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目的建立面粉、玉米及其制品中3种伏马菌素的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法样品用乙腈-水(50∶50,V/V)溶液提取,经MultiSep 211净化柱富集净化后,用甲醇-甲酸(99∶1,V/V)溶液洗脱,洗脱液用UPLC-MS/MS进行测定。UPLC-MS/MS检测伏马菌素的条件为梯度洗脱,流动相为0.2%甲酸水和乙腈;质谱采集模式为电喷雾正离子多反应监测模式。结果 UPLC-MS/MS检测方法对3种伏马菌素的检出限均为0.2μg/kg,最低定量限为0.6μg/kg。不同加标水平的3种伏马菌素平均回收率为69.44%～114.69%。用所建方法对2011年甘肃及天津生产的39份玉米及30份面粉样品进行了分析,结果以伏马菌素B1的检出率最高,污染水平最为严重。结论 UPLC-MS/MS法具有操作简单、灵敏度高、重现性好等特点,可用于面粉、玉米及其制品中伏马菌素的检测。
Objective To establish a method for the determination of three fumonisins in flour, corn and their products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The samples were extracted with acetonitrile-water (50:50, V / V) and purified by MultiSep 211 purification column. The samples were eluted with methanol-formic acid (99:1 V / V) -MS / MS. The conditions for the determination of fumonisin by UPLC-MS / MS were gradient elution, the mobile phase was 0.2% formic acid water and acetonitrile, and the mass acquisition mode was electrospray positive ion multiple reaction monitoring. Results The detection limits of three fumonisins by UPLC-MS / MS were 0.2μg / kg and the limit of quantification was 0.6μg / kg. The average recoveries of three fumonisins at different spiked levels ranged from 69.44% to 114.69%. The results showed that the detection rate of fumonisin B1 was the highest and the pollution level was the most serious in the analysis of 39 maize and 30 flour samples produced in Gansu and Tianjin in 2011. Conclusion UPLC-MS / MS has the advantages of simple operation, high sensitivity and good reproducibility. It can be used for the determination of fumonisins in flour, corn and their products.