速、准确,结合 GC/ MS 可以满足豆芽中植物生长调节剂多残留检测要求。%A sequential clean-up method was developed for the quantification of 10 plant growth regulators in bean sprout by the gas chromatography / mass spectrometry (GC / MS). The analytes were firstly extracted by the acided acetonitrile. Extraction was concentrated and re-dissovled by methanol. Then, it was divided to two aliquots. One of that was analyzed for 2,4-D-butyl ester and 2,4-D-ethyl ester after the purification by QuECHERS cartridge. Another one was treated by MCS solid phase extraction column including diverse eluting steps. After eluting by 5 mL methanol, composition 1 was obtain, concentrated, and methyl esterified by 10% boron trifluoride methanol solution. The treated extract was used for the determination of 4-chlorophenoxy acetic acid, β-naphthyl acetic acid, 2,4-dichlorophenoxy acetic acid, indole

  17. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  18. Potential of needle trap microextraction-portable gas chromatography-mass spectrometry for measurement of atmospheric volatile compounds

    Science.gov (United States)

    Feijó Barreira, Luís Miguel; Xue, Yu; Duporté, Geoffroy; Parshintsev, Jevgeni; Hartonen, Kari; Jussila, Matti; Kulmala, Markku; Riekkola, Marja-Liisa

    2016-08-01

    Volatile organic compounds (VOCs) play a key role in atmospheric chemistry and physics. They participate in photochemical reactions in the atmosphere, which have direct implications on climate through, e.g. aerosol particle formation. Forests are important sources of VOCs, and the limited resources and infrastructures often found in many remote environments call for the development of portable devices. In this research, the potential of needle trap microextraction and portable gas chromatography-mass spectrometry for the study of VOCs at forest site was evaluated. Measurements were performed in summer and autumn 2014 at the Station for Measuring Ecosystem-Atmosphere Relations (SMEAR II) in Hyytiälä, Finland. During the first part of the campaign (summer) the applicability of the developed method was tested for the determination of monoterpenes, pinonaldehyde, aldehydes, amines and anthropogenic compounds. The temporal variation of aerosol precursors was determined, and evaluated against temperature and aerosol number concentration data. The most abundant monoterpenes, pinonaldehyde and aldehydes were successfully measured, their relative amounts being lower during days when particle number concentration was higher. Ethylbenzene, p- and m-xylene were also found when wind direction was from cities with substantial anthropogenic activity. An accumulation of VOCs in the snow cover was observed in the autumn campaign. Results demonstrated the successful applicability of needle trap microextraction and portable gas chromatography-mass spectrometry for the rapid in situ determination of organic gaseous compounds in the atmosphere.

  19. Determination of Volatile Flavor Compounds of Shrimp Head by Headspace Solid Phase MicroextractionGas Chromatography-Mass Spectrometry%顶空固相微萃取-气相色谱-质谱法测定北极虾虾头的挥发性成分

    Institute of Scientific and Technical Information of China (English)

    解万翠; 杨锡洪; 章超桦; 吉宏武; 张丽风

    2011-01-01

    For determination the volatile flavor compounds of sweet shrimp heads (P. Borealis), solid phase microextraction-gas chromatography-mass spectrometry was used to separate and identify, then standards of hydrocarbons of C5 -C20 were adapted to verify by Kovats retention index (RI), finally, the standard compounds of unknown were analyzed to confirm these identifications. Based on these, 62 kinds of volatile compounds in shrimp heads (P. Borealis) were analyzed by qualitative and semi-quantitative method, in which include 18 hydrocarbons (27. 98%), 6 alcohols (9. 57%), 14 ketones (21. 93%), 5 esters (13. 20%), 8 aldehydes (2. 86%), 1 furan compound (0. 41%), 4 nitrogenous compounds (19.58%), 1 sulphurs (0. 71%), and 4 unknowns (3. 76%). Considering the threshold perception and odour active values, ketones of (E,Z) 3,5-octadien-2-one, (E,E) 3,5-octadien-2-one, 1-penten-3-one, 3-penten-2-one (E), and 6-methyl-2-heptanone that have sweet, fresh mushroom flavor were identified as the key compounds for the shrimp head flavor. Esters (ethyl acetate) and alcohols (1-penten-3-ol, 1-octen-3-ol, and 2-ethyl-1-hexanol) have high contribution to shrimp head flavor too. Moreover, the high concentration of nitrogenous compounds such as trimeth-ylamine can cause a fishy flavor of shrimp head. The results indicated that by combining with GC-MS, RI and standard confirm, the credibility of the data increased. The SPME-GC-MS method could be used as a reference for analysis of complicated volatile flavor of aquatic products.%为了测定北极虾(P.Borealis)虾头中的挥发性风味成分,采用顶空固相微萃取-气相色谱-质谱(HS-SPME-GC-MS)分离及初步鉴定,以C5~C20正构烷烃系列标准品进行Kovats保留指数(Rentention index,RI)验证,在此基础上利用未知物标准品匹配法最终确证.对虾头中的62种挥发性化合物进行了定性及半定量分析,主要有烃类18种(27.98%)、醇类6种(9.57%)、酮类14种(21.93%)、脂类5种(13.20

  20. Determination of potential carcinogenic and genotoxic sulfonate impurities in imatinib mesylate by a highly sensitive liquid chromatography-mass spectrometry method%LC-MS法同时检测甲磺酸伊马替尼中3个磺酸酯基因毒杂质

    Institute of Scientific and Technical Information of China (English)

    冯慧敏; 杭太俊; 高新桃; 崔浩; 龚心实; 张斐; 肖柏明

    2014-01-01

    Objective:To determine three sulfonic acid esters,methyl methanesulfonate (MMS),ethyl methanesulfonate (EMS),and isopropyl methanesulfonate (IPMS),known as potential carcinogenic and genotoxic impurities in imatinib mesylate by liquid chromatography-mass spectrometry (LC-MS).Methods:The separation was carried out on a Poroshell SB-C18 column (2.7 μm,4.6 mm × 100 mm) with the mobile phase consisting of 10 mmol · L-1 ammonium formate containing O.1% (V/V) formic acid (A) and methanol (B) by gradient elution [0min(80% A-20% B) →5 min (10% A-90% B) →10 min (10% A-90% B) → 10.5 min (80% A-20% B) →18.5 min(80% A-20% B)] at a flow rate of 0.4mL · min-1 The results of quadrupole mass spectrometer was equipped with an ESI (in the positive mode).The conditions were as follows:nitrogen drying gas with nebulizer pressure of O.3 MPa,the flow rate of 10 L · min-1,the temperature of 300 ℃,the capillary voltage of 3 kV and the fragmentation voltage of 30 V.Results:The results of limit of quantification (LOQ) of MMS,EMS and IPMS were 10 ng· mL-1,5 ng · mL-1 and 10 ng· mL-1,respectively.Recoveries of MMS,EMS and IPMS were 99.86%,101.7% and 103.8%,respectively.The linear calibration curves of MMS and IPMS were obtained over the concentration range of 10-100 ng· mL-1,while the curve of EMS over 5-50 ng· mL-1.Conclusion:The methodology validation showed that this LC-MS method is useful as a quality control method for the simultaneous trace analysis of MMS,EMS and IPMS in imatinib mesylate.%目的:建立LC-MS法对甲磺酸伊马替尼原料中的3个磺酸酯基因毒杂质一甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)、甲磺酸异丙酯(IPMS)进行定量检测.方法:选用Agilent Poroshell 120 SB-C18色谱柱(2.7 μm,4.6 mm×100 mm),以10mmol·L-甲酸铵(含0.1%甲酸)为流动相A,甲醇为流动相B,梯度洗脱[0 min(80%A-20%B)→5 min(10%A-90%B)→10 min(10%A-90%B)→10.5 min(80%A-20%B)→18.5 min(80%A-20

  1. Determination of 2-methylisoborneol and geosmin in drinking water using headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry%顶空固相微萃取-气相色谱-质谱联用测定饮用水中的2-甲基异莰醇和土臭素

    Institute of Scientific and Technical Information of China (English)

    成建国; 刘开颖; 白敏冬; 程超; 余忆玄; 周新颖

    2015-01-01

    2-甲基异莰醇(2-methylisoborneol,2-MIB)和土臭素(geosmin,GSM)在水源水中大量分泌排放是造成饮用水土霉异味突发事件、引发居民用水恐慌的重用因素之一。使用顶空固相微萃取( HS-SPME)与气相色谱-质谱联用技术( GC-MS)建立了水库水、水库附近土壤、居民自来水中2-MIB 和 GSM 的测定方法。结合正交分析优化了加盐量、萃取温度、萃取时间条件,在电子轰击( EI)-选择离子扫描( SIM)模式下进行了目标物的定性定量分析。结果表明:在5~1000 ng/L 范围内,2-MIB 和 GSM 的色谱峰面积与其质量浓度的线性关系良好( r2≥0.998),2-MIB与 GSM的检出限分别为0.72 ng/L和0.34 ng/L,定量限分别为2.40 ng/L 和1.13 ng/L;目标物加标水平为10~600 ng/L时,平均回收率为93.6%~107.7%,相对标准偏差( RSD)≤6.1%( n=6)。基于上述方法,对辽宁省某地区水库水、水库附近土壤、居民自来水中的目标物进行检测,结果表明:水库水目标物质量浓度范围为3.0~3.6 ng/L,水库附近土壤中提取的2-MIB为8.1 ng/L、提取的GSM为17.8 ng/L,居民自来水中的目标物未检出。该方法操作简便、准确可靠,灵敏度高,无需有机溶剂,适合于饮用水中2-MIB和 GSM的分析检测。%The odorous compounds of 2-methylisoborneol(2-MIB)and geosmin(GSM)heavi-ly produced and released in water source are one of the most important factors leading to off-flavor emergencies and resident water consumption panic in drinking water. A headspace solid phase micro-extraction ( HS-SPME ) combined with gas chromatography-mass spectrometry ( GC-MS)method was established for the simultaneous determination of these two trace earthy and musty compounds in reservoir water,reservoir soil and tap water. The conditions of HS-SPME,such as salt amount,extraction time and extraction temperature,were optimized based on

  2. Determination of Listeria Monocytogenes in Agricultural Products by-High Resolution Pyrolysis Gas Chromatography-Mass Spectrometry%高分辨热裂解气相色谱/质谱法快速定性检测农产品中的单增李斯特菌

    Institute of Scientific and Technical Information of China (English)

