液相色谱-串联质谱法测定猪可食性组织中脱氧雪腐镰刀菌烯醇残留量的方法研究  

Study on the Determination of Dexynivalenol in Edible Tissues of Swine by Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

作　　者：李维铖[1] 沈祥广[1] 刘戎[1] 张嘉慧[1] 余静贤[1] 谢玉萍[1] 邓衔柏[1] 

机构地区：[1]华南农业大学兽医学院,广东广州510642

出　　处：《华南农业大学学报》2013年第1期101-105,共5页Journal of South China Agricultural University

基　　金：国家重点基础研究发展计划项目(2009CB118805);省部产学研结合项目(2011B090400228)

摘　　要：针对猪可食性组织中脱氧雪腐镰刀菌烯醇(DON)的残留,建立了一种液相-电喷雾质谱检测法.样品用纯水提取,C18柱净化,体积分数为30%的甲醇洗脱后进行LC-MS/MS分析.色谱柱采用Phenomenex Luna 5μC18(2),流动相采用体积比为3∶7的甲醇-体积分数为0.1%甲酸水溶液.质谱采用电喷雾离子源,正离子多重反应监测模式进行定量和定性分析.方法的最低检测限为25μg.kg-1,最低定量限为50μg.kg-1;在50、100、500μg.kg-13个水平的回收率为80.2%～99.4%,相对标准偏差为2.47%～9.47%.A method has been developed for the determination of dexynivalenol in edible tissues of swine by liquid chromatography coupled with electrospray ionization tandem mass spectrometry （LC-MS/MS）. The samples were extracted by pure water and purified by Cls solid phase extraction, and then analyzed by the LC-MS/MS after redissolved by 30% methanol. The chromatographic column was Phenomenex Lu- na 5 μ ClS （2）, and the flowing phase was comprised with methanol -0. 1% formic acid solution （ V/V = 3 ： 7 ）. The mass spectrometry was run with electrospray ion source and in positive ions multiple reaction monitoring mode for the quantitative and qualitative analyses. Limit of detection （LOD） was 25 μg · kg^- 1, and limit of quantitation （LOQ） was 50μg · kg^- 1. The recoveries of dexynivalenol in edible tissues of swine ranged from 80. 2% to 99.4% in 50, 100 and 500 μg · kg^- 1 concentration levels. The relative standard deviation ranged from 2.47% to 9.47%.

关 键 词：脱氧雪腐镰刀菌烯醇 猪可食性组织 固相萃取 电喷雾串联质谱 

分 类 号：S859.84[农业科学—临床兽医学]