HPLC-QAMS法同时测定前列平胶囊中7种成分的含量  

Quantitative determination of seven components in Qianlieping capsule by HPLC-QAMS

作　　者：刘德军[1] 贺玲 樊苗苗 陶弘武[4] 慕扬娜 LIU De-jun;HE Ling;FAN Miao-miao;TAO Hong-wu;MU Yang-na(Department of Preparation Center,the Third Affiliated Hospital of Liaoning University of Traditional Chinese Medicine,Shenyang 110003,China;Shenyang Hongqi Pharmaceutical Co.,Ltd,Shenyang 110179,China;Liaoyang Drug Inspection Institute,Liaoyang 111000,China;The Second Affiliated Hospital of Liaoning University of Traditional Chinese Medicine&Liaoning Province Chinese Medicine Research Institute,Shenyang 110034,China)

机构地区：[1]辽宁中医药大学附属第三医院制剂中心,辽宁沈阳110003 [2]沈阳红旗制药有限公司,辽宁沈阳110179 [3]辽阳市药品检验所,辽宁辽阳111000 [4]辽宁中医药大学附属第二医院&辽宁省中医药研究院,辽宁沈阳110034

出　　处：《实用药物与临床》2020年第12期1119-1125,共7页Practical Pharmacy and Clinical Remedies

基　　金：辽宁省科技厅公益基金(20170019)。

摘　　要：目的建立高效液相一测多评法(HPLC-QAMS)同时测定前列平胶囊中菊苣酸、羟基红花黄色素A、红花黄色素A、丹参素、丹酚酸B、丹参酮Ⅰ和丹参酮ⅡA的含量。方法采用高效液相色谱法,以Agilent ZORBAX SB-C 18柱(250 mm×4.6 mm,5μm)为色谱柱,流动相:乙腈-0.4%磷酸水溶液,梯度洗脱,流速为1.0 ml/min,检测波长分别为330 nm(检测菊苣酸)、403 nm(检测羟基红花黄色素A和红花黄色素A)和280 nm(检测丹参素、丹酚酸B、丹参酮Ⅰ和丹参酮ⅡA),柱温为30℃。以丹酚酸B为内参物,建立其他6个成分的相对校正因子,计算各成分含量。结果菊苣酸、羟基红花黄色素A、红花黄色素A、丹参素、丹酚酸B、丹参酮Ⅰ和丹参酮ⅡA分别在0.66~16.50μg/ml(r=0.9991)、4.59~114.75μg/ml(r=0.9993)、3.87~96.75μg/ml(r=0.9997)、0.81~20.25μg/ml(r=0.9995)、12.63~315.75μg/ml(r=0.9996)、1.09~27.75μg/ml(r=0.9994)、1.78~44.50μg/ml(r=0.9998)范围内线性关系良好,平均加样回收率(RSDs)分别为97.86%(1.44%)、99.42%(0.96%)、99.18%(0.83%)、96.97%(1.11%)、100.02%(0.59%)、97.91%(1.37%)和98.90%(0.76%),一测多评法计算结果与外标法实测结果无明显差异。结论所建立的HPLC-QAMS结果准确,可用于前列平胶囊的质量控制。Objective To develop an HPLC-QAMS method for the determination of chicoric acid,hydroxysafflor yellow A,safflor yellow A,Danshensu,salvianolic acid B,tanshinone Ⅰ and tanshinone ⅡA in Qianlieping capsule.Methods Separation was carried out using Agilent ZORBAX SB-C18(250 mm×4.6 mm,5μm)with mobile phase of acetonitrile-0.4% phosphoric acid solution in gradient elution.The detection wavelength was set at 330 nm for chicoric acid,403 nm for hydroxysafflor yellow A and safflor yellow A,and 280 nm for Danshensu,salvianolic acid B,tanshinone Ⅰ and tanshinone ⅡA.The flow rate was 1.0 ml/min,and the column temperature was 30℃.Using salvianolic acid B as an internal standard,the relative correction factors of the other six constituents were established,after which the content determination was made.Results Chicoric acid,hydroxysafflor yellow A,safflor yellow A,Danshensu,salvianolic acid B,tanshinone Ⅰ and tanshinone ⅡA showed good linear relationships within the ranges of 0.66~16.50μg/ml(r=0.9991),4.59~114.75μg/ml(r=0.9993),3.87~96.75μg/ml(r=0.9997),0.81~20.25μg/ml(r=0.9995),12.63~315.75μg/ml(r=0.9996),1.09~27.75μg/ml(r=0.9994)and 1.78~44.50μg/ml(r=0.9998),whose average recoveries(RSD s)were 97.86%(1.44%),99.42%(0.96%),99.18%(0.83%),96.97%(1.11%),100.02%(0.59%),97.91%(1.37%)and 98.90%(0.76%),respectively.No significant difference in quantitative results was observed between ESM and QAMS method.Conclusion The established HPLC-QAMS method is accurate and can be used for the quality control of Qianlieping capsule.

关 键 词：一测多评法 前列平胶囊 相对校正因子 含量测定 

分 类 号：R927.2[医药卫生—药学]