Temperature-Programmed Gas Chromatographic Determination of Polychlorinated and Polybrominated Biphenyls in Serum

1981 ◽  
Vol 64 (5) ◽  
pp. 1131-1137
Author(s):  
Larry L Needham ◽  
Virlyn W Burse ◽  
Harold A Price
Keyword(s):  
Gas Chromatography ◽  
Human Serum ◽  
Analytical Method ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Polybrominated Biphenyls ◽  
Coefficients Of Variation ◽  
Temperature Programmed

Abstract An analytical method was developed to quantitate polychlorinated and polybrominated biphenyls (PCBs and PBBs, respectively) in human serum. The method includes denaturation of the proteins in serum, extraction, adsorption chromatography, and gas chromatography with electron capture detection. The coefficients of variation for determining the in vivo bound PCBs and PBBs ranged from 11.7 to 29.8% and 7.1 to 14.0%, respectively. The method is capable of measuring 10 ng PCBs and PBBs/mL in 4 mL serum.

Gas Chromatographic Determination of Captan, Folpet, and Captafol Residues in Tomatoes, Cucumbers, and Apples Using a Wide-Bore Capillary Column: Interlaboratory Study

1991 ◽  
Vol 74 (5) ◽  
pp. 830-835 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Capillary Column ◽  
Chromatographic Determination ◽  
Interlaboratory Study ◽  
Electron Capture Detection ◽  
Coefficients Of Variation ◽  
Capillary Column Gas Chromatography ◽  
Ppm Level

Abstract An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multlresidue method modified to Include additional solvent elutlon in the optional Florisll column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol In apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.

scholarly journals Gel Permeation and Florisil Chromatographic Cleanup and Gas Chromatographic Determination of Organochlorine Pesticides in Eggs

1998 ◽  
Vol 81 (5) ◽  
pp. 1033-1036 ◽  
Author(s):  
Naoto Furusawa ◽  
Kunio Okazaki ◽  
Sachiko Iriguchi ◽  
Hidemasa Yamaguchi ◽  
Minoru Saitoh
Keyword(s):  
Gas Chromatography ◽  
Organochlorine Pesticides ◽  
Mobile Phase ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Coefficients Of Variation ◽  
Gel Permeation ◽  
Whole Egg

Abstract Cleanup of residual organochlorine pesticides (OCPs; α-, β-, γ-, and δ-BHC; aldrin; dieldrin; p,p′-DDE; o,p′-DDT; p,p′-DDD; and p,p′-DUX) in eggs by gel permeation chromatography (GPC) and Florisil minicolumn chromatography is described. Ten OCPs in purified extract are determined by gas chromatography with electron capture detection. The lipids extracted from whole egg are cleaned up first by GPC with an Envirogel column and an ethyl acetate-cychlohexane (1 + 1, v/v) mobile phase and then by Florisil minicolumn chromatography with 15% (v/v) diethyl ether-hexane eluant. Cleanup is highly efficient. Average recoveries of 10 spiked OCPs (0.0025-0.0125 ppm) ranged from 81 to 101%, with coefficients of variation between 1 and 14%. The detection limit was 0.001 ppm for the 10 OCPs

Evaluation of Potential Analytical Approach for Determination of Polychlorinated Biphenyls in Serum: Interlaboratory Study

1983 ◽  
Vol 66 (4) ◽  
pp. 956-968
Author(s):  
Virlyn W Burse ◽  
Larry L Needham ◽  
Chester R Lapeza ◽  
Margaret P Korver ◽  
John A Liddle ◽  
...  
Keyword(s):  
Polychlorinated Biphenyls ◽  
Ethyl Ether ◽  
Analytical Approach ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Coefficients Of Variation ◽  
The Mean

Abstract Forty-four laboratories participated in evaluation of a method for determining polychlorinated biphenyls (PCBs) as AR 1254 in serum at the parts per billion level. The method involves deproteinating serum with methanol, extracting with hexane-ethyl ether, and eluting PCBs from deactivated silica gel for gasliquid chromatographic determination with electron capture detection. Compounds are quantitated by using the Webb-McCall factors. Five serum pools, 4 containing in vivo-fortified PCBs (as AR 1254) or 8 in vitro-f ortif ied chlorinated hydrocarbons (CHs), or both, were used. For PCB fortification levels of 9.89 (EP 2), 24.74 (EP 3), and 74.20 ppb (EP 4), interlaboratory coefficients of variation (CVs) for collaborators that adhered to protocol were 92.7, 67.6, and 25.8%, respectively. CVs on the same pools analyzed by the Centers for Disease Control (CDC) were 7.4, 7.8, and 4.6%, respectively. Average interlaboratory recoveries for pools EP 2, EP 3, and EP 4 were 138.1,111.2, and 91.1%, respectively, and 99.8,89.6, and 90.4%, respectively, for CDC on the same pools. There was a general decrease in the mean error for those laboratories that had participated in an earlier study in which they were allowed to use their own methods.

Extraction and determination of chloroform in rat blood and tissues by gas chromatography-electron-capture detection: distribution of chloroform in the animal body.

