Collaborative Study of Clopidol in Chicken Tissues and Eggs, Using Gas-Liquid Chromatography

1974 ◽  
Vol 57 (4) ◽  
pp. 914-918
Author(s):  
E Leroy Bjerke ◽  
James L Herman
Keyword(s):  
Gas Chromatography ◽  
Exchange Resin ◽  
Anion Exchange Resin ◽  
Collaborative Study ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Improved Method ◽  
Average Recovery ◽  
Chicken Tissues ◽  
Unknown Sample

Abstract Ten collaborators participated in a study of an improved method for determining residues of the coccidiostat clopidol (3,5-dichloro-2,6- dimethyl-4-pyridinol) in chicken tissues and eggs. Tissues are extracted with methanol and the extract is cleaned up with columns of alumina and anion exchange resin. After methylation with diazomethane reagent, clopidol methyl ether is determined by gas chromatography with electron capture detection. The method is applicable to levels as low as 0.1 ppm in chicken tissues and 0.05 ppm in eggs. Results from 9 collaborators gave an average recovery of 84% from muscle, 90% from liver, and 84% from eggs. Results from an unknown sample of each substrate were excellent. The method has been adopted as official first action.

Gas Chromatographic Determination of Deoxynivalenol in Wheat with Electron Capture Detection: Collaborative Study

1986 ◽  
Vol 69 (5) ◽  
pp. 899-901 ◽  
Author(s):  
George M Ware ◽  
Octave J Francis ◽  
Allen S Carman ◽  
Shia S Kuan ◽  
◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Collaborative Study ◽  
Control Sample ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Average Recovery ◽  
Repeatability And Reproducibility ◽  
The Mean

Abstract Ten laboratories participated in a collaborative study of a method for the determination of deoxynivalenol in wheat by gas chromatography with electron capture detection. Each laboratory analyzed 6 samples in duplicate. Each collaborator received samples spiked at the 100.3, 501.3, and 1002.6 ng/g levels; a control sample; and 2 naturally contaminated samples. The average recovery (outliers excluded) for the spiked samples was 92.2%. The mean repeatability and reproducibility, respectively, were 32.2 and 41.3% for the spiked samples and 30.9 and 47.6% for the naturally contaminated samples. The method was adopted official first action.

Quantitative Determination of FD&C Colors in Foods

1975 ◽  
Vol 58 (2) ◽  
pp. 278-282
Author(s):  
Charles Graichen
Keyword(s):  
Quantitative Determination ◽  
Anion Exchange ◽  
Salt Solution ◽  
Exchange Resin ◽  
Anion Exchange Resin ◽  
Collaborative Study ◽  
Chromatographic Technique ◽  
Different Color ◽  
Selection Of

Abstract A published procedure using Amberlite LA-2 (a liquid anion exchange resin) solutions to extract colors from food and the salt solution cellulose chromatographic technique to separate colors from each other were updated and submitted to collaborative study. Three batches of cookies and 4 purchased products were analyzed by 13 collaborators. The 3 batches of cookies contained different color mixtures requiring the selection of various procedures. The 4 purchased products were selected principally to include a variety of foods. Some results were partially deficient. The deficiencies reflect certain inadequacies in the directions as written rather than basic flaws in the method. Some improvements were suggested by the collaborators. The Associate Referee recommends that the method be further revised to correct the present inadequacies and to include some improvements, and that the revised method be submitted to another collaborative study.

Collaborative Study of Three Methods for the Determination of Fluoride in Vegetation

1978 ◽  
Vol 61 (1) ◽  
pp. 150-153
Author(s):  
Jay S Jacobson ◽  
Laurence I Heller
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Polychlorinated Biphenyls ◽  
Collaborative Study ◽  
Bald Eagle ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Florisil Column ◽  
Average Recovery

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2ffcyclobuta[ cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2S04-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography (GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry

Gas Chromatography with Electron Capture and Mass Spectrometric Detection of Deoxynivalenol in Wheat and Other Grains

1981 ◽  
Vol 64 (6) ◽  
pp. 1364-1371 ◽  
Author(s):  
Peter M Scott ◽  
Pui-Yan Lau ◽  
Shriniwas R Kanhere
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Sulfate Solution ◽  
Mass Spectrometric ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Ammonium Sulfate Solution ◽  
Sample Extract ◽  
Coefficients Of Variation ◽  
Made In

Abstract A method for determining deoxynivalenol (DON) in wheat has been developed in conjunction with an assessment of contamination in Canada. The sample is extracted with methanol-water; the extract is treated with 30% aqueous ammonium sulfate solution and extracted with 4 portions of ethyl acetate. After further cleanup by column chromatography, the sample extract is derivatized with AT-heptafluorobutyrylimidazole, and the DON tris-heptafluorobutyrate is determined by gas-liquid chromatography with electron capture detection. Mass spectrometric single ion monitoring at m/z 884 is used for confirmation. Detection limits are ≤0.01 μg DON/g and recoveries from wheat, using the proposed method, averaged 72 and 80% in 2 different laboratories, with coefficients of variation of 10.2 and 10.0%, respectively. The method is also applicable to determining DON in barley and corn and T-2 toxin in wheat. Virtually 100% contamination by DON of the 1980 Ontario white winter wheat and Quebec red spring wheat crops was found, based on 72 analyses made in this laboratory, but western Canadian wheat contained little or no DON.