    苏靖; 李晓晶; 韦琰琰; 柳婷; 郭爱玲

    2013-01-01

    A method was developed for the qualitative determination of Listeria monocytogenes in the agricultural products by high resolution pyrolysis gas chromatography-mass spectrometry-selected ion monitoring (HPRGC/MS-MIS) technology. The method was accurate, highly sensitive and easy to operate. The operation conditions of HRPGC/MS system were as follows; pyrolysis conditions were as follows; starting temperature was 50 t , heating rate was 20℃/min, the temperature of the pyrolysis room was 230 ℃, and pyrolysis temperature was 650 ℃ for 10 s. Gas chromatography was accomplished with a carrier gas of helium at a flow rate of 0.9 ml/min. The GC column was a DB-WAXTER capillary column. The GC column temperature initially was kept at 45℃ for 4 min, then programmed to 100 ℃ at 6 t/min, 200 ℃ at 10 t/min, 250 ℃ at 12 ℃/min and held for 25 min. The total flow rate was spilt at ratio of 50 to 1. EI was used as ion source. The retention time of 19.056 min was selected for SIM, the ions of m/z were 54, 98. L. monocytogens, two kinds of agricultural products with and without L. monocytogens samples were evaluated by this method according to the characteristics of the selected ion of L. monocytogens. An expected result was observed using the HRPGC/ MS to detect L. monocytogens in different kinds of food, cucumber and beef. This method does not need the complex pre-treatment, the analysis time was comparatively short, and handing is easy for the operator. Retention time and mass spectra were used for qualitative analysis at the same time to eliminate the interference of different kinds of agricultural product impurities. The accurateness, good selectivity and reproducibility of the results demonstrate that HRPGC/MS is a useful method for rapid detection of L. monocytogens in agricultural products.%要在高分辨率热裂解气相色谱/质谱(HRPGC/MS)系统中采用选择离子检测法(SIM),建立了准确可靠、灵敏度高、快速简便的检测农产品中

  3. Multi-class method for biomonitoring of hair samples using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martín, Julia; Möder, Monika; Gaudl, Alexander; Alonso, Esteban; Reemtsma, Thorsten

    2015-11-01

    Currently, non-invasive biomonitoring of human exposure to organic pollutants bases upon the analysis mainly of urine and human breast milk. While mostly persistent organic pollutants are the center of interest, the aim of our study was to develop a method for the determination of different chemical classes of emerging pollutants (organophosphorus flame retardants, plastic additives such as phthalates, bisphenol A, insecticides, antimicrobials, preservatives and musk fragrances) in hair by gas chromatography-mass spectrometry. The preferred sample preparation included hydrolysis of the hair with trifluoroacetic acid in methanol followed by a liquid-liquid extraction using hexane/ethyl acetate. The validated method is characterized by recoveries higher than 77 % for most analytes, relative standard deviations below 16 % and limits of detection between 2 pg mg(-1) (HHCB) and 292 pg mg(-1) (propylparaben) using 50 mg of dry hair. After respective blank corrections, bis-(2-ethylhexyl)phthalate (DEHP) and the musk fragrance HHCB were the predominant compounds determined in all hair samples at concentrations between 32 and 59 ng mg(-1) and 0.8-13 ng mg(-1), respectively. The bactericide triclosan and the insect repellent N,N-diethyl-3-methylbenzamide (DEET) were detected in selected hair samples at 2 and 0.8 ng mg(-1), respectively. PMID:26427497

  4. Multi-class method for biomonitoring of hair samples using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Martín, Julia; Möder, Monika; Gaudl, Alexander; Alonso, Esteban; Reemtsma, Thorsten

    2015-11-01

    Currently, non-invasive biomonitoring of human exposure to organic pollutants bases upon the analysis mainly of urine and human breast milk. While mostly persistent organic pollutants are the center of interest, the aim of our study was to develop a method for the determination of different chemical classes of emerging pollutants (organophosphorus flame retardants, plastic additives such as phthalates, bisphenol A, insecticides, antimicrobials, preservatives and musk fragrances) in hair by gas chromatography-mass spectrometry. The preferred sample preparation included hydrolysis of the hair with trifluoroacetic acid in methanol followed by a liquid-liquid extraction using hexane/ethyl acetate. The validated method is characterized by recoveries higher than 77 % for most analytes, relative standard deviations below 16 % and limits of detection between 2 pg mg(-1) (HHCB) and 292 pg mg(-1) (propylparaben) using 50 mg of dry hair. After respective blank corrections, bis-(2-ethylhexyl)phthalate (DEHP) and the musk fragrance HHCB were the predominant compounds determined in all hair samples at concentrations between 32 and 59 ng mg(-1) and 0.8-13 ng mg(-1), respectively. The bactericide triclosan and the insect repellent N,N-diethyl-3-methylbenzamide (DEET) were detected in selected hair samples at 2 and 0.8 ng mg(-1), respectively.

  5. Development of liquid chromatography mass spectrometric methods for quantification of metabolites from cellular level to clinical biomarkers

    OpenAIRE

    Tohmola, Niina

    2015-01-01

    Metabolites are low molecular weight compounds participating in different functions of cellular systems. Metabolites can be used as diagnostic biomarkers for numerous diseases. Liquid chromatography tandem mass spectrometry (LC-MS/MS) is a powerful tool in quantification of metabolites from various sample matrices. Good sensitivity and specificity are the main benefits of the technique. Mass spectrometry is commonly used in industry, drug research and clinical diagnostics. Extensive validatio...

  6. Pyrolysis of Polytrimethylene Terephthalate (PTT) Fiber by Pyrolysis Gas Chromatography-Mass Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    QIAN He-sheng

    2007-01-01

    Pyrolysis of polytrimethylene terephthalate (PTT) fiber has been investigated by pyrolysis gas chromatography-mass spectroscopy in the temperature range from 400℃ to 750℃ in order to observe the possible effect of the temperature on its composition of pyrolysates. At 400℃, pyrolysis of molecular chain could occur, only 13 pyrolysates could be identified. The trimethylene moieties bound to the macromolecular core by ester bonds are cleaved at around 400℃. At 550℃ -750℃, pyrolysis of molecular chain could completely take place, 46 pyrolysates could be found. As the temperature increases, the compositions of pyrolysate are distinctly increased. Several compounds, especially benzoic acid, monopropenyl-p-phthalate, 2 - propenyl benzoate, di - 2 - propenyl ester, 1,4 -benzenedicarboxylic acid, benzene, 1, 5 - hexadiene, biphenyl and 1, 3 - propanediol dibenzoate could be formed. The thermal degradation mechanism, which is determined by structure and amount of the thermal decomposition products, are described. During pyrolysis of polytrimethylene terephthalate, polymeric chain scissions take place a peeling reaction as a successive removal of the dimer units from the polymeric chain. The chain scissions are followed by the elimination reaction, linkage action and secondary reactions, which bring about a variety fragment.

  7. A liquid chromatography-mass spectrometry approach to study "glucosinoloma" in broccoli sprouts.

    Science.gov (United States)

    Maldini, Mariateresa; Baima, Simona; Morelli, Giorgio; Scaccini, Cristina; Natella, Fausta

    2012-09-01

    Glucosinolates are an important class of secondary plant metabolites, possessing health-promoting properties. Young broccoli plants are a very good source of glucosinolates with concentrations several times greater than in mature plants. The aim of our study was to develop a liquid chromatography-mass spectrometry and liquid chromatography/tandem mass spectrometry qualitative and quantitative method for the measure of glucosinolates in broccoli sprouts. The described method provides high sensitivity and specificity, allowing a rapid and simultaneous determination of 14 glucosinolates. The proposed method has been validated for eight glucosinolates: glucobrassicin, glucoraphanin, glucoiberin, glucoerucin, progoitrin, gluconapin, sinigrin and glucocheirolin. The linear range was 1-150 µg ml(-1), the intra-day and inter-day precision values are within 6% and 8% at the lower limit of quantification, while the overall recovery of the eight glucosinolates was 99 ± 9%. This validated method was used successfully for analysis of glucosinolates content of broccoli sprouts grown in different conditions.

  8. Recent progress in polar metabolite quantification in plants using liquid chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Zhiqian Liu; Simone Rochfort

    2014-01-01

    Metabolite analysis or metabolomics is an impor-tant component of systems biology in the post-genomic era. Although separate liquid chromatography (LC) methods for quantification of the major classes of polar metabolites of plants have been available for decades, a single method that enables simultaneous determination of hundreds of polar metabolites is possible only with gas chromatography-mass spectrometry (GC-MS) techniques. The rapid expansion of new LC stationary phases in the market and the ready access of mass spectrometry in many laboratories provides an excellent opportunity for developing LC-MS based methods for multi-target quantification of polar metabolites. Although various LC-MS methods have been developed over the last 10 years with the aim to quantify one or more classes of polar compounds in different matrices, currently there is no consensus LC-MS method that is widely used in plant metabolomics studies. The most promising methods applicable to plant metabolite analysis wil be reviewed in this paper and the major problems encountered highlighted. The aim of this review is to provide plant scientists, with limited to moderate experience in analytical chemistry, with up-to-date and simplified information regarding the current status of polar metabolite analysis using LC-MS techniques.

  9. Metabolic Fingerprinting of Three Malaysian Ginger (Zingiber officinale Roscoe Using Gas Chromatography-Mass Spectromertry

    Directory of Open Access Journals (Sweden)

    H. J. Mahdi

    2010-01-01

    Full Text Available Problem statement: There is a chemical variation among different ginger cultivars detected by previous studies including the volatile and non-volatile oleo-resins. In this study we try to determine whether these variations are related to a genetic factor rather than environmental or intrinsic factors. Approach: A comprehensive metabolic fingerprinting from the leaves of three micro-propagated ginger cultivars Bukit Tinggi, Tanjung Sepat and Sabah was performed using a Gas Chromatography-Mass Spectrometry (GC-MS. Constituents of the ginger leaves were first extracted and then fractionated into methanolic and chloroform. The samples were subsequently methoximated and silylated prior to GC-MS analysis. Results: By applying this technique, we detected more than 300 compounds (polar and non-polar in total originated from each ginger cultivar. Based on the GC-MS fragmentation, three different classes of metabolites were detected from the ginger cultivars, namely amino acids, carbohydrates and organic acids. A qualitative variation on the type of ginger metabolites was observed, albeit no marked different found in the level of the metabolites. Conclusion: Apparently the chemical variations among the three ginger cultivars were due to genetic effects since almost all other environmental and intrinsic factors were eliminated.

