UPLC-MS/MS法测定降血压类保健食品中13种二氢吡啶类钙拮抗剂  

Determination of 13 Dihydropyridine Calcium Antagonists in Antihypertensive Health Food by UPLC-MS/MS

作　　者：李林益 张高勤 冯星桥 温毓秀 李健 刘玫 杨瑞琴[1] LI Lin-yi;ZHANG Gao-qin;FENG Xing-qiao;WEN Yu-xiu;LI Jian;LIU Mei;YANG Rui-qin(School of Criminal Investigation,People's Public Security University of China,Beijing 100038,China;Shanxi Provincial Institute of Forensic Science for Public Security,Jinzhong 030601,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]山西省公安厅刑事科学技术研究所,山西晋中030601

出　　处：《分析测试学报》2024年第7期987-994,共8页Journal of Instrumental Analysis

基　　金：中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06)。

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测降血压类保健食品中非法添加13种二氢吡啶类钙拮抗剂的方法。片剂、功能茶样品用甲醇-水(4∶1)溶液超声提取,口服液样品用甲醇超声提取,采用Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm)分离,以2 mmol/L甲酸铵-0.1%甲酸水溶液和乙腈为流动相梯度洗脱,采用电喷雾离子源(ESI)正离子模式,多反应监测(MRM)模式进行检测。结果显示,13种分析物在对应质量浓度范围内线性关系良好,相关系数均不低于0.998 0,平均回收率为85.1%~119%,日内相对标准偏差(RSD)为0.37%~5.6%,日间RSD为1.6%~13%。各组分在片剂、功能茶、口服液3种基质中的检出限分别为0.1~2μg/kg、0.1~5μg/kg、0.1~1.7μg/L。采用该法对46个市售样品进行检测,有2个阳性样品分别检出硝苯地平(178.1μg/kg)与马尼地平(260.2μg/kg)。该方法操作简单、灵敏度高、精密度好,适用于保健食品中非法添加二氢吡啶类钙拮抗剂的筛查与定量分析。A method for the detection of 13 kinds of dihydropyridine calcium antagonists in antihy⁃pertensive health foods by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Tablets and functional tea samples were extracted by ultrasonic ex⁃traction with methanol-water(4∶1)solution but methanol used by oral liquid samples.The separa⁃tion was performed on a Waters ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm)with a gradient elution of 0.1%formic acid aqueous solution(containing 2 mmol/L ammonium for⁃mate)and acetonitrile at the flow rate of 0.4 mL/min.Electrospray ionization source was done in the positive ion mode and analytes were detected in the MRM mode to complete the detection.Thirteen analytes had a good linear relationship in their own linear ranges,and the correlation coefficients were not less than 0.9980.The average recoveries were 85.1%-119%,the intraday relative stan⁃dard deviations(RSDs)were 0.37%-5.6%and the interday RSDs were 1.6%-13%.The detection limits of each analytes in tablets,functional teas,and oral liquids were in the ranges of 0.1-2μg/kg,0.1-5μg/kg,and 0.1-1.7μg/L,respectively.The 46 samples procured were tested by this method,and 2 positive samples were found,one of which detected nifedipine 178.1μg/kg and the other detected 260.2μg/kg of manidipine.This method is simple,high sensitivity and good preci⁃sion,which is suitable for the screening and quantitative analysis of illegally added dihydropyridine calcium antagonists in health food.

关 键 词：降血压类保健食品 二氢吡啶类钙拮抗剂 UPLC-MS/MS 非法添加 

分 类 号：O657.7[理学—分析化学] R917[理学—化学]