摘要
建立了粮谷中三环锡和苯丁锡同时测定的气相色谱-质谱联用(GC-MS)测定方法.样品中残留的三环锡和苯丁锡经用乙腈提取,乙腈饱和正己烷进行液液分配,与乙基溴化镁-乙醚溶液衍生化后,经弗罗里硅土柱净化,洗脱液浓缩并定容后,用气相色谱-质谱联用仪测定,外标法定量.方法的回收率范围为75.1%~99.8%,相对标准偏差为2.20%~8.78%.检出限均为20 μg/kg.该方法准确、灵敏度高,可用于粮谷中三环锡和苯丁锡残留的同时测定.
To establish a detection method for the determination of cyhexatin and fenbutatin pesticide residues in grains by GC-MS. The eyhexatin and fenbutatin in the test sample are extracted with acetonitrile, partitioned with n-Hexane saturated by acetonitrile. And then the extract is ethylated by ethyl magnesium bromide-diethyl ether solution, then cleaned up is performed on a florisil cartridge. The residues are determined by gas chromatography - mass spectrum after it is concentrated, quantificated by normalization method. The recoveries was 75.1%-99.8 %, the relative standard derivations (RSD) of pesticide residues was 2.20 %-8.78 %. The method limit of detection was 20 txg/kg. The method was a simple, sensitive assay for the grains inspection.
出处
《食品研究与开发》
CAS
北大核心
2013年第22期17-20,共4页
Food Research and Development
基金
国家质检总局科研项目(2013IK176)
山东检验检疫局科研项目(SK201353)
关键词
气相色谱-质谱联用
三环锡
苯丁锡
粮谷
gas chromatography-mass spectrometry(GC-MS )
cyhexatin
fenbutatin
grain