食品科学 ›› 2017, Vol. 38 ›› Issue (10): 297-304.doi: 10.7506/spkx1002-6630-201710048

• 安全检测 • 上一篇    下一篇

花生油和玉米油中多组分真菌毒素高效 液相色谱-串联质谱检测方法的建立

刘 丹,韩小敏,李凤琴,王 畅,罗晓林,卢大新,   

  1. 1.北京农学院食品科学与工程学院,北京 102206;2.农产品有害微生物及农残安全检测与控制北京市重点实验室, 北京 102206;3.国家食品安全风险评估中心,卫生部食品安全风险评估重点实验室,北京 100021; 4.中山大学公共卫生学院,广东 广州 510080
  • 出版日期:2017-05-25 发布日期:2017-05-23
  • 基金资助:
    国家自然科学基金青年科学基金项目(31301489);北京市自然科学基金项目(7163235)

Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry for Detection of Multi-Mycotoxins in Peanut Oil and Corn Oil

LIU Dan , HAN Xiaomin , LI Fengqin , WANG Chang , LUO Xiaolin , LU Daxin ,   

  1. 1. College of Food Science and Engineering, Beijing University of Agriculture, Beijing 102206, China; 2. Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides, Beijing 102206, China; 3. Key Laboratory of Food Safety Risk Assessment, Ministry of Health, China National Centre for Food Safety Risk Assessment, Beijing 100021, China; 4. School of Public Health, Sun Yat-Sen University, Guangzhou 510080, China
  • Online:2017-05-25 Published:2017-05-23

摘要: 建立花生油和玉米油中黄曲霉毒素、玉米赤霉烯酮、单端孢霉烯族化合物等13 种真菌毒素的高效液相 色谱-串联质谱检测方法。样品经乙腈-水提取、MultiSep 226多功能净化柱净化后,分别用电喷雾正离子模式和 负离子模式检测。经优化,正离子模式流动相为含2 mmol/L甲酸铵的0.1%甲酸-甲醇溶液,负离子模式流动相为 0.1%氨水-乙腈溶液。该方法对花生油和玉米油中13 种真菌毒素的检出限为0.05~3.00 μg/kg,定量限为0.10~ 10.00 μg/kg,平均加标回收率为66.6%~114.9%。所建方法操作简单、灵敏度高、重复性好,可用于花生油和玉米 油中多组分真菌毒素的协同测定。

关键词: 真菌毒素, 花生油, 玉米油, 高效液相色谱-串联质谱

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous detection of 13 mycotoxins including aflatoxins, zearalenone, and trichothecenes in peanut and corn oils. Samples were extracted with acetonitrile-water, followed by clean-up with a MultiSep 226 multifunctional column. The positive electrospray ionization mode (ESI+) and negative electrospray ionization mode (ESI-) were respectively employed to acquire signals. The mobile phase for ESI+ was composed of 0.1% formic acid containing 2 mmol/L ammonium formate (solvent A) and methanol (solvent B), while that for ESI- consisted of 0.1% ammonia water (solvent A) and acetonitrile (solvent B). The limits of detections (LODs) for 13 mycotoxins in peanut and corn oils ranged from 0.05 to 3.00 μg/kg and the limits of quantification (LOQ) ranged from 0.10 to 10.00 μg/kg. The mean recoveries ranged from 66.6% to 114.9%. The method developed in the present study had the advantages of simple operation, high sensitivity and good reproducibility, and so it could be used for the detection of multi-mycotoxins in peanut and corn oils.

Key words: mycotoxin, peanut oil, corn oil, high performance liquid chromatography-tandem mass spectrometry

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