从水溶液中用有机溶剂提取合成代谢类固醇

Q4 Chemistry
S. Leschev, Y. Pakhadnia, O. N. Tchekhovskaya, A. A. Ahabalayeu, M. Zayats
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引用次数: 0

摘要

提取合成代谢类固醇(睾酮;epitestosterone;epimethenediol;17α-methyltestosterone;19-norethiocholanolone;18-normethenol;19-norandrosterone;3α-hydroxy-2α-methyl-5α-androstan-17-one;9α-fluoro-17、17 dimethyl-18-norandrostan-4 13-dien-11β-ol-3-one;1α-methyl-5α-androstan-3α-ol-17-one;1α-methyl-5αandrostan-3α,17β二醇;epioxandrolone;methasterone;oxandrolone;formestane;在20℃的条件下,用有机溶剂从水和盐水溶液中提取16β-羟基呋喃唑酚(16β-hydroxyfurazabol),在此基础上计算合成代谢类固醇(AS)的分配比,并以此为依据,优化运动员尿液中合成代谢雄激素(AAS)及其代谢物测定过程中的标准样品制备工艺。结果表明,水溶液和含水盐溶液中选择性最强的萃取剂是己烷,它能萃取出大部分的AAS。对于己烷萃取效果较差的原子吸收光谱,建议采用硫酸钠或硫酸铵盐析,并选用活性较强的有机萃取剂二氯甲烷或乙醚。建立了一种提取样品制备技术,用于气相色谱-质谱检测法测定运动员尿液中的合成代谢类固醇及其代谢物。该方法的标准偏差为10 - 15%,检出限约为10 ng/ml。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Organic solvent extraction of anabolic steroids from aqueous solutions
The extraction of anabolic steroids (testosterone; epitestosterone; epimethenediol; 17α-methyltestosterone; 19-norethiocholanolone; 18-normethenol; 19-norandrosterone; 3α-hydroxy-2α-methyl-5α-androstan-17-one; 9α-fluoro-17,17dimethyl-18-norandrostan-4,13-dien-11β-ol-3-one; 1α-methyl-5α-androstan-3α-ol-17-one; 1α-methyl-5αandrostan-3α,17β-diol; epioxandrolone; methasterone; oxandrolone; formestane; 16β-hydroxyfurazabol) with organic solvents from water and aqueous salt solutions was studied at 20 ° C. Based on the experimental data obtained, the partition ratios of anabolic steroids (AS) were calculated, which were used to optimize the standard sample preparation procedure in the process of determining anabolic androgenic steroids (AAS) and their metabolites in the urine of athletes. It was found that the most selective extractant from aqueous and aqueous salt solutions is hexane, which extracts the majority of AAS. To increase the recovery of AAS, poorly extracted by hexane, it is advisable to use salting out with sodium or ammonium sulfate and use more active organic extractants – methylene chloride or diethyl ether. An extraction sample preparation technique has been developed for the subsequent determination of anabolic steroids and their metabolites in athletes’ urine by gas chromatography with mass spectrometric detection method. The proposed method is characterized by a standard deviation of 10 – 15 % and a detection limit of about 10 ng/ml of urine.
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CiteScore
0.30
自引率
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发文量
38
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