凝胶渗透色谱净化-超高效液相色谱-串联质谱法同时检测玉米粉中10种真菌毒素

Simultaneous determination of ten mycotoxins in corn flour by gel permeation chromatography-ultra performance liquid chromatography-tandem mass spectrometry

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 detection of ten common mycotoxins in corn flour with gel permeation chromatography（ GPC） pretreatment and ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. Methods The samples were extracted by acetonitrile-water（ 90 ∶ 10,V/V） and evaporated to dryness under nitrogen,reconstituted by cyclohexane / ethyl-acetate mixture（ 1 ∶ 1,V / V）,then purified by GPC and concentrated.The reconstituted solution was filtered through 0. 22 μm nylon syringe filter. Chromatography was performed using a Waters ACQUITY UPLC HSS T3 column（ 2. 1 mm × 100 mm,1. 8 μm）. Quantitation was performed in the electrospray ionization mode and multiple reaction monitoring（ MRM）. Results Quantified by matrix matching external standard method,all mycotoxins had good linear relationship within linear ranges,the correlation coefficients of the standard curve were 0. 995 9-0. 999 8. The limits of quantitation（ LOQ） of ten mycotoxins were 0. 003-1. 2 μg / kg,the recoveries at low,middle and high spiked levels were from 71. 3%-91. 3%, and the relative standard deviations（ RSDs） were 3. 1%-13. 2%.Conclusion The method was high sensitive,accurate,safe,low cost,simple and suitable for determination of mycotoxins in corn flour products.