食品科学 ›› 2020, Vol. 41 ›› Issue (14): 307-313.doi: 10.7506/spkx1002-6630-20190725-328

• 安全检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定保健食品中90 种那非类药物

马俊美,王 敬,孙文毅,蒋 杰,李 强,范素芳   

  1. (河北省食品检验研究院,河北省食品安全重点实验室,河北 石家庄 050091)
  • 发布日期:2020-07-29
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603403)

Determination of 90 Nafils in Health Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Junmei, WANG Jing, SUN Wenyi, JIANG Jie, LI Qiang, FAN Sufang   

  1. (Key Laboratory of Food Safety of Hebei Province, Hebei Food Inspection and Research Institute, Shijiazhuang 050091, China)
  • Published:2020-07-29

摘要: 建立高效液相色谱-串联质谱检测保健食品中90 种那非类药物的分析方法。样品经甲醇直接提取,用Waters Acquity BEH C18柱(2.1 mm×100 mm,2.5 μm)分离,以0.1%甲酸溶液和乙腈为流动相进行梯度洗脱,多反应模式监测,外标法定量。结果表明:90 种那非类药物在0.2~50 ng/mL质量浓度范围内线性关系良好,相关系数大于0.995;检出限范围为2.5~25.0 μg/kg;定量限范围为5.0~50.0 μg/kg;加标水平为5.0~500 μg/kg时,回收率范围为78.0%~109.9%;相对标准偏差小于10%;此方法简便快速、选择性强、灵敏度高,可用于保健食品中90 种那非类药物的测定。

关键词: 那非类药物;超高效液相色谱-串联质谱法;保健食品

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to determine 90 nafils in health foods. The samples were extracted with methanol, and the extracts were then separated on a Waters Acquity UPLC BEH C18 (2.1 mm × 100 mm, 2.5 μm) using a gradient mobile phase composed of acetonitrile and 0.1% formic acid in water. Multiple reaction monitoring was used to acquire mass spectrometric data. An external standard method was adopted for quantification. The results showed that good linearity was obtained in the concentration range of 0.2–50 ng/mL for the 90 nafils with correlation coefficients higher than 0.995. The limits of detection (LODs) were in the range of 2.5–25.0 μg/kg, and the limits of quantitation (LOQs) were in the range of 5.0–50.0 μg/kg. The recoveries were in the range of 78.0%–109.9% at spiked concentration levels between 5.0 and 500 μg/kg with relative standard deviations (RSDs) lower than 10%. The developed method was successfully used for accurate and quantitative measurement of the 90 nafils in health foods.

Key words: nafils; ultra-high performance liquid chromatography-tandem mass spectrometry; health foods

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