论文部分内容阅读
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20μg/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。
A gas chromatography-mass spectrometry (GC-MS) method was developed for the simultaneous determination of tricyclic tin and dibenzyl tin in grain. The tricyclotine and benzidine in the sample were extracted with acetonitrile, and saturated with n-hexane, then liquid-liquid was partitioned. After derivatization with ethyl magnesium bromide-diethyl ether, the residue was purified by Florisil column and the eluate was concentrated After the volume was determined by gas chromatography - mass spectrometry, external standard method. The recoveries ranged from 75.1% to 99.8% with relative standard deviations from 2.20% to 8.78%. Detection limits were 20μg / kg. The method is accurate and sensitive and can be used for the simultaneous determination of tricyclotine and phenyltin residues in grain.