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本文用反相分配层析从样品中分离醋酸脱氧皮质甾酮,然后加入孕甾酮作内标,用反相高压液相层析进行定量,结果稳定、可靠。反相分配层析用溶剂:取95%乙醇95份、水5份,层析用正庚烷50份,于分液漏斗中振摇,平衡后分层取上层液作固定相,下层液作流动相。高压液相用流动相:按表1的比例配制水和乙腈或水和甲醇的混合液,脱气后供用。标准储备液和内标储备液:分别精密秤定美国药典规格醋酸脱氧皮质甾酮和孕甾酮标准品约10mg,用甲醇溶解,分别定量转移至50ml容量瓶中,用甲醇稀释至刻度。高压液相用标准液:精密取标准储备液和内标储备液各5.0ml置50ml容量瓶中,用甲醇稀释至刻度。
In this paper, RP-HPLC was used to separate the deoxycorticosterone acetate from the sample, and then the progesterone was added as internal standard and quantified by reversed-phase high pressure liquid chromatography. The result was stable and reliable. The solvent for reversed-phase partition chromatography was 95 parts of 95% ethanol and 5 parts of water. 50 parts of n-heptane for chromatography was shaken in a separatory funnel. After the equilibration, the supernatant liquid was taken as the stationary phase, Mobile phase. High pressure liquid phase mobile phase: according to the ratio of Table 1 Preparation of water and acetonitrile or water and methanol mixture, degassing for use. Standard stock solution and internal standard stock solution: respectively, the United States Pharmacopoeia precision scale specifications deoxycorticosterone and progesterone acetate about 10mg, dissolved in methanol, were quantitatively transferred to 50ml volumetric flask, diluted with methanol to the mark. High-pressure liquid standard solution: Take standard precision stock solution and internal standard stock solution of 5.0ml set 50ml volumetric flask, diluted with methanol to the mark.