Rapid Determination of Glutethimide (Doriden) by Gas-Liquid Chromatography

1967 ◽  
Vol 13 (7) ◽  
pp. 589-594 ◽  
Author(s):  
Seymour Winsten ◽  
Daniel Brody
Keyword(s):  
Liquid Chromatography ◽  
Rapid Determination ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic

Abstract A rapid simple gas liquid chromatographic technic has been developed for the identification and quantitation of glutethimide in biologic fluids. The method requires no evaporation of extracting fluid and will estimate glutethimide levels in the range of 1 mg./100 ml. or higher.

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 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.

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.

Liquid Chromatographic Determination of Bromide Ion in Cereals, Fruit, Vegetables, and Blood with a Silver Electrode in an Electrochemical Detector System

1995 ◽  
Vol 78 (3) ◽  
pp. 841-845 ◽  
Author(s):  
Bertil Lindgren ◽  
Tomas Berglöf ◽  
Åsa Ramberg ◽  
Anna Stepdmska ◽  
Malin Åkerblom
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Rapid Determination ◽  
Chromatographic Determination ◽  
Electrochemical Detector ◽  
Satisfactory Precision ◽  
Bromide Ion ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for rapid determination of bromide ion in commodities and blood by paired-ion liquid chromatography with electrochemical detection. The method involves extraction of samples with water and filtration. Blood is passed through a Sep-Pak C18 minicolumn. Recoveries are usually close to 100%, with satisfactory precision. The detection limit is 1 mg/kg. The method needs little labor and uses no noxious solvents or reagents.

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.

Gas—Liquid Chromatographic Measurement of Guanidino Acids

1975 ◽  
Vol 21 (7) ◽  
pp. 838-843 ◽  
Author(s):  
Harini Patel ◽  
Burton D Cohen
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Liquid Chromatography ◽  
Liquid Phase ◽  
Magnetic Resonance ◽  
Gas Liquid Chromatography ◽  
Butyl Esters ◽  
Silicone Liquid ◽  
Chromatographic Measurement ◽  
Liquid Chromatographic

Abstract We present a method for separating and measuring guanidino acids by gas—liquid chromatography. Compared to ion-exchange techniques, this system is faster, more sensitive, requires smaller sample volumes, is independent of colorimetric reactions, and permits simultaneous determination of both amino and guanidino acids. N-Trifluoroacetyl-n-butyl esters are formed and then are separated by using a column containing a mixed silicone liquid phase coated on Chromosorb W-HP. Analytical recoveries from plasma ranged from 86 to 112% and were optimal when purification and derivatization were done without prior protein precipitation. Speculations as to the cause of this interference by protein include coprecipitation, protein-binding, and cyclization of the guanidines in the acids used for denaturation. Evidence presented suggests that all three occur: ultrafiltrability is diminished in the presence of protein and nuclear magnetic resonance demonstrates cyclization of some of these esters.

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