QuEChERS-超高效液相色谱-串联质谱法测定花生及土榨花生油中9种真菌毒素

Determination of 9 kinds of mycotoxins in peanuts and flavor peanut oil by QuEChERS-ultra performance liquid chromatographytandem mass spectrometry

目的建立QuEChERS净化-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定花生及土榨花生油中9种真菌毒素的分析方法。方法样品经1%甲酸甲醇溶液提取,用QuEChERS分散吸附剂净化除杂,以0.1%甲酸水溶液和乙腈为流动相梯度洗脱,经ACE Excel 3 C18色谱柱(2.1 mm×100 mm,3μm)分离,在电喷雾(electrospray ionization,ESI)正负离子切换扫描模式下,采用多反应监测(multiple reaction monitoring,MRM)进行分析,外标法进行定量。结果9种真菌毒素在0.5~50μg/L的浓度范围内线性关系良好,相关系数(r 2)≥0.9937,检出限和定量限分别为0.03~1.14μg/kg和0.10~3.50μg/kg。在低、中、高3个添加水平(2、10、20μg/kg)下的回收率为73.1%~117.7%,相对标准偏差范围为0.6%~6.5%之间(n=6)。结论本方法操作简单、灵敏度高、适用性强,适用于花生及土榨花生油等9种真菌毒素的快速筛查及定量检测。

Objective To establish a method for the determination of 9 kinds of mycotoxins in peanuts and flavor peanut oil by QuEChERS extraction technology and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted with 1%formic acid methanol solution,purified with QuEChERS dispersed adsorbent,eluted with 0.1%formic acid aqueous solution and acetonitrile as mobile phase,and separated by ACE Excel 3 C18 column(2.1 mm×100 mm,3μm).In the electrospray ionization(ESI)positive and negative ion switching scanning mode,the samples were analyzed by multi-reaction monitoring multiple reaction monitoring(MRM)and quantified by external standard method.Results Nine kinds of mycotoxins had good linear relationships in the concentration range of 0.5-50μg/L,the correlation coefficient(r2)≥0.9937,the detection limits and quantitative limits were 0.03-1.14μg/kg and 0.10-3.50μg/kg,respectively.The recoveries at low,medium and high addition levels(2,10,20μg/kg)were 73.1%-117.7%,and the relative standard deviation were 0.6%-6.5%(n=6).Conclusion This method has the advantages of simple operation,high sensitivity and strong applicability,and is suitable for rapid screening and quantitative detection of 9 kinds of mycotoxins such as peanut and flavor peanut oil.