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类固醇与高血压。1--3,15-及3,16-二羟基-17-氧代类固醇的气液色谱法和气-相色谱-质谱分析法

Steroids and hypertension. 1--Gas-liquid chromatography and gas chromatography mass spectrometry of 3,15- and 3, 16-dihydroxy-17-oxosteroids.

作者信息

Bègue R J, Dumas M, Morinière M, Nivois C, Padieu P

出版信息

Biomed Mass Spectrom. 1979 Nov;6(11):476-81. doi: 10.1002/bms.1200061104.

Abstract

In order to analyse and quantitate the urinary 16-oxysteroids known or thought to be associated with hypertension, we have established for six 16-oxy-C19 reference steroids the following parameters: elution volume on lipophilic gel columns, gas chromatographic retention data expressed as methylene unit values of trimethylsilyl ether and O-methoxime trimethylsilyl ether derivatives on OV-1 and OV-17 packed columns and on SE-30 capillary column, and mass spectra of these compounds. These reference steroids were: 3 alpha, 16 alpha-dihydroxy-5 alpha-androstan-17-one, 3 alpha, 16 alpha-dihydroxy-5 beta-androstan-17-one, 3 beta, 16 alpha-dihydroxy-5 alpha-androstan-17-one, 3 beta, 16 alpha-dihydroxy-5-androsten-17-one, 3 beta, 16 beta-dihydroxy-5-androsten-17-one, 3 beta, 17 beta-dihydroxy-5-androsten-16-one and 3 alpha, 15 alpha-dihydroxy-5 beta-androstan-17-one. The proposed method was shown to be applicable to the specific analysis of 16-oxy-C19-steroids in biological samples since it achieved the selective isolation of these compounds from other steroids and their quantitative elution in a single fraction. The analysis of the urinary steroids of two patients with arterial hypertension demonstrated an elevated rate of 3 beta, 16 alpha-dihydroxy-5-androsten-17-one.

摘要

为了分析和定量已知或被认为与高血压相关的尿16 - 氧代甾体,我们针对六种16 - 氧代 - C19参考甾体建立了以下参数:亲脂性凝胶柱上的洗脱体积、在OV - 1和OV - 17填充柱以及SE - 30毛细管柱上以三甲基硅醚和O - 甲肟三甲基硅醚衍生物的亚甲基单位值表示的气相色谱保留数据,以及这些化合物的质谱。这些参考甾体为:3α, 16α - 二羟基 - 5α - 雄甾烷 - 17 - 酮、3α, 16α - 二羟基 - 5β - 雄甾烷 - 17 - 酮、3β, 16α - 二羟基 - 5α - 雄甾烷 - 17 - 酮、3β, 16α - 二羟基 - 5 - 雄烯 - 17 - 酮、3β, 16β - 二羟基 - 5 - 雄烯 - 17 - 酮、3β, 17β - 二羟基 - 5 - 雄烯 - 16 - 酮和3α, 15α - 二羟基 - 5β - 雄甾烷 - 17 - 酮。所提出的方法被证明适用于生物样品中16 - 氧代 - C19 - 甾体的特异性分析,因为它能够从其他甾体中选择性分离这些化合物,并将它们定量洗脱在单一馏分中。对两名动脉高血压患者尿甾体的分析表明,3β, 16α - 二羟基 - 5 - 雄烯 - 17 - 酮的含量升高。

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