新型脱脂前处理技术联合净化－同位素稀释－超高效液相色谱－串联质谱法测定花生中15种真菌毒素

潘晨; 于建; 吴思霖; 简龙海; 郑荣; 王柯

doi:10.19428/j.cnki.sjpm.2020.20057

新型脱脂前处理技术联合净化－同位素稀释－超高效液相色谱－串联质谱法测定花生中15种真菌毒素

Simultaneous determination of 15 mycotoxins in peanuts by ultra high performance liquid chromatography-tandem mass spectrometry with QuEChERS EMR-Lipid approach and stable isotope dilution

摘要

摘要:
目的建立新型脱脂前处理(QuEChERS EMR-Lipid)技术联合净化－同位素稀释－超高效液相色谱－串联质谱法检测花生中15种真菌毒的方法。
方法样品用含2%甲酸的乙腈-水(50 : 50，V/V)溶液提取，通过QuEChERS EMR-Lipid技术净化后，以五氟苯基柱为分离柱，用甲醇-0.01%甲酸水溶液进行梯度洗脱，采用超高效液相色谱－串联质谱(UPLC-MS/MS)测定、多反应模式(MRM)监测和同位素内标法定量。
结果该方法测定花生中15种真菌毒素在一定范围内线性良好(r＞0.995)，检出限为0.1~10 μg/kg，平均回收率为81.2%~115.3%，相对标准偏差(RSD，n=6)为2.1%~10.7%。
结论该方法操作简便、灵敏度高，适用于花生中15种真菌毒素的快速准确检测。

Abstract:
ObjectiveTo develop a method for the simultaneous determination of 15mycotoxins in peanuts by ultra high performance liquid chromatography-tandem mass spectrometry with QuEChERS EMR-Lipid approach and stable isotope dilution.
MethodsThe samples were extracted by 2% formic acid acetonitrile-water (50 : 50, V/V) and then purified with QuEChERS EMR-Lipid approach.The mycotoxins were fully separated on a pentafluorophenyl column under a gradient elution with methonal-0.01%formic acid aqueous solution.The mycotoxins were analyzed by UPLC-MS/MS with multiple reaction monitoring (MRM) mode and quantified by isotope internal standard method.
ResultsFifteen mycotoxins had good linear relationship in the certain correlation ranges with the correlation coefficients all above 0.995 and the detection limits were 0.1－10 μg/kg.The mean recoveries ranged from 81.2% to 115.3% with RSD (n=6) varying from 2.1% to 10.7%.
ConclusionThe method is simple, highly sensitive, practical, and proves to be suitable for quantitative analysis of 15 mycotoxins in peanuts.

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