Multiresidue Gas Chromatographic Method for Determining Organochlorine Pesticides in Meats: Validation Study for Swine and Beef Fats

1985 ◽  
Vol 68 (5) ◽  
pp. 941-944
Author(s):  
James A Ault ◽  
Timothy E Spurgeon ◽  
Douglas S Gillard ◽  
Edward T Mallinson
Keyword(s):  
Organochlorine Pesticides ◽  
Validation Study ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Heptachlor Epoxide ◽  
Average Recovery ◽  
Coefficients Of Variation ◽  
Poultry Fat ◽  
Gas Chromatographic Method

Abstract A validation of a previously studied method for determining organochlorine residues in poultry fat was conducted to extend the usefulness of the method to beef and swine fats. The validation samples consisted of 16 materials all analyzed in duplicate. Fortification levels ranged from 0.02 to 1.2 ppm for a-BHC, lindane, cis- and Irans-chlordane, octachlor epoxide, o,p'- and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 101 % with a range of 7 9 - 113%, not including toxaphene. The ranges of coefficients of variation wtreCV. = 0-23.37% and CVX = 3.74-26.19%. The results were comparable to the previous collaborative study of the same method for poultry fat. The extended method has been adopted official first action

Multiresidue Gas Chromatographic Method for Determining Organochlorine Pesticides in Poultry Fat: Collaborative Study

1984 ◽  
Vol 67 (2) ◽  
pp. 284-289 ◽  
Author(s):  
James A Ault ◽  
Tim E Spurgeon ◽  
◽  
M M Anderson ◽  
R Bowers ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Gel Permeation Chromatography ◽  
Accuracy And Precision ◽  
Coefficients Of Variation ◽  
Poultry Fat ◽  
Gel Permeation ◽  
Detector Method ◽  
Gas Chromatographic Method

Abstract A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for a-BHC, lindane, cis- and frans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.

Collaborative Study of a Gas Chromatographic Method for Ronnel in Feeds

1969 ◽  
Vol 52 (3) ◽  
pp. 435-438
Author(s):  
Albert J Gehrt
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Flame Ionization Detector ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Chromatographic Measurement ◽  
Cattle Feeds ◽  
Gas Chromatographic Method

Abstract A GLC method (flame ionization detector) for ronnel in cattle feeds at levels of 0.038, 0.041, and 0.055% was studied by 11 collaborators. The method involves extraction of ronnel by shaking with acetone followed by direct chromatographic measurement. The method is simple and rapid (no cleanup required), measures true ronnel, and is free from interferences present in the UV methods previously studied. Agreement between laboratories was satisfactory; coefficients of variation were 11.0, 12.0, and 7.2%. Ronnel recoveries were 81.1, 93.5, and 98.0%. Low recovery from the first sample may be due to ronnel hydrolysis or binding during storage (sample was 8 months old). The Associate Keferee recommends that the method be adopted as official first action.

Gas Chromatographic Method for Determination of Cypermethrin in Pesticide Formulations: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 51-53
Author(s):  
J F C Tyler
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Coefficients Of Variation ◽  
Pesticide Formulations ◽  
Glass Column ◽  
Technical Material ◽  
Gas Chromatographic Method ◽  
Ethylhexyl Phthalate

Abstract A gas chromatographic method for determination of total cypermethrin in technical and formulated products has been developed and subjected to a collaborative study involving IS participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing di(2-ethylhexyl) phthalate as internal standard and analyzed by gas chromatography on a glass column with 3% OV-101 on Chromosorb W-HP. Each collaborator was furnished with reference stdard and 4 samples of technical material, 3 emulsifiable concentrates, one wettable powder, and one ultralow volume formulation for analysis. The coefficients of variation of the results obtained ranged from 0.955 to 1.7462%. The method has been adopted as official first action by AOAC.

Gas Chromatographic Method for Determination of Permethrin in Pesticide Formulations: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 53-55
Author(s):  
J F C Tyler
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Isobutyl Ketone ◽  
Coefficients Of Variation ◽  
Pesticide Formulations ◽  
Glass Column ◽  
Technical Material ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for determination of permethrin in technical and formulated products has been developed and subjected to a collaborative study involving 19 participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing n-octacosane as internal standard and analyzed by gas chromatography on a glass column with 3% OV-210 on Chromosorb W-HP. Each collaborator was furnished with reference standard and 5 samples of technical material (90-95%), 8 emulsifiable concentrates (10-50%), 2 wettable powders (20-30%), one dustable powder (1-2%), and one mter-dispersible granules (1-2%) for analysis. The coefficients of variation of the results obtained ranged from 0.79 to 4.24%. The method has been adopted as official first action by AOAC.

Gas Chromatographic Determination of Fensulfothion in Formulations: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 488-490
Author(s):  
William R Betker ◽  
◽  
E W Balcer ◽  
O O Bennett ◽  
W R Coffman ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Chromatograph ◽  
Technical Product ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A collaborative study was conducted on a gas chromatographic method for determination of fensulfothion. Eleven laboratories analyzed 2 technical and two 6 lb/U.S. gal. spray concentrate samples. In the analysis, samples are dissolved in methylene chloride which contains 4-chlorophenyl sulfoxide as an internal standard, and solutions are injected into a gas chromatograph equipped with an OV-330 column. Withinlaboratory repeatability was 0.79% for technical product and 0.37% for the spray concentrate samples, with coefficients of variation of 0.88 and 0.58%, respectively. Among-laboratories reproducibility was 0.81% for technical product and 0.53% for the spray concentrate, with coefficients of variation of 0.91 and 0.84%, respectively. The method has been adopted official first action.

