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OA北大核心CSTPCD
Determination of 13 Dihydropyridine Calcium Antagonists in Antihypertensive Health Food by UPLC-MS/MS
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 C18色谱柱(2.1 mm×100 mm,1.7 μm)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、0.1~5 μg/kg、0.1~1.7 μg/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(260.2 μg/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 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.
李林益;张高勤;冯星桥;温毓秀;李健;刘玫;杨瑞琴
中国人民公安大学 侦查学院,北京 100038山西省公安厅刑事科学技术研究所,山西 晋中 030601
化学
降血压类保健食品二氢吡啶类钙拮抗剂UPLC-MS/MS非法添加
antihypertensive health fooddihydropyridine calcium antagonistsUPLC-MS/MSillegal additions
《分析测试学报》 2024 (007)
987-994 / 8
中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06)
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