去氢孕酮有关物质的合成、确证和检测  

Synthesis,Characterization and Detection of Related Substances of Dydrogesterone

作　　者：邹明慧 Zou Minghui(School of Pharmacy,Jiangsu Ocean University,Lianyungang 222000,China)

机构地区：[1]江苏海洋大学药学院,江苏连云港222000

出　　处：《山东化工》2024年第13期85-89,93,共6页Shandong Chemical Industry

摘　　要：目的:依据去氢孕酮的合成路线,合成去氢孕酮3个有关物质并进行来源分析,建立其有关物质的定量测定方法。方法:以9β,10α-孕甾-4,7二烯-3,20-二酮为起始原料,经四氯苯醌氧化得有关物质A,在无水乙醇/氯化氢溶液作用下发生双键重排得有关物质C,以9α,10β-孕甾-4,6-二烯-3,20-二酮为起始原料,经对甲苯磺酸水解重排得有关物质B,有关物质测定采用RP-HPLC法,Hypersil ODS(4.6 mm×150 mm,3μm)色谱柱,以乙醇-乙腈-水(V_(乙醇)∶V_(乙腈)∶V_(水)=10∶30∶60)为流动相,等度洗脱,检测波长为290 nm。结果与结论:通过化学合成得到了3个有关物质,其结构经MS、^(1)H NMR和^(13)C NMR确证;有关物质测定方法灵敏度高、专属性强,可用于去氢孕酮有关物质的测定。Objective:According to the synthesis route of dydrogesterone,make the source analysis of three related substances and establish the quantitative determination method of the related substances.Method:With 9β,10α-pregna-4,7-diene-3,20-dione as the starting material,related substance A,oxidized by chloranil,C after double bond rearrangement in absolute ethanol/hydrogen chloride solution,At 9α,10β-pregna-4,6-diene-3,20-dione as the starting material,related substance B by hydrolysis of p-toluene sulfonic acid,related substances were determined using the RP-HPLC method,hypersil ODS(4.6 mm×150 mm,3μm)column,with ethanol-acetonitrile-water(10∶30∶60,volume ratio)as the mobile phase,isocratic elution,the wavelength was detected at 290 nm.Results and conclusions:Three related substances were obtained by chemical synthesis,and their structures were confirmed by MS,^(1)H NMR and^(13)C NMR,the determination methods are highly sensitive and specific,and can be used for the determination of dydrogesterone.

关 键 词：去氢孕酮 有关物质 合成 确证 RP-HPLC 

分 类 号：TQ463.24[化学工程—制药化工]