液相色谱-串联质谱法测定小麦中T-2、ZEN及DON3种镰刀菌毒素

Determination of T-2,Zearalenone and Deoxynivalenol in Wheat Using Liquid Chromatography-Tandem Mass Spectrometry

采用液相色谱-串联质谱建立了小麦中T-2、玉米赤霉烯酮(ZEN)和脱氧镰刀菌烯醇(DON)的测定方法。样品经80%乙腈-水提取,氨基柱(500 mg,6 mL)杂质吸附模式净化,以5 mmol/L乙酸铵溶液和甲醇为流动相,ZORBAX Extend-C18柱(150 mm×2.1 mm,1.8μm)进行色谱分离;在电喷雾正离子化模式下,多反应监测方式测定。结果表明:T-2、ZEN和DON分别在0.5～500、5～500、10～2 000μg/L质量浓度范围内呈良好线性,相关系数分别为0.998 9、0.999 7和0.999 1。通过对空白小麦样品进行3个水平的加标回收实验,T-2、ZEN和DON的回收率分别为86%～94%、80%～101%和81%～105%,相对标准偏差(RSD)分别为2.6%～5.5%、3.6%～8.9%和2.2%～8.1%,方法检出限分别为0.5、8.0、10.0μg/kg。该方法准确、灵敏、成本低,适用于小麦中T-2、ZEN和DON的同时分析。

A liquid chromatography tandem mass spectrometric（LC-MS/MS）method was developed for the simultaneous determination of T-2,zearalenone（ZEN） and deoxynivalenol（DON） in wheat.The sample was extracted with acetonitrile-water（80 ∶ 20）.The extract was purified with an Amino column（AccuBond AMINO,500 mg,6 mL）.Three myctoxins were completely separated on a ZORBAX Extend-C18 column（150 mm×2.1 mm,1.8 μm）by gradient elution with methanol and 5 mmol/L ammonium acetate as mobile phase,and detected by positive ion electrospray ionization mass spectrometry（ESI MS） under multiple reaction monitoring（MRM） mode.The results showed that the linearities of T-2,ZEN and DON were in the concentration ranges of 0.5-500,5-500,10-2 000 μg/L,respectively,with correlation coefficients of 0.998 9,0.999 7 and 0.999 1,respectively.The spiked recoveries of T-2,ZEN and DON at three spiked levels in wheat were in the ranges of 86%-94%,80%-101% and 81%-105%,with relative standard deviations（RSDs,n=5） of 2.6%-5.5%,3.6%-8.9% and 2.2%-8.1%,respectively.The limits of detection for T-2,ZEN and DON were 0.5,8.0,10.0 μg/kg,respectively.The method was low cost,sensitive and accurate,and was suitable for the simultaneous determination of T-2,ZEN and DON in wheat.