IDENTIFICATION AND DETERMINATION OF NEUTRAL STEROID SULPHATES IN HUMAN FOETAL ADRENAL AND LIVER TISSUE

1970 ◽  
Vol 64 (2) ◽  
pp. 273-286 ◽  
Author(s):  
I. Huhtaniemi ◽  
T. Luukkainen ◽  
R. Vihko
Keyword(s):  
Mass Spectrometry ◽  
Liver Tissue ◽  
Keto Group ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Silyl Ethers ◽  
Adrenal Tissue ◽  
Neutral Steroid

ABSTRACT The endogenous neutral steroids in adrenal and liver tissue obtained from foetuses of 12–17 weeks gestation were investigated. After extractions, the steroids were fractionated into a monosulphate and a disulphate fraction on Sephadex LH-20. The conjugates were cleaved by solvolysis, and purified on silicic acid and their trimethyl silyl ethers were analysed by gas-liquid chromatography and gas chromatography-mass spectrometry. Only neutral steroid monosulphates were found. The following compounds were identified in the monosulphate fraction of adrenal tissue: dehydroepiandrosterone, 16α-hydroxydehydroepiandrosterone, pregnenolone and 17α-hydroxypregnenolone, and of liver tissue; dehydroepiandrosterone, 16α-hydroxydehydroepiandrosterone, androst-5-ene-3β,16α,17β-triol, pregnenolone, 17α-hydroxypregnenolone and 16α-hydroxypregnenolone. The identifications and the results of the quantitative determinations of endogenous neutral steroid sulphates suggest that pregnenolone is synthesised in vivo in the foetal adrenal and converted to 17α-hydroxypregnenolone and dehydroepiandrosterone sulphates. The latter compound is further transformed to 16α-hydroxydehydroepiandrosterone sulphate. No 16α-hydroxylation of pregnenolone was observed in adrenal tissue, whereas liver tissue seems to form 16α-hydroxypregnenolone. Reduction of a 17-keto group to 17β-hydroxyl and a 20-keto group to 20α-hydroxyl seems to take place in liver but not in adrenal tissue.

Monitoring drug concentrations in a case of combined overdosage with primidone and methsuximide.

1976 ◽  
Vol 22 (6) ◽  
pp. 915-921 ◽  
Author(s):  
G F Johnson ◽  
C J Least ◽  
J W Serum ◽  
E B Solow ◽  
H M Solomon
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Therapeutic Decision ◽  
Serum Samples ◽  
Monitoring Drug ◽  
Drug Concentrations

Abstract We describe a case of fatal overdosage with primidone and methsuximide. During the early phase of the patient's hospital course we found concentrations of methsuximide, N-desmethylmethsuximide, and primidone in serum that far exceeded the usual therapeutic concentrations, as determined by gas-liquid chromatography. Determination of N-desmethylmethsuximide in peritoneal fluid demonstrated concentrations comparable to those in serum. This led to the therapeutic decision to manage the patient by dialysis. Subsequently, serum samples collected during the course of hospitalization were analyzed quantitatively by gas-liquid chromatography for methsuximide, N-desmethylmethsuximide, primidone, phenobarbital, and diphenylhydantoin. Selected serum specimens were also analyzed by gas chromatography-mass spectrometry, and N-methyl-2-hydroxymethyl-2-phenylsuccinimide, a metabolite of methsuximide not previously described in human serum, was identified by analysis of its mass spectrum.

NEUTRAL STEROID SULPHATES IN AMNIOTIC FLUID

1970 ◽  
Vol 46 (3) ◽  
pp. 391-399 ◽  
Author(s):  
T. LUUKKAINEN ◽  
A. SIEGEL ◽  
R. VIHKO
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Amniotic Fluid ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Human Amniotic Fluid ◽  
Main Compound ◽  
Neutral Steroid

SUMMARY Steroid monosulphate and disulphate fractions were obtained by chromatography on Sephadex LH-20 from human amniotic fluid collected at term. Only 16α-hydroxydehydroepiandrosterone could be identified in the monosulphate fraction, the detection limit being 5–8 μg./1000 ml. amniotic fluid. In the disulphate fraction 5-androstene-3β,17α-diol, 5-androstene-3β,17β-diol, 5-pregnene-3β,20α-diol, 5α-pregnane-3β,20α-diol, 16α-hydroxydehy-droepiandrosterone, 16β-hydroxydehydroepiandrosterone, 3β, 17β-dihy-droxy-5-androsten-16-one and 5-pregnene-3β,17α,20α-triol were identified by gas—liquid chromatography and gas chromatography—mass spectrometry. The concentrations of these steroids were determined in a pool of human amniotic fluid taken at term. The main compound was 5-androstene-3β,17α-diol.

Gas-Liquid Chromatographic Determination of Congeners in Alcoholic Products with Confirmation by Gas Chromatography/Mass Spectrometry

1981 ◽  
Vol 64 (1) ◽  
pp. 186-190
Author(s):  
Glenn E Martin ◽  
James M Burggraff ◽  
Randolph H Dyer ◽  
Peter C Buscemi
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Chromatographic Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for the separation and determination of the following compounds which are found as congeners in alcoholic products: acetaldehyde, ethyl acetate, methanol, ethanol, n-propanol, isobutanol, n-butanol, acetic acid, and the amyl alcohols (2-methyl-l-butanol and 3-methyl-l-butanol). These compounds were separated by gas-liquid chromatography (GLC) using 5% Carbowax 20M on Carbopack B as the column packing. The results obtained by using this method were compared with those obtained using the present AOAC methods for these compounds. GLC chromatograms show better resolution by the method presented.

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