超高效液相色谱-质谱/质谱联用法快速测定苦碟子注射液中两种倍半萜内酯类成分的含量  

Simultaneous Content Determination of Two Sesquiterpene Lactones in Ku-Die-Zi Injection by UPLC-ESI-MS/MS

作　　者：董鲁艳[1] 刘颖[2] 张加余[2] 蔡伟[1] 刘荣荣[1] 卢建秋[2] 

机构地区：[1]北京中医药大学中药学院,北京100102 [2]北京中医药大学科研实验中心,北京100029

出　　处：《世界科学技术-中医药现代化》2014年第12期2671-2675,共5页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：科学技术部国家"973"计划项目(2012CB518406):治疗心血管疾病有效方剂组分配伍规律研究--组分配伍方药临床应用基础研究;主课题负责人:张允岭;子课题负责人:卢建秋

摘　　要：目的:建立快速测定苦碟子注射液中两种倍半萜内酯类成分Ixerin Z、11,13α-dihydroixerin Z含量的超高效液相色谱-质谱/质谱联用方法(UPLC-ESI-MS/MS)。方法:采用Waters ACQUITY BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为乙腈-水系统梯度洗脱,流速为0.4 m L·min-1,柱温为40℃;在ESI负离子模式下,采用多反应离子监测(MRM)扫描方式进行检测。结果:苦碟子注射液中两种倍半萜内酯类成分在2 min内完全分离,Ixerin Z的线性范围在5.70-182.50 ng·m L-1,11,13α-dihydroixerin Z的线性范围在4.60-131.25 ng·m L-1,相关系数r均大于0.999 0,加样回收率(n=6)分别为98.18%、97.52%,RSD值均小于1.5%。应用所建立的方法对市售苦碟子注射液中两种倍半萜内酯类成分Ixerin Z、11,13α-dihydroixerin Z进行含量测定,两个厂家6个批次苦碟子注射液中Ixerin Z、11,13α-dihydroixerin Z的含量有一定的差异。结论:所建立的方法快速、准确、灵敏,可用于苦碟子注射液中两种倍半萜内酯类成分的含量测定。This study was aimed to establish a method for the rapid content determination of Ixerin Z and 11,13α-dihydroixerin Z in Ku-Die-Zi （KDZ） injection by UPLC-ESI-MS/MS. The separation was performed on a Waters ACQUITY BEH C18 column （2.1 mmx 50 mm, 1.7μm） by using a gradient elution with the mobile phase of acetonitrile-water at the flow rate of 0.4 mL·min-1. The column temperature was set at 40℃. Multi-reaction moni-toring （MRM） scanning was employed for quantification in ESI negative mode. The results showed that two sesquit-erpene lactones in KDZ injection were totally separated within 2 min. The linear range of Ixerin Z was 5.70-182.50 ng·mL-1, and the linear range of 11,13α-dihydroixerin Z was 4.60-131.25 ng·mL-1. The correlation coefficient r was more than 0.999 0. The recovery rates （n = 6） were 98.18% and 97.52%, with RSDs 〈 1.5%. The established method was successfully applied for simultaneous content determination of Ixerin Z and 11,13α-dihydroixerin Z in 6 batches of KDZ injection from 2 factories, which had some variations on the content determination results. It was concluded that the method was rapid, accurate and sensitive, which can be used for the content determination of two sesquiterpene lactones in KDZ injection.

关 键 词：超高效液相色谱-质谱/质谱联用方法 苦碟子注射液 倍半萜内酯 Ixerin Z 11 13α-dihy-droixerin Z 

分 类 号：R284.1[医药卫生—中药学]