QuEChERS-高效液相色谱-串联质谱法测定小麦中的8种真菌毒素

Determination of Eight Mycotoxins in Wheat by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

【目的】建立了基于QuEChERS技术的高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定小麦中8种真菌毒素的方法。【方法】对QuEChERS前处理技术条件进行改进和优化,最终确定样品经甲酸水溶液分散后采用乙腈提取,然后加入氯化钠和无水硫酸镁盐析分层,上层清液加入C18、PSA和无水硫酸镁净化;以Waters C18(5μm,150 mm 4.6 mm i.d.)色谱柱分离,梯度洗脱,质谱分析采用电喷雾电离源(ESI)和多反应监测方式(MRM),以基质匹配标准曲线外标法进行定量。【结果】8种真菌毒素在小麦中线性良好,相关系数(r)均大于0.99,方法检出限为0.10～1.0μg/kg,样品的平均加标回收率为85.1%～95.4%,相对标准偏差为3.8%～8.5%。【结论】该方法简便、快捷、灵敏、准确、环保,可用于小麦中8种真菌毒素的同时检测。

[Objective] A method based on QuEChERS technique was developed for the simuhaneous determination of eight mycotoxins in wheat by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. [Method] The QuEChERS technique was improved and optimized. As a result, the samples were firstly extracted with acetonitrile after dispersed with formic acid aqueous solution, and salted out with sodium chloride and anhydrous magnesium, and finally the extracts were cleaned up with C 18 and PSA sorbents and anhydrous magnesium. Chromatographic analysis was carried out using a Waters C18 （5 μm, 150 mm 4.6 mm i.d.） column with gradient elution. The mycotoxins were analyzed by electrospray ionization source and muhiple reaction monitoring mode （MRM） in tandem mass spectrometry. The quantification was achieved using matrix-matched standard calibrations as the external standard. [Result] The results showed that all the mycotoxins in wheat were determined with excellent linear relationships under the correlation coefficients （r） above 0.99. The limits of detection for all mycotoxins were in the range of 0.10-1.0 μg/kg. The average recoveries were 85.1%-95.4% with the relative standard deviations of 3.8%-8.5%. [Conclusion] The method has been proven to be simple, quick, sensitive, accurate, environmental protection, and thus suitable for the simuhaneous determination of the eight mycotoxins in wheat samples.