Analysis of Potato Glycoalkaloids by Gas-Liquid Chromatography of Alkaloid Components

1980 ◽  
Vol 63 (6) ◽  
pp. 1226-1230 ◽  
Author(s):  
Russell R King
Keyword(s):  
Liquid Chromatography ◽  
Lower Limit ◽  
Direct Determination ◽  
Gas Liquid Chromatography ◽  
Potato Tubers ◽  
Potato Glycoalkaloids ◽  
Nitrogen Phosphorus Detector ◽  
Liquid Chromatographic ◽  
Nitrogen Phosphorus

Abstract A gas-liquid chromatographic (GLC) method has been developed for the analysis of potato glycoalkaloids by direct determination of the alkaloid components isolated by hydrolysis with IN ethanolic HCl. Recoveries of solanidine from potato tubers and foliage fortified with solanine over a range approximately 0.5 to 5 times the glycoalkaloid originally present averaged greater than 95%, and the lower limit of sensitivity was 0.25 mg/100 g using a nitrogen-phosphorus detector. A means of distinguishing solanidine and demissidine by formation of their respective 3β-trifluoroacetates with trifluoroacetic anhydride (TFAA) is demonstrated.

Gas-liquid chromatographic determination of nicotine and cotinine in plasma.

1978 ◽  
Vol 24 (1) ◽  
pp. 50-53 ◽  
Author(s):  
N Hengen ◽  
M Hengen
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Nitrogen Phosphorus Detector ◽  
Liquid Chromatographic ◽  
Nitrogen Phosphorus ◽  
Respective Concentration

Abstract We report a procedure for determining nicotine and cotinine in plasma. Nicotine is extracted from 1 ml of plasma with diethyl ether, back extracted, and analyzed by gas-liquid chromatography with a nitrogen/phosphorus detector. Nicotine and its internal standard, modaline, had retention times of 1.9 and 2.9 min, respectively. Cotinine is then extracted from the same plasma with dichloromethane and similarly analyzed. Cotinine and its internal standard, lidocaine, had retention times of 3.8 and 4.9 min. Day-to-day reproducibilities (CV) within 14% for nicotine and within 6% for cotinine are attainable for the respective concentration ranges 1-100 microgram/liter and 1-200 microgram/liter. Nornicotine and related alkaloids do not interfere. The sensitivity was such that less than 0.1 microgram (0.62 nmol) of nicotine and 0.1 microgram (0.62 nmol) of nicotine and 0.1 microgram (0.57 nmol) of cotinine could be detected per liter.

Gas-liquid Chromatography and Nitrogens-Phosphorus Detection of N-Nitroso-di-n-Propylamine in Trifluralin Products

1983 ◽  
Vol 66 (5) ◽  
pp. 1209-1213
Author(s):  
Ronald B Maybury ◽  
Ralph G Grant
Keyword(s):  
Liquid Chromatography ◽  
High Resolution ◽  
Silica Gel ◽  
Detection System ◽  
Gas Liquid Chromatography ◽  
Sample Extraction ◽  
Nitrogen Phosphorus Detector ◽  
Minimum Detectable Amount ◽  
Nitrogen Phosphorus

Abstract A method is described for the determination of trace levels of N-nitroso-di-n-propylamine (NDPA) in trifluralin herbicide formulations. Following sample extraction, NDPA is separated on a silica gel column and determined by gas-liquid chromatography with a nitrogen-phosphorus detector (NPD). A comparison between the results obtained using this detection system and the thermal energy analyzer (TEA) for 0.5-5 ppm levels of NDPA in 17 samples showed no significant differences. Close agreement was also demonstrated with the results obtained by high resolution gas-liquid chromatography/mass spectrometry (GLC/MS). The minimum detectable amount of NDPA with the NPD was 5 pg, for the TEA system 50 pg, and for high resolution GLC/MS 100 pg. A number of other nitrosamines were detected by all systems in one sample but these were not fully characterized. The nitrogen-phosphorus detector is useful for monitoring traces of NDPA in trifluralin when preceded by cleanup on a silica gel column.

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.

Extraction and Cleanup of Fish, Sediment, and Water for Determination of Triaryl Phosphates by Gas-Liquid Chromatography

1981 ◽  
Vol 64 (1) ◽  
pp. 79-84
Author(s):  
Derek C G Muir ◽  
Norbert P Grift ◽  
John Solomon
Keyword(s):  
Liquid Chromatography ◽  
Soxhlet Extraction ◽  
Gel Permeation Chromatography ◽  
Gas Liquid Chromatography ◽  
Fish Samples ◽  
Alumina Treatment ◽  
Diphenyl Phosphate ◽  
Nitrogen Phosphorus ◽  
Acetone Hexane

Abstract Several techniques were evaluated for extracting triphenyl phosphate (TPP), 14C-labeled TPP, cresyl diphenyl phosphate, and tricresyl phosphate isomers (o-TCP, m-TCP, and p-TCP) from fish and sediment samples. Extracts of fish samples were cleaned up by gel permeation chromatography/alumina column chromatography; sediment extracts received alumina treatment only. Compounds were determined by gas-liquid chromatography (GLC) with nitrogenphosphorus detection. Methanol/Polytron and hexane/ball mill extraction of fish samples fortified at 0.01, 0.1, and 1.0 μg/g levels gave overall recoveries of the 5 compounds of 89 and 97%, respectively. Methanol recovered more radioactivity (97%) from fish exposed to 14C-TPP in aquaria for 24 h than did hexane from fish exposed for 16 h (79%). Refluxing fortified sediment (0.05 and 0.5 μg/g) with methanol-water (9+1) gave significantly higher recoveries (88%) of the 5 triaryl phosphates than did dichloromethane-methanol (1+1) reflux or acetone-hexane (1+1) Soxhlet extraction. Recoveries of TPP and o-, m- and p-TCP from fortified river water (0.5, 5.0, and 50 μg/L) by shaking with dichloromethane ranged from 91 to 118%. Some problems were encountered with interfering GLC peaks at low (μg/g) levels in fish and sediment extracts despite the use of nitrogen-phosphorus specific detectors.

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.

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