液相色谱-串联质谱法同时测定中成药与保健食品中非法添加的9种尿酸调节类药物  

Determination of Nine Uric Acid Regulation Drugs Illegally Added in Chinese Traditional Patent Medicine and Health-care Food by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张秋炎 罗辉泰[1] 黄晓兰[1] 吴惠勤[1] 朱志鑫[1] 黄芳[1] 林晓珊[1] 谢梦婷 吴庆晖 马叶芬[1] ZHANG Qiu-yan;LUO Hui-tai;HUANG Xiao-lan;WU Hui-qin;ZHU Zhi-xin;HUANG Fang;LIN Xiao-shan;XIE Meng-ting;WU Qing-hui;MA Ye-fen(Guangdong Engineering and Technology Research Center for Quality and Safety of Traditional Chinese Medicine,Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,Guangdong Institute of Analysis, Guangzhou 510070,China)

机构地区：[1]广东省测试分析研究所广东省化学危害应急检测技术重点实验室广东省中药质量安全工程技术研究中心,广东广州510070

出　　处：《分析测试学报》2018年第9期989-994,共6页Journal of Instrumental Analysis

基　　金：广东省省级科技计划项目(2014B070705001)

摘　　要：建立了液相色谱-串联质谱同时快速测定中成药和保健食品中9种非法添加尿酸调节类药物的新方法。样品经水分散后,加入乙腈涡旋、超声提取,提取液用Poroshell 120 Bonus-RP(100 mm×2. 1 mm,2. 7μm)色谱柱进行分离,以0. 1%(体积分数)乙酸溶液(含5 mmol/L甲酸铵)-乙腈为流动相,梯度洗脱。在电喷雾正离子模式下,以多反应监测(MRM)模式采集数据并作定性鉴别和定量分析。结果表明,9种药物在相应的质量浓度范围内线性关系良好,相关系数均大于0. 99,在3个不同加标水平下的平均回收率为79. 2%~108%,相对标准偏差(RSD)为1. 2%~12%,检出限(LOD)和定量下限(LOQ)分别为0. 03~0. 6 mg/kg及0. 1~2. 0mg/kg。结果表明,该法简单、快速、灵敏、准确、可靠,适用于中成药和保健食品中9种非法添加尿酸调节类药物的同时快速定性定量分析。A comprehensive analytical method was developed for the simultaneous determination of nine uric acid regulation drugs illegally added in Chinese traditional patent medicine and health-care food by liquid chromatography-tandem mass spectrometry(LC-MS/MS).The sample was dipersed with water,and the analytes were ultrasonically extracted using vortex mixer with acetonitrile.The chromatographic separation was performed on a Poroshell 120 Bonus-RP chromatographic column(100 mm×2.1 mm,2.7μm),with 0.1%(by volume)acetic acid aqueous solution containing 5 mmol/L ammonium formate and acetonitrile as mobile phases by gradient elution.The qualitative and quantitative analyses were performed by electrospray ionization mass spectrometry in positive mode under multiple reaction monitoring(MRM)mode.Results showed that the calibration curves for nine drugs were linear in the corresponding concentration ranges with their correlation coefficients larger than 0.99.The average recoveries for 9 drugs at three spiked levels ranged from 79.2%to 108%,with relative standard deviations(RSDs)of 1.2%-12%.The limits of detection(LOD)and quantitation(LOQ)were in the ranges of 0.03-0.6 mg/kg and 0.1-2.0 mg/kg,respectively.The established method is simple,rapid,sensitive,accurate and reliable,and is suitable for the determination of nine uric acid regulation drugs illegally added in Chinese traditional patent medicine and health-care food.

关 键 词：液相色谱-串联质谱 中成药 保健食品 尿酸调节类药物 非法添加 

分 类 号：O657.7[理学—分析化学] R914.1[理学—化学]