基于HPLC-QAMS法对清心安神合剂中9种成分的含量测定  

Content determination of nine components in Qingxin Anshen Heji by HPLC-QAMS method

作　　者：曲颂扬[1] 关开[1] 周慧 陈巍然[1] 毛清雯 QU Songyang;GUAN Kai;ZHOU Hui;CHEN Weiran;MAO Qingwen(Department of Pharmacy,Affiliated Hospital of Liaoning University of Traditional Chinese Medicine,Shenyang 110032,China;College of Graduate Studies,Liaoning University of Traditional Chinese Medicine,Shenyang 110847,China)

机构地区：[1]辽宁中医药大学附属医院药学部,辽宁沈阳110032 [2]辽宁中医药大学研究生学院,辽宁沈阳110847

出　　处：《沈阳药科大学学报》2021年第6期567-574,共8页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立一测多评法同时测定清心安神合剂中斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B、毛蕊花糖苷、白桦脂酸、焦地黄苯乙醇苷B1、麦冬甲基黄烷酮A、马替诺皂苷、甲基麦冬二氢高异黄酮B的含量。方法采用Sepax Sapphire C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-体积分数0.2%磷酸水溶液,梯度洗脱,流速为1.0 mL·min-1,检测波长分别为204 nm(检测斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B和白桦脂酸)、330 nm(检测毛蕊花糖苷、焦地黄苯乙醇苷B1和马替诺皂苷)和296 nm(检测麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B),柱温为30℃。以毛蕊花糖苷为内参物,建立其他8个成分的相对校正因子,计算各成分的含量,同时与外标法结果进行对比,验证一测多评法的准确性。结果9种目标成分分别在2.98~59.60、1.72~34.40、1.39~27.80、2.57~51.40、1.96~39.20、0.74~14.80、1.63~32.60、1.26~25.20、0.69~13.80 mg·L^(-1)范围内线性关系良好(r≥0.9991),平均加样回收率(RSD)分别为99.28%(1.33%)、98.59%(1.08%)、98.28%(1.16%)、100.07%(0.78%)、99.01%(0.97%)、96.94%(0.94%)、98.73%(1.55%)、97.60%(1.01%)、97.83%(0.83%),采用校正因子计算的含量值与外标法实测值之间无显著差异。结论该方法可用于同时测定清心安神合剂中9种成分含量。Objective To establish an HPLC-QAMS method for the determination of spinosin,jujuboside A,jujuboside B,verbascoside,betulinic acid,jionoside B1,methylophiopogonanone A,martinoside and methylophiopogonanone B in Qingxin Anshen Heji.Methods The separation was developed on a Sepax Sapphire C18 column(250 mm×4.6 mm,5μm)by gradient elution with acetonitrile-0.2%phosphoric acid aqueous solution as the mobile phase.The flow rate was 1.0 mL·min-1.The detection wavelengths were set at 204 nm for spinosin,jujuboside A,jujuboside B and betulinic acid,330 nm for verbascoside,jionoside B1 and martinoside,296 nm for methylophiopogonanone A and methylophiopogonanone B.The column temperature was set at 30℃.Using verbascoside as an internal standard,the relative correction factors between the eight components and verbascoside were calculated and used to assay the contents of eight components,which were compared with external standard method to verify the accuracy of the QAMS method.Results The linear ranges of nine components were 2.98-59.60,1.72-34.40,1.39-27.80,2.57-51.40,1.96-39.20,0.74-14.80,1.63-32.60,1.26-25.20,0.69-13.80 mg·L^(-1)(r≥0.9991),respectively.The average recoveries and RSDs were 99.28%(1.33%),98.59%(1.08%),98.28%(1.16%),100.07%(0.78%),99.01%(0.97%),96.94%(0.94%),98.73%(1.55%),97.60%(1.01%)and 97.83%(0.83%),respectively.There were no significant difference between the calculated values using the relative correction factors and the measured values of the external standard method.Conclusion The QAMS method can simultaneously determine the content of nine components in Qingxin Anshen Heji.

关 键 词：高效液相一测多评法 清心安神合剂 毛蕊花糖苷 酸枣仁皂苷A 麦冬甲基黄烷酮A 含量测定 

分 类 号：R917[医药卫生—药物分析学]