超高效液相色谱-四极杆/静电场轨道阱质谱快速测定保健食品中13种β-受体阻滞剂  

Rapid determination of 13β⁃blockers in health foods by ultra performance liquid chromatography⁃quadrupole/electrostatic field orbitrap mass spectrometry

作　　者：李彤辉 冯峰[1] 申一鸣 张峰[1] LI Tonghui;FENG Feng;SHEN Yiming;ZHANG Feng(Institute of Food Safety,Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Henan Institute of Food and Salt Industry Inspection Technology,Key Laboratory of Food Safety Quick Tesking and Smart Superbision Technology for State Market Regulation,Zhengzhou 450000,China)

机构地区：[1]中国检验检疫科学研究院食品安全研究所,北京100176 [2]河南省食品和盐业检验技术研究院,国家市场监管重点实验室(食品安全快速检测与智慧监管技术),河南郑州450000

出　　处：《色谱》2023年第11期1030-1037,共8页Chinese Journal of Chromatography

基　　金：河南省医学科技攻关计划联合共建项目(LHGJ20210813)。

摘　　要：建立了基于超高效液相色谱-四极杆/静电场轨道阱质谱快速测定保健食品中13种β-受体阻滞剂的分析方法,并对其质谱裂解规律进行了分析研究。实验对质谱条件、色谱条件、提取溶剂及基质效应等进行了详细探究,使用甲醇对样品进行稀释提取,高速离心、超声处理,用Acquity UPLC BEH C18柱(100 mm×21 mm,17μm)分离,以乙腈和01%(v/v)甲酸水溶液作为流动相进行梯度洗脱,采用正离子模式检测,数据采集使用一级母离子全扫描和数据依赖的二级离子扫描(Full MS/dd-MS2)模式,在10 min内实现了保健食品中13种β-受体阻滞剂的分离和高精度一级、二级扫描,得到准确的质量数和准确碎片离子信息。通过方法学验证,13种β-受体阻滞剂在05~100μg/L内线性关系良好,相关系数(r)均≥09912,检出限为1~10μg/kg。空白加标样品中13种β-受体阻滞剂的平均回收率为753%~1084%,相对标准偏差为09%~100%(n=6)。用本方法对市售的30批次保健食品进行筛查,均未检出13种β-受体阻滞剂。该方法检测速度快,准确性强,灵敏度高,可用于保健食品中β-受体阻滞剂的快速测定。A method based on ultra performance liquid chromatography-quadrupole/electrostat-ic field orbitrap mass spectrometry was developed for the rapid determination of 13β-blockers in health foods.The MS fragmentation pathways of the analytes were subsequently investigated.The optimal MS conditions,extraction solvents,mobile phases,and matrix effects were evalu-ated in detail.The samples were extracted with methanol,filtered by high-speed centrifugation and ultrasonic treatment,and then separated on an Acquity UPLC BEH C18 column(100 mm×21 mm,17μm)with gradient elution using acetonitrile and 01%(v/v)formic acid aqueous solution as mobile phases.MS analysis was conducted in positive-ion mode,and the data were collected using full mass and data-dependent MS2 scans(Full MS/dd-MS2).The efficient sepa-ration and high-precision primary and secondary scanning of the 13β-blockers in health foods were realized within 10 min,and accurate mass numbers and fragment-ion information were obtained.The methodological validation showed good linear relationships in the range of 05-100μg/L,with correlation coefficients(r)≥09912.The limits of detection ranged from 1 to 10μg/kg.When the standard substances were added to the blank sample in the amount of 10-200μg/kg,the recoveries were in the range of 753%-1084%,and the relative standard devia-tions ranged from 09%to 100%(n=6).The method was used to screen 30 batches of com-mercially available health foods,and none of the 13β-blockers was detected.The proposed method is fast,accurate,and sensitive,and can be used for the rapid determination ofβ-block-ers in health foods.

关 键 词：超高效液相色谱-四极杆/静电场轨道阱质谱法 Β-受体阻滞剂 保健食品 

分 类 号：O658[理学—分析化学]