应用串联液质技术检测玉米中伏马菌毒素的研究

Simultaneous determination of three kinds of fumonisin contaminants in corn by ultra-performance liquid chromatography tandem mass spectrometry

目的：建立简单、快速、同时测定玉米中伏马菌素的超高效液相色谱三重四极杆质谱确证方法。方法：样品经混合溶剂50/50的乙腈/水溶液（V/V）提取,SPE柱净化、离心、吹干、定容和过滤。进样,经超高压液相BEH C18（50 mm×2.1 mm I.D.,粒径1.7μm）柱分离,选用0.1%甲酸溶液和乙腈/甲醇（50/50,V/V）作为流动相,经梯度洗脱将3种伏马菌毒素完全分离。采用基质加标法定量。结果：经方法学研究验证：在ESI＋电离方式下3种伏马菌毒素的最低定量限LOQ：FB1为3.08μg/kg,FB2为1.00μg/kg,FB3为0.45μg/kg,均低于欧盟、美国的最低限量。相关系数r均大于0.999;低、中、高浓度加标回收率：88.6±6.4%～93.7±4.1%,80.9±2.0%～96.1±6.9%,84.9±1.6%～97.0±2.9%。结论：该方法具有预处理简单、检测速度快、灵敏度高的优点,可适用于玉米样品中伏马菌毒素的确认和准确定量检测,可满足各国对伏马菌毒素的最低检出要求。

Objective：A new approach for simple and rapid simultaneous determination of 3 kinds of fumonisin contaminants in corn by ultra-performance liquid chromatography-tandem mass spectrometry is described.Methods：Homogenized samples were sequentially extracted by 50%（v/v） of acetonitrile aqueous solution,SPE clean-up with MultiSep211 FUM columns,centrifuge,evaporate,re-dissolve and filtration.Then injected,the analytes were separated by UPLC BEH C18 column（50 mm×2.1 mm I.D.,1.7 μm）,and eluted with 0.1% formic acid and acetonitrile /methanol（50＋50）.The method is spiked with standard for quantitative analysis.Results：The LOQ of selected analytes ranged from 0.45 to 3.08 μg/kg,which was lower than the criteria of EU,USA and other countries on the determination of the minimum limiting level of Fumonisin in foods including baby foods and corn.Meanwhile,reasonable recoveries（80.9%～97.0%） of them were also demonstrated in different spiked levels.Conclusion：This quantitative method has many advantages including simple pretreatment,rapid determination and high sensitivity,which could be applied to the determination and quantification of Fumonisin contaminants in maize.Meanwhile,the method successfully fulfilled the minimum limiting level requests from various countries.