超高效液相色谱-串联质谱法同时测定谷物及其制品中11种真菌毒素

Determination of 11 kinds of mycotoxins in grains and its products by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法同时测定谷物及其制品中11种常见真菌毒素的分析方法。方法样品采用70%的甲醇水溶液超声提取,经多功能净化柱净化,Waters ACQUITY UPLC HSS T3 C_(18)色谱柱分离,以0.2%氨水溶液和乙腈流动相梯度洗脱,利用串联三重四极杆质谱多反应模式,负离子监测方式检测,并采用内标法和外标法结合定量。结果 11种真菌毒素在相应范围内线性关系良好,相关系数均大于等于0.997,通过低、中、高3个浓度进行加标回收实验,加标回收率范围为65.4%～108.2%,相对标准偏差(RSD)范围为0.68%～9.25%,检出限范围为0.02～0.10μg/kg,定量限范围为0.15～2.0μg/kg,通过真菌毒素质控样的测定,检测值在参考值允许范围内。结论该方法具有灵敏度高、重复性好、准确度高、样品前处理操作便捷和检测速度快的优点,适用于谷物及其制品中11种真菌毒素的检测。

Objective To establish a method for simultaneous determination of 11 kinds of mycotoxins in grains and its products by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods After extracted by 70% methanol and purification by multifunction cleaning column, the mycotoxins of grains and its products were separated by a chromatographic column of Waters ACQUITY UPLCTMBEH C（18）, gradient eluted with 0.2% ammonia solution and acetonitrile as the mobile phase. The mass spectrometry was conducted by using negative electrospray ionization（ESI-） and multi-reactions monitoring（MRM） models, and internal and external standard methods were used to quantify. Results The 11 kinds of mycotoxins had good linear relationships in the corresponding ranges, with correlation coefficients greater than or equal to 0.997. The recovery experiments were carried out through 3 concentrations of low, medium and high concentration, the recovery rates were from 65.4% to 108.2%, the relative standard deviations（RSDs） were 0.68%～9.25%, the limits of detection were 0.02～0.10 μg/kg, and the limits of quantification were 0.15～2.0 μg/kg. Through the determination of the quality control of mycotoxin, the detection values were within the reference values. Conclusion This method has the advantages of high sensitivity, good repeatability, high accuracy, convenient operation and quick detection speed, which is suitable for the detection of 11 kinds of mycotoxins in grains and its products.