超高效液相色谱串联质谱法同时测定小麦及其制品中玉米赤霉烯酮和伏马毒素的方法优化

Optimization of the method for simultaneous determination of zearalenone and fumonisins in wheat and its products by ultra high performance liquid chromatography-tandem mass spectrometry

目的建立和优化超高效液相色谱串联质谱法同时测定小麦及其制品中玉米赤霉烯酮和伏马毒素的方法。方法样品经粉碎后经乙腈∶水∶甲酸(70∶29∶1,V/V/V)提取,Oasis PRiME HLB小柱净化,乙腈洗脱,流出液氮吹后复溶,质谱MRM多重反应离子模式检测,内标法定量,比较3个不同阶段加入内标的测定结果。结果在样品提取后过柱前加入内标,标物结果满足不确定度要求的同时节省内标,4种真菌毒素在其各自的线性范围内具有良好的线性关系,相关系数r均大于0.998,方法检出限为2~5μg/kg,定量限为6~15μg/kg,高中低3个浓度的加标回收率在88.8%~97.1%之间,RSD在1.26%~5.01%之间。结论该方法经济、可靠、灵敏、快捷,可以满足小麦及其制品中玉米赤霉烯酮和伏马毒素大批量检测的工作要求。

Objective To establish and optimize a method for simultaneous determination of zearalenone and fumonisins in wheat and its products by ultra high performance liquid chromatography-tandem mass spectrometry.Methods The samples were crushed,purified by Oasis PRiME HLB column and extracted with acetonitrile:water:formic acid.The samples were eluted with acetonitrile and resoluted by nitrogen in the effluent.The samples were detected by MRM multiple reaction ion model and quantified by internal standard method.The determination results of internal standard in three different stages were compared.Results After the extraction of the sample,the internal standard was added before the column,and the standard result met the requirement of uncertainty while saving the internal standard.The four mycotoxins had a good linear relationship in their respective linear range,and the correlation coefficients were all greater than 0.998.The detection limit of the method was 2-5μg/kg,the quantitative limit was 6-15μg/kg,and the recoveries of three concentrations in high,medium and low concentration were between 88.8%and 97.1%.RSD is between 1.26%and 5.01%.Conclusion The method is economical,reliable,sensitive and rapid,and can meet the requirements of mass detection of zearalenone and fumonisins in wheat and its products.