柱前衍生化UPLC-MS/MS法测定川芎药材中二氯喹啉酸残留  

Determination of Quinclorac Residue in Szechwan Lovage Rhizome by UPLC-MS/MS with Precolumn Derivatization

作　　者：董自艳 马晓英 毕瑞锋 章晨峰[1] 王团结[1] 刘茫茫 Dong Ziyan;Ma Xiaoying;Bi Ruifeng;Zhang Chenfeng;Wang Tuanjie;Liu Mangmang(State Key Laboratory of New-Tech for Chinese Traditional Medicine Pharmaceutical Process,Jiangsu Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China;Merieux Nutri Sciences Testing Technology(Qingdao)Co.,Ltd.,Qingdao 266000,China)

机构地区：[1]江苏康缘药业股份有限公司中药制药过程新技术国家重点实验室,江苏连云港222001 [2]梅里埃检测技术(青岛)有限公司,山东青岛266000

出　　处：《亚太传统医药》2024年第3期40-43,共4页Asia-Pacific Traditional Medicine

基　　金：国家重点研发计划中医药现代化项目:基于筋骨理论的腰椎间盘突出症中医药方案循证评价及机制研究(2021YFC1712802)。

摘　　要：目的:建立川芎中二氯喹啉酸残留的UPLC-MS/MS分析方法,为川芎药材的安全性研究提供依据。方法:药材中的二氯喹啉酸用0.5%氨水-甲醇溶液提取,提取液吹干,甲醇复溶后,用三甲基硅烷化重氮甲烷衍生化,采用电喷雾离子源(ESI+),多反应监测模式(MRM)下分析。结果:在0.01、0.05、0.1 mg/kg加标水平下,二氯喹啉酸回收率为83.2%~98.5%,RSD为0.9%~8.2%。结论:该方法简单快速准确,适用于川芎中二氯喹啉酸残留的检测,并按欧盟法规制定川芎中二氯喹啉酸的最大残留限量为0.01 mg/kg,能够保证川芎的用药安全。Objective:To establish a UPLC-MS/MS method for the determination of quinclorac residue in Szechwan Lovage Rhizome,and provide a basis for the safety research of Szechwan Lovage Rhizome.Methods:Sample was extracted with 0.5%ammonia-methanol solution,after dryness under nitrogen blowing,redissolved with methanol,derivatized with(Trimethylsilyl)diazomethane,and detected with electrospray ion source(ESI+)and multiple reaction monitoring mode(MRM).Results:At the spiked levels of 0.01,0.05,and 0.1mg/kg,the recoveries of quinclorac were 83.2%~98.5%with RSD 0.9%~8.2%.Conclusion:The method is simple,rapid,accurate,and suitable for the detection of quinclorac residue in Szechwan Lovage Rhizome.The maximum residue limit of quinclorac is 0.01mg/kg according to EU regulation,the propasal method could guarantee the quality safety of Szechwan Lovage Rhizome.

关 键 词：川芎 液相色谱-串联质谱 二氯喹啉酸 残留 

分 类 号：R282[医药卫生—中药学]