LC-MS法同时测定雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量  

Determination of contents of euonine and wilforidine in Tripterygium wilfordii hook.F.extract by liquid chromatography coupled with mass spectrometry

作　　者：陈晓红[1] 何世伟[2] 沈称意[3] 蔡美强[3] 金米聪[1] 

机构地区：[1]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,宁波315010 [2]浙江大学化学工程与生物工程学系,杭州310027 [3]浙江工商大学环境科学与工程学院固废处理与资源化研究所,杭州310035

出　　处：《中国临床药学杂志》2013年第2期81-85,共5页Chinese Journal of Clinical Pharmacy

基　　金：浙江省公益性技术应用研究计划项目(2011C37002);宁波市自然科学基金项目(2011A610058)

摘　　要：目的建立一种灵敏、准确的雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的LC-MS法。方法雷公藤浸膏样品经氯仿溶解后用稀盐酸(2.0 mol·L^(-1))溶液提取,上清液移入Oasis(?)MCX固相萃取小柱进行净化,然后样品在Zorbax Plus RRHD C_(18)柱(50 mm×2.1 mm,1.8μm)上,以醋酸铵缓冲液[0.05%醋酸-酸酸铵溶液(5 mmol·L^(-1))]-乙腈(30:70)为流动相进行分离,应用LC-MS法,在大气压化学电离正离子选择离子监测模式(SIM)下测定,雷公藤新碱和雷公藤碱戊的定量离子分别为m/z806和m/z 779。结果雷公藤新碱和雷公藤碱戊的绝对回收率为87.0%~97.5%,在含量1.0~200.0μg·kg^(-1)内均具有良好线性,日内RSD均<9.8%,日间RSD均<14.7%,定量检出限均为1.0μg·kg^(-1)。结论本方法简便、灵敏、干扰少、特异性好,可用于雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的监测。AIM To establish a sensitive and accurate method for the determination of contents of trace euonine and wilforidine in Tripterygium wilfordii hook. F. extract by liquid chromatography coupled with mass spectrometry （LC- MS）. METHODS After the alkaloids in Tripterygium wilfordii hook. F. extract was dissolved by chloroform and ex- tracted by hydrochloric acid solution （2.0 mol L-1）, the supernatant was cleaned by the solid-phase extraction （SPE） using Oasis MCX cartridges. The separation was performed on a Zorbax Plus RRHD C18 column（50 mm × 2.1 mm, 1.8 μm）using a mobile phase consisting of 0.05 % acetic acid-ammonium acetate （5 mmol L- 1 ）.acetonitrile （30 ： 70）. Detection was carried out by a positive atmospheric-pressure chemical ionization mass spectrometry （APCI-MS） in the se- lected ion monitoring （SIM） mode with the protonated molecular ions m/z 806 [M ＋ H]＋ and m/z 779 [M ＋ H]＋ for euonine and wilforidine, respectively. RESULTS Calibration curves were linear within the range of 1.0 - 200.0 μg kg- 1, and the extraction recoveries were from 87.0 % to 97.5 %. The intra-day RSD was less than 9.8 %, the inter-day RSD was less than 14.7 %, and the limits of quantification （LOQ） were 1.0 μg kg-l for the two alkaloids. CONCLU- SION This method is found to be simple, sensitive and little interferential, and can be used for the determination of trace euonine and wilforidine in Tripterygium wilfordii hook. F. extract.

关 键 词：液相色谱-质谱法 固相萃取 选择离子监测 雷公藤浸膏 雷公藤新碱 雷公藤碱戊 

分 类 号：R286.0[医药卫生—中药学]