  10. Presence of phthalate esters in intravenous solution evaluated using gas chromatography-mass spectrometry method.

    Science.gov (United States)

    Strac, Ivona Vidić; Pušić, Maja; Gajski, Goran; Garaj-Vrhovac, Vera

    2013-03-01

    Di-(2-ethylhexyl) phthalate (DEHP) is a plasticizer widely used in the production of poly-(vinyl) chloride (PVC) materials. It is a reproductive and developmental toxicant in animals and a suspected endocrine modulator in humans. DEHP is not covalently bound within the PVC molecule, which is why migration into a suitable medium can be expected. Since application of infusion solutions is one of the most common medical treatments, the objective of this study was to determine the migration of phthalates from softened PVC storage bags into infusion solution in different time periods within one year from date of production using a gas chromatography-mass spectrometry method. The measured values of DEHP ranged between 0.22 and 14.00 µg l(-1) , but the unexpected presence of other phthalate esters was also detected. It was concluded that values obtained in infusion solutions match the reference data and represent a minor risk for the patient. The presence of other phthalate esters leads to the conclusion that the pharmacopeic requirement for polymer cleanness was not fully met. Since phthalate esters are among the most extensively used industrial chemicals and are widely distributed in the environment, special precautions and further monitoring should be conducted to minimize any possible health risks. PMID:22034089

  11. Comparison of motor oils using high-temperature gas chromatography-mass spectrometry.

    Science.gov (United States)

    Reardon, Michelle R; Allen, Lance; Bender, Edward C; Boyle, Katherine M

    2007-05-01

    The analysis of motor oils has wide applications in the forensic science field from comparing lubricants transferred between an automobile and a victim or crime scene to differentiating the compositions of plastic explosives. In this study, 40 unused motor oils were analyzed and compared by high-temperature gas chromatography-mass spectrometry to determine the potential for oil individualization. Oil samples were also collected from the crankcase dipsticks of 30 cars. Twenty-six of these oils could be differentiated from each other based on visual comparisons of the unresolved envelope (baseline rise due to incomplete separation) and the resolved hydrocarbons in the raw total ion chromatograms (TICs) and smoothed TIC data. Four of these oils were analyzed as unknowns and were correctly related to the corresponding vehicle. The use of extracted ion profiles (EIPs) was explored as a means to further discriminate between the indistinct samples based on the polycyclic aromatic hydrocarbon (PAH) content. The research discussed in this paper demonstrated that differentiation of motor oils was possible by examining the TIC, smoothed TIC, and EIP data. PMID:17456092

  12. Quantification of busulfan in plasma by gas chromatography-mass spectrometry following derivatization with tetrafluorothiophenol.

    Science.gov (United States)

    Quernin, M H; Poonkuzhali, B; Montes, C; Krishnamoorthy, R; Dennison, D; Srivastava, A; Vilmer, E; Chandy, M; Jacqz-Aigrain, E

    1998-05-01

    A specific and highly sensitive method has been developed for the determination of busulfan in plasma by gas chromatography-mass spectrometry using a deuterium-labeled busulfan (busulfan-d8) as internal standard. Plasma containing busulfan and busulfan-d8 were extracted with ethyl acetate and derivatized with 2,3,5,6-tetrafluorothiophenol prior to the monitoring of specific ions. The limit of quantification of the assay was 20 ng/ml and the calibration curve was linear over the range of 10 to 2000 ng/ml of derivatized busulfan. This method was in good agreement with the GC-MS assay using derivatization with sodium iodide and measuring diiodobutane. In addition, a pharmacokinetic study of busulfan was conducted in six children. The apparent oral clearance was 5.7+/-1.9 ml/kg/min and the volume of distribution was 1.0+/-0.4 l/kg and were similar to those previously reported in pediatric patients.

  13. Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

    Science.gov (United States)

    Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn M.

    2000-01-01

    A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

  14. Solid-phase extraction-gas chromatography and solid-phase extraction-gas chromatography-mass spectrometry determination of corrosion inhibiting long-chain primary alkyl amines in chemical treatment of boiler water in water-steam systems of power plants.

    Science.gov (United States)

    Kusch, Peter; Knupp, Gerd; Hergarten, Marcus; Kozupa, Marian; Majchrzak, Maria

    2006-04-28

    Gas chromatography with simultaneous flame-ionization detection (FID) and a nitrogen-phosphorus detection (NPD) as well as gas chromatography-mass spectrometry (GC/MS) has been used to characterize long-chain primary alkyl amines after derivatization with trifluoroacetic anhydride (TFAA). Electron impact ionization- (EI) and negative chemical ionization (NCI) mass spectra of trifluoroacetylated derivatives of the identified tert-octadecylamines are presented for the first time. The corrosion inhibiting alkyl amines were applied in a water-steam circuit of energy systems in the power industry. Solid-phase extraction (SPE) with octadecyl bonded silica (C18) sorbents followed by gas chromatography were used for quantification of the investigated tert-octadecylamines in boiler water, superheated steam and condensate samples from the power plant. The estimated values were: 89 microg l(-1)(n = 5, RSD = 7.8%), 45 microg l(-1) (n = 5, RSD = 5.4%) and 37 microg l(-1)(n = 5, RSD = 2.3%), respectively. PMID:16483586

  15. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

    DEFF Research Database (Denmark)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin;

    2014-01-01

    This paper reports an analytical method for the determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation......, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference...... values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of 239+240Pu by alpha spectrometry agreed very well with the sum of 239Pu and 240Pu measured by ICP-MS. ICP-MS can not only measure 239Pu and 240Pu separately but also 241...

  16. Determination of Typical Odorous Compounds in Water Using Purge-and-trap Gas Chromatography-Mass Spectrometry Combined with Stable Isotope Dilution%稳定性同位素稀释吹扫捕集-气质联用法测定水中典型臭味物质

    Institute of Scientific and Technical Information of China (English)

    许冬梅; 许俊鸽; 苑宝玲; 吕华东; 林麒

    2011-01-01

    A stable isotope dilution technique based on purge-and-trap coupled to gas chromatography with mass spectrometric detection was developed and optimized for the trace determination of the typical odorous compounds, geosmin (GSM) and 2-methylisoborneol (MIB). The selection of quantitation ions and the factors of temperature program, the sample purge temperature, salt content on the extraction of odorous compounds were studied. Under the experimental conditions, the optimal operating conditions were the addition of 20% (m/V) NaC1, purging at 60 ℃ on the temperature program of 5 ℃/min. D5-Geosmin and d3-MIB as the isotopes internal standards were added to improve the stability of recovery. Using this method, both the calibration curves of MIB and GSM were good linear correlation in the range of 5-500 ng/L. Recoveries were 82 %-95 % for GSM and 99%-101% for MIB, and precision was 5.2% for GSM and 0.8% for MIB. The limits of detection for GSM and MIB were 3.6 and 4.1 ng/L, respectively.%采用稳定性同位素稀释吹扫捕集-气相色谱/质谱联用法测定水中典型臭味物质土臭素(GSM)和2-甲基异莰醇(MIB).研究了特征离子、升温程序、样品吹扫温度及盐浓度等因素对臭味物质萃取过程的影响.本实验测定臭味物质的最佳条件为:盐浓度20%(m/V),样品吹扫温度60℃,程序升温速率5℃/min.通过加人同位素内标d5-GSM和d3-MIB,可以提高样品回收率的稳定性.土臭素(GSM)和2-甲基异莰醇(MIB)浓度在5~500 ng/L,范围内线性良好;在100 ng/L加标浓度水平下,GSM和MIB回收率范围分别为82%~95%和99%~101%;相对标准偏差为5.20%和0.78%.方法检出限分别为3.60和4.12 ng/L.本方法操作简单、快速、准确,用于实际水样的检测效果良好.

  17. Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Multielement instrumental neutron activation (INAA), inductively coupled plasma-atomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses were utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth, respectively. (author)

  18. Determination of sulfadiazine, trimethoprim, and N(4) -acetyl-sulfadiazine in fish muscle plus skin by Liquid Chromatography-Mass Spectrometry. Withdrawal-time calculation after in-feed administration in gilthead sea bream (Sparus aurata L.) fed two different diets.

    Science.gov (United States)

    Zonaras, V; Tyrpenou, A; Alexis, M; Koupparis, M

    2016-10-01

    This study presents a depletion study for sulfadiazine and trimethoprim in muscle plus skin of gilthead sea bream (Sparus aurata L.). N(4) -acetyl-sulfadiazine, the main metabolite of sulfadiazine (SDZ), was also examined. The fish were held in seawater at a temperature of 24-26 °C. SDZ and trimethoprim (TMP) were administered orally with medicated feed for five consecutive days at daily doses of 25 mg SDZ and 5 mg TMP per kg of fish body weight per day. Two different diets, fish oil- and plant oil-based diets, were investigated. Ten fish were sampled at each of the days 1, 3, 5, 6, 8, 9, 10, and 12 after the start of veterinary medicine administration. However for the calculation of the withdrawal periods, sampling day 1 was set as 24 h after the last dose of the treatment. Fish samples were analyzed for SDZ, TMP, and acetyl-sulfadiazine (AcSDZ) residues by liquid chromatography-mass spectrometry. SDZ and TMP concentrations declined rapidly from muscle plus skin. Considering a maximum residue limit of 100 μg/kg for the total of sulfonamides and 50 μg/kg for TMP residues in fish muscle plus skin, the withdrawal periods of the premix trimethoprim-sulfadiazine 50% were calculated as 5 and 6 days, at 24-26 °C, in fish oil (FO) and plant oil (PO) groups, respectively. The investigation of this work is important to protect consumers by controlling the undesirable residues in fish. PMID:26987772

  19. Mass spectrometric immunoassay

    Science.gov (United States)

    Nelson, Randall W; Williams, Peter; Krone, Jennifer Reeve

    2007-12-04

    Rapid mass spectrometric immunoassay methods for detecting and/or quantifying antibody and antigen analytes utilizing affinity capture to isolate the analytes and internal reference species (for quantification) followed by mass spectrometric analysis of the isolated analyte/internal reference species. Quantification is obtained by normalizing and calibrating obtained mass spectrum against the mass spectrum obtained for an antibody/antigen of known concentration.

  20. Urine Mescaline Screening With a Biochip Array Immunoassay and Quantification by Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Battal, Dilek; Barnes, Allan J; Castaneto, Marisol S; Martin, Thomas M; Klette, Kevin L; Huestis, Marilyn A

    2015-12-01

    Mescaline, the primary psychoactive chemical in peyote cactus, has been consumed for thousands of years in ancient religious ceremonies. The US military wanted to determine if mescaline intake was a problem for personnel readiness. Twenty thousand seventeen urine specimens negative for cannabinoids, cocaine, opiates, and amphetamines were tested for mescaline with the Randox Drugs of Abuse V (DOA-V) biochip array immunoassay at the manufacturer's recommended cutoff of 6 mcg/L. A sensitive and specific method for mescaline quantification in urine was developed and fully validated. Extracted analytes were derivatized with pentafluoropropionic anhydride and pentafluoropropanol and quantified by gas chromatography-mass spectrometry (GC/MS) with electron impact ionization. Standard curves, using linear least squares regression with 1/x weighting, were linear from 1 to 250 mcg/L with coefficients of determination >0.994. Intra- and inter-assay imprecision was 90.4%. Mean extraction efficiencies were >92.0% across the linear range. This fully validated method was applied for the confirmation of urinary mescaline in 526 presumptive-positive specimens and 198 randomly selected presumptive-negative specimens at the manufacturer's 6 mcg/L cutoff. No specimen confirmed positive at the GC/MS limit of quantification of 1 mcg/L. Results indicated that during this time frame, there was insufficient mescaline drug use in the military to warrant routine screening in the drug testing program. However, mescaline stability, although assessed, could have contributed to lower prevalence. We also present a validated GC/MS method for mescaline quantification in urine for reliable confirmation of suspected mescaline intake.

