高效液相色谱-串联质谱法测定不同畜禽配合饲料中伏马毒素的含量  

Determination of Fumonisin B_1 and Fumonisin B_2 in Formula Feeds for Livestock and Poultry by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭文博[1,2] 杨俊花[1] 韩铮[1] 陈慧英[1,2] 孙真真[1,2] 赵志辉[1] 

机构地区：[1]上海市农业科学院农产品质量标准与检测技术研究所,上海201403 [2]上海海洋大学食品学院,上海201306

出　　处：《分析化学》2015年第3期414-418,共5页Chinese Journal of Analytical Chemistry

基　　金：上海市农委科技兴农重点攻关项目沪农科攻字(2013)第3-8号;沪农科攻字(2014)第3-2号项目资助~~

摘　　要：为摸清复杂基质中FB1和FB2污染的准确水平,本研究建立了高效液相色谱-串联质谱法（LC-MS/MS）测定不同畜禽配合饲料中伏马毒素B1（FB1）和B2（FB2）的分析方法。样品用乙腈-水（50∶50,V/V）提取,MAX强阴离子固相萃取柱富集净化后,以0.1%甲酸和甲醇为流动相,经Thermo C18色谱柱（100 mm×2.1 mm,5μm）分离,采用电喷雾正电离（ESI＋）多反应模式（MRM）监测,外标法定量。结果表明：不同饲料样品中FB1和FB2在1-500μg/kg之间线性关系良好,相关系数（R2）均大于0.9990,定量限分别为0.098和0.197μg/kg,检出限分别为0.328和0.656μg/kg;低、中、高浓度加标回收率为89.7%-95.1%,相对标准偏差（RSD）为3.2%-8.6%。用本方法对市场上采集的106份不同畜禽配合饲料中FB1和FB2含量进行测定,样品检出率为98.11%。本方法适用于基质复杂的畜禽配合饲料中伏马毒素FB1和FB2的准确、快速定性与定量分析。A method was developed for the determination of fumonisin B1（ FB1） and fumonisin B2（ FB2） in livestock and poultry formula feeds by high performance liquid chromatography-tandem mass spectrometry（ LC-MS /MS. After extracted by acetonitrile-water（ 50 ∶ 50,V/V） and purified with MAX solid phase extraction column,the fumonisins were separated by Thermo C18（ 100 mm×2. 1 mm,5 μm） column with0. 1% formic acid in water and methanol as the mobile phase. Multiple reaction monitoring（ MRM） was used to acquire mass spectrometric data under electrospray positive ionization mode（ ESI＋）. The results showed that the linear correlation coefficients（ R2） of fumonisin FB1 and FB2were all greater than 0. 999 in the range of 1-500 μg / L. The limits of quantitation（ LOQ） were 0. 098 and 0. 197 μg / L,and the limits of detection（ LOD） were 0. 328 and 0. 656 μg /L,respectively. At different spiked levels,the recoveries of FB1 and FB2were ranged from 89. 7% to 95. 1%,and the relative standard deviation（ RSD） was ranged from 3. 2% to8. 6%. Additionally,the detection rate reached 98. 11% screening through the established method in the 106 livestock and poultry formula feeds collected from markets. This result indicates that the method is suitable for accurate quantitative analysis of FB1 and FB2in different complicated livestock and poultry formula feeds.

关 键 词：伏马毒素 阴离子固相萃取柱 液相色谱-串联质谱法 畜禽配合饲料 

分 类 号：S816.17[农业科学—饲料科学] O657.63[农业科学—畜牧学]