Further studies on the gas-liquid chromatographic determination of C10 steroids in human plasma using nickel-63 electron capture detection

1969 ◽  
Vol 41 ◽  
pp. 22-36 ◽  
Author(s):  
G.Lakshmi Kumari ◽  
William P. Collins ◽  
Ian F. Sommerville
1971 ◽  
Vol 54 (6) ◽  
pp. 1277-1282 ◽  
Author(s):  
Robert J Daun

Abstract A procedure is described for the gas-liquid chromatographic determination of sulfathiazole, sulfamerazine, sulfamethazine, and sulfaquinoxaline in finished feeds at levels from 0.002 to 0.05%. The procedure utilizes a double derivatization technique to modify the sulfonamides so that they can be determined by gas-liquid chromatography with electron capture detection. The conditions for extraction, derivatization, and gas-liquid chromatography are given, along with recovery data.


1978 ◽  
Vol 61 (5) ◽  
pp. 1054-1057
Author(s):  
Hisaya Tobioka ◽  
Ryoji Kawashima

Abstract A gas-liquid chromatographic (GLC) method with electron capture detection was developed for determining hexestrol residues based on a GLC method for diethylstilbestrol residues. The extraction and purification procedures were based on a published procedure. Pentafluoropropionic (PFP) and heptafluorobutyric (HFB) anhydrides and other halogenated compounds were compared as acylation reagents. PFP anhydride was selected because it provided reproducible GLC responses. Of the 3 column packing materials tested, OV-17, OV-210, and QF-1, OV-17 was the most stable under the GLC conditions used. A pH 10.5—10.6 in the purification step gave higher recoveries than pH 10.3 or pH 10.8 and was selected for use. The method is suitable for determining residues of 0.5 ppb. The limit of sensitivity ranges from 0.1 to 0.2 ppb.


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.


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