  1. Impurity profiling of trinitrotoluene using vacuum-outlet gas chromatography-mass spectrometry

    NARCIS (Netherlands)

    Brust, H.; Willemse, S.; Zeng, T.; Asten, A. van; Koeberg, M.; Heijden, A.E.D.M. van der; Bolck, A.; Schoenmakers, P.

    2014-01-01

    In this work, a reliable and robust vacuum-outlet gas chromatography-mass spectrometry (GC-MS) method is introduced for the identification and quantification of impurities in trinitrotoluene (TNT). Vacuum-outlet GC-MS allows for short analysis times the analysis of impurities in TNT was performed in

  2. Incorporation of Gas Chromatography-Mass Spectrometry into the Undergraduate Organic Chemistry Laboratory Curriculum

    Science.gov (United States)

    Giarikos, Dimitrios G.; Patel, Sagir; Lister, Andrew; Razeghifard, Reza

    2013-01-01

    Gas chromatography-mass spectrometry (GC-MS) is a powerful analytical tool for detection, identification, and quantification of many volatile organic compounds. However, many colleges and universities have not fully incorporated this technique into undergraduate teaching laboratories despite its wide application and ease of use in organic…

  3. Characterization of typical chemical background interferences in atmospheric pressure ionization liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Guo, Xinghua; Bruins, Andries P.; Covey, Thomas R.

    2006-01-01

    The structures and origins of typical chemical background noise ions in positive atmospheric pressure ionization liquid chromatography/mass spectrometry (API LC/MS) are investigated and summarized in this study. This was done by classifying chemical background ions using precursor and product ion sc

  4. Datura stramonium poisoning. Identification of tropane alkaloids in urine by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Nogué, S; Pujol, L; Sanz, P; de la Torre, R

    1995-01-01

    A case of acute poisoning by ingestion of Datura stramonium infusion is reported. The patient presented with a typical anticholinergic syndrome (dryness of mouth, mydriasis, flushing, tachycardia, agitation, hallucinations) and was treated with symptomatic and supportive measures. The presence of tropane belladona alkaloids in a urine sample was demonstrated by gas chromatography-mass spectrometry. PMID:7601297

  5. Identification of Synthetic Polymers and Copolymers by Analytical Pyrolysis-Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

    An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In…

  6. Comparative analysis of essential oils found in Rhizomes Curcumae and Radix Curcumae by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Di-Ya Lu; Yan Cao; Ling Li; Zhen-Yu Zhu; Xin Dong; Hai Zhang; Yi-Feng Chai; Zi-Yang Lou

    2011-01-01

    A comparison of the volatile compounds in Rhizomes Curcumae (Ezhu) and Radix Curcumae (Yujin) was undertaken using gas chromatography mass spectrometi-y (GC-MS). Ultrasonic extraction and GC-MS methods were developed for the simultaneous determination of five sesquiterpenes, namely, α-pinene, β-elemene, curcumol, germacrone and curdione, in Ezhu and Yunjin. Good linearity (r〉0.999) and high inter-day precision were observed over the investigated concentration ranges. The validated method was successfully used for the simultaneous determination of five sesquiterpenes in Ezhu and Yujin. The quantitative method can be effectively used to evaluate and monitor the quality of Chinese curcuma in clinical use.

  7. Analysis of volatile components in a Chinese fish sauce,Fuzhou Yulu, by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Yuan-fan YANG; Shen-ru CHEN; Hui NI; Xing-qian YE

    2008-01-01

    Volatile components of Fuzhou Yulu, a Chinese fish sauce, were analyzed by gas chromatography-mass spectrometry (GC-MS), and two pretreatment methods, i.e., purge and trap (P&T) GC-MS and ethyl acetate extraction followed by GC-MS, were compared. P&T-GC-MS method determined 12 components, including sulfur-containing constituents (such as dimethyl disulfide), nitrogen-containing constituents (such as pyrazine derivatives), aldehydes and ketones. Ethyl ace tate extraction fol-lowed by GC-MS method detected 10 components, which were mainly volatile organic acids (such as benzenepropanoic acid) and esters. Neither of the two methods detected alcohols or trimethylamine. This study offers an important reference to determine volatile flavor components of traditional fish sauce through modem analysis methods.

  8. 气相色谱-质谱联用法同时测定污水中 对羟基苯甲酸酯和甾体雌激素%Simultaneous determination of parabens and steroid estrogens in sewage water using gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    王亮; 毛茜慧; 袁守军; 黄德英; 张继彪

    2016-01-01

    A method was developed for the simultaneous detamination of seven parabens and five steroid estrogens in sewage water using gas chromatography-mass spectrometry coupled by solid phase extraction. The sample derivatization was optimized and the best derivatization was obtained when target compounds reacted with bis ( trimethylsilyl ) trifluoroacetamide at 40 ℃ for 60 min. The optimum extraction conditions were as follow: HC-C18 cartridge was selected and the pH value of 7 was optimized for samples extraction, then ethyl acetate:acetone (1:1, V:V) was used for elution. Under the optimized conditions, the linear detection range of 12 analytes was 20—2000 ng·L-1( r>0.990). The limit of detection was 1.8—5.7 ng·L-1, and the recovery of 82.2-128.5%was obtained for most of the analytes, and the relative standard deviation was 4.4%—21.2%.%利用气相色谱-质谱联用仪( GC-MS) ,结合固相萃取技术,建立了同时测定污水中7种对羟基苯甲酸酯和5种甾体雌激素的定量分析方法.结果表明,目标物在40 ℃衍生化反应60 min可达最佳衍生化效果;最佳萃取剂净化条件为:使用HC-C18型SPE柱,pH=7条件下萃取,洗脱液为乙酸乙酯:丙酮( 1:1,V:V) .该方法检出限(LOD)为1.8—5.7 ng·L-1,线性范围20—2000 ng·L-1(r>0.990),除少量目标物回收率稍高外,大部分目标物的回收率为82.2%—128.5%,相对标准偏差介于4.4%—21.2%之间.

  9. Bioassay- and liquid chromatography/mass spectrometry-guided acetylcholinesterase inhibitors from Picriafel-terrae

    Directory of Open Access Journals (Sweden)

    Lu Wen

    2013-01-01

    Full Text Available Background: Picria fel-terrae is a traditional Chinese medicine. Materials and Methods: A new approach to the search for acetylcholinesterase (AChE inhibitors from Picria fel-terrae is presented. Results: Bioassay- and LC-MS-guided fractionation of the ethyl acetate extract was from traditional Chinese medicine P.fel-terrae. Following primary extraction, the ethyl acetate extracts fraction of P.fel-terrae showed strong AChE inhibitory activities. So the sample was separated using highperformance liquid chromatography (HPLC. The effluent was split towards two identical 96-well fraction collectors, and the presence of the biologically interesting portion and chromatographic fractions could be readily detected by analyzing selected ion chromatograms through an electrophoresis-electrospray ionization mass spectrometry (ESIMS system for accurate mass measurement. One 96-well plate was used for a bioassay (AChE-inhibitory assay and detected the bioactivity and position of the relevant peak in the chromatogram. The positive well in the second 96-well plate was used for identification by LC-(+ ESIMS. Conclusion: As abovementioned, the AChE inhibitory constituents from P.fel-terrae by LC-bioassay-ESIMS were rapid identified. Liquid chromatography/ mass spectrometry (LC-MS screening detected the presence of six active compounds, identified as picfeltarraenin IA (1, picfeltarraenin IB (2, picfeltarraenin IV (3, picfeltarraenin X (4, picfeltarraenin XI (5, and one unknown compound. The structures were further determined by 13C NMR. The six compounds expressed stronger AChE inhibition than the known AChE inhibitorTacrine. Above all, the value of this LC-bioassay-ESIMS methodology is highlighted by the finding and structure elucidation of the active constituents from many other structural families of natural products.

  10. Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

  11. Biomedical applications of gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Gas chromatography coupled with mass-spectrometry (GC/MS) is a modern technique, which has very important applications in the biomedical area. A large number of qualitative and quantitative determinations of drugs, amino acids, vitamins, lipids, aroma compounds, important nutrients, herb extracts were developed. The extraction procedure is the first important step in the analytical work. The internal standard is usually added at the very begin ing of the quantitative work. The best one is the stable isotopic labeled compound, usually the analogue of the compound of interest. Stable isotopic internal standard or compounds from the same chemical class having boiling point close to that of the compound of interest were used. Quantitation needs very well selected standards and method validation. Some validated methods for the determination of drugs and some active principles in biological media are presented. Several preconcentration extraction procedures were used. The quantitative determinations by detection (GC-MS) were performed. Good validation parameters were obtained: precision, accuracy, linearity in the range of interest, good limit of detection and quantitation, selectivity and specificity. Chromatography was performed on a 5% phenyl methyl polysiloxane column (15 or 30 m x 0.25 mm I.D., 0.25 μm film thickness) operated in suitable temperature programs. Helium carrier gas flow was 1ml/min. Ionization was performed by electron impact and detection in scan or selected ion monitoring (SIM) modes. The methods provided high response linearity (mean r = 0.99), precision and accuracy (< 10% C.V.). Applications of the quantitative methods in biomedical area are described. (author)

  12. Flame atomic absorption spectrometric determination of trace cadmium in alloys and biological samples after solid-liquid extraction and preconcentration with use of nitroso-S

    International Nuclear Information System (INIS)

    Cadmium is quantitatively retained by 2-nitroso-1-naphthol-4-sulfonic acid (nitroso-S) and tetradecyldimethylbenzylammonium chloride (TDBA) on microcrystalline naphthalene in the pH range 5.7-10.5 from a large volumes of aqueous solutions of various samples. After filtration, the solid mass consisting of cadmium complex and naphthalene is dissolved with 5 mL of dimethylformamide and the metal was determined by flame atomic absorption spectrometric. Cadmium complex can alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. About 25 ng of cadmium can be concentrated in a column from 500 mL of aqueous sample, where its concentration is as low as 0.05 ng/mL. Eight replicate determinations of 0.1 μg/mL of cadmium in final DMF solution gave a mean absorbance of 0.060 with a relative standard deviation of 1.8 %. The sensitivity for 1 % absorption was 7.3 ng/mL. The interference of a large number of anions and cations has been studied and the optimized conditions developed were utilized for the trace determination of cadmium in various alloys and biological samples. (author)

  13. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  14. Rapid and Accurate Identification of Animal Species in Natural Leather Goods by Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Izuchi, Yukari; Takashima, Tsuneo; Hatano, Naoya

    2016-01-01

    The demand for leather goods has grown globally in recent years. Industry revenue is forecast to reach $91.2 billion by 2018. There is an ongoing labelling problem in the leather items market, in that it is currently impossible to identify the species that a given piece of leather is derived from. To address this issue, we developed a rapid and simple method for the specific identification of leather derived from cattle, horses, pigs, sheep, goats, and deer by analysing peptides produced by the trypsin-digestion of proteins contained in leather goods using liquid chromatography/mass spectrometry. We determined species-specific amino acid sequences by liquid chromatography/tandem mass spectrometry analysis using the Mascot software program and demonstrated that collagen α-1(I), collagen α-2(I), and collagen α-1(III) from the dermal layer of the skin are particularly useful in species identification. PMID:27313979

  15. Rapid and Accurate Identification of Animal Species in Natural Leather Goods by Liquid Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Izuchi, Yukari; Takashima, Tsuneo; Hatano, Naoya

    2016-01-01

    The demand for leather goods has grown globally in recent years. Industry revenue is forecast to reach $91.2 billion by 2018. There is an ongoing labelling problem in the leather items market, in that it is currently impossible to identify the species that a given piece of leather is derived from. To address this issue, we developed a rapid and simple method for the specific identification of leather derived from cattle, horses, pigs, sheep, goats, and deer by analysing peptides produced by the trypsin-digestion of proteins contained in leather goods using liquid chromatography/mass spectrometry. We determined species-specific amino acid sequences by liquid chromatography/tandem mass spectrometry analysis using the Mascot software program and demonstrated that collagen α-1(I), collagen α-2(I), and collagen α-1(III) from the dermal layer of the skin are particularly useful in species identification.

