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利用正相半制备柱和反相分析柱的两步高效液相色谱法,在实验室规模制备了毫克是级维生素D_3的三个重要异构体——维生素D_3前体、光甾醇_3和速甾醇_3·维生素D_3原体,7-去氢胆固醇的光照是在一个装有UVB荧光灯的光治疗室中进行。采用紫外分光光度法和高效液相色谱法对制得的三个异构体进行了定性定量分析。在这三个异构体检测极限下,除了维生素D_3前体中有不超过0.25％的维生素D_3杂质外,三个产品中均没有发现任何除它本身之外的其他异构体杂质。
Using a two-step high performance liquid chromatography with a normal-phase semi-preparative column and a reversed-phase analysis column, milligrams of three important isomers of vitamin D 3 were produced on a laboratory scale—vitamin D 3 precursor, phytosterol _3, and Tachysterol _3·Vitamin D_3 protoplasm, 7-dehydrocholesterol irradiation was performed in a light treatment room equipped with a UVB fluorescent lamp. The three isomers were qualitatively and quantitatively analyzed by UV spectrophotometry and high performance liquid chromatography. At the limit of detection of these three isomers, no impurity other than itself was found in any of the three products except for the vitamin D 3 impurity in the vitamin D 3 precursor.