超高效液相色谱-四极杆静电场轨道阱质谱法快速筛查测定抗疲劳类保健食品中112种化学药  

Rapid Screening of 112 Kinds of Illegally Added Chemical Compounds in Anti-fatigue Health Food by Ultra-high Performance Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap Mass Spectrometry

作　　者：黄芳 邓欣 张秋炎 周熙 梁梓洋 徐翠芳 赖晓娜 罗辉泰 吴惠勤 HUANG Fang;DENG Xin;ZHANG Qiu-yan;ZHOU Xi;LIANG Zi-yang;XU Cui-fang;LAI Xiao-na;LUO Hui-tai;WU Hui-qin(Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070,China)

机构地区：[1]广东省科学院测试分析研究所(中国广州分析测试中心),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》2023年第10期1221-1232,共12页Journal of Instrumental Analysis

基　　金：广东省科学院打造综合产业技术创新中心行动资金项目“高端医疗健康与高效生物转化关键技术研究及应用”(2022GDASZH-2022010110)。

摘　　要：建立了一种超高效液相色谱-四极杆静电场轨道阱质谱法(UPLC-Q-Orbitrap HRMS)快速筛查测定抗疲劳保健中112种非法添加化学药物的方法。收集了现有补充检验方法规定的90种以及实际工作中发现的化学药共112种,利用Q-Orbitrap HRMS和Trace Finder软件采集并记录每种药物的信息,建立高分辨质谱数据库。样品采用90%甲醇(含0.1%甲酸)超声萃取,加热电喷雾电离源(H-ESI)、正离子扫描方式采集数据。通过数据库筛查和鉴定非法添加化学成分。分别对样品前处理、色谱、质谱条件进行优化,并考察了每种物质的检出限、定量下限、线性范围。结果表明,112种化合物的检出限为0.0125~0.0625 mg/kg,定量下限为0.025~0.125 mg/kg,相关系数(r^(2))均不低0.999,方法的线性关系良好,回收率为62.0%~124%,相对标准偏差(RSD)为2.4%~8.9%。方法可用于保健食品中非法添加化学药物的高通量快速筛查。利用全扫描结果,还能发现数据库以外的可疑化合物,鉴定新的非法添加物。方法已用于实际工作,适用于抗疲劳类保健食品及普通食品中非法添加化学药的快速筛查。An efficient method was developed to screening 112 illegally added chemical compounds in anti-fatigue health food based on ultra-high performance liquid chromatography quadrupole electro-static field orbital trap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Otherwise,a HRMS database was established through acquiring each chemical compound data by Q-Orbitrap HRMS and analyzing it by Trace Finder software.The samples were prepared by ultrasonic extraction of 90%methanol(containing 0.1%formic acid)and the data were acquired by heat-electrospray ion-ization(H-ESI)process in the positive ion polarity mode.Through database screening,illegal chem-ical components were identified.And according to the identification,the sample prepared condi-tions,chromatographic conditions and MS conditions were optimized,respectively.Then,the veri-fication of the quantitative method of each chemical compound identified was investigated,including its detection limit(LOD),quantitation limit(LOQ)and linear range.The results showed that the LODs and LOQs of 112 compounds were in the range of 0.0125-0.0625 mg/kg,and 0.025-0.125 mg/kg,respectively.The linear ranges were linear within a certain ranges,with correlation coeffi-cients(r^(2))not less than 0.999.The average recoveries were between 62.0%and 124%,with relative standard deviations(RSDs)of 2.4%-8.9%.Thus,the method could achieve the purpose of high-throughput rapid screening of illegal compounds in health care food.Besides,some suspicious com-pounds outside the database were found through the full scan mode after the data re-analysis.Further-more,the identification of suspicious compound was beneficial for discovering new illegal additions.The method has been applied to practical work,and was suitable for the rapid screening of illegal chemical substances in anti-fatigue health products and food.

关 键 词：抗疲劳 保健食品 非法添加 超高效液相色谱-四极杆静电场轨道阱质谱(UPLC-Q-Orbitrap HRMS) 快速筛查 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]