  16. Analysis of volatile chemical components of Radix Paeoniae Rubra by gas chromatography-mass spectrometry and chemometric resolution

    Institute of Scientific and Technical Information of China (English)

    LI Xiao-ru; LAN Zheng-gang; LIANG Yi-zeng

    2007-01-01

    The volatile chemical components of Radix Paeoniae Rubra (RPR) were analyzed by gas chromatography-mass spectrometry with the method of heuristic evolving latent projections and overall volume integration.The results show that 38 volatile chemical components of RPR are determined.accounting for 95.21% of total contents of volatile chemical components of RPR.The main volatile chemical components of RPR are(Z,Z)-9, 12-octadecadienoic acid, n-hexadecanoic acid, 2-hydroxy benzaldehyde, 1-(2-hydroxy-4-methoxyphenyl)-ethanone, 6,6-dimethyl-bicyclo[3.1.1]heptane-2-methanol, 4,7-dimethyl-benzofuran, 4-(1-methylethenyl)-1-cyclohexene-1-carboxaldehyde, and cyclohexadecane.

  17. Rapid and Accurate Identification of Animal Species in Natural Leather Goods by Liquid Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Izuchi, Yukari; Takashima, Tsuneo; Hatano, Naoya

    2016-01-01

    The demand for leather goods has grown globally in recent years. Industry revenue is forecast to reach $91.2 billion by 2018. There is an ongoing labelling problem in the leather items market, in that it is currently impossible to identify the species that a given piece of leather is derived from. To address this issue, we developed a rapid and simple method for the specific identification of leather derived from cattle, horses, pigs, sheep, goats, and deer by analysing peptides produced by the trypsin-digestion of proteins contained in leather goods using liquid chromatography/mass spectrometry. We determined species-specific amino acid sequences by liquid chromatography/tandem mass spectrometry analysis using the Mascot software program and demonstrated that collagen α-1(I), collagen α-2(I), and collagen α-1(III) from the dermal layer of the skin are particularly useful in species identification. PMID:27313979

  18. Urinary metabonomics study in a rat model in response to protein-energy malnutrition by using gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Zeming; Li, Min; Zhao, Chunxia; Zhou, Jia; Chang, Yuwei; Li, Xiang; Gao, Peng; Lu, Xin; Li, Yousheng; Xu, Guowang

    2010-11-01

    Systematic studies were performed on the biological perturbations in metabolic phenotype responding to protein-energy malnutrition through global metabolic profiling analysis, in combination with pattern recognition. The malnutrition rat model was established through five weeks of strict diet restriction, and the metabonome data obtained from gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) were integrated to approximate the comprehensive metabolic signature. Principal component analysis and orthogonal projection to latent structure analysis were used for the classification of metabolic phenotypes and discovery of differentiating metabolites. The perturbations in the urine profiles of malnourished rats were marked by higher levels of creatine, threitol, pyroglutamic acid, gluconic acid and kynurenic acid, as well as decreased levels of succinic acid, cis-aconitic acid, citric acid, isocitric acid, threonic acid, trimethylglycine, N-methylnicotinic acid and uric acid. The alterations in these metabolites were associated with perturbations in energy metabolism, carbohydrate, amino acid, and fatty acid metabolism, purine metabolism, cofactor and vitamin metabolism, in response to protein and energy malnutrition. Our findings show the integration of GC-MS and LC-MS techniques for untargeted metabolic profiling analysis was promising for nutriology. PMID:20717558

  19. 基于阳离子交换-反相混合分离模式的液相色谱-质谱联用检测河豚毒素新方法%Determination of tetrodotoxin using a cation exchange-reverse phase liquid chromatography-mass spectrometric method

    Institute of Scientific and Technical Information of China (English)

    刘希; 陈佳; 刘勤; 郭磊; 毛军文; 谢剑炜

    2012-01-01

    Objective To establish a highly sensitive method suitable for detection of intoxicated biomedical samples with regard to tetrodotoxin ,one of the most toxic non-proteins as well as a hydrophilic small biotoxin . Methods A novel method for detection of tetrodotoxin in human blood plasma by liquid chromatography -time of flight/mass spectrometry ( LC-TOF/MS) technique was established using a cation exchange -reverse phase separation mode. The LC-MS analysis and extraction conditions were systematically optimized. Results For the tetrodotoxin standard sample , the linear calibration curve ranged from 0.1 to 50 mg/L and the limit of detection ( LOD) was 0.01 mg/L. For the tetrodotoxin exposed human plasma sample, the linear calibration curve ranged from 0.5 to 10 mg/L and the LOD was 0.25 mg/L, respectively. Conclusion Such an LC-TOF/MS established for the detection of tetrodotoxin is highly specific and sensitive , and it can be feasible for the detection of tetrodotoxin at mg/L level in puffer fish biosamples.%目的 建立一种可用于检测中毒生物医学样品中小分子生物毒素--河豚毒素的高灵敏度分析方法.方法 选用阳离子交换-反相混合色谱柱,针对河豚毒素亲水性强的特点,建立了一种新型的液相色谱-飞行时间质谱方法对人血浆中河豚毒素进行检测,优化了液相色谱-质谱条件,考察了血浆中河豚毒素的提取方法.结果 对于参考品溶液,河豚毒素的线性范围为0.1~50 mg/L,检测限为0.01 mg/L;对于染毒人血浆样品,河豚毒素的线性范围为0.5~10 mg/L,检测限为0.25 mg/L.结论 所建立的液相色谱-飞行时间质谱方法专属性强、灵敏度高,可适用于实际测定河豚鱼头样品中 mg/L水平的河豚毒素.

  20. A novel method for the identification of illegal cooking oil (2) :determination of special odd-chain fatty acids by multidimensional gas chromatography-mass spectrometry%非正常食用油鉴别新方法(二):特征奇数碳脂肪酸的多维气相色谱-质谱检测

    Institute of Scientific and Technical Information of China (English)

    金静; 王龙星; 陈吉平; 田玉增; 邹黎黎; 张保琴; 王淑秋; 王幸福

    2012-01-01

    通过对脂肪酸的非靶标/靶标筛查,确立了非正常食用油(俗称地沟油)的内源性特征指示物:两种奇数碳脂肪酸,包括源自动物油的13-甲基十四烷酸和源自加热植物油的十一烷酸.并借助多维气相色谱-质谱技术,依据不同极性气相色谱柱的保留作用,不仅实现了不同碳数烷酸以及同碳数烷酸异构体之间的有效分离,达到了对13-甲基十四烷酸和十一烷酸准确定量的目的;而且实现了对目标化合物的在线净化、富集.凭借该项检测方法,参加了国家食品安全风险评估中心组织的第四、五批地沟油盲样考核.经过不断完善,该方法阴性样品的正确率提高到100%,阳性样品的正确率分别达到71%和75%.再结合辣椒碱指标,从内、外源指示物两方面全面、准确地对食用油样品进行判定,使得阳性样品的正确率分别提高至89%和100%.目前,该方法已经人选国家卫生部公布的四大地沟油鉴定仪器分析方法,正等待权威部门的协同性验证.%Endogenesis referents from illegal cooking oil (ICO), namely, 13-methyl-tetrade-canoic acid and undecanoic acid have been confirmed via non-target and target screening of fatty acids. The former is mainly originated from animal oil, and the later from heated vegetable oil. Based on the retention interactions between gas chromatographic columns with different polarities and alkyl acids, the alkyl acids with various carbon chain or their isomers with the same carbon chains can be separated effectively using multidimensional gas chromatography-mass spectrometry. And the accurate quantification of 13-methyl-tetradecanoic acid and undecanoic acid was obtained. The target compounds can be cleaned up online and enriched with the developed method. Subsequently, the fourth and fifth assessments organized by China National Center for Food Safety Risk Assessment were performed in our laboratory. After continuous improvement, the

  1. Optimization of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    International Nuclear Information System (INIS)

    The suitability of spectrometric backscattered gamma - gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma - ray source of very low radioactivity (1.8 MBq) is used. The logging tools is tested using 133 Ba and 137 Cs sources with a 37 mm (diameter) x 750 mm NaI (TI) scintillation detector. Five source - to - detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a 133 Ba source was determined to be 52 mm source - to - detector spacing. This configuration gives the best results for both Pb and ZME grade. The r.m.s deviations for Pb and ZME were 0.33 and 2.3%, respectively. The optimum configuration for the logging probe using a 137 Cs source was determined to be 64 mm source - to - detector spacing. This configuration gives the best results for both Pb and ZME grade. The r.m.s deviations for Pb and ZME were 0.36 and 2.2%, respectively. (author)

  2. Optimisation of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    International Nuclear Information System (INIS)

    The suitability of spectrometric backscattered gamma-gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma-ray source of very low radioactivity (1.8 MBq) is used. The logging tool is tested using 133Ba and 137Cs sources with a 37 mm (diameter)x75 mm NaI (TI) scintillation detector. Five source-to-detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a 133Ba source was determined to be 52 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0.33 and 2.3%, respectively. The optimum configuration for the logging probe using a 137Cs source was determined to be 64 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0. 3 6 and 2.2 %, respectively

  3. Evaluation of mass spectrometric data using principal component analysis for determination of the effects of organic lakes on protein binder identification.

