分析测试学报2024，Vol.43Issue(7)：987-994,8.DOI:10.12452/j.fxcsxb.24040303
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
摘要
Abstract
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 C18 column(2.1 mm × 100 mm,1.7 μm)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 0.998 0.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 0.1-2 μg/kg,0.1-5 ptg/kg,and 0.1-1.7 μg/L,respectively.The 46 samples procured were tested by this method,and 2 positive samples were found,one of which detected nifedipine 178.1 μg/kg and the other detected 260.2 μg/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Key words
antihypertensive health food/dihydropyridine calcium antagonists/UPLC-MS/MS/illegal additions分类
化学化工引用本文复制引用
李林益,张高勤,冯星桥,温毓秀,李健,刘玫,杨瑞琴..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[J].分析测试学报,2024,43(7):987-994,8.基金项目
中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06) （2023SYL06）
