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

摘要

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 C 18 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.%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0.5~100 μg/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0.05~0.5 μg/kg.在2、30 、60 μg/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.