    Science.gov (United States)

    Hrdlickova Kuckova, Stepanka; Rambouskova, Gabriela; Hynek, Radovan; Cejnar, Pavel; Oltrogge, Doris; Fuchs, Robert

    2015-11-01

    Matrix-assisted laser desorption/ionisation-time of flight (MALDI-TOF) mass spectrometry is commonly used for the identification of proteinaceous binders and their mixtures in artworks. The determination of protein binders is based on a comparison between the m/z values of tryptic peptides in the unknown sample and a reference one (egg, casein, animal glues etc.), but this method has greater potential to study changes due to ageing and the influence of organic/inorganic components on protein identification. However, it is necessary to then carry out statistical evaluation on the obtained data. Before now, it has been complicated to routinely convert the mass spectrometric data into a statistical programme, to extract and match the appropriate peaks. Only several 'homemade' computer programmes without user-friendly interfaces are available for these purposes. In this paper, we would like to present our completely new, publically available, non-commercial software, ms-alone and multiMS-toolbox, for principal component analyses of MALDI-TOF MS data for R software, and their application to the study of the influence of heterogeneous matrices (organic lakes) for protein identification. Using this new software, we determined the main factors that influence the protein analyses of artificially aged model mixtures of organic lakes and fish glue, prepared according to historical recipes that were used for book illumination, using MALDI-TOF peptide mass mapping. PMID:26505772

  4. Validation of method for determination of different classes of pesticides in aqueous samples by dispersive liquid-liquid microextraction with liquid chromatography-tandem mass spectrometric detection.

    Science.gov (United States)

    Caldas, Sergiane Souza; Costa, Fabiane Pinho; Primel, Ednei Gilberto

    2010-04-14

    In this study, a simple, rapid and efficient method has been developed for the extraction and preconcentration of different classes of pesticides, carbofuran (insecticide), clomazone (herbicide) and tebuconazole (fungicide) in aqueous samples by dispersive liquid-liquid microextraction (DLLME) coupled with liquid chromatography-tandem mass spectrometric detection. Some experimental parameters that influence the extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, speed of centrifugation, pH and addition of salt were examined and optimized. Under the optimum conditions, the recoveries of pesticides in water at spiking levels between 0.02 and 2.0 microg L(-1) ranged from 62.7% to 120.0%. The relative standard deviations varied between 1.9% and 9.1% (n=3). The limits of quantification of the method considering a 50-fold preconcentration step were 0.02 microg L(-1). The linearity of the method ranged from 1.0 to 1000 microg L(-1) for all compounds, with correlation coefficients varying from 0.9982 to 0.9992. Results show that the method we propose can meet the requirements for the determination of pesticides in water samples. The comparison of this method with solid-phase extraction indicates that DLLME is a simple, fast, and low-cost method for the determination of pesticides in natural waters.

  5. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    Science.gov (United States)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation. PMID:24401459

  6. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    Science.gov (United States)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation.

  7. Scope and limitations of flash pyrolysis-gas chromatography-mass spectrometry as revealed by the thermal behaviour of high-molecular-weight lipids derived from the green microalga Botryococcus braunii

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Gelin, F.; Leeuw, J.W. de; Derenne, S.; Largeau, C.; Metzger, P.

    1994-01-01

    Curie point pyrolysis—gas chromatography/mass spectrometry studies of four types of high-molecular-weight (HMW) lipids isolated from the green microalga Botryococcus braunii race A were performed to determine the thermal behaviour of these lipids and to propose mechanisms of pyrolysis for these type

  8. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Roos, Per

    2008-01-01

    spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer...

  9. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    International Nuclear Information System (INIS)

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l-1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  10. Flame atomic absorption spectrometric determination of cadmium(II) and lead(II) after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493

    International Nuclear Information System (INIS)

    An enrichment procedure for cadmium and lead after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493 has been established prior to their flame atomic absorption spectrometric determinations. The analytical parameters including pH, amounts of dibenzyldithiocarbamate, sample volume, etc., were investigated. The effects of alkaline and earth alkaline ions and some metal ions on the retentions of analytes on Dowex Optipore V-493 resin were examined. Under the optimized conditions, the detection limits (3s, n = 21) for cadmium and lead were 0.43 μg L-1 and 0.65 μg L-1, respectively. The relative standard deviation (R.S.D.), and the recoveries of standard addition for this method were lower than 5% (n = 11) and 95-102%, respectively. Three standard reference samples (LGC 6010 Hard drinking water, NIST SRM 2711 Montana soil and GBW 07605 Tea) were introduced for accuracy and precision of analytical data. The proposed solid phase extraction system was successfully applied to the analysis of environmental samples

  11. Liquid chromatography-tandem mass spectrometric methods for the determination of spinosad, thiacloprid and pyridalyl in spring onions and estimation of their pre-harvest interval values.

    Science.gov (United States)

    Dasenaki, Marilena E; Bletsou, Anna A; Hanafi, Ahmad H; Thomaidis, Nikolaos S

    2016-12-15

    Two liquid chromatography-tandem mass spectrometric methods were developed and validated to determine spinosyn A and D, thiacloprid and pyridalyl in spring onions cultivated under Egyptian field conditions. The degradation rates, the pre-harvest interval (PHI) values and the half-life values of the three pesticides were estimated. QuEChERS was used for sample preparation and the separation was performed on an X-Bridge C18 column with ACN-formic acid 0.1% as the mobile phase. Linear range, method detection limits (MDLs), precision, recovery and matrix effects were estimated. The multi-residue MDLs ranged from 0.02μg/kg (spinosyn A & D) to 0.05μg/kg for pyridalyl. All the investigated pesticides showed high degradation rates. For spinosad the half-life value was 1.2days, for thiacloprid it reached 2.2days and for pyridalyl 4.4days. Furthermore, the calculated PHI values, according to the maximum residue levels set by the EU, were 0days for spinosad, 9.8days for thiacloprid and 39.4days for pyridalyl. PMID:27451196

  12. [Determination of nine estrogenic steroids in milk using matrix solid phase dispersion-ultra performance liquid chromatography with mass spectrometric detector].

    Science.gov (United States)

    Liu, Hongcheng; Li, Ning; Lin, Tao; Shao, Jinliang; Li, Qiwan

    2015-11-01

    An analytical method for the multiresidue determination of nine estrogenic steroids in milk was developed by modified matrix solid phase dispersion (MSPD) purification and ultra performance liquid chromatography (UPLC) with mass spectrometric detector (MSD). The sensitivity and accuracy of MSD were better than that of ultraviolet detector. In comparison with traditional mass spectrometry, the merits of MSD were simpler in operation and shorter in starting time (5 min). The results showed that the limits of detection of the compounds with nucleophilic substitution were high in positive ion mode of MSD and were easily affected by environmental conditions. The matrix effects of milk samples reduced from 84%-160% to 80%-121% after MSPD purification. The intraday precision and interday precision of the nine estrogenic steroids were 0.87%-1.78% and 1.82%-3.79%, respectively. The average recoveries were 68.7%-94.7%, and the relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) were 0.5-10 μg/kg. The limits of quantification (LOQ) were 2-20 μg/kg. PMID:26939362

  13. Optimisation of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    CERN Document Server

    Asfahani, J

    1999-01-01

    The suitability of spectrometric backscattered gamma-gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma-ray source of very low radioactivity (1.8 MBq) is used. The logging tool is tested using sup 1 sup 3 sup 3 Ba and sup 1 sup 3 sup 7 Cs sources with a 37 mm (diameter)x75 mm NaI (TI) scintillation detector. Five source-to-detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a sup 1 sup 3 sup 3 Ba source was determined to be 52 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0.33 and ...

  14. A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric method for the determination of organosulfur compounds in petroleum asphalt cements.

    Science.gov (United States)

    da Silveira, Géssica Domingos; Faccin, Henrique; Claussen, Luis; Goularte, Rayane Bueno; Do Nascimento, Paulo C; Bohrer, Denise; Cravo, Margareth; Leite, Leni F M; de Carvalho, Leandro Machado

    2016-07-29

    We present a sensitive liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the determination of selected organosulfur compounds in Brazilian asphalt cements. It was possible to detect 14 organosulfur compounds of different classes where sulfoxides and sulfones presented higher sensibility in ionization than thiophenes and aromatic sulfides. A dopant-assisted APPI method was also tested, however, when chromatographic flow rate was optimized a decrease in signal was observed for all compounds. PAHs were tested and ruled out as possible interfering compounds and the matrix effect of asphalt cements was within an acceptable range for the quantification of organosulfur compounds. The proposed method was found to have satisfactory linearity and accuracy with recoveries between 83.85 and 110.28% for thianaphthene and 3-methylbenzothiophene, respectively. Therefore, the method allowed the characterization of organosulfur compounds in Brazilian asphalt cements and demonstrated changes in the amount quantified in asphaltenic and maltenic fractions after the RTFOT+SUNTEST aging process. PMID:27342135

  15. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    Science.gov (United States)

    Reyes, Mariela N. Matos; Campos, Reinaldo C.

    2005-06-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation ( n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits ( k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l - 1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples.

  16. Influence of particle size of wear metal on the spectrometric oil analysis programme (SOAP), demonstrated by the determination of iron by AAS

    International Nuclear Information System (INIS)

    The possibility that there might be a relation between particle size of wear metal and spectrometric determination, (e.g. of the iron content in used lubricating oils) has been examined. In this connection it had to be clarified from which particle size of the iron wear the Fe content determined by direct AAS (solution of the oil sample) is in agreement with the true value in the used oil. The determination of the absolute iron content was performed by a colorimetric method preceded by an incineration of the used oil. Contrary to other publications, in which work is based on spherical iron particles as a simulated wear, the test described here relates to true wear particles. To obtain the total iron wear from a gear oil it was filtered off from the used oil and afterwards separated into defined particle size ranges by a procedure specially developed for this purpose. The different groups of scaly particles, which were collected in this way, were then mixed homogeneously into fresh luboil samples according to their sizes. The determination of the iron content from these newly mixed luboil samples was carried out 1. by direct AAS, 2. by AAS after incineration of the oil samples and 3. by a colorimetric method (to obtain the absolute value of the iron content). The results showed a recovery of the iron of only 50% if the wear particles were bigger than about 2 μm. That means that the true value of the iron content in a used lubricating oil is found by direct AAS only if the particle size is <=1 μm. (orig.)

  17. A high-performance liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric method for determination of risperidone and 9-hydroxyrisperidone in human plasma.

