HPLC测定吴茱萸及其制剂中吴茱萸碱和吴茱萸次碱含量

 目的:建立吴茱萸药材及其制剂华佗再造丸中吴茱萸碱和吴茱萸次碱的含量测定方法。方法:反相高效液相色谱法。主要色谱条件包括:吴茱萸药材:流动相为乙腈-水(50∶50),流速1.0ml·min^-1,内标物为醋酸甲羟孕酮;华佗再造丸:流动相为乙腈-水(40∶60),流速1.0ml·min^-1,内标物为联苯;紫外检测波长均为225nm。结果:吴茱萸药材中吴茱萸碱和吴茱萸次碱的线性浓度范围均为5～50μg·ml^-1;回收率分别为96.6%和96.4%;批内RSD分别为0.8%～1.5%和1.1%～2.3%(n=6);批间RSD分别为2.3%～3.6%和2.5%～3.9%(n=6)。华佗再造丸中二组分的线性浓度范围均为0.5～20μg·ml^-1;回收率分别为97.6%和94.6%。经测定,同种不同产地的4种吴茱萸中吴茱萸碱和吴茱萸次碱的含量分别为0.118%和0.092%,0.213%和0.106%,0.581%和0.609%,0.478%和0.459%;华佗再造丸中二组分的含量分别为0.1123mg·g^-1和0.0981mg·g^-1。结论:该方法可用于吴茱萸药材及其制剂的质量控制。

Determination of evodiamine and rutaecarpine in Evodia rutaecarpa and Huatuo Zaizao Pill by HPLC

OBJECTIVE:To establish a quantitative method for the determination of two main active ingredients,evodiamine and rutaecarpine,in Chinese medicinal crop Evodia rutaecarpaand its preparation Huatuo Zaizao pill.METHOD:Evodiamine and rutaecarpine were determined by RP-HPLC for Evodia rutaecarpa,the mobile phase consisted of acetonitrile-water(50∶50),the flow rate was 1.0ml·min^-1,medroxyprogesteron acetate was used as internal standard.For Huatuo Zaizao pill,the mobile phase consisted of acetonitrile-water(40∶60),the flow rate was 1.0ml·min^-1,biphenyl was used as internal standard.The eluent was monitored with UV detector at225nm.RESULTS:For Evodia rutaecarpa,the standard curves of evodiamine and rutaecarpine were all linear over the concentration range of 5～50μg·min^-1.The average recoveries were 96.6% and 96.4% respectively.The intra-run relative standard deviations were 0.8%～1.5% and 1.1%～2.3%(n=6),respectively,the inter-run relative standard deviations were 2.3%～3.6% and 2.5 %～3.9%(n=6),respectively.For Huatuo Zaizao pill,the standard curve of evodiamine and rutaecarpine were all linear over the range of 5～20μg·ml^-1,the average recoveries were 97.6% and 94.6%,respectively.The contents of evodiamine and rutaecarpine in Evodia rutaecarpa from four localities of growth were 0.118% and 0.092%,0.213% and 0.106%,0.581% and 0.609%,0.4 78% and 0.459%,respectively.In Huatuo Zaizao pill,the contents of two ingredients were 0.1123mg·g^-1 and 0.0981mg·g^-1,respectively.CONCLUSION:This method is accurate,convenient and sensitive.It is satisfactory for the quality control of Evodia rutaecarpa and its preparations.