Gas-liquid chromatographic determination of gossypol as the trimethylsilyl ether derivative

1967 ◽  
Vol 44 (7) ◽  
pp. 465-466 ◽  
1979 ◽  
Vol 62 (3) ◽  
pp. 604-609
Author(s):  
Henry B S Conacher ◽  
Jagannath R Iyengar ◽  
Walter F Miles ◽  
Herbert G Botting

Abstract A method is given for determining monosodium glutamate (MSG) in soups and soup bases by gas-liquid chromatography (GLC) of the trimethylsilyl ether derivative of glutamic acid. This method compared favorably with existing methods including GLC of the trifluoroacetate (TFA) /butyl ester derivative, and analysis on an amino acid analyzer. In addition, some samples were analyzed by GLC/mass spectrometry. The MSG content of various products ranged from approximately 0.2% in some condensed soups to 13.1% in bouillon cubes. The method, which can detect as little as 0.05%, requires only a 10 min single step derivatization at room temperature and is preferred to the TFA/butyl ester technique.


1976 ◽  
Vol 59 (1) ◽  
pp. 221-223
Author(s):  
Chester J Mirocha ◽  
Sadanand V Pathre ◽  
Jerome Behrens

Abstract Two substances interfering with the gas-liquid chromatographic (GLC) detection of the T-2 mycotoxin were identified as 1-glycerylmonooleate and 1-glycerylmonolinoleate. These monoglycerides are natural products formed by species of Fusarium growing on cereal grains and are also additives contained in liquid vegetable and animal fats added to the feed mixture. The monoglycerides can be removed from the analytical sample by resolution by thin layer chromatography prior to separation by GLC. Trimethylsilyl ether derivatives of the monoglycerides and T-2 toxin have almost identical retention times on 3% OV-1 columns, whereas the trifluoroacetyl and pentafluoropropionyl derivatives give baseline separation on the same column. The monoglycerides can be misidentified as the T-2 toxin in analyses involving GLC.


2016 ◽  
Vol 12 (6) ◽  
pp. 560-567
Author(s):  
Marwa F. Mansour ◽  
Ehab F. El-Kady ◽  
Mona M. Abd El-Moety ◽  
Nabawia M. El-Guindi ◽  
Ann Van Schepdael ◽  
...  

1975 ◽  
Vol 58 (5) ◽  
pp. 1051-1061
Author(s):  
William P Cochrane ◽  
James F Lawrence ◽  
Young W Lee ◽  
Ronald B Maybury ◽  
Brian P Wilson

Abstract An interlaboratory investigation of technical chlordane residues in food crops was carried out to determine the most practical and consistent method of reporting results. Using a technical chlordane reference standard, 8 gas chromatographic stationary phases were studied for their resolution capabilities. The best separations were obtained with SE-30 and its OV-1 equivalent. Using these columns and electron capture detection, potatoes and carrots from supervised field experiments were analyzed in duplicate and quantitated by using 4 methods of calculation. The data were statistically treated to determine the precision and bias for each method. Also, 1 sample was analyzed in duplicate on 2 different occasions by 6 laboratories to substantiate the initial conclusions. Based on the criterion of high precision it is suggested that a comparison of total area under the chromatogram of the sample with total area of a standard technical chlordane be the method of quantitation. Only peaks which are common to both standard and sample have any significance in this type of calculation.


1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.


1988 ◽  
Vol 455 ◽  
pp. 271-277 ◽  
Author(s):  
Emiko Mochizuki ◽  
Akira Nakayama ◽  
Yoshimi Kitada ◽  
Koichi Saito ◽  
Hiroyuki Nakazawa ◽  
...  

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