Gas-Liquid Chromatographic Determination of m-Phenoxybenzyl cis, trans-(±)-3-(2,2-Dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate in Aqueous Formulations

1977 ◽  
Vol 60 (1) ◽  
pp. 9-13
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail ◽  
James M Zehner ◽  
Roy E Bry
Keyword(s):  
Aqueous Solution ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Chromatographic Determination ◽  
Good Precision ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Collaborative Study of the Gas-Liquid Chromatographic Determination of Sorbitol in Bakery Products

1973 ◽  
Vol 56 (1) ◽  
pp. 66-67
Author(s):  
Harvey K Hundley
Keyword(s):  
Aqueous Solution ◽  
Acetic Anhydride ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Bakery Products ◽  
Sugar Alcohols ◽  
Flame Ionization ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A GLC method for the determination of sorbitol has been collaboratively studied. Sugar and sugar alcohols are extracted from the bakery products by methanol and the solvent is evaporated. Acetate derivatives are then formed by addition of acetic anhydride in pyridine, and the derivatives are extracted from an aqueous solution with chloroform and analyzed by flame ionization GLC. Collaborative results show a recovery ranging from 90 to 102% sorbitol from bakery products containing 1.5 to 7% sorbitol. The method has been adopted as official first action.

Gas-Liquid Chromatographic Determination of p-Chloroacetanilide in Acetaminophen

1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Glass Column ◽  
Retention Characteristics ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.

Gas-Liquid Chromatographic Determination of IV-Octylbicycloheptene Dicarboximide

1975 ◽  
Vol 58 (4) ◽  
pp. 845-849
Author(s):  
Vernon J Meinen
Keyword(s):  
Quantitative Determination ◽  
Chromatographic Determination ◽  
Flame Ionization Detector ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Preliminary Work ◽  
Technical Material ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Sorbitol in Cooked Sausage Products

1978 ◽  
Vol 61 (1) ◽  
pp. 164-166
Author(s):  
Fred A Moseley ◽  
Joel S Salinsky ◽  
Robert W Woods
Keyword(s):  
Chromatographic Determination ◽  
Flame Ionization Detector ◽  
Gas Chromatograph ◽  
Ionization Detector ◽  
Simple Method ◽  
Flame Ionization ◽  
Freeze Dried ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Acephate and Ortho 9006 Residues in Crops

1974 ◽  
Vol 57 (1) ◽  
pp. 189-191
Author(s):  
James B Leary
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Ether Solution ◽  
Liquid Chromatographic Determination ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Levamisole Residues in Bovine Milk

1976 ◽  
Vol 59 (5) ◽  
pp. 954-958 ◽  
Author(s):  
John E Smith ◽  
N Robert Pasarela ◽  
John C Wyckoff
Keyword(s):  
Bovine Milk ◽  
Chromatographic Determination ◽  
Ionization Detector ◽  
Flame Ionization ◽  
External Standard ◽  
Liquid Chromatographic Determination ◽  
Control Milk ◽  
Water Saturated ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Morphine, Heroin, and Cocaine

1979 ◽  
Vol 62 (2) ◽  
pp. 304-307
Author(s):  
Manfred J Prager ◽  
Shirley M Harrington ◽  
Thomas F Governo
Keyword(s):  
Chromatographic Determination ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Accuracy And Precision ◽  
Forensic Samples ◽  
Glass Column ◽  
Computer Based ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Kepone Residues in Finfish, Shellfish, and Crustaceans

1978 ◽  
Vol 61 (4) ◽  
pp. 877-883
Author(s):  
Richard A Carver ◽  
Arnold P Borsetti ◽  
Laverne R Kamps
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Petroleum Ether ◽  
Ethyl Ether ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Finfish, shellfish, and crustacean samples are extracted with isopropanol and benzene; the extract is filtered and then concentrated. The extract, dissolved in hexane, is treated with oleum and extracted with aqueous alkali. The aqueous phase is acidified and extracted with petroleum ether-ethyl ether (1+1). The Kepone residue is determined by electron capture gas-liquid chromatography (GLC). Recoveries obtained by 8 laboratories from 15 species of finfish fortified at 0.02-0.23 ppm ranged from 37 to 107% with a mean ± relative standard deviation of 79.4±14.5%. For oysters fortified at 0.01- 0.10 ppm, recoveries range from 63 to 129% with a mean of 78.2 ±20.8%. For crustaceans fortified at 0.05—0.26 ppm, recoveries ranged from 52 to 110% with a mean of 78.8±16.4%. The approximate limits of quantitation for finfish and for shellfish and crustaceans are 0.02 and 0.05 ppm, respectively, under the GLC conditions used in this study.

Gas-Liquid Chromatographic Determination of Aniline Metabolites of Substituted Urea and Carbamate Herbicides in Aqueous Solution

1981 ◽  
Vol 64 (4) ◽  
pp. 833-840
Author(s):  
Erika E Hargesheimer ◽  
Ronald T Coutts ◽  
Franco M Pasutto
Keyword(s):  
Aqueous Solution ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Distilled Water ◽  
Substituted Anilines ◽  
Flame Ionization ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Derivatives Of

Abstract A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and IV-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 ml distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

Gas-Liquid Chromatographic Determination of d-trans-Allethrin

1972 ◽  
Vol 55 (5) ◽  
pp. 907-912
Author(s):  
Vernon J Meinen
Keyword(s):  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Technical Material ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

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.

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