延胡索炮制前后多组分质量控制方法的研究

Study on the method of multi-component quality control before and after processing of corydalis yanhusuo

[目的]建立超高效液相色谱法(UPLC)同时测定延胡索药材中四氢非洲防己碱、原阿片碱、四氢黄连碱、非洲防己碱、延胡索乙素、盐酸小檗碱、盐酸巴马汀、去氢紫堇碱8种生物碱含量的方法,并对延胡索生品及炮制品进行测定。[方法]采用UPLC检测方法,ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),乙腈(B)-0.2%甲酸水溶液,梯度洗脱,流速:0.3 mL/min,柱温55℃,检测波长280 nm。[结果]四氢非洲防己碱,原阿片碱、四氢黄连碱、非洲防己碱、延胡索乙素、盐酸小檗碱、盐酸巴马汀、去氢紫堇碱在0.395～98.8、0.4～100.2、0.99～247.5、0.197～49.4、1.004～251、0.198～49.5、0.398～99.6、1～250μg/mL浓度范围内线性良好,平均加样回收率在98.10%～100.87%,RSD≤1.94(n=6)。[结论] UPLC所建立的方法简便、快速、准确,可应用于延胡索药材中多种成分含量测定,为延胡索药材质量控制提供更加科学、便捷的方法。

[Objective]To establish an UPLC method for the simultaneous determination of eightalkaloids(tetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahy-dropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline)in corydalis yanhusuofrom the products and processed products.[Methods]The separationwas performed on an ACQUITY UPLCBEH C18(100 mm×2.1 mm,1.7 μm)columnin the UPLC method.The mobile phases consisted of acetonitrile(B)and 0.2% formic acid aqueous solutionwith gradient elution.The flow rate was 0.3 mL/min,the column temperature was 55 ℃,and the detection wavelength was 280 nm.[Results]Good linearities oftetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahydropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline were achievedwithin the range of 0.395~98.8、0.4~100.2、0.99~247.5、0.197~49.4、1.004~251、0.198~49.5、0.398~99.6、1~250 μg/mL,respectively.The average recoveries were in the range of 98.10%-100.87%,RSD≤1.94(n=6).[Conclusion]The method established by UPLC is simple,rapid and accurate,and it can be applied to the determination of various components in Corydalis yanhusuo,and provide a more scientific and convenient method for the quality control of Corydalis yanhusuo.