复合免疫亲和柱净化-UPLC-MS/MS测定饲料中黄曲霉毒素B_(1)、玉米赤霉烯酮和T-2毒素  

Determination of aflatoxin B_(1),zearalenone and T-2 toxin in feeds by UPLC-MS/MS combined with immunoaffinity clean-up column

作　　者：李洪波 宋志超[2] 陈蔷[2] 刘传辉[3] LI Hongbo;SONG Zhichao;CHEN Qiang;LIU Chuanhui(Zhumadian quality inspection and supervision center of Veterinary Drugs,feed and animal product,Zhumadian,Henan Province 463000,China;Hennan Institute of Veterinary Drug Control,Zhengzhou,Henan Province 450008,China;Shangqiu animal product quality monitoring and inspection center,Shangqiu,Henan Province 476000,China)

机构地区：[1]驻马店市兽药伺料动物产品质量检验监测中心,河南驻马店463000 [2]河南省兽药监察所,河南郑州450008 [3]商丘市畜产品质量监测检验中心,河南商丘476000

出　　处：《中国饲料》2022年第5期79-83,共5页China Feed

摘　　要：为建立饲料(浓缩饲料、配合饲料、植物性饲料原料)中黄曲霉毒素B_(1)、玉米赤霉烯酮和T-2毒素残留量的复合免疫亲和柱净化-UPLC-MS/MS检测方法,实验样品经86%乙腈提取,复合免疫亲和柱净化,定容后经液相快速分离,电喷雾离子化,采用MRM监测模式,正负离子扫描,外标法定量。结果表明:黄曲霉毒素B_(1)检测限为0.02μg/kg,定量限为0.05μg/kg,在0.05~2.0μg/L线性关系良好,r≥0.9990,在添加不同倍数定量限浓度水平上回收率为90.5%~97.8%,变异系数≤2.6%;玉米赤霉烯酮检测限为0.2μg/kg,定量限为0.5μg/kg,在0.5~10.0μg/L线性关系良好,r≥0.9992,在添加不同倍数定量限浓度水平上回收率为85.4%~93.7%,变异系数≤4.6%;T-2毒素检测限为0.02μg/kg,定量限为0.05μg/kg,在0.05~2.0μg/L线性关系良好,r≥0.998,在添加不同倍数定量限浓度水平上回收率为87.4%~95.2%,变异系数≤3.9%。本方法分析速度快、灵敏度高、准确可靠,可用于饲料中黄曲霉毒素B_(1)、玉米赤霉烯酮和T-2毒素的检测分析。A new method for determination of aflatoxin B_(1),zearalenone and T-2 in feeds by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The samples were extracted using the solution of 86%acetonitrile,and purified through immunoaffinity clean-up column,rapid separation by liquid phase after constant volume.The identification and quantification of the target compounds were carried out by positive and negative electrospray ionization(ESI±)in the multiple reaction monitoring(MRM)mode using external standard method.The results showed that the limits of detection(LOD)and the limits of quantification(LOQ)for aflatoxin B_(1) were 0.02μg/kg and 0.05μg/kg.The calibration curves showed good linearity in the range of 0.05~2.0μg/L(r≥0.9990).The recovery rates were90.5%~97.8%at different concentration levels,with the relative standard deviations(RSD)less than or equal to 2.6%.The limits of detection(LOD)and the limits of quantification(LOQ)for zearalenone were 0.2μg/kg and 0.5μg/kg.The calibration curves showed good linearity in the range of 0.5~10.0μg/L(r≥0.9992).The recovery rates were 85.4%~93.7%at different concentration levels,with the relative standard deviations(RSD)less than or equal to 4.6%.The limits of detection(LOD)and the limits of quantification(LOQ)for T-2 toxin were 0.02μg/kg and 0.05μg/kg.The calibration curves showed good linearity in the range of 0.05~2.0μg/L(r≥0.998).The recovery rates were 87.4%~95.2%at different concentration levels,with the relative standard deviations(RSD)less than or equal to 3.9%.The method was simple,rapid,sensitive,accurate,reliable for the determination of aflatoxin B_(1),zearalenone and T-2 toxin in feeds.

关 键 词：黄曲霉毒素B_(1) 玉米赤霉烯酮 T-2毒素 复合免疫亲和柱 液相色谱-串联质谱 

分 类 号：S816.17[农业科学—饲料科学]