1980 ◽  
Vol 26 (1) ◽  
pp. 66-68 ◽  
Author(s):  
C R Vogt ◽  
J C Liao ◽  
A Y Sun
Keyword(s):  
Gas Chromatography ◽  
Detection Limit ◽  
Accurate Method ◽  
Electron Capture Detection ◽  
Fat Tissue ◽  
Rat Blood ◽  
Kidney Liver ◽  
Different Tissues

Abstract We have developed a simple, sensitive, and accurate method for the determination of chloroform in rat blood, brain, kidney, liver, and fat. The detection limit is 2.5 ng of chloroform per gram of tissue. Studies of in vivo distribution of chloroform in rat blood and target tissues after intragastric intubation of chloroform/water show that the amount of chloroform accumulated in the different tissues increases with increasing doses. Fat tissue contains the greatest amount of chloroform. The accumulation of chloroform in rat blood and target tissues seems to be maximum 1.5 h after administration, and the apparent chloroform concentration is almost at baseline value 8 h later.

Gas Chromatographic Determination of Primary and Secondary Amines as Pentafluorobenzamide Derivatives

1982 ◽  
Vol 65 (5) ◽  
pp. 1066-1072
Author(s):  
Brian D Ripley ◽  
Bruce J French ◽  
Lloyd V Edgington
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Analytical Method ◽  
Chromatographic Determination ◽  
Sample Volume ◽  
Secondary Amines ◽  
Primary And Secondary Amines

Abstract An analytical method is described for the determination of mono- and dialkylamines in foodstuffs. Amines are derivatized to their pentafluorobenzamides which may be separated by gas chromatography (GC) and determined using an N-P detector. Analysis of the derivatives by GC-mass spectrometry indicated they were all mono-substituted. The amines were isolated from foodstuffs by alkaline distillation of ≥75% sample volume. The distribution of dimethylamine (DMA) in distillate volumes indicated 2 maxima from barley and malt, which could represent 2 or more sources of DMA. DMA concentrations of 6.6-8.8 ppm in barley, 11 ppm in malt, and 1.2 ppm in beer are higher than previously reported.

Gas-Chromatographic Determination of Theophylline in Human Serum and Saliva

1975 ◽  
Vol 21 (1) ◽  
pp. 144-147 ◽  
Author(s):  
George F Johnson ◽  
Walter A Dechtiaruk ◽  
Harvey M Solomon
Keyword(s):  
Gas Chromatography ◽  
Human Serum ◽  
Patient Compliance ◽  
Alkylating Agent ◽  
Chromatographic Determination ◽  
Allergy Clinic ◽  
Pediatric Allergy ◽  
Chromatographic Procedure

Abstract We report a gas-chromatographic procedure for routine determination of the bronchodilator, theophylline (1,3-dimethylxanthine), in serum and saliva. Volatile butyl derivatives for gas chromatography were prepared by the method of Greeley [Clln. Chem. 20, 192 (1974)], with butyliodide as the alkylating agent. Substances that interfere in the classical determination of theophylline, such as theobromine (3,7-dimethylxanthine) and phenobarbital, are well separated from theophylline by the gas-chromatographic procedure and can be quantitated if desired. It is possible to determine 1 µg of theophylline in 1 ml of serum or saliva. Between-run precision for 15 µg/ml samples was 5.3%. This determination is useful in assessing patient compliance with medication instructions and in adjusting dosage schedules of theophylline in patients attending a pediatric allergy clinic.

scholarly journals Determination of Fluvalinate Residues in Beeswax by Gas Chromatography with Electron-Capture Detection

2000 ◽  
Vol 83 (5) ◽  
pp. 1225-1228 ◽  
Author(s):  
Angeliki Tsigouri ◽  
Urania Menkissoglu-Spiroudi ◽  
Andreas T Thrasyvoulou ◽  
Grigorios C Diamantidis
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Diethyl Ether ◽  
Capillary Gas Chromatography ◽  
Diatomaceous Earth ◽  
Accurate Method ◽  
Electron Capture Detection ◽  
Limit Of Determination ◽  
Coefficients Of Variation

Abstract A simple, rapid, and accurate method is described for the determination of residual fluvalinate in beeswax. The procedure consists of partitioning on a disposable column of diatomaceous earth (Extrelut®), followed by chromatographic cleanup on a Florisil cartridge. The final extract is analyzed by capillary gas chromatography with electron-capture detection (GC–ECD). Briefly, wax samples were dissolved in n-hexane, and the solutions were sonicated and transferred to Extrelut columns. The fluvalinate was extracted with acetonitrile, and a portion of the extract was cleaned up on a Florisil cartridge. The fluvalinate was eluted with diethyl ether–n-hexane (1 + 1) and directly determined by GC–ECD. Recoveries from wax samples spiked at 5 fortification levels (100–1500 μg/kg) ranged from 77.4 to 87.3%, with coefficients of variation of 5.12–8.31%. The overall recovery of the method was 81.4 ± 3.2%, and the limit of determination was 100 μg/kg.

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