高效液相色谱-串联质谱法同时测定参麦注射液中9种皂苷  

Simultaneously Quantification of Ginsenoside Rg1,Re,Rf,Rd,Rc,Rb2,Rb1,Ro and Ophiopogonin D in Shenmai Injection by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：余健[1] 徐晓珍[1] 顾利强[1] 高海燕[1] 辛艳飞[1] 宣尧仙[1] 

机构地区：[1]浙江省医学科学院安全性评价研究中心,浙江杭州310000

出　　处：《中华中医药学刊》2014年第1期71-74,共4页Chinese Archives of Traditional Chinese Medicine

基　　金：国家"十二五"科技重大专项(2011ZX09301-003);浙江省科技计划项目(2011C37079;2013F 20005);浙江省中医药管理局项目(2013ZZ003)

摘　　要：目的：本研究采用高效液相色谱-串联质谱检测方法,建立同时测定参麦注射液中人参皂苷Rg1,Re,Rf,Rc,Rd,Rb1,Rb2,Ro和麦冬皂苷D的分析方法。方法：本实验应用ThermoBDSHypersilC18柱（150mm×2.1mm,5μm）,柱温30℃。以乙腈（A）-0.02%醋酸溶液（B）为流动相进行梯度洗脱,流速0.2mL.min-1,以电喷雾离子源选择反应监测（SRM）方式正离子模式分别检测离子对m/z823.5→643.75（人参皂苷Rg1）,m/z969.4→789.46（人参皂苷Re）,m/z823.6→371.94（人参皂苷Rf）,m/z1101.7→343.17（人参皂苷Rc）,m/z969.4→789.46（人参皂苷Rd）,m/z1131→371.80（人参皂苷Rb1）,m/z1101.7→343.35（人参皂苷Rb2）,m/z979.7→641.65（人参皂苷Ro）;负离子模式检测离子对m/z889.4→853.67（麦冬皂苷D）。结果：本法专属性良好,各成分均能达到有效分离,线性关系良好（r〉0.99）,人参皂苷Rg1,Re,Rf,Rc,Rd,Rb1,Rb2,Ro和麦冬皂苷D最低定量限分别为0.03、0.003、0.3、0.03、0.003、0.03、0.03、5、3ng.mL-1,回收率均在97.10%～102.14%范围内,重复进样精密度均小于2.63%（RSD）。讨论：与文献中报道方法相比,本方法快速、灵敏度高、准确性好、重复性好,可以对参麦注射液中含量差异较大的四类皂苷类成分进行同时定量,能够用于参麦注射液的含量测定和质量控制。Objective： In order to simultaneously determine the amounts of ginsenoside Rgl, Re, Rf, Rd, Rc, Rb2, Rbl, Ro and ophiopogonin D in Shenmai Injection,liquid chromatographytandem mass spectrometry was involved in the experiment. Method： Separations of analytes were achieved by a Thermo BDS HYPERSIL CIS column （ 150 mm × 2.1 mm,5μm） at 30℃. Acetonitrile （A）/0.02% acetic acid solution （B） （3： 7,v： v） was used as mobile phase and flow rate was 200μL/min. Quantification was performed using selected reaction monitor （SRM） mode of the transition of m/ z 1131→371.80 for Rbl , m/z 1101.7→343.35 for Rb2, m/z 1101.7→343.17 for Rc, m/z 969.4→789.46 for Rd, m/z 969.4→789.46 for Re ,m/z 823.6→371.94 for Rf,m/z 823.5→ 643.75 for Rgl ,m/z 979.1→641.65 for Ro by positive ionization mass spectrometry, m/z 889.4→853.67 for ophiopogonin D by negative ionization mass spectrometry. Result ： The linear over the investigated concentration range with a good correlation coefficient was higher than 0.99. The LOQ of Rgl, Re, Rf, Rd, Re, Rb2, Rbl, Ro and ophiopogonin D was 0.03,0. 003,0.3,0.03,0. 003,0.03,0.03,5,3 ng · mL-1. The recovery of the method ranges was from 97.10 % to 102.14% and the precisions were all no more than 2.63%. According to validation, our method was proved to be rapid and high sensitive. Conclusion： Present method could be easily applied to the determination and quality control of ginsenoside Rgl, Re, Rf, Rd, Re, Rb2, Rbl, Ro and ophiopogonin D in Shenmai Injection.

关 键 词：参麦注射液 人参皂苷 麦冬皂苷 高效液相色谱-串联质谱法 

分 类 号：R284.1[医药卫生—中药学]