    Science.gov (United States)

    Moody, David E; Laycock, John D; Huang, Wei; Foltz, Rodger L

    2004-09-01

    Risperidone, a benzisoxazole derivative, is an antipsychotic agent used for the treatment of schizophrenia. We developed a liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS-MS) method with improved sensitivity, selectivity, and dynamic range for determination of risperidone and 9-hydroxyrisperidone in human plasma. A structural analogue of risperidone, RO68808 (5 ng/mL), is added as the internal standard to 1 mL of human plasma. Plasma is made basic, extracted with pentane/methylene chloride (3:1), the organic phase evaporated to dryness, and the residue is reconstituted in water with 0.1% formic acid/acetonitrile (20:1). For LC-MS-MS analysis, a Metachem Inertsel HPLC column (2.1 x 150 mm, 5-microm particle size) is connected to a Finnigan TSQ7000 tandem MS via the Finnigan API interface. Both electrospray (ESI) and APCI produced predominantly MH(+) ions for the two analytes and the internal standard. Ions detected by selected reaction monitoring correspond to the following transitions: m/z 411 to 191 for risperidone, m/z 427 to 207 for 9-hydroxyrisperidone, and m/z 421 to 201 for the internal standard. APCI provided a larger dynamic range (0.1 to 25 ng/mL) and better precision and accuracy than ESI. Intrarun accuracy and precision determined at 0.1, 0.25, 2.5, and 15 ng/mL were within 12% of target with %CVs not exceeding 10.9%. Interrun accuracy and precision determined at the same concentrations were within 9.6% of target with %CVs not exceeding 6.7%. Analytes were stable in plasma after 24 h at room temperature, 2 freeze-thaw cycles, and 490 days at -20 degrees C. PMID:15516302

  18. New approaches for the mass spectrometric determination of trace concentrations and congener group patterns of chlorinated paraffins in biota

    OpenAIRE

    Reth, Margot

    2006-01-01

    The determination of chlorinated paraffins (CPs) in the environment is important, since CPs are persistent, bioaccumulative and toxic. However, the analysis of these complex mixtures containing thousands of isomers is also a demanding task. CP analysis and especially the quantification of CPs are far from being well established. In this work, new methodologies were developed for the determination of CPs in biota by low-resolution mass spectrometry (LRMS). The use of expensiv...

  19. The bridge between thin layer chromatography-mass spectrometry and high-performance liquid chromatography-mass spectrometry: The realization of liquid thin layer chromatography-mass spectrometry (LTLC-MS).

    Science.gov (United States)

    Li, Yafeng; Wang, Jianing; Zhan, Lingpeng; Wleklinski, Michael; Wang, Jiyun; Xiong, Caiqiao; Liu, Huihui; Zhou, Yueming; Nie, Zongxiu

    2016-08-19

    The combination of thin layer chromatography (TLC) and mass spectrometry (MS) has been studied for decades, but for most cases MS detection is done after TLC separation is finished. Here, an online simultaneous TLC-MS analysis system, liquid thin layer chromatography-mass spectrometry (LTLC-MS), is developed which successfully synchronize TLC separation process and MS detection process like GC-MS and HPLC-MS do. And there's no need to use specially designed TLC, just regular TLC plates are enough. LTLC-MS method is composed of a newly developed ambient ionization method, glow discharge-matrix assisted infrared desorption ionization (GD-MAIRDI), and forced-flow TLC (FFTLC) technique, which guarantees the MS detection process does not disturb the TLC separation process throughout the whole analysis. The whole LTLC-MS analysis only need two steps and less than 15min. Mixtures as well as the two main components of a pain relief pills have been successfully analyzed by LTLC-MS. This proof of concept study opens up new possibilities of combining TLC with MS, and will further broaden the application abilities of TLC. PMID:27452991

  20. Integration of Gas Chromatography Mass Spectrometry Methods for Differentiating Ricin Preparation Methods

    Energy Technology Data Exchange (ETDEWEB)

    Wunschel, David S.; Melville, Angela M.; Ehrhardt, Christopher J.; Colburn, Heather A.; Victry, Kristin D.; Antolick, Kathryn C.; Wahl, Jon H.; Wahl, Karen L.

    2012-05-17

    The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of the castor plant Ricinus communis. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatographic - mass spectrometric (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method and independent of the seed source. In particular the abundance of mannose, arabinose, fucose, ricinoleic acid and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation.

  1. Confirmation of patulin and 5-hydroxymethylfurfural in apple juice by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Rupp, H S; Turnipseed, S B

    2000-01-01

    A gas chromatographic/mass spectrometric (GC/MS) method was developed for the confirmation of patulin and 5-hydroxymethylfurfural (HMF) extracted from apple juice. The extraction is based on the official AOAC method for liquid chromatographic analysis. Juice extracts are quickly and easily derivatized with bis(trimethylsilyl)trifluoracetamide under mild conditions, and the trimethylsilyl ethers of the analytes are stable for at least several hours. The analytes are determined by GC/MS using an electron-impact source and selected ion monitoring of characteristic ions. For both analytes, the interassay differences between base-peak ratios for samples and standards were all <7.1% (absolute). The presence of patulin was confirmed at fortification levels of about 30-400 microg/L and naturally occurring levels of about 80-400 microg/L. The presence of HMF was also confirmed at levels < or = 2 mg/L. The proposed mass spectral fragmentation pathways of the analytes are presented. PMID:10868584

  2. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  3. Preconcentration of submicrogram amounts of metals from natural water for X-ray energy spectrometric determination using pyrrolidinecarbodithioic acid

    International Nuclear Information System (INIS)

    A method was developed for the routine determination of several trace metals in natural waters by X-ray energy spectrometry following precipitation with pyrrolidinecarbodithioate. Preoxidation with persulfate eliminates interferences by organic matter. By optimizing carrier ion selection and measurement conditions, one may determine dithioate-reactive elements with Z less than or equal to 50 by means of their K X-rays, and some with Z greater than or equal to 80 by means of their L X-rays. Determinations are feasible for several elements at concentrations down to 250 ng L-1, or below. Recoveries are generally greater than 90%, although some exceptions are noted. Reproducibility with real samples averaged about 25% relative standard deviation for five representative elements at concentrations above 250 ng L-1. 24 references, 5 figures, 4 tables

  4. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed. PMID:25830900

  5. Electrothermal atomic absorption spectrometric determination of lithium, sodium, potassium and copper in uranium without preliminary chemical separation

    International Nuclear Information System (INIS)

    Graphite furnace atomization is used for the direct determination of Li (0.25-4 ppm), Na (8-70 ppm), K (20-300 ppm) and Cu (0.5-25 ppm) in uranium dissolved in nitric acid, with relative standard deviations of 4-9%. Only iron seriously depresses the signals from the alkali metals. (Auth.)

  6. Development of a cloud point extraction and preconcentration method for Cd and Ni prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Manzoori, Jamshid L. [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: manzoori@tabrizu.ac.ir; Karim-Nezhad, Ghasem [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2004-09-13

    In this work a new cloud point extraction (CPE) methodology was developed for the separation and preconcentration of cadmium and nickel. The analyte in the initial aqueous solution was complexed with dithizone and Triton X-114 was added as surfactant. After phase separation, based on the cloud point of the mixture, and dilution of the surfactant-rich phase with tetrahydrofuran (THF), the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions and preconcentration of only 10 ml of sample in the presence of 0.05% Triton X-114, the enhancement factors of 52 and 39 and the detection limits of 0.31 {mu}g l{sup -1} and 1.2 {mu}g l{sup -1} were obtained for cadmium and nickel respectively. The proposed method was applied satisfactorily to the determination of cadmium and nickel in water samples.

  7. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Robert De Levie

    2009-09-01

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements may need an unexpectedly high precision to yield accurate answers, because of an artifact of inverse cancellation, in which a small noise or drift signal is misinterpreted in terms of a concentration difference. The computed sum of the concentrations is not affected.

  8. Chemical characterization using gas chromatography/mass spectrometry of two extracts from Phyllanthus orbicularis HBK

    International Nuclear Information System (INIS)

    The objective of this paper was the chemical characterization of two extracts from Phyllanthus orbicularis HBK through gas chromatography/mass spectrometry. To this end, maceration with N-hexane and ethyl acetate was used to obtain the respective extracts. The study of the hexane extract identified 17 components in which hydrocarbonate structures prevailed, mainly cyclooctacosane. In the ethyl acetate extract, 19 compounds were detected, being the terpenoids the predominant, although the most abundant was sterol g-sitosterol. For the first time, the identified compounds are reported for this species

  9. Analysis of the citric acid cycle intermediates using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kombu, Rajan S; Brunengraber, Henri; Puchowicz, Michelle A

    2011-01-01

    Researchers view analysis of the citric acid cycle (CAC) intermediates as a metabolomic approach to identifying unexpected correlations between apparently related and unrelated pathways of metabolism. Relationships of the CAC intermediates, as measured by their concentrations and relative ratios, offer useful information to understanding interrelationships between the CAC and metabolic pathways under various physiological and pathological conditions. This chapter presents a relatively simple method that is sensitive for simultaneously measuring concentrations of CAC intermediates (relative and absolute) and other related intermediates of energy metabolism using gas chromatography-mass spectrometry.

  10. Screening for N-glycosylated proteins by liquid chromatography mass spectrometry

    DEFF Research Database (Denmark)

    Bunkenborg, Jakob; Pilch, Bartosz J; Podtelejnikov, Alexandre V;

    2004-01-01

    in complex mixtures by reducing sample complexity and enriching glycoprotein content. Glycosylated proteins are selected by an initial lectin chromatography step and digested with endoproteinase Lys-C. Glycosylated peptides are then selected from the digest mixture by a second lectin chromatography step....... The glycan components are removed with N-glycosidase F and the peptides digested with trypsin before analysis by on-line reversed-phase liquid chromatography mass spectrometry. Using two different lectins, concanavalin A and wheat germ agglutinin, this procedure was applied to human serum and a total of 86 N...

  11. Development of a high-speed MALDI-triple quadrupole mass spectrometric method for the determination of 3,4-methylenedioxymethamphetamine (MDMA) in oral fluid.

    Science.gov (United States)

    Poetzsch, Michael; Steuer, Andrea E; Hysek, Cedric M; Liechti, Matthias E; Kraemer, Thomas

    2016-02-01

    3,4-Methylenedioxymethamphetamine (MDMA, ecstasy) is still a widely used illicit designer drug and its detection in different matrices is of major importance for forensic purposes (e.g. driving under the influence) as well as for workplace drug testing or abstinence control. Established analytical methods for the determination of MDMA are mainly employing high performance liquid chromatography (HPLC) or gas chromatography (GC) coupled to mass spectrometric detection. Matrix assisted laser desorption/ionization-triple quadrupole-tandem mass spectrometry (MALDI-QqQ-MS/MS) is so far rarely used in forensics and offers an ultrafast high-throughput platform. The Quantisal™ Oral Fluid Collection Device was used for sample collection. After addition of the deuterated internal standard and a carbonate buffer (0.75 M Na2 CO3 ), oral fluid samples were liquid-liquid extracted (ButOAc/EtOAc, 1:1). As little as 1 microlitre of a mixture of this extract and the MALDI matrix (alpha-cyano-4-hydroxycinnamic acid) was spotted onto the MALDI plate and could directly be analyzed. With MALDI omitting chromatographic separation, very short analysis times of about 10 s per sample were possible. The method was developed and validated according to international guidelines including specificity, recovery, matrix effects, accuracy and precision, stabilities and limit of quantification. All validation criteria were fulfilled except for ion suppression/enhancement. Comparison with a routine liquid chromatography-tandem mass spectrometry (LC-MS/MS) method showed good agreement of the results. Applicability of the method was shown by analyzing about 250 oral fluid samples collected after controlled administration of 125 mg MDMA in a pharmacokinetic study. The whole lot of samples could be analyzed in less than 1 h, proving the ultra-high-speed of the method. PMID:25990956

  12. 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

  13. An ultra-high-performance liquid chromatography-tandem mass spectrometric method for the determination of hederacoside C, a drug candidate for respiratory disorder, in rat plasma.

