Gas-Liquid Chromatographic Determination of IV-Octylbicycloheptene Dicarboximide

1975 ◽  
Vol 58 (4) ◽  
pp. 845-849
Author(s):  
Vernon J Meinen

Abstract A gas-liquid chromatographic (GLC) method is described for the quantitative determination of /V-octylbicycloheptene dicarboximide (MGK 264 synergist) in technical materials and in various formulations. The samples are diluted with acetone and analyzed by GLC, using a flame ionization detector and a column packed with OV-1 on Chromosorb W (HP). Preliminary work indicates that satisfactory results can be obtained with the technical material and several different formulations.

1978 ◽  
Vol 61 (1) ◽  
pp. 164-166
Author(s):  
Fred A Moseley ◽  
Joel S Salinsky ◽  
Robert W Woods

Abstract A rapid and simple method of analysis has been developed for sorbitol in cooked sausage products. Sorbitol is extracted from cooked sausage products with water, an aliquot of the extract is freeze-dried, and the trimethylsilyl (TMS) derivative of sorbitol is formed. An aliquot of the TMS-sorbitol is injected into a gas chromatograph and measured by a flame ionization detector. Analysis of fortified samples shows that the recovery compares well with known amounts of sorbitol added.


1972 ◽  
Vol 55 (5) ◽  
pp. 907-912
Author(s):  
Vernon J Meinen

Abstract A gas chromatographic method is described for the quantitative determination of d-trans-allethrin in the technical product and in various formulations. The samples are diluted with acetone and analyzed by gas chromatography, using a flame ionization detector and a column packed with OV-1 on Chromosorb W (HP). Preliminary work indicates that satisfactory results can be obtained with the technical material and several different formulations. Since this method is more rapid and specific than the present AOAC titrimetric method, it is expected that it will be a valuable supplement to or alternative for the AOAC method for the analysis of allethrin.


1975 ◽  
Vol 58 (5) ◽  
pp. 1032-1036
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail

Abstract gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cistraras-(±)- 2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.


1976 ◽  
Vol 59 (1) ◽  
pp. 93-97 ◽  
Author(s):  
John M Newton

Abstract A gas-liquid chromatographic (GLC) method, using a 4% XE-60 on 80-100 mesh Gas-Chrom Q column, a flame ionization detector, and anthracene as the internal standard, has been developed for the direct determination of nikethamide. Eight collaborators analyzed 4 samples, using methanol as the solvent; the coefficients of variation obtained ranged from 1.19 to 3.20%. In a limited study with acetone as the solvent, the coefficients of variation ranged from 0.59 to 1.96%. The GLC method with acetone as a solvent has been adopted as official first action.


1974 ◽  
Vol 57 (1) ◽  
pp. 189-191
Author(s):  
James B Leary

Abstract A gas chromatographic method is described for determining acephate (O,S-dimethyl acetylphosphoramidothioate) and a metabolite, Ortho 9006 (O,S-dimethyl phosphoramidothioate), in a variety of crops. After extraction of the sample with ethyl acetate, the solvent is evaporated, and an ether solution of the residue is passed through a silica gel column to remove interferences. Acephate and Ortho 9006 are eluted from the column with 10% methanol in ether and measured simultaneously by programmed temperature gas chromatography, using an alkali flame ionization detector.


1976 ◽  
Vol 59 (5) ◽  
pp. 954-958 ◽  
Author(s):  
John E Smith ◽  
N Robert Pasarela ◽  
John C Wyckoff

Abstract A gas-liquid chromatographic (GLC) method is described for determining residues of levamisole, (1-)-(2,3,5,6-tetrahydro-6-phenylimidazo[2,1-b] thiazole), in milk. Levamisole is extracted from an alkaline milk sample with water-saturated ethyl acetate. After co-extractives are removed by various partitionings, the levamisole concentration is measured by GLC by using an alkali (RbSO4) flame ionization detector, vs. an external standard. This method is satisfactory for determining levamisole residues as low as 0.01 ppm in bovine milk. Apparent residues in control milk samples averaged <0.001 ppm. Recoveries of 0.01–2.0 ppm added levamisole ranged from 86.5 to 113%. Animals treated with various Tramisol® formulations showed apparent levamisole residues below the validated sensitivity of the method (0.01 ppm) at sampling periods exceeding 48 hr.


1979 ◽  
Vol 62 (2) ◽  
pp. 304-307
Author(s):  
Manfred J Prager ◽  
Shirley M Harrington ◽  
Thomas F Governo

Abstract Morphine, heroin, and cocaine are quantitatively determined with the same gas-liquid chromatographic system. The compounds are separated on a 6 ft × 2 mm id glass column packed with a 1:1 mixture of 5% SE-30 on 80-100 mesh Chromosorb W and 3% OV-17 on 80-100 mesh Varaport 30. The column is temperatureprogrammed. Flame ionization detector responses are measured with a computer-based data system. Heroin and cocaine are chromatographed directly; morphine is derivatized first. The procedure was evaluated with previously analyzed commercial and forensic samples. Accuracy and precision were 5 and 3%, respectively.


1977 ◽  
Vol 60 (1) ◽  
pp. 9-13
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail ◽  
James M Zehner ◽  
Roy E Bry

Abstract A simple and rapid gas-liquid chromatographic (GLC) method was developed for the analysis of aqueous solutions of FMC 33297 (m-phenoxybenzyl cis,trans-(±)-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate). The compound is extracted from aqueous solution with benzene and cleaned up by liquid chromatography. The sample extracts are analyzed by GLC with a flame ionization detector and quantitated by comparing integrator counts of extracts with those of standards. Recoveries of FMC 33297 were 90—100%. The method has good precision (the standard deviation for 4 determinations of a 0.002394% formulation was 6 × 10−6) and is sensitive to 0.00004% active ingredient by weight.


1971 ◽  
Vol 54 (5) ◽  
pp. 1160-1163
Author(s):  
Walter Fiddler ◽  
Robert C Doerr ◽  
John R Ertel ◽  
Aaron E Wasserman

Abstract A method is described for the gas chromatographic determination of N-nitrosodimethylamine in ham. The use of a commercial rubidium sulfate alkali flame ionization detector for nitrogen-containing compounds permits a simple cleanup procedure and a rapid analysis. This method consists of digesting the ham sample with methanolic KOH, distillation from aqueous alkali, washing the distillate with hexane, acidification and extraction of the aqueous layer with methylene chloride, and washing the extracts with base prior to concentration. The sensitivity of the method is 25 ppb; the average recoveries at this level range from 73 to 100%. Ten hams including 4 varieties were analyzed and found to contain less than 1 ppb apparent N-nitrosodimethylamine.


1978 ◽  
Vol 61 (3) ◽  
pp. 561-563
Author(s):  
Robert L Smallidge

Abstract A gas-liquid chromatographic method is presented for determining ethopabate in 0.8 and 8.0% premixes. A sample is extracted with tetrahydrofuran containing an internal standard, by sonication or overnight soaking. The extract is clarified by centrifugation, diluted if necessary, and injected into a gas chromatograph equipped with a flame ionization detector. Average per cent recoveries for spiked blank samples were 100.6 at the 0.8% level and 100.4 at the 8.0% level. Precision, as indicated by replicate analyses of several premixes, ranged from 0.5 to 1.7% relative standard deviation


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