食品科学 ›› 2019, Vol. 40 ›› Issue (10): 325-330.doi: 10.7506/spkx1002-6630-20180305-045

• 安全检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定乳制品中的莫奈太尔及其代谢物

吴映璇,林 峰,陈思敏   

  1. 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室,广东 广州 510623
  • 出版日期:2019-05-25 发布日期:2019-05-31
  • 基金资助:
    广东省科技计划项目(2015A030401074;2014A040401064)

Determination of Monepantel and Its Metabolite Residues in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

WU Yingxuan, LIN Feng, CHEN Simin   

  1. Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province, Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China
  • Online:2019-05-25 Published:2019-05-31

摘要: 建立测定乳制品中莫奈太尔及其代谢物的高效液相色谱-串联质谱法。试样加水-饱和氯化钠-乙腈溶液提取,正己烷净化,经Inertsil C8(2.1 mm×100 mm,3 μm)色谱柱分离,以甲醇-0.5 mmol/L乙酸铵溶液为流动相进行梯度洗脱,采用电喷雾离子源串联质谱,在负离子扫描方式下以多反应监测模式检测,外标法定量。结果表明:莫奈太尔及其代谢物在0.1~5.0 μg/L范围内线性关系良好,定量限为2.0 μg/kg。在3 个加标水平下的平均回收率为79.5%~102.9%,相对标准偏差为2.0%~5.3%。该方法操作简便、快速、准确、灵敏度高、抗干扰能力强、回收率和重复性良好,适合于乳制品中莫奈太尔及其代谢物的测定。

关键词: 莫奈太尔, 代谢物, 高效液相色谱-串联质谱法, 乳制品

Abstract: A method was developed for the determination of monepantel and its metabolite residues in dairy products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was ultrasonically extracted with a mixture of saturated sodium chloride solution and acetonitrile, and then the extract was purified by hexane. The target compounds were separated on an inertsil C8 column (2.1 mm × 100 mm, 3 μm) using a gradient elution program with a mobile phase composed of methanol and 0.5 mmol/L ammonium acetate, and detected by tandem mass spectrometry using negative electrospray ionization in multiple reaction monitoring (MRM) mode. The quantification of monepantel and its metabolite residues was performed by the external standard method. The calibration curves showed a good linearity within the concentration range of 0.1–5.0 μg/L and the limit of quantitation (LOQ) was 2.0 μg/kg. The recoveries for dairy products at three spiked levels were in the range of 79.5%–102.9% with relative standard deviations (RSDs) between 2.0% and 5.3%. With the advantages of simplicity, rapidity, accuracy, high sensitivity, strong anti-interference capacity and good recovery and repeatability, the method could be suitable for the analysis of monepantel and its metabolite residues in dairy products.

Key words: monepantel, metabolite, high performance liquid chromatography-tandem mass spectrometry, dairy products

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