农产品与饲料中T-2毒素免疫亲和柱净化-液相色谱串联质谱检测技术研究  

Investigation on Determination of T-2 Toxin in Cereal and Feed by Immunoaffinity Column Purification /LC- MS /MS

作　　者：李静[1,2,3] 马飞[1,4,5] 李培武[1,2,4,3,5] 张奇[1,2,4] 丁小霞[1,2,3] 张文[1,2,5] 

机构地区：[1]中国农业科学院油料作物研究所,湖北武汉430062 [2]农业部生物毒素检测重点实验室,湖北武汉430062 [3]农业部油料产品质量安全风险评估实验室(武汉),湖北武汉430062 [4]农业部油料作物生物学与遗传育种重点实验室,湖北武汉430062 [5]农业部油料及制品质量监督检验测试中心,湖北武汉430062

出　　处：《分析测试学报》2014年第10期1095-1101,共7页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(31101299);国家科技支撑计划(2012BAB19B09);公益性行业科研专项(201203094);国家农产品质量安全风险评估重大项目(GJFP2014006)

摘　　要：利用T-2毒素单克隆抗体2G7和CNBr活化的Sepharose 4B研制出T-2免疫亲和柱，考察了T-2免疫亲和柱的最佳应用条件。利用免疫亲和柱，建立了农产品与饲料中T-2毒素免疫亲和柱净化/液相色谱-串联质谱（ IAC/LC-MS/MS）确证性检测技术，并考察该方法的准确度和精密度。结果表明，T-2毒素在0.5-500.0 ng/g范围内线性关系良好，相关系数为0.9997，检出限为0.05 ng/g，定量下限为0.17 ng/g。大米、玉米、饲料样品在T-2毒素10，50，100 ng/g的加标水平下，回收率为92.9％-109.7％，相对标准偏差为2.1％-8.3％。对市售36份农产品与饲料样品进行测定，检测结果的相对标准偏差均小于10.0％。lmmunoaffinity column（ lAC ）for T-2 toxin was prepared with anti-T-2 toxin monoclonal antibody 2G7 and CNBr activated Sepharose 4B. The experimental conditions for T-2 immunoaffinity column were optimized and the columns were applied in cereals and feed pretreatment. An lAC/LC-MS/MS method was established for the determination of T-2 toxin in cereals and feed. The calibration curve for T-2 toxin standard solution was linear in the range of 0. 5-500. 0 ng/g with correlation coef-ficient of 0. 999 7. The limit of detection（LOD）and limit of quantitation（LOQ）was 0. 05 ng/g and 0. 17 ng/g,respectively. The average recoveries of T-2 toxin in rice,maize and feed samples at three spiked levels of 10,50,100 ng/g ranged from 92. 9% to 109. 7% ,with relative standard de-viations（ RSDs）of 2. 1% -8. 3% . The method was applied in the detection of T-2 toxin in 36 real samples with RSDs less than 10. 0% .

关 键 词：T-2毒素 免疫亲和柱 定量分析 农产品与饲料 

分 类 号：O657.63[理学—分析化学]