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

2017-06-05韩小敏李凤琴罗晓林卢大新

食品科学 2017年10期

刘丹，韩小敏，李凤琴，王畅，罗晓林，卢大新,*

（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）

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1,2，韩小敏3，李凤琴3，王畅4，罗晓林4，卢大新1,2,*

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

真菌毒素是由某些真菌在特定条件下产生的有毒代谢产物，人畜摄入后可导致中毒[1-3]。目前国际上普遍关注的真菌毒素包括黄曲霉毒素（aflatoxin，AF）、单端孢霉烯族化合物、玉米赤霉烯酮（zearalenone，ZEN）等。……

登录APP查看全文