超高效液相色谱-串联质谱法测定面粉、玉米及其制品中的伏马菌素研究

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。

Ultra performance liquid chromatography-tandem mass spectrometry method for determination of fumonisins in wheat flour,corn and corn-based products

Objective To develop a solid-phase extraction method coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) for determination of three fumonisins(fumonisin B1,fumonisin B2 and fumonisin B3) in wheat flour,corn and corn-based products.Methods The samples were extracted by 50%(V/V) acetonitrile-water,followed by cleaning up on a MultiSep 211 column.Three toxins were eluted by methanol-formic acid(99∶ 1,V/V) and analyzed by UPLC-MS/MS with gradient elution.Acetonitrile and 0.2%(V/V) formic acid-water were used as the mobile phases in the gradient elution.The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring(MRM) in electrospray positive ionization mode.Results The limits of detection(LOD) and the limits of quantification(LOQ) for three fumonisins were 0.2 μg/kg and 0.6 μg/kg.The mean recoveries of three fumonisins at the different spiked levels ranged from 69.44% to 114.69%.39 corn samples and 30 wheat flour samples collected from Gansu and Tianjin harvested in 2011 were analyzed with the developed method.Fumonisin B1 was the predominant toxin detected in terms of frequency and contamination level.Conclusion The developed method is simple,sensitive and reproducible,and meets the requirement for determination of the three fumonisins in wheat flour,corn and corn-based products.