THE ESTIMATION OF 3α-HYDROXY-5α-ANDROST-16-ENE AND OTHER C19-Δ16-STEROIDS IN URINE BY GAS-LIQUID CHROMATOGRAPHY

1970 ◽  
Vol 63 (1) ◽  
pp. 79-90 ◽  
Author(s):  
B. W. L. Brooksbank ◽  
D. B. Gower
Keyword(s):  
Liquid Chromatography ◽  
Excretion Rate ◽  
Quantitative Estimation ◽  
Colorimetric Method ◽  
Gas Liquid Chromatography ◽  
Urinary Excretion Rate ◽  
Men And Women ◽  
Accuracy And Precision ◽  
Preliminary Purification ◽  
Normal Men

ABSTRACT A method is described for the quantitative estimation of C19-Δ16-steroids in human urine. After extraction and preliminary purification by the method of Brooksbank & Haslewood (1961), the steroids were analyzed as chloromethyl dimethylsilyl ethers by gas-liquid chromatography. The specificity, accuracy and precision of the method were found to be satisfactory and comparison with the colorimetric method of Brooksbank & Haslewood (1961) for urinary 3α-hydroxy-5α-androst-16-ene showed a high correlation coefficient, r = 0.97 (P < 0.001). Figures are given for the urinary excretion rate of 3α-hydroxy-5α-androst-16-ene of normal men and women and of some women suffering from hirsutism and from adrenocortical overactivity. The values are given for 3α-hydroxy-5β-androst-16-ene and 3β-hydroxyandrosta-5,16-diene in pools of urine from healthy men and women.

Amphetamines in Human Urine: Rapid Estimation by Gas—Liquid Chromatography

1970 ◽  
Vol 16 (9) ◽  
pp. 786-788 ◽  
Author(s):  
J W Schweitzer ◽  
A J Friedhoff
Keyword(s):  
Liquid Chromatography ◽  
Human Urine ◽  
Excretion Rate ◽  
Low Ph ◽  
Gas Liquid Chromatography ◽  
Reference Compound ◽  
Internal Reference ◽  
Rapid Estimation ◽  
Amphetamine Psychosis

Abstract A procedure is described for the quantitative determination of amphetamine and p-methoxyamphetamine and for the semiquantitative determination of methamphetamine, mephentermine, and normephentermine in human urine. An internal reference compound, phenethylamine, is added to 5 ml of urine. The urine is extracted at low pH to remove acidic contaminants, then at high pH with chloroform, in which the amines were acetylated with acetic anhydride. After evaporation, the residue, dissolved in dioxane, is injected onto a column at 215°C, packed with 8% ethyleneglycol adipate on Chromosorb W, 100-120 mesh, except at both ends, where the packing was 8% silicon rubber SE 30 on Chromosorb W, 100-120 mesh. The excretion rate of amphetamines by patients admitted with a diagnosis of amphetamine psychosis was measured.

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