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目的建立凝胶渗透色谱净化-超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定玉米粉中10种常见的真菌毒素分析方法。方法样品中的目标化合物经乙腈-水(90∶10,V/V)提取,将收集的上清液用氮气吹至近干后经乙酸乙酯-环己烷(1∶1,V/V)溶解,再经凝胶渗透色谱净化,净化液浓缩后经过0.22μm尼龙滤膜过滤,采用Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm)色谱柱分离,在电喷雾电离源(ESI)和多反应监测(MRM)方式下测定。结果采用基质匹配外标法测定,10种真菌毒素在曲线范围内有良好的线性关系,其相关系数为0.995 9~0.999 8,10种真菌毒素在玉米粉样品中的定量下限为0.003~1.2μg/kg,三个浓度水平的加标回收率为71.3%~91.3%,相对标准偏差(RSD)为3.1%~13.2%。结论该方法选择性好,操作简单安全,成本低,快速准确,适用于玉米粉中多种真菌毒素的测定。
OBJECTIVE To establish a method for the simultaneous determination of ten common mycotoxins in corn meal by gel permeation chromatography-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). The target compound in the method sample was extracted with acetonitrile-water (90:10, V / V) and the supernatant collected was blown with nitrogen to near-dryness and eluted with ethyl acetate-cyclohexane (1: Dissolved and purified by gel permeation chromatography. The concentrated solution was filtered through a 0.22 μm nylon membrane and separated on a Waters ACQUITY UPLC HSS T3 (2.1 mm × 100 mm, 1.8 μm) column. Electrospray ionization (ESI) And multiple reaction monitoring (MRM) mode. Results The matrix matched external standard method was used to determine the mycotoxins. The 10 mycotoxins had a good linear relationship in the curve range with a correlation coefficient of 0.995 9 to 0.999 8. The lower limit of quantification of 10 mycotoxins in the corn flour samples was 0.003-1.2 μg / kg, the spiked recoveries of three concentrations ranged from 71.3% to 91.3%, and the relative standard deviations (RSDs) ranged from 3.1% to 13.2%. Conclusion The method has good selectivity, simple and safe operation, low cost, fast and accurate, and is suitable for the determination of various mycotoxins in corn flour.