食品科学 ›› 2018, Vol. 39 ›› Issue (22): 283-288.doi: 10.7506/spkx1002-6630-201822043

• 安全检测 • 上一篇    下一篇

高效液相色谱-串联质谱测定食品中15 种有毒生物碱

范素芳1,马俊美1,刘茁2,俞婧1,翟洪稳1,李强1,*,张岩1,*   

  1. (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;2.河北科技大学生物科学与工程学院,河北?石家庄 050018)
  • 出版日期:2018-11-25 发布日期:2018-11-21
  • 基金资助:
    国家重大科学仪器设备开发专项(2012YQ03011110)

Determination of 15 Toxic Alkaloids in Food Samples by High Performance Liquid Chromatography-Tandem Mass Spectrometry

FAN Sufang1, MA Junmei1, LIU Zhuo2, YU Jing1, ZHAI Hongwen1, LI Qiang1,*, ZHANG Yan1,*   

  1. (1. Hebei Food Inspection and Research Institute, Hebei Food Safety Key Laboratory, Shijiazhuang 050091, China; 2. College of Bioscience and Bioengineering, Hebei University of Science and Technology, Shijiazhuang 050018, China)
  • Online:2018-11-25 Published:2018-11-21

摘要: 建立高效液相色谱-串联质谱法测定食品中15?种有毒生物碱。研究和优化提取条件、净化方式、色谱-质谱参数等指标,样品经体积分数20%乙醇溶液提取、离心后,经高效液相色谱分离、质谱测定,外标法定量。结果表明,15?种有毒生物碱的检出限范围为4~20?μg/kg,定量限范围为10~80?μg/kg,在1、3、5?倍定量限添加水平时,方法的回收率范围为80.9%~119.8%,相对标准偏差低于10%,符合分析方法要求。该方法可用于植物源饮料、粮谷类食品及果蔬中15?种有毒生物碱的快速筛查和定量分析。

关键词: 高效液相色谱-串联质谱, 食品, 有毒生物碱

Abstract: In this paper, a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of 15 toxic alkaloids in food samples. Extraction conditions, purification methods and instrumental parameters were optimized. Samples were extracted with 20% ethanol solution, and the supernatant was separated and analyzed after centrifugation. The external standard method was used for quantification. The limits of detection (LODs) of 15 alkaloids were in range of 4–20 μg/kg and the limits of quantification (LOQ) were in range of 10–80 μg/kg. The recoveries of the method were in range of 80.9%–119.8% at spiked levels of LOQ, 3 LOQ and 5 LOQ, with relative standard deviations (RSDs) lower than 10%, which met the analytical requirements. This method was found to be useful for rapid screening and quantitative analysis of 15 toxic alkaloids in plant-derived drinks, cereal products, fruits and vegetables.

Key words: high performance liquid chromatography-tandem mass spectrometry, food, toxic alkaloids

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