食品科学 ›› 2018, Vol. 39 ›› Issue (18): 320-325.doi: 10.7506/spkx1002-6630-201818049

• 安全检测 • 上一篇    

超高效液相色谱-串联质谱法检测辅助降血脂保健食品中6 种非法添加化学药物

李晓蕾1,陈军2,杨朝芬1,杨俊1   

  1. (1.昆明理工大学分析测试研究中心,云南?昆明 650000;2.中国林业科学研究院资源昆虫研究所,云南?昆明 650000)
  • 出版日期:2018-09-25 发布日期:2018-09-18
  • 基金资助:
    昆明理工大学自然科学基金项目(KKSY201532062)

Determination of Six Antilipemic Chemicals Illegally Added in Antilipemic Functional Foods by UPLC-MS/MS

LI Xiaolei1, CHEN Jun2, YANG Chaofen1, YANG Jun1   

  1. (1. Research Center of Analysis and Measurement, Kunming University of Science and Technology, Kunming 650000, China; 2. Research Institute of Resources Insects, Chinese Academy of Forestry, Kunming 650000, China)
  • Online:2018-09-25 Published:2018-09-18

摘要: 建立超高效液相色谱-串联质谱法同时快速检测辅助降血脂类保健食品中6 种降血脂药物(烟酸、普伐他汀钠、氟伐他汀钠、美伐他汀、洛伐他汀、辛伐他汀)的方法。样品经甲醇提取,Waters Acquity BEH-C18色谱柱分离,0.1%甲酸-乙腈溶液梯度洗脱,流速0.2?mL/min,电喷雾离子源正离子模式扫描,多反应监测模式测定,外标法定量。结果表明:在实验条件下4?min内可快速、准确地定性定量分析6?种降血脂化学药物,分离度良好,方法检出限为4~39?μg/kg,加样回收率为80.2%~106.1%。利用本方法检测20?批降血脂类保健食品,其中3?批分别含有烟酸和洛伐他汀。本方法线性关系良好、快速、简便、准确,可作为辅助降血脂类保健食品中非法添加化学药物的定性定量检测方法。

关键词: 超高效液相色谱-串联质谱法, 辅助降血脂, 化学药物, 保健食品, 非法添加

Abstract: A method for the simultaneous determination of six blood lipid regulating drugs (nicotinicacid, pravastatin sodium, fluvastatin sodium, mevastatin, lovastatin and simvastatin) illegally added to antilipemic functional foods by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The samples were extracted with methanol. The analytes were separated on a Waters Acquity BEH-C18 column with a mobile phase consisting of 0.1% aqueous formic acid solution and acetonitrile using gradient elution at a flow rate of 0.2 mL/min, detected by multiple reaction monitoring (MRM) with an electrospray ionization source in the positive ion mode, and quantified by the external standard method. Under the experimental conditions in this study, all analytes were separated well, and they were quantified accurately and rapidly within 4 min. The limits of detection of the method ranged from 4 and 39 μg/kg, and the recoveries for spiked samples were 80.2%–106.1%. Twenty batches of antilipemic functional foods were tested by the method and out of these, 3 were found to contain nicotinic acid and lovastatin. This method exhibited good linear relationships and it was fast, simple and highly accurate, and thus could be used for the simultaneous determination of the six drugs illegally added in antilipemic functional foods.

Key words: ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), antilipemic, chemicals, healthy foods, illegal additives

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