Capillary Gas Chromatographic Determination of Technical Chlordane in Emulsifiable Concentrates and Aqueous Dilutions

1985 ◽  
Vol 68 (2) ◽  
pp. 175-176
Author(s):  
Rodger W Stringham ◽  
Ray P Schulz
Keyword(s):  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Regression Coefficient ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Average Recovery ◽  
Titrimetric Method ◽  
Relative Standard ◽  
Aoac Official

Abstract Technical chlordane is extracted in acetone, diluted with hexane, and determined via capillary gas chromatography with electron capture detection. Quantitation is based on the sum of areas or heights of 6 well resolved major peaks. The method was tested for precision, linearity, recovery, and applicability to aqueous dilutions of emulsifiable concentrate formulations. Comparison of quadruplicate analysis of 5 formulations by this method with the AOAC official titrimetric method gave average relative standard deviations of 1.4 and 0.9 %, respectively. Results were comparable for the 72% formulations, but were lower using this method for the 45% samples. Linearity and recovery were excellent (regression coefficient = 0.9996, recovery = 100.7%). Application of this method to aqueous dilutions was simple and resulted in an average recovery of 97%. The method is faster, safer, and more specific than the AOAC titrimetric method.

scholarly journals Determination of Pesticide Residues in Lettuce by Gas Chromatography with Electron-Capture Detection

2007 ◽  
Vol 90 (6) ◽  
pp. 1670-1676 ◽  
Author(s):  
Jose Fenoll ◽  
Pilar Hellin ◽  
Josefa Lopez ◽  
Alberto Gonzalez ◽  
Pilar Flores
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Electron Capture Detection ◽  
Selected Ion Monitoring ◽  
Average Recovery ◽  
Relative Standard ◽  
Different Types ◽  
Confirmation Analysis ◽  
Subsequent Sample

Abstract A sensitive, rapid, and simple multiresidue method for the simultaneous determination of 19 pesticides in different varieties of lettuce (Lactuca sativum) was developed. Lettuce samples were extracted by homogenization with acetone and partitioned into ethyl acetatecyclohexane. Subsequent sample cleanup was not needed. Final determination was made by capillary gas chromatography (GC) with electron-capture detection (ECD). Confirmation analysis of pesticides was performed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recovery by the GCECD method obtained for these compounds varied from 66.4 to 119.2 with relative standard deviations <7.7. The GCECD method has good linearity, and the detection limit for the pesticides studied varied from 0.1 to 3.8 g/kg. The proposed method was used to determine pesticide levels in different types of lettuce grown in soils from experimental fields.

scholarly journals Determination of Hydrazine in Maleic Hydrazide Technical and Pesticide Formulations by Gas Chromatography: Collaborative Study

2008 ◽  
Vol 91 (1) ◽  
pp. 5-12 ◽  
Author(s):  
Anthony S Riggs ◽  
David M Borth ◽  
David G Tutty ◽  
Wan S Yu ◽  
B Barclay ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Gas Chromatography ◽  
Electron Capture ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Test Sample ◽  
Electron Capture Detection ◽  
Pesticide Formulations ◽  
Liquid Concentrate

Abstract Twelve collaborating laboratories assayed hydrazine in technical maleic hydrazide (MH), 6-hydroxy-2H-pyridazin-3-one, and 2 formulated products, a liquid concentrate and a soluble granule, using gas chromatography (GC) with electron capture detection. The hydrazine content in the samples ranged from 0.03 ppm, in the liquid concentrate, to 0.26 ppm, in MH technical. Hydrazine and MH are dissolved in an aqueous solution. The MH is then precipitated out of solution by acidification. The solution containing hydrazine is treated with excess pentafluorobenzaldehyde (PFB) to form pentafluorobenzaldehyde azine (PFBA). The PFBA is extracted with hexane for analysis by GC using an electron capture detector. Peak area responses of PFBA are measured and quantified by external standardization. Hydrazine concentration is calculated from the PFBA determination. The laboratories weighed each test sample in duplicate with duplicate analysis for each weighing. Data from these laboratories were statistically analyzed. The average relative repeatability was determined to be 5.34 and the average relative reproducibility was 27.99.

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