Synthesis,Characterization and Detection of Related Substances of Dydrogesterone
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,3 μm)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,1H NMR and 13C NMR,the determination methods are highly sensitive and specific,and can be used for the determination of dydrogesterone.
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