一测多评法同时测定复方金蒲片中10种成分的质控方法研究  

An HPLC-QAMS method for simultaneous determination of ten components in Compound Jinpu Tablet for quality control

作　　者：李苏颖 王晶[2] LI Su-ying;WANG Jing(Department of Pharmacy,Henan Medical College,Zhengzhou 451191,China;Department of Pharmacy,Nanjing Hospital of Chinese Medicine Affiliated to Nanjing University of Chinese Medicine,Nanjing 210022,China)

机构地区：[1]河南医学高等专科学校药学系,郑州451191 [2]南京中医药大学附属南京中医院药学部,南京210022

出　　处：《国际药学研究杂志》2019年第12期937-945,共9页Journal of International Pharmaceutical Research

基　　金：河南省医学科技攻关计划项目(2018020530);江苏省药学会-奥赛康医院药学基金(A201808);南京药学会-常州四药医院药学科研基金(2018YX001)。

摘　　要：目的建立一测多评法(QAMS)同时测定复方金蒲片中绞股蓝皂苷XLⅨ、绞股蓝皂苷A、绞股蓝皂苷XⅦ、丹参素、丹酚酸B、丹参酮ⅡA、荭草苷、异荭草苷、牡荆苷和异牡荆苷的含量。方法采用高效液相色谱法,以Wondasil C18柱(250 mm×4.6 mm,5μm)为色谱柱,柱温为30℃;流动相甲醇-乙腈(3∶1)∶0.1%甲酸水溶液,梯度洗脱,流速为0.9 ml/min;检测波长分别为203 nm(检测绞股蓝皂苷XLⅨ、绞股蓝皂苷A和绞股蓝皂苷XⅦ)、280 nm(检测丹参素、丹酚酸B和丹参酮ⅡA)和340 nm(检测荭草苷、异荭草苷、牡荆苷和异牡荆苷)。外标法(ESM)用10种对照品分别测定复方金浦片中各成分的含量;QAMS法则仅以丹参酮ⅡA为内参物,建立其他9种成分的相对校正因子,并以外标法测定的丹参酮Ⅱ含量为基准,利用相对校正因子计算其他9种成分的含量;通过对比分析9种成分含量的QAMS法计算值和ESM法实测值,考察QAMS法的可行性。结果上述10种成分依次分别在2.848~56.96、5.304~106.08、7.776~155.52、1.248~24.96、13.28~265.6、1.976~39.52、1.112~22.24、0.928~18.56、0.696~13.92、0.648~12.96μg/ml范围内线性关系良好(r≥0.9992),平均加样回收率(RSD)分别为99.35%(0.97%)、99.07%(1.10%)、98.81%(0.83%)、97.69%(1.39%)、100.05%(0.79%)、97.90%(1.20%)、98.21%(1.52%)、97.59%(1.44%)、96.93%(1.07%)和96.99%(0.89%)。复方金蒲片中9种成分的QAMS计算结果与外标法(ESM)实测结果无明显差异。结论本文建立的QAMS法仅用一种对照品可同时测定多成分含量,该法简捷,结果准确,可用于同时测定复方金蒲片中10种成分含量。Objective To develop an HPLC method for quantitative analysis of multi-components by single marker(QAMS)to simultaneously determine gypenoside XLⅨ,gypenoside A,gypenoside XⅦ,danshensu,salvianolic acid B,tanshinoneⅡA,orientin,isoorientin,vitexin and isovitexin in Compound Jinpu Tablet(CJT).Methods HPLC was performed on a Wondasil C18 column(250 mm×4.6 mm,5μm)at 30℃.The mobile phase was methanol-acetonitrile(3∶1)and 0.1%formic acid aqueous solution,in a gradient elution,and the flow rate was 0.9 ml/min.The detection wavelength was set at 203 nm for gypenoside XLⅨ,gypenoside A and gypenoside XⅦ,280 nm for danshensu,salvianolic acid B and tanshinoneⅡA,and 340 nm for orientin,isoorientin,vitexin and isovitexin.The content of the ten components in CJT was determined at first by the external standard method(ESM)using ten related standards.For the QAMS method,only tanshinoneⅡA was used as an internal standard,whereas the relative correction factors of the other nine components in CJT were determined using the internal tanshinoneⅡA as reference standard,and their content was calculated on the basis of the correction factors and the tanshinoneⅡA content determined by ESM.The QAMS method was validated by comparison of the calculated values with the measured data by ESM.Results The 10 components all showed a good linearity within the concentration ranges of 2.848-56.96,5.304-106.08,7.776-155.52,1.248-24.96,13.28-265.6,1.976-39.52,1.112-22.24,0.928-18.56,0.696-13.92,and 0.648-12.96μg/ml(r≥0.9992),with the average recoveries(RSDs)of 99.35%(0.97%),99.07%(1.10%),98.81%(0.83%),97.69%(1.39%),100.05%(0.79%),97.90%(1.20%),98.21%(1.52%),97.59%(1.44%),96.93%(1.07%)and 96.99%(0.89%),respectively.No significant differences were found in the content of the nine components in CJT between the QAMS-calculated values and the ESM-measured data.Conclusion The established QAMS method could simultaneously determine multi-components using only one standard.It is simple and accurate,which could be used for simultaneous d

关 键 词：一测多评法 复方金蒲片 相对校正因子 含量测定 

分 类 号：R927.2[医药卫生—药学]