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分析化学  2015 

液相色谱-串联质谱法测定饲料原料中26种霉菌毒素

DOI: 10.11895/j.issn.0253-3820.140769, PP. 264-270

Keywords: 液相色谱-串联质谱,饲料原料,多功能净化柱,霉菌毒素

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Abstract:

建立了同时检测玉米、豆粕等饲料原料中脱氧雪腐镰刀菌烯醇等26种霉菌毒素的液相色谱-串联质谱(LC-MS/MS)方法.玉米和豆粕样品经乙腈-水-甲酸(84:15.9:0.1,V/V)超声提取1h,取1mL上清液经Mycospin400多功能净化柱净化,浓缩干燥,0.25mL水-甲醇-甲酸(95:4.9:0.1,V/V)复溶,上机测定.采用反相C18色谱柱分离,以0.1%甲酸-水和0.1%甲酸-甲醇溶液作为流动相进行梯度洗脱,采用多反应监测离子模式进行定性分析.基质效应考察发现,样品提取液经Mycospin400多功能净化柱净化后,大部分毒素仍有较强的基质效应.因此,采用基质匹配标准曲线外标法进行定量分析.在高、中、低3种添加浓度水平下,26种霉菌毒素的平均回收率为61.9%~119.5%,相对标准偏差介于0.8%~18.6%之间.针对不同目标物,本方法的定量限为0.5~25μg/kg.

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