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

LI Lin-yi; ZHANG Gao-qin; FENG Xing-qiao; WEN Yu-xiu; LI Jian; LIU Mei; YANG Rui-qin

doi:10.12452/j.fxcsxb.24040303

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

Scientific Papers | 更新时间：2024-07-08

- Determination of 13 Dihydropyridine Calcium Antagonists in Antihypertensive Health Food by UPLC-MS/MS
- Journal of Instrumental Analysis Vol. 43, Issue 7, Pages: 987-994(2024)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24040303
  CLC： O657.7;R917
- Published：15 July 2024，
  
  Received：03 April 2024，
  
  Revised：08 May 2024，
- 稿件说明：
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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(07):987-994.

LI Lin-yi,ZHANG Gao-qin,FENG Xing-qiao,WEN Yu-xiu,LI Jian,LIU Mei,YANG Rui-qin.Determination of 13 Dihydropyridine Calcium Antagonists in Antihypertensive Health Food by UPLC-MS/MS[J].Journal of Instrumental Analysis,2024,43(07):987-994.
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(07):987-994. DOI： 10.12452/j.fxcsxb.24040303.

LI Lin-yi,ZHANG Gao-qin,FENG Xing-qiao,WEN Yu-xiu,LI Jian,LIU Mei,YANG Rui-qin.Determination of 13 Dihydropyridine Calcium Antagonists in Antihypertensive Health Food by UPLC-MS/MS[J].Journal of Instrumental Analysis,2024,43(07):987-994. DOI： 10.12452/j.fxcsxb.24040303.

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

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0.1~2 μg/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（178.1 μg/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。

Abstract

A method for the detection of 13 kinds of dihydropyridine calcium antagonists in antihypertensive health foods by ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was established. Tablets and functional tea samples were extracted by ultrasonic extraction with methanol-water（4∶1） solution but methanol used by oral liquid samples. The separation was performed on a Waters ACQUITY UPLC BEH C

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 formate） 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 standard 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 μg/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 precision，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

Keywords

antihypertensive health fooddihydropyridine calcium antagonistsUPLC-MS/MSillegal additions

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