亲水作用液相色谱串联质谱法测定糙米中灭瘟素残留量  

Determination of Blasticidin-S in Brown Rice by HILIC-MS/MS

作　　者：苏红伟[1] 赵华锋 周嘉明 罗司玉 

机构地区：[1]华测检测技术股份有限公司上海分公司,上海201206 [2]青岛市华测检测技术有限公司,山东青岛266101

出　　处：《粮油加工（电子版）》2014年第6期47-49,共3页Machinery for Cereals Oil and Food Processing Main Contents

摘　　要：建立了糙米中灭瘟素残留量的亲水作用液相色谱-质谱联用测定方法。样品用80％甲醇／水提取，经MCX固相萃取小柱净化，以WatersHPLCBEHHILIC色谱柱（100mm×2．1mm，1．7μm）分离，采用U—PLC—MS／MS多反应监测（MRM）正离子模式测定，外标法定量。灭瘟素最低检测浓度为0．02mg／kg，在0．02、0．05和0．20mg／kg3个添加水平下平均回收率为78％～95％，相对标；住偏差为2．9％～5．2％。A method of determination for blasticidin-S in brown rice by HILIC-MS/MS was established. Analytes were extracted from samples using methanol and water （V/V, 8：2） , and purified with MCX solid phase extraction columns, then analyzed using UPLC-MS/MS multiple reaction monitoring （MRM） mode via positive electrospray ionization with a Waters HPLC BEH HILIC column （ 100mm×2.1mm, 1.7μm） as the analytical column. All analytes were quantified by external standard method. Limit of quantification was 0.02mg/kg. Results showed that average recoveries at fortified levels of 0.02, 0.05 and 0.2 mg/kg ranged from 78% to 95%, and RSD were 2.9% -5.2%.

关 键 词：灭瘟素 残留 糙米 亲水作用液相色谱-质谱 质谱 

分 类 号：TQ450.7[化学工程—农药化工]