液相色谱-串联质谱法测定粮谷中的伏马毒素

Determination of Fumonisins in Cereals Using Liquid Chromatography-Tandem Mass Spectrometry

建立了液相色谱-串联质谱同时测定玉米、小麦、大米和黄豆中伏马毒素FB1、FB2的分析方法.样品经甲醇-水-乙酸（74∶25∶1）提取,强阴离子交换柱（SAX）净化后,以0.1％乙酸水溶液-乙腈为流动相,ZORBAX Extend-C18反相色谱柱（150 mm ×2.1 mm,1.8 μm）进行色谱分离,在电喷雾正离子化模式下,选择反应监测（SRM）方式进行测定.结果表明：FB1和FB2分别在2.5～1000、5.0～1 000 μg/L范围内线性关系良好,相关系数分别为0.999 5和0.999 7.对4种空白基质分别进行0.02、0.50、2.00 mg/kg 3个水平的加标回收实验,FB1和FB2的加标回收率分别为67.5％ ～ 90.5％和70.5％ ～ 95.3％,相对标准偏差（RSD）分别为1.3％ ～ 11.4％和1.5％ ～ 10.6％,检出限分别为2.00 μg/kg和4.00μg/kg.该方法稳定、可靠,适用于谷物中FB1和FB2的同时检测与确证.

A method was developed for the determination of fumonisin B1 （FB1） and fumonisin B2 （FB2） in cereals by high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）.The sample was extracted with methanol-water-acetic acid （74 ∶ 25 ∶ 1）,and cleaned up by strong anion exchange column（SAX）.FB1 and FB2 were completely separated on a ZORBAX Extend-C18 column（150 mm ×2.1 mm,1.8 μm） with gradient elution by using 0.1% acetic acid water solution-acetonitrile as mobile phase,and detected by positive ion electrospray ionization mass spectrometry（ESI-MS） under select reaction monitoring（SRM） mode.The results showed that the linearities of FB1 and FB2 were in the concentration ranges of 2.5-1 000 μg/L,5.0-1 000 μg/L,respectively,with correlation coefficients of 0.999 5 and 0.999 7,respectively.The average recoveries of FB1 and FB2 from four kind of blank matries at three spiked levels of 0.02,0.50,2.00 mg/kg were in the range of 67.5%-90.5% and 70.5%-95.3%,respectively,with relative standard deviations（RSDs,n =5） of 1.3%-11.4% and 1.5%-10.6%,respectively.The limits of detection were 2.00 μg/kg for FB1and 4.00 μg/kg for FB2.This method was stable,reliable,and could be used for detection of FB1 and FB2 in cereals simultaneously.