    Science.gov (United States)

    Rehman, Shaheed Ur; Choi, Min Sun; Kim, In Sook; Kim, Seung Hyun; Yoo, Hye Hyun

    2016-09-10

    Hederacoside C is a principal bioactive pharmaceutical ingredient of Hedera helix leaf extracts. H. helix extracts have long been used in folk medicine for the treatment of respiratory disorders. Currently, hederacoside C is investigated as a promising candidate for the treatment of respiratory diseases. In this study, an accurate, sensitive, rapid, and reliable bioanalytical method was developed for the determination of hederacoside C in rat plasma using ultra high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). For sample preparation, plasma proteins were precipitated with 0.1% acetic acid in acetonitrile. Waters UPLC BEH C18 (2.1mm I.D.×100mm, 1.7μm) column was used for chromatographic separation. A gradient elution of mobile phases consisting of 0.02% acetic acid in distilled water (solvent A) and 0.02% acetic acid in acetonitrile (solvent B) was used at a flow rate of 0.3mL/min. The multiple reaction monitoring (MRM) mode was used for mass spectrometric detection; the MRM transitions were m/z 1219.7→m/z 469.2 for hederacoside C and m/z 1108.3→m/z 221.2 for ginsenoside Rb1 (internal standard) in the negative ionization mode. A calibration curve was constructed in the range of 10-1000ng/mL. The intra- and inter-day precision and accuracy were within 5%. The developed UPLC-MS/MS method was successfully applied in a pharmacokinetic study of hederacoside C in rats. Hederacoside C was quickly but inadequately absorbed from the gastrointestinal tract of rats resulting in extremely low bioavailability and relatively slow clearance.

  14. Simultaneous determination of major type A and B trichothecenes, zearalenone and certain modified metabolites in Finnish cereal grains with a novel liquid chromatography-tandem mass spectrometric method.

    Science.gov (United States)

    Nathanail, Alexis V; Syvähuoko, Jenna; Malachová, Alexandra; Jestoi, Marika; Varga, Elisabeth; Michlmayr, Herbert; Adam, Gerhard; Sieviläinen, Elina; Berthiller, Franz; Peltonen, Kimmo

    2015-06-01

    A reliable and sensitive liquid chromatography-tandem mass spectrometric method was developed for the simultaneous quantitative determination in cereals of the Fusarium mycotoxins HT-2 toxin, T-2 toxin, deoxynivalenol, nivalenol and zearalenone, as well as the modified metabolites 3-acetyl-deoxynivalenol, α-zearalenol, β-zearalenol, deoxynivalenol-3-glucoside, HT-2-3-glucoside, nivalenol-3-glucoside, zearalenone-14-glucoside, zearalenone-14-sulphate, zearalenone-16-glucoside, α-zearalenol-14-glucoside and β-zearalenol-14-glucoside. The 'dilute and shoot' approach was used for sample preparation after extraction with acetonitrile:water:acetic acid (79:20:1, v/v/v). Separation was carried out using reversed-phase liquid chromatography, and detection was performed using tandem mass spectrometry in the selected reaction monitoring mode. The method was in-house validated according to performance characteristics, established in Commission Regulation EC No 401/2006 and Commission Decision EC No 657/2002, prior to its application in a nationwide survey for the analysis of barley, oat and wheat samples (n = 95) harvested in Finland during 2013. Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively. Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing. All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

  15. Determination of trace elements in various kinds of bean by X-ray spectrometric techniques (1995-96)

    International Nuclear Information System (INIS)

    Various kinds of bean such as Peanut, Gram Whole, Black Eye Bean, Small Red Bean, Lab Lab Bean, Green Mung Bean, Filed Pea, Seasame Seed, Sultani, Maize, Butter Bean, Dolichos Lab Lab, Toor Whole, Small Yellow Bean, Cow Pea have been collected and analysed by EDXRF analysis for trace elements. The measurement system consists of a Cd-109 annual excitation source, a Si (Li) detector, H V power supply, a spectrometry amplifier, a multichannel analyser and a personal computer. The samples were prepared as pressed pellets and measured by Emission Transmission Technique. The accuracy was determined by analysing standard reference material, SOIL-7 form IAEA. (author)

  16. Analysis for chloroanisoles and chlorophenols in cork by stir bar sorptive extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Callejon, R M; Troncoso, A M; Morales, M L

    2007-03-30

    A complete methodology for the determination of chloroanisoles and chlorophenols in cork material is proposed. The determination is accomplished by means of a previous liquid-solid extraction followed by stir bar sorptive extraction (SBSE) coupled to gas chromatography-mass spectrometry (GC-MS). Two different liquid-solid extraction experiments were conducted and eight compounds considered (2,6-dichloroanisole, 2,4-dichloroanisole, 2,4,6-trichloroanisole, 2,4,6-trichlorophenol, 2,3,4,6-tetrachloroanisole, 2,3,4,6-tetrachlorophenol, pentachloroanisole and pentachlorophenol). From the results obtained we can conclude that high volume extraction extending extraction time up to 24h is the best choice if we have to release compounds from the inner surfaces of cork stoppers. Recovery percentages ranged from 51% for pentachloroanisole to 81% for 2,4-dichloroanisole. This method allows the determination of an array of compounds involved in cork taint at very low levels from 1.2ng g(-1) for 2,4,6-tricholoroanisole to 23.03ng g(-1) for 2,3,4,6-tetrachlorophenol. PMID:19071569

  17. Development of a Gas Chromatography-Mass Spectrometry Method for the Quantification of Glucaric Acid Derivatives in Beverage Substrates

    Directory of Open Access Journals (Sweden)

    Ana Paula Craig

    2014-01-01

    Full Text Available A gas chromatography-mass spectrometry (GC-MS method using the standard addition methodology was developed for the determination of glucuronolactone (GL and glucuronic acid (DGuA in four beverages categorized as detoxification, recovery, or energy drinks. The method features a precolumn derivatization step with a combination of BSTFA (N,O-bis(trimethylsilyltrifluoroacetamide and TMCS (trimethylchlorosilane to silylate the analytes. The sample pretreatment required no extraction, filtration, or reduction step prior to the injection. The quantification of the analytes was performed using a five-point standard addition protocol. The proposed method presented excellent intraday precision (%RSD 0.995 and acceptable linearity for DGuA calibration curves (correlation coefficients > 0.97. The estimated limits of detection (LOD and quantification (LOQ for GL ranged from 0.006 ppm to 0.14 ppm, and 0.02 ppm to 0.47 ppm, respectively. The estimated LOD and LOQ for DGuA determination ranged, respectively, from 0.06 ppm to 1.1 ppm and 0.2 ppm to 3.8 ppm. The results demonstrated that the method should be regarded as a reliable alternative to the simultaneous determination of GL and DGuA.

  18. Development of a gas chromatography-mass spectrometry method for the quantification of glucaric Acid derivatives in beverage substrates.

    Science.gov (United States)

    Craig, Ana Paula; Fields, Christine C; Simpson, John V

    2014-01-01

    A gas chromatography-mass spectrometry (GC-MS) method using the standard addition methodology was developed for the determination of glucuronolactone (GL) and glucuronic acid (DGuA) in four beverages categorized as detoxification, recovery, or energy drinks. The method features a precolumn derivatization step with a combination of BSTFA (N,O-bis(trimethylsilyl)trifluoroacetamide) and TMCS (trimethylchlorosilane) to silylate the analytes. The sample pretreatment required no extraction, filtration, or reduction step prior to the injection. The quantification of the analytes was performed using a five-point standard addition protocol. The proposed method presented excellent intraday precision (%RSD 0.995) and acceptable linearity for DGuA calibration curves (correlation coefficients > 0.97). The estimated limits of detection (LOD) and quantification (LOQ) for GL ranged from 0.006 ppm to 0.14 ppm, and 0.02 ppm to 0.47 ppm, respectively. The estimated LOD and LOQ for DGuA determination ranged, respectively, from 0.06 ppm to 1.1 ppm and 0.2 ppm to 3.8 ppm. The results demonstrated that the method should be regarded as a reliable alternative to the simultaneous determination of GL and DGuA. PMID:25024704

  19. Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography - mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cardellicchio, N.; Giandomenico, S.; Decataldo, A.; Di Leo, A. [CNR - Istituto Sperimentale Talassografico, Taranto (Italy)

    2001-03-01

    A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry.The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown. (orig.)

  20. Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography mass spectrometry.

    Science.gov (United States)

    Cardellicchio, N; Giandomenico, S; Decataldo, A; Di Leo, A

    2001-03-01

    A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry. The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown. PMID:11336336

  1. Quantitative analysis of arbutin and hydroquinone in strawberry tree (Arbutus unedo L., Ericaceae) leaves by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jurica, Karlo; Karačonji, Irena Brčić; Šegan, Sandra; Opsenica, Dušanka Milojković; Kremer, Dario

    2015-09-01

    The phenolic glycoside arbutin and its metabolite with uroantiseptic activity hydroquinone occur naturally in the leaves of various medicinal plants and spices. In this study, an extraction procedure coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine arbutin and hydroquinone content in strawberry tree (Arbutus unedo L., Ericaceae) leaves. The method showed good linearity (R2>0.9987) in the tested concentration range (0.5-200 μg mL(-1)), as well as good precision (RSDarbutin and hydroquinone, respectively). The results obtained by the validated GC-MS method corresponded well to those obtained by high performance liquid chromatography (HPLC) method. The proposed method was then applied for determining arbutin and hydroquinone content in methanolic leaf extracts. The amount of arbutin in the leaves collected on the island of Koločep (6.82 mg g(-1) dry weight) was found to be higher (tpaired=43.57, tc=2.92) in comparison to the amount of arbutin in the leaves collected on the island of Mali Lošinj (2.75 mg g(-1) dry weight). Hydroquinone was not detected in any of the samples. The analytical features of the proposed GC-MS method demonstrated that arbutin and hydroquinone could be determined alternatively by gas chromatography. Due to its wide concentration range, the method could also be suitable for arbutin and hydroquinone analysis in leaves of other plant families (Rosaceae, Lamiaceae, etc.). PMID:26444340

  2. A novel, donor-active solvent-ass