STEROIDS AND HYPERTENSION .1. GAS-LIQUID-CHROMATOGRAPHY AND GAS-CHROMATOGRAPHY MASS-SPECTROMETRY OF 3,15-DIHYDROXY-17-OXOSTEBOIDS AND 3,16-DIHYDROXY-17-OXOSTEROIDS

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 columuns and on SE‐30 capillary column, and mass spectra of these compounds. These reference steroids were: 3α, 16α‐dihydroxy‐5α‐androstan‐17 one, 3α,16α‐dihydroxy‐5β‐androstan‐17‐one, 3β,16α‐dihydroxy‐5α‐androstan‐17‐one, 3β,16α‐dihydroxy‐5‐androsten‐17‐one, 3β,16β‐dihydroxy‐5‐androsten‐17‐one, 3β,17β‐dihydroxy‐5‐androsten‐16‐one and 3α,15α‐dihydroxy‐5β‐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 3β,16α‐dihydroxy‐5‐androstan‐17‐one. Copyright © 1979 Heyden & Son Ltd