食品科学 ›› 2024, Vol. 45 ›› Issue (19): 235-241.doi: 10.7506/spkx1002-6630-20240226-137

• 安全检测 • 上一篇    下一篇

反相/强阳离子交换固相萃取净化-超高效液相色谱-串联质谱法测定动物源性食品中的曲美他嗪和氯米芬

卢兰香, 薛霞, 田翠, 张艳侠, 宿书芳, 李新玲, 刘艳明, 王骏, 胡梅   

  1. (1.山东省食品药品检验研究院,国家市场监管重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,山东 济南 250101;2.泸州市农业农村局,四川 泸州 646000)
  • 出版日期:2024-10-15 发布日期:2024-10-12
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2017YEC1601600)

Determination of Trimetazidine and Clomiphene in Animal-Derived Foods by Mixed-Mode Reversed-Phase Strong Cation Exchange Solid Phase Extraction Cleanup Followed by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

LU Lanxiang, XUE Xia, TIAN Cui, ZHANG Yanxia, SU Shufang, LI Xinling, LIU Yanming, WANG Jun, HU Mei   

  1. (1. Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation, Industrial Technology Foundation Public Service Platform, Shandong Institute for Food and Drug Control, Jinan 250101, China; 2. Luzhou Municipal Bureau of Agriculture and Rural Affairs, Luzhou 646000, China)
  • Online:2024-10-15 Published:2024-10-12

摘要: 建立反相/强阳离子交换固相萃取净化-超高效液相色谱-串联质谱法测定动物源性食品中曲美他嗪和氯米芬的分析方法。试样用0.5%甲酸乙腈提取,经反相/强阳离子交换混合模式固相萃取柱PRiME MCX净化。目标物经Waters ACQUITY UPLC HSS T3色谱柱分离,以乙腈-0.1%甲酸作为流动相进行梯度洗脱,在电喷雾正离子模式下以多反应监测模式检测,用内标法定量。结果表明:曲美他嗪与氯米芬在0.3~100.0 ng/mL范围内线性关系良好,决定系数均大于0.999。方法回收率范围为93.4%~112.1%,相对标准偏差为0.68%~4.81%(n=6),检出限均为0.1 μg/kg,定量限为0.3 μg/kg。该方法灵敏度高、稳定性好、实用性强,适用于动物源性食品中曲美他嗪和氯米芬的检测,可为体育赛事中的食品安全保障工作提供有效的技术支撑。

关键词: 超高效液相色谱-串联质谱法;食源性兴奋剂;曲美他嗪;氯米芬;固相萃取;动物源性食品

Abstract: A method for the determination of trimetazidine and clomiphene in animal-derived foods was developed by mixed-mode reversed-phase strong cation exchange solid phase extraction cleanup followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with 0.5% (V/V) formic acid in acetonitrile, and purified on a mixed-mode reversed phase strong cation exchange column (PRiME MCX). The chromatographic separation was performed on a Waters ACQUITY UPLC HSS T3 column by gradient elution using a mobile phase composed of acetonitrile and 0.1% formic acid. The analytes were detected in the positive ion mode using multiple reaction monitoring (MRM). Quantification was performed by the internal standard method. The results showed that good linearity was observed for trimetazidine and clomiphene in the concentration range of 0.3–100.0 ng/mL with determination coefficients (R2) > 0.999. The average recoveries of this method ranged from 93.4% to 112.1%, with relative standard deviations (RSDs) of 0.68%–4.81% (n = 6). The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.1 and 0.3 μg/kg, respectively. The developed method is sensitive, stable, practical, and suitable for the determination of trimetazidine and clomiphene in animal-derived foods, which can provide effective technical support for food safety assurance for sports events.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; foodborne stimulants; trimetazidine; clomiphene; solid phase extraction; animal-derived foods

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