HPLC-QAMS法同时测定补益蒺藜丸中10种成分的含量  

Simultaneous quantitative determination of ten components in Buyi Jili Wan by HPLC-QAMS

作　　者：李苏颖 张明亮 LI Suying;ZHANG Mingliang(Department of Pharmacy,Henan Medical College,Zhengzhou 451191,China;Henan Province Engineering Laboratory for Clinical Evaluation Technology of Chinese Medicine,The First Affiliated Hospital of Henan University of CM,Zhengzhou 450000,China)

机构地区：[1]河南医学高等专科学校药学系,河南郑州451191 [2]河南中医药大学第一附属医院中药临床评价技术河南省工程实验室,河南郑州450000

出　　处：《沈阳药科大学学报》2021年第12期1286-1295,共10页Journal of Shenyang Pharmaceutical University

基　　金：河南省医学科技攻关计划项目(2018020530);河南省中医药科学研究专项(2019ZY2144);河南省医学教育研究项目(Wjlx2021119)。

摘　　要：目的建立高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single marker,HPLC-QAMS)法同时测定补益蒺藜丸中沙苑子苷、毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素、柚皮芸香苷、橙皮苷、川陈皮素、白术内酯Ⅲ和白术内酯Ⅰ的含量。方法采用高效液相色谱法,Kromasil C_(18)色谱柱(250 mm×4.6 mm,5μm),柱温为30℃;以乙腈:甲醇(体积比为9∶1)-体积分数0.1%甲酸水溶液为流动相,梯度洗脱,流速1.0 mL·min^(-1),检测波长分别为260 nm(检测沙苑子苷、毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮和芒柄花素)、300 nm(检测柚皮芸香苷、橙皮苷和川陈皮素)和220 nm(检测白术内酯Ⅲ和白术内酯Ⅰ);以橙皮苷为内参物,建立其与其他9种待测成分的相对校正因子(relative correction factor,f)并进行一测多评,同时采用外标法(external standard method,ESM)对这10种成分进行实测,比较一测多评法和外标法的含量测定结果。结果沙苑子苷、毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素、柚皮芸香苷、橙皮苷、川陈皮素、白术内酯Ⅲ和白术内酯Ⅰ的线性范围分别为2.064~41.28、1.816~36.32、1.248~24.96、1.112~22.24、3.568~71.36、2.304~46.08、5.256~105.12、0.584~11.68、0.488~9.76、0.432~8.64 mg·L^(-1),r为0.9991~0.9997;平均加样回收率分别为98.20%、99.06%、97.96%、97.59%、98.68%、96.98%、100.05%、99.35%、97.81%和96.93%,RSD分别为1.16%、0.93%、1.05%、1.61%、1.38%、1.14%、0.79%、1.27%、0.96%和0.86%;高效液相色谱一测多评法计算值和外标法实测值无显著性差异。结论所建立的HPLC-QAMS法操作便捷,结果准确,可用于补益蒺藜丸的质量评价研究。Objective To establish a high performance liquid chromatography-quantitative analysis of multi-components by single marker(HPLC-QAMS) method for the simultaneous determination of complanatuside,calycosin 7-O-β-D-glucopyranoside,ononin,calycosin,formononetin,narirutin,hesperidin,nobiletin,atracylenolide Ⅲ and atracylenolide Ⅰ in Buyi Jili Wan.Methods Kromasil C_(18) column(250 mm×4.6 mm,5 μm)was used for high performance liquid chromatography with acetonitrile-methanol(V∶V=9∶1)-0.1% formic acid solution as mobile phase,gradient elution,flow rate of 1.0 mL·min^(-1),column temperature of 30 ℃.The detection wavelength were set at 260 nm for complanatuside,calycosin 7-O-β-D-glucopyranoside,ononin,calycosin and formononetin,300 nm for narirutin,hesperidin and nobiletin,and 220 nm for atracylenolide Ⅲ and atracylenolide Ⅰ.Using hesperidin as the internal reference,relative correction factors(RCF) of other nine components were calculated respectively,and the contents of other nine components were calculated by RCF.The contents of ten components were determined by external standard method(ESM).The results of content determination by QAMS were compared with ESM.Results Complanatuside,calycosin7-O-β-D-glucopyranoside,ononin,calycosin,formononetin,narirutin,hesperidin,nobiletin,atracylenolide Ⅲ and atracylenolide Ⅰhad good relations within the range of 2.064-41.28,1.816-36.32,1.248-24.96,1.112-22.24,3.568-71.36,2.304-46.08,5.256-105.12,0.584-11.68,0.488-9.76,0.432-8.64 mg·L^(-1)(r=0.999 1-0.999 7);the average recovery were 98.20%,99.06%,97.96%,97.59%,98.68%,96.98%,100.05%,99.35%,97.81% and 96.93%;RSDs were 1.16%,0.93%,1.05%,1.61%,1.38%,1.14%,0.79%,1.27%,0.96% and 0.86%,respectively.There was no significant difference between the calculated value of HPLC-QAMS method and the measured value of ESM.Conclusion The HPLC-QAMS method is simple and accurate,and can be used for quality evaluation of Buyi Jili Wan.

关 键 词：高效液相色谱一测多评法 相对校正因子 补益蒺藜丸 含量测定 

分 类 号：R917[医药卫生—药物分析学]