HPLC-MS/MS法同时测定杜仲饮片及其单方制剂中11种成分的含量  

Simultaneous Determination of 11 Compounds in Eucommia Ulmoides Pieces and its Single Prescription Preparations by HPLC-MS/MS

作　　者：郭琴 高焕[2] 李小锋 王欢欢[2] 张立石[1] 柏冬[1] Guo Qin;Gao Huan;Li Xiaofeng;Wang Huanhuan;Zhang Lishi;Bai Dong(Institute of Basic Theory of Chinese Medicine,China Academy of Chinese Medical Sciences,Beijing 100700,China;Shaanxi University of Chinese Medicine;Jiangxi Puzheng Pharmaceutical Co.Ltd.)

机构地区：[1]中国中医科学院中医基础理论研究所,北京100700 [2]陕西中医药大学 [3]江西普正制药股份有限公司

出　　处：《中国药师》2022年第2期369-372,385,共5页China Pharmacist

基　　金：国家自然科学基金青年科学基金项目(编号:81403282);江西省博士后科研项目(编号:2018KY23);中央级公益性科研院所基本科研业务费专项资金资助(编号:YZ202027)。

摘　　要：目的:建立HPLC-MS/MS法同时测定杜仲及其单方制剂中桃叶珊瑚苷、京尼平苷酸、原儿茶酸、丁香树脂醇双葡萄糖苷、松脂醇二葡萄糖苷、芦丁、无梗五加苷B、松脂醇葡萄糖苷、京尼平苷、槲皮素、咖啡酸和绿原酸11种成分的方法。方法:采用安捷伦SB C_(18)色谱柱(2.1 mm×50 mm,1.8μm),流动相为0.1%甲酸水-含0.1%甲酸的乙腈,梯度洗脱,流速为0.3 ml·min^(-1),进样量为2μl,柱温为35℃,质谱采用ESI源,雾化器压力为40 psi,在多反应监测负离子模式下进行检测。结果:桃叶珊瑚苷、京尼平苷酸、原儿茶酸、丁香树脂醇双葡萄糖苷、松脂醇二葡萄糖苷、芦丁、无梗五加苷B、松脂醇葡萄糖苷、京尼平苷、槲皮素、咖啡酸、绿原酸在16.20~10120 ng·ml^(-1)、3.30~10220 ng·ml^(-1)、3.20~1000 ng·ml^(-1)、3.20~1008 ng·ml^(-1)、3.20~10140 ng·ml^(-1)、3.20~1000 ng·ml^(-1)、2.80~885 ng·ml^(-1)、3.30~1018 ng·ml^(-1)、3.20~2004 ng·ml^(-1)、3.30~1045 ng·ml^(-1)、2.60~798 ng·ml^(-1)的范围内线性关系良好(r≥0.9989),平均加样回收率为91.3%~104.3%,RSD为0.5%~6.5%(n=6)。结论:本研究建立的方法专属性好,稳定可靠,可为杜仲及其单方制剂的质量控制提供依据。Objective:To establish a method for the simultaneous determination of geniposidic acid,protocatechuic acid,syringaresinol-di-O-glucoside,pinoresinol diglucoside,rutin,eleutheroside B,pinoresinol glucoside,geniposide,quercetin,caffeic acid and chlorogenic acid in Eucommia ulmoides pieces and its preparations.Methods:The determination of 11 compounds was performed on a 35℃thermostatic Agilent SB C_(18)column(2.1 mm×50 mm,1.8μm)with the mobile phase consisting of 0.1%formic acid water-acetonitrile containing 0.1%formic acid at a flow rate of 0.3 ml·min^(-1)with gradient elution.The injection volume was 2μl.Mass spectrometry was performed by using an ESI source at 40 psi atomizer pressure in a multiple reaction monitoring negative ion mode.Results:Good linear relationships were found for geniposidic acid,protocatechuic acid,syringaresinol-di-O-glucoside,pinoresinol diglucoside,rutin,eleutheroside B,pinoresinol glucoside,geniposide,quercetin,caffeic acid and chlorogenic acid within the ranges of 16.20-10120 ng·ml^(-1),3.30-10220 ng·ml^(-1),3.20-1000 ng·ml^(-1),3.20-1008 ng·ml^(-1),3.20-10140 ng·ml^(-1),3.20-1000 ng·ml^(-1),2.80-885 ng·ml^(-1),3.30-1018 ng·ml^(-1),3.20-2004 ng·ml^(-1),3.30-1045 ng·ml^(-1)and 2.60-798 ng·ml^(-1),respectively.The RSD values of precision results were less than 5%.The average recoveries were 91.3%-104.3%with the RSDs of 0.5%-6.5%(n=6).Conclusion:The method established in this study has good specificity,stability and reliability,and can provide reference for the quality control of Eucommia ulmoides and its preparations.

关 键 词：杜仲 高效液相色谱-串联质谱 含量测定 制剂 

分 类 号：R927.2[医药卫生—药学]