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 Total Inorganic Iodine in Milk

1977 ◽  
Vol 60 (6) ◽  
pp. 1307-1309 ◽  
Author(s):  
Hendrik J Bakker
Keyword(s):  
Liquid Chromatography ◽  
Iodine Content ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Inorganic Iodine ◽  
Liquid Chromatographic

Abstract Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively.

Column Chromatographic Cleanup and Gas-Liquid Chromatographic Determination of Hydroxybenzoic Esters in Food

1973 ◽  
Vol 56 (6) ◽  
pp. 1515-1517
Author(s):  
Paul Daenens ◽  
Leander Laruelle
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Hydroxybenzoic Acid ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Acid Esters ◽  
Column Chromatographic

Abstract Hydroxybenzoic acid esters are isolated on a column of silica gel while interferences are removed with petroleum ether. The preservatives are then eluted with petroleum ether-diethyl ether (8+2), derivatives are formed by reaction with bis(trimethylsilyl)acetamide, and the concentrations are determined by gas-liquid chromatography.

Gas-Liquid Chromatographic Determination of Pydrin, a Synthetic Pyrethroid, in Cabbage and Lettuce

1978 ◽  
Vol 61 (4) ◽  
pp. 869-871
Author(s):  
Young W Lee ◽  
Neil D Westcott ◽  
Randy A Reichle
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Synthetic Pyrethroid ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Pydrin, a-cyano-3-phenoxybenzyI 2-(4-chlorophenyl)-3-methylbutyrate, a synthetic pyrethroid ester, is extracted from vegetables with acetonitrile, partitioned into petroleum ether before cleanup on a Florisil column, and analyzed by electron capture gas-liquid chromatography. Recoveries of 88-102% at 0.01 ppm, 99-102% at 0.1 ppm, and 98—104% at 1.0 ppm were obtained from fortified cabbage and lettuce samples. The method appears applicable to detection of the residues of Pydrin in the foliage of many types of crops.

Gas-Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080)

1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker
Keyword(s):  
Liquid Chromatography ◽  
Tissue Sample ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Fluoroacetic Acid ◽  
Pentafluorobenzyl Bromide ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.

Gas-Liquid Chromatographic Determination of Maleic Hydrazide in Tobacco and Tobacco Smoke

1979 ◽  
Vol 62 (1) ◽  
pp. 171-175 ◽  
Author(s):  
Alfred F Haeberer ◽  
Orestes T Chortyk
Keyword(s):  
Liquid Chromatography ◽  
Tobacco Smoke ◽  
Plant Growth Regulator ◽  
Maleic Hydrazide ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Trimethylsilyl Derivative ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of the plant growth regulator maleic hydrazide (MH; l,2-dihydro-3,6-pyridazinedione) in tobacco and tobacco smoke. Residues are converted to the bis(trimethylsilyl) derivative before analysis by gas-liquid chromatography. The method has been applied to cigarettes and condensed smoke and has been used to determine the per cent transfer of MH into cigarette smoke. Free MH residues could be determined directly on the tobacco samples, whereas total MH values were obtainable only after acid hydrolysis. In spite of large MH residues in tobacco, only 0.2% of the MH was transferred into smoke.

Gas-Liquid Chromatographic Determination of Choline in Low and High Potency Multiple Vitamin Tablets and Liver Preparations

1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
High Potency ◽  
Average Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.

Gas-Liquid Chromatographic Determination of Residues from the Herbicide 2-Chloro-l-(3-Ethoxy-4-Nitrophenoxy)-4-(Trifluoromethyl) Benzene

1978 ◽  
Vol 61 (3) ◽  
pp. 636-639 ◽  
Author(s):  
Irving L Adler ◽  
Linwood D Haines ◽  
Brent Marco Jones
Keyword(s):  
Liquid Chromatography ◽  
Sodium Hydroxide ◽  
Methanol Extract ◽  
Chromatographic Determination ◽  
Extraction Process ◽  
Gas Liquid Chromatography ◽  
Simultaneous Distillation Extraction ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Residues of 2 - chloro - 1 - (3 - ethoxy- 4 - nitrophenoxy)-4-(trifluoromethyl) benzene and reduced metabolites are determined by digesting a sample methanol extract with aluminum in aqueous 10% sodium hydroxide to convert residues to 4-[2-chloro-4-(trifluoromethyl)-phenoxy]-2-ethoxybenzenamine. This compound is partitioned into hexane, using a simultaneous distillation-extraction process. The heptafluorobutyryl derivative is then prepared, partially purified by chromatography on Florisil, and measured by electron capture gas-liquid chromatography. The method is sensitive to 0.01 ppm.

Gas-Liquid Chromatographic Determination of β-Asarone in Wines and Flavors

1976 ◽  
Vol 59 (3) ◽  
pp. 675-677
Author(s):  
Randolph H Dyer ◽  
Glenn E Martin ◽  
Peter C Buscemi
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Ethyl Palmitate ◽  
Ultraviolet Spectra ◽  
Liquid Chromatographic Determination ◽  
Mass Spectrometery ◽  
Liquid Chromatographic

Abstract Wine samples containing β-asarone (cis-2,4,5-trimethoxy-1-propenylbenzene) are distilled; β-asarone is extracted by hexane and then quantitatively determined by gas-liquid chromatography (GLC), using ethyl palmitate as the internal standard. The GLC procedure is rapid and yields precise and accurate results. Mass spectrometery confirmed the identity of the GLC peak as β-asarone. The ultraviolet spectra of β-asarone and its isomer were also determined.

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.

Stability-Indicating Liquid Chromatographic Determination of Alpha-Ionone in Toothpaste

1988 ◽  
Vol 71 (1) ◽  
pp. 36-37
Author(s):  
Ramesh J Trivedi
Keyword(s):  
Standard Deviation ◽  
Chromatographic Method ◽  
Cost Effective ◽  
Chromatographic Determination ◽  
Average Recovery ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, sensitive, and rapid liquid chromatographic method for quantitating α-ionone in toothpaste at levels of 20 ppm in the presence of large amounts of flavor has been developed. The method is accurate, precise, cost-effective, and specific for α-ionone. Average recovery of a laboratory-prepared sample was 99.0% with the relative standard deviation was 1.29% (n = 6).

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