全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16种真菌毒素

考察高效液相色谱-串联质谱-全碳标记的稳定同位素内标法精确测定小麦和玉米中16种真菌毒素方法的适用性。样品经提取稀释、加入内标,高效液相色谱-串联质谱测定。结果表明,16种真菌毒素线性相关系数大于0.997,3个水平的添加回收率为83%~114.3%,相对标准偏差为0.9%~13%,定量限为0.5~200μg/kg,通过检测FAPAS04223质控样品和小麦、玉米样品验证了方法的准确性和适用性,能够快速、批量、准确的测定小麦和玉米中16种真菌毒素,为我国粮食真菌毒素污染监测提供便利。

Suitability of Fully 13C Isotope Labeled Internal Standards for the Simultaneous Determination of 16 Mycotoxins in Grains by UPLC-MS/MS

This work investigated the suitability of applying fully 13C isotope labeled mycotoxins as internal standards for the accurate determination of 16 mycotoxins in maize and wheat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target analytes in samples were extracted, diluted, and detected by UPLC-MS/MS after addition of internal standards. The results showed that all 16 mycotoxins displayed good linear relationships with correlation coefficients more than 0.997. Recoveries of the analytes were in the range of 83%–114.3% with relative standard deviations of 0.9%–13%. The limits of quantification (LOQs) of the method ranged from 0.5 to 200 μg/kg. Maize reference materials, and corn and wheat samples were analyzed by this method to validate its accuracy and applicability. The method could accurately, quickly detect 16 mycotoxins in grains in batch.