固相萃取-气相色谱-串联质谱法检测粮食作物中的T-2与HT-2毒素

Determination of T-2 and HT-2 toxins in cereal grains by solid phase extraction and gas chromatography-tandem mass spectrometry

目的建立粮食作物中T-2与HT-2毒素的高灵敏度气相色谱-串联质谱(GC-MS/MS)检测方法。方法染毒的粮食样品以柱淋洗方式用甲醇提取后,采用C18固相萃取柱净化富集,再经七氟丁酰咪唑衍生化后,在气相色谱-串联质谱仪上采用选择反应监测(SRM)模式进行检测。结果在染毒大米、小米、糯米和玉米样品中,T-2与HT-2毒素在0.5～100μg/kg范围内均呈现良好的线性关系。在最优分析条件下,两种毒素的最低检出限均在0.05～0.5μg/kg。在2、30、60μg/kg 3个加标浓度下,T-2与HT-2毒素的方法回收率均在47.2%～110.8%。结论该方法操作简便,灵敏度高,适用于各类粮食样品中T-2与HT-2毒素的检测。

Objective To establish a high sensitive gas chromatography-tandem mass spectrometric（GC-MS/MS） method for the detection of T-2 and HT-2 toxins in cereal grains.Methods The spiked samples packed into tubes were eluted with methanol and cleaned up by C18 solid phase extraction（SPE）.The eluant was analyzed after heptafluorobutyryl derivatization by GC-MS/MS-selected reaction monitoring（SRM）.Results The calibration curves of T-2 and HT-2 toxin showed good linearity in the range of 0.5-100 μg/kg for the samples of rice,millet,glutinous rice and corn.Under optimal conditions,the limits of detection（LOD） of two toxins ranged from 0.05 to 0.5 μg/kg.The spiked recovery of T-2 and HT-2 toxin at concentration levels of 2,30 and 60 μg/kg ranged from 47.2% to 110.8%.Conclusion Such a GC-MS/MS method is simple and sensitive,and is feasible for the detection of T-2 toxin and HT-2 toxin in various crop samples.