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“抗孕-53”是甾体口服避孕药。在合成过程中产生两个差向异构体,即“2α,17α-双炔基-A-失碳-雄烷-2β,17β-双羟基双丙酸酯”和“2β,17α-双炔基-A-失碳-雄烷-2α,17β-双羟基双丙酸酯”,用高效液相色谱法对此两异构体分离和定量测定进行了研究。用2.6mm×250mm不锈钢色谱柱,填充硅胶A,柱温30℃,以1%乙腈+1%异丙醇+98%正己烷的三元体系混合溶剂作流动相,以紫外分光光度计作检测器,可使此两异构体分离度达1.05。2α-构型化合物定量误差±3%,最低检测量2α型5×10~(-7)g,2β型2.5×10~(-7)g。分析时间15分钟。
“Anti-pregnancy -53” is a steroid oral contraceptive. Two epimers were produced during the synthesis, namely “2α, 17α-diynyne-A-nor-androstane-2β, 17β-bis-hydroxy dipropionate” and “ A-nor-C-androstane-2α, 17β-bishydroxypropyl diphosoate ”was prepared and the separation and quantitation of the two isomers were studied by high performance liquid chromatography. The column was filled with silica gel A on a 2.6 mm × 250 mm stainless steel column with a column temperature of 30 ℃ and a ternary system mixed solvent of 1% acetonitrile + 1% isopropanol + 98% n-hexane as mobile phase and UV spectrophotometer The resolution of the two isomers was 1.05.2. The quantitative error of the 2-a-configuration compounds was ± 3%. The lowest detection limit was 2 × 5 × 10 -7 g and 2 × 2.5 × 10 -7. g. Analysis time 15 minutes.