饲料用玉米和小麦麸皮中伏马毒素含量的测定

Determination of Fumonisins in Maize and Wheat Bran Feeds

通过对仪器条件、提取溶剂的选择与优化,建立了饲料用玉米和小麦麸皮中伏马毒素(FB1、FB2、FB3)的液相色谱-串联质谱分析方法。样品用水-2%甲酸乙腈(50:50,V/V)提取,经分散固相萃取净化管和PRIME HLB固相萃取柱净化后,用液相色谱-串联质谱仪进行测定。结果表明:玉米和小麦麸皮基质溶液中,3种伏马毒素在1.0~250 ng/mL浓度范围内呈现良好的线性,相关系数(R2)均大于0.999,方法的检出限(LOD)和定量限(LOQ)分别为1.0、3.0μg/kg。不同添加浓度水平下,玉米和小麦麸皮样品中伏马毒素的加标回收率分别为83.65%~107.3%、88.79%~103.5%,相对标准偏差(RSD)分别为2.03%~7.00%、1.41%~8.98%。该方法净化效果好,杂质干扰小,且回收率高,可满足饲料用玉米和小麦麸皮中伏马毒素的检测要求。

Via the selection and optimization of apparatus parameters and extraction solvents,an efficient method for the determination of Fumonisins(FB1,FB2 and FB3)in maize and wheat bran feeds was de⁃veloped based on liquid chromatography-tandem mass spectrometry(LC-MS/MS).Samples were extract⁃ed by water-acetonitrile with 2%formic acid(50:50,V/V),preliminary purified by dispersive solid phase extraction tube and followed by PRIME HLB solid phase extraction column.All purified sample so⁃lutions were then determined by LC-MS/MS.The limit of detection(LOD)for these three compounds in maize and wheat bran feeds was estimated to be 1.0μg/kg,and the limit of quantification(LOQ)was 3.0μg/kg,showing good linearity in the matrix solution concentration range of 1.0~250 ng/mL with coeffi⁃cient R2 more than 0.999.At different spiked levels,the average recoveries of three compounds in maize were in the range of 83.65%~107.3%(with RSD of 2.03%~7.00%),the average recoveries of three com⁃pounds in wheat bran were in the range of 88.79%~103.5%(with RSD of 1.41%~8.98%),respectively.The proper impurity purification,small impurity interference and high recovery rate make this method suit⁃able for the determination of fumonisins in maize and wheat bran feeds.