Collaborative Study of a Gas Chromatographic Method for Ipronidazole in Feeds

1971 ◽  
Vol 54 (1) ◽  
pp. 72-74
Author(s):  
Elmer De Ritter ◽  
Modest Osadca
Keyword(s):  
Electron Capture ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Electron Capture Detector ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A GLC method for ipronidazole in turkey feeds at levels of 0.0033, 0.0066, and 0.0099% was studied by 7 laboratories. Ipronidazole is extracted by shaking with warm 0.2N HCl. An aliquot of the extract is made alkaline and the ipronidazole is extracted with benzene and diluted further for GLC with an electron capture detector. The method is simple, rapid, and free from interference. Agreement between laboratories was very satisfactory; coefficients of variation were 7.1, 3.0, and 8.0%. Recoveries of ipronidazole were 97, 96, and 99%. It is recommended that the method be adopted as official first action and that the study be continued.

Headspace Gas Chromatographic Method for Determination of Ethanol in Canned Salmon: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 524-526
Author(s):  
Thomas A Hollingworth ◽  
Harold R Throm ◽  
Marleen M Wekell ◽  
William F Trager ◽  
Michael W O’Donnell ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Sampling Technique ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Headspace Gas ◽  
The Mean ◽  
Gas Chromatographic Method

Abstract Six laboratories collaboratively studied a headspace gas chromatographic method for determination of ethanol in the aqueous phase of canned salmon. Ethanol is determined by a headspace sampling technique with tert-butanol as the internal standard, using a gas chromatograph equipped with a Super Q column and a flame ionization detector. With outliers excluded, the mean recoveries from samples spiked with 25.1 and 78.4 ppm ethanol were 112 and 110%, respectively. For the 4 sample pairs quantitated, repeatability coefficients of variation ranged from 1.42 to 4.25% and reproducibility coefficients of variation from 2.55 to 8.09%, with 3 of the 4 reported values less than 5%. The method has been adopted official first action.

Gas Chromatographic Determination of Isofenphos in Technical and Formulated Products: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 55-57
Author(s):  
Daniel E Terry
Keyword(s):  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of isofenphos (OFTANOL®) in isofenphos technical and liquid formulations has been developed and collaboratively studied by 11 laboratories. Two technical samples and 2 liquid flowable samples were analyzed after shaking/extracting in methanol which contained diisobutyl phthalate as an internal standard. The extracts were analyzed by gas chromatography using an SP-2100 column and either flame ionization or thermal conductivity detection. Coefficients of variation were 0.57 and 1.27% for the technical and formulated products, respectively. The GC method has been adopted official first action as a AOACCTPAC method.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 419-421
Author(s):  
George Yip
Keyword(s):  
Gas Chromatography ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method ◽  
Hydrolysis Of ◽  
Ppm Level

Abstract Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1 % SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.

Determination of Several Chlorinated Pesticides by the AOAC Multiresidue Method with Additional Quantitation of Perthane after Dehydrochlorination: Collaborative Study

1973 ◽  
Vol 56 (3) ◽  
pp. 721-727
Author(s):  
Richard T Krause
Keyword(s):  
Parent Compound ◽  
Collaborative Study ◽  
Heptachlor Epoxide ◽  
Chlorinated Pesticides ◽  
Average Recovery ◽  
Multiresidue Method ◽  
Coefficients Of Variation ◽  
Before And After ◽  
Coefficients Of Variations

Abstract The AOAC multiresidue method for chlorinated pesticides, 29.001–29.017, was studied collaboratively by 7 laboratories. Perthane, heptachlor epoxide, mirex, and dieldrin were determined in apple and cauliflower samples fortified at 2 levels, and Perthane was determined in butterfat samples fortified at 2 levels. Perthane was quantitatively measured before and after a simplified dehydrochlorination procedure. Average recoveries and coefficients of variations for pesticides in the apple samples for both levels were: Perthane 100±10%, heptachlor epoxide 102±14%, mirex 96±9%, dieldrin 101±14%, and Perthane (after dehydrochlorination and recalculation to the parent compound) 100±9%. Average recoveries and coefficients of variation for pesticides in the cauliflower samples for both levels were: Perthane 105±9%, heptachlor epoxide 103± 15%, mirex 103±7%, dieldrin 98±11%, and Perthane (after dehydrochlorination and recalculation) 100±10%. The average recovery for both levels of Perthane (after dehydrochlorination and recalculation) in the butterfat samples was 91±10%. For a spinach sample with field-incurred residues the collaborators found an average of 4.47 ppm Perthane before dehydrochlorination and 5.09 ppm Perthane as the olefin after dehydrochlorination. In most instances, the identities of all the residues were confirmed by TLC. The dehydrochlorination technique has been adopted as official first action.

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