超高效液相色谱-串联质谱法准确测定食品中非法添加的3种新型降压药  

Accurate determination of three new antihypertensive drugs illegally added to food using ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：张居舟 李静 章萍萍 杨梅 周迪 ZHANG Juzhou;LI Jing;ZHANG Pingping;YANG Mei;ZHOU Di(Anhui Provincial Institute for Food and Drug Control,China National Center for Quality Inspection and Test of Agricultural-Avocation Processed Food,Hefei 230051,China)

机构地区：[1]安徽省食品药品检验研究院,国家农副加工食品质量检验检测中心,安徽合肥230051

出　　处：《色谱》2024年第10期954-962,共9页Chinese Journal of Chromatography

基　　金：国家市场监督管理总局委托研究项目(食品补充检验方法);安徽省市场监督管理局科技计划项目(2022MK031);市场监管总局科技计划项目(2023MK064).

摘　　要：为解决食品中非法添加化学降压药并以此宣称具有降压功能的食品安全问题,本研究基于超高效液相色谱-串联质谱(UHPLC-MS/MS)技术,建立了一种同时测定压片糖果、固体饮料、代用茶、茶饮料、饼干、果冻、配制酒和保健食品(口服液、茶剂、片剂、硬胶囊、软胶囊)等12种典型食品基质中阿齐沙坦、坎地沙坦酯和拉西地平等3种新型降压药的分析方法。样品以0.2%(v/v)甲酸乙腈提取,选择性采用QuEChERS净化,再用水稀释,经聚四氟乙烯膜过滤,以5 mmol/L甲酸铵水溶液-乙腈为流动相,通过Agilent Eclipse Plus RRHD C 18色谱柱(50 mm×2.1 mm,1.8μm)进行分离,在电喷雾正离子扫描(ESI+)、多反应监测(MRM)模式下进行测定,基质匹配外标法定量。方法学研究表明,3种降压药在各自的线性范围内线性关系良好,相关系数(r 2)均大于0.996;拉西地平的检出限(LOD)为0.02 mg/kg,定量限(LOQ)为0.04 mg/kg,阿齐沙坦和坎地沙坦酯的LOD均为0.01 mg/kg,LOQ均为0.02 mg/kg;对12种基质进行低、中、高3个水平的加标试验(n=6),3种降压药的平均回收率为86.6%~107.5%,相对标准偏差(RSD)为1.1%~10.9%。该方法简单、快速、灵敏、准确,适用于食品中阿齐沙坦、坎地沙坦酯、拉西地平的同时测定,解决了这3种药物在食品基质中检测方法缺失的难题,可为监管部门提供技术支撑。Effective strategies are required to address food safety issues related to the illegal addition of antihypertensive drugs to food and claims of antihypertensive function.In this study,a novel ultra-high performance liquid chromatography-triple-quadrupole mass spectrometry(UHPLC-MS/MS)method was developed for the simultaneous determination of three antihypertensive drugs(azilsartan,candesartan cilexetil,and lacidipine)in 12 food matrices(pressed candies,solid beverages,alternative teas,tea drinks,biscuits,jellies,mixed liquors,oral liquids,medicinal teas,tablets,hard capsules,and soft capsules).Initially,mass spectrometry parameters,such as the collision energies of the three antihypertensive drugs,were optimized.Subsequently,the response intensities and chromatographic separation conditions of the three drugs in different mobile phases were compared.In addition,to enhance the recoveries,various extraction solvents and purification methods,including solid-phase extraction(SPE)columns and the QuEChERS technique,were investigated.In the developed method,sample determination involved three steps.First,the sample was extracted using 0.2%(v/v)formic acid in acetonitrile and then filtered using high-speed centrifugation,in addition,the extracted solution of alternative tea and medicinal tea was purified using the QuEChERS technique.Second,the supernatant was diluted with water,and filtered through a 0.22μm polytetrafluoroethylene(PTFE)membrane.Finally,the analytes were separated on an Agilent Eclipse Plus RRHD C 18 column(50 mm×2.1 mm,1.8μm)using a 5 mmol/L ammonium formate aqueous solution and acetonitrile as the mobile phases under gradient elution conditions and then detected using UHPLC-MS/MS with positive electrospray ionization(ESI)in the multiple reaction monitoring(MRM)mode.Quantitative analysis was performed using a matrix-matched external standard method.Methodological validation showed good linear relationships for all three antihypertensive drugs in the investigated concentration ranges,with correlation c

关 键 词：超高效液相色谱-串联质谱法 降压药 阿齐沙坦 坎地沙坦酯 拉西地平 食品 

分 类 号：O658[理学—分析化学]