大米及玉米中6种环己烯酮类除草剂的液相色谱-串联质谱测定  

Analysis of Cyclohexanedione Herbicides in Rice and Corn by LC-MS/MS

作　　者：沈金灿[1] 叶卫翔[1] 谢丽琪[1] 赵琼辉[1] 肖来龙[1] 

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,广州深圳518067

出　　处：《质谱学报》2009年第4期201-207,共7页Journal of Chinese Mass Spectrometry Society

基　　金：国家质检总局计划项目(No.B126-2004);深圳出入境检验检疫局博士资金(SZ2007106)资助

摘　　要：建立了大米和玉米中6种环己烯酮类除草剂吡喃草酮,禾草灭,噻草酮,苯草酮,稀禾定和烯草酮的高效液相色谱-串联质谱(LC-MS/MS)测定方法。样品制备后,采用乙腈进行提取,经C18和Envi-Carb固相萃取柱净化处理后,采用LC-MS/MS电喷雾电离(ESI),多反应监测(MRM)正离子模式检测,外标法定量。在1～100μg.L-1范围内,6种环己烯酮类除草剂的线性相关系数均大于0.999。在添加浓度5～20ng.g-1范围内,6种环己烯酮类除草剂的回收率在70.0%～97.9%,相对标准偏差(RSD)均在10%以内。A method for determination of 6 cyclohexanedione herbicides, tepraloxydim, alloxydim, cycloxydim, tralkoxydim, sethoxydim and clethodim in rice and corn was developed. After homogenization, sample was extracted with acetonitrile. The extracts were cleaned by C18 and Envi-Carb solid phase extraction （SPE） cartridge. Identification and detection were achieved by electrospray ionization （ESI） in positive mode using multiple reaction monitoring of liquid chromatography coupled with tandem mass spectrometry. The linearity of all the 6 cyclohexanedione herbicides in the range from 1 to 100μg · L^-1 is correlation coefficient greater than 0. 999. Cyclohexanedione herbicides are quantified by external standard method. Recoveries of 6 cyclohexanedione herbicides are within 70.0%-97.9%at the spiked levels of 5-20 ng · g^ -1. The relative standard deviations （RSDs） for the 6 herbicides are less than 10%.

关 键 词：环己烯酮 除草剂 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]