THE GAS-LIQUID CHROMATOGRAPHY OF STEROID FORMATES; AN APPLICATION IN CONGENITAL ADRENAL HYPERPLASIA

1970 ◽  
Vol 47 (1) ◽  
pp. 55-64 ◽  
Author(s):  
H. L. J. MAKIN
Keyword(s):  
Liquid Chromatography ◽  
Periodate Oxidation ◽  
Oxygenation Index ◽  
Rapid Screening ◽  
Gas Liquid Chromatography ◽  
Adrenal Hyperplasia ◽  
Trimethylsilyl Ethers ◽  
Rapid Screening Test ◽  
Speed Up ◽  
Urinary Steroid

SUMMARY The gas-liquid chromatography (GLC) of some C19 steroid formates has been investigated in an attempt to speed up the final stages of the estimation of the 11-oxygenation index. SE-30 was found to give the best separation of the urinary C19 steroids formed after borohydride reduction and periodate oxidation of urine. Formates, acetates, propionates, n-butyrates, valerates and trimethylsilyl ethers were examined; formate esters gave the best separation of androsterone and aetiocholanolone. Estimation of the 11-oxygenation index by GLC increases the specificity and speed of single estimations and it is suggested that this method may find use as a rapid screening test for abnormal urinary steroid patterns.

A MODIFIED METHOD FOR THE ANALYSIS OF URINARY 17-KETOSTEROIDS, PREGNANEDIOL AND PREGNANETRIOL BY GAS LIQUID CHROMATOGRAPHY IN NORMAL SUBJECTS AND SUBJECTS WITH VARIOUS ENDOCRINE DISORDERS

1967 ◽  
Vol 54 (1) ◽  
pp. 37-50 ◽  
Author(s):  
Roberto Rivera ◽  
Ralph I. Dorfman ◽  
Enrico Forchielli
Keyword(s):  
Liquid Chromatography ◽  
Normal Subjects ◽  
Endocrine Disorders ◽  
Gas Liquid Chromatography ◽  
Modified Method ◽  
Trimethylsilyl Ethers ◽  
Normal Males ◽  
Steroid Excretion ◽  
Urinary Steroid

ABSTRACT A modified method using gas-liquid chromatography (GLC) is described for the determination of androsterone*, aetiocholanolone, dehydroepiandrosterone, pregnanediol and pregnanetriol in the same urine aliquot. After sequential enzymatic hydrolysis and solvolysis, the urine extract is separated into 3 main fractions by silica gel column chromatography; one containing mainly the 17-ketosteroids, androsterone, aetiocholanolone and dehydroepiandrosterone; a second containing pregnanediol and the third pregnanetriol. After formation of the trimethylsilyl ethers (TMSi), the respective fractions are subjected to gas-liquid chromatography for quantitation. Tritiated androsterone, pregnanediol and pregnanetriol are added prior to extraction of the urines to check for recoveries. The method is specific and reproductible and is sufficiently sensitive to permit determination of urinary steroid excretion levels as low as 0.025 mg/24 hours. Results obtained with this method in the study of normal males and females and various pathological conditions are presented.

Collaborative Study of the Extraction of Plant Sterols from Adulterated Butter Oil Using a Digitonin-impregnated Celite Column

1970 ◽  
Vol 53 (3) ◽  
pp. 535-538
Author(s):  
Denis E Lacroix
Keyword(s):  
Liquid Chromatography ◽  
Vegetable Oil ◽  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Screening Method ◽  
Rapid Screening ◽  
Gas Liquid Chromatography ◽  
Butter Oil ◽  
Average Coefficient ◽  
Rapid Screening Method

Abstract A rapid screening method for the analysis of the phytosterol, β-sitosterol, in butter oil adulterated with vegetable oil has been studied collaboratively. The sterols are removed from the adulterated butter oil by passing the sample through a digitonin-impregnated Celite 545 column, eluting the sterols with dimethyl sulfoxide, and analyzing the eluate for β-sitosterol by gas-liquid chromatography using a 3% JXR column. The average coefficient of variation for those samples containing more than 4 mg β-sitosterol/100 g adulterated butter oil is 12.6%. Therefore, β-sitosterol can be used as an index to qualitatively detect vegetable oil adulteration of butter oil.

Simultaneous Determination of Urinary Estriol, Pregnanediol, and Pregnanolone by Gas-Liquid Chromatography

1969 ◽  
Vol 15 (3) ◽  
pp. 190-196 ◽  
Author(s):  
Robert D Baynton ◽  
Donald J Campbell
Keyword(s):  
Liquid Chromatography ◽  
Glycol Succinate ◽  
Urine Specimen ◽  
Gas Liquid Chromatography ◽  
Large Hospital ◽  
Flame Ionization ◽  
Trimethylsilyl Ethers ◽  
Hydrogen Flame ◽  
Progesterone Metabolites ◽  
Temperature Programmed

Abstract A simplified method for following the urinary excretion of estriol, pregnanediol, and pregnanolone during the course of pregnancy is presented. The procedure has been used successfully in a large hospital laboratory. An important advantage is that the estrogen and progesterone metabolites are measured simultaneously, and separate extraction and gas-liquid chromatography is not required. The urine specimen is hydrolyzed enzymatically, extracted, and the steroids are converted to trimethylsilyl ethers. Temperature-programmed gas-liquid chromatography is carried out on a 2% neopentyl glycol succinate column using a hydrogen flame ionization detector.

The steroid 11-oxygenation index by gas-liquid chromatography

1971 ◽  
Vol 31 (2) ◽  
pp. 435-438 ◽  
Author(s):  
Qutub H. Qazi ◽  
J. Gilbert Hill ◽  
Margaret W. Thompson
Keyword(s):  
Liquid Chromatography ◽  
Oxygenation Index ◽  
Gas Liquid Chromatography

CONGENITAL ADRENAL HYPERPLASIA AND OTHER CONDITIONS ASSOCIATED WITH A RAISED URINARY STEROID 11-OXYGENATION INDEX

1971 ◽  
Vol 50 (2) ◽  
pp. 251-265 ◽  
Author(s):  
BARBARA E. CLAYTON ◽  
R. W. H. EDWARDS ◽  
H. L. J. MAKIN
Keyword(s):  
Congenital Heart Disease ◽  
Heart Disease ◽  
Congenital Adrenal Hyperplasia ◽  
Congenital Heart ◽  
Oxygenation Index ◽  
Adrenocortical Function ◽  
Adrenal Hyperplasia ◽  
Severe Diarrhoea ◽  
Adrenocortical Tumours ◽  
Urinary Steroid

SUMMARY Raised values of the 11-oxygenation index (11-OI) were found in 164 children, although it was only possible to record 97 fully. Seventy-four were fully diagnosed as having congenital adrenal hyperplasia (CAH) and among the others five had high 11-OI values which fell to normal by the 8th day of life and two gave high values due to methodological interference by 1-oxygenated steroids. Severe diarrhoea was associated with a raised 11-OI in ten boys and this presented difficulty in diagnosis; CAH was considered a possible diagnosis by the referring physician but was finally excluded. Impaired adrenocortical function probably accounted for the raised 11-OI observed in six children who were never considered to have CAH. They had a variety of conditions including congenital heart disease. Normal 11-OI values were found in six patients with adrenocortical tumours. Prednisone and prednisolone administration interfered with the determination.

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