液相色谱-串联质谱法测定小麦中T-2、ZEN及DON 3种镰刀菌毒素

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,1.8 μm）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、10~2 000 μg/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、10.0 μg/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。

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

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.