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建立了1种高效测定聚氯乙烯(PVC)塑料制品中一丁基锡、二丁基锡、三丁基锡、四丁基锡、一辛基锡、二苯基锡和三苯基锡等7种有机锡化合物的气相色谱-质谱(GC-MS)检测方法。以四氢呋喃盐酸溶液溶解PVC样品,超声提取其中的微量有机锡,经四乙基硼酸钠(NaBEt4)水溶液衍生化后,用正己烷萃取分离,再进行GC-MS的定性定量分析。对样品前处理、衍生化条件等进行优化,并考察了方法的线性关系、检出限和精密度等。对实际PVC样品进行测定,检出3种丁基锡,样品加标回收率为84.14%～111.71%,相对标准偏差皆小于10%。结果表明:该法简便、灵敏,能很好地应用于PVC制品中有机锡的测定。
A high performance liquid chromatography-mass spectrometry (GC-MS) method was developed for the determination of seven organotin compounds, such as monobutyltin, dibutyltin, tributyltin, tetrabutyltin, monooctyltin, diphenyltin and triphenyltin in polyvinyl chloride (PVC) (GC-MS) detection method. The samples were dissolved in tetrahydrofuran and hydrochloric acid, and the trace organotin was extracted by sonication. After derivatization with sodium tetraethylborate (NaBEt4), the mixture was extracted with n-hexane and then qualitatively and quantitatively analyzed by GC-MS. The sample pretreatment, derivatization conditions were optimized, and the linear relationship between the method, the detection limit and precision and so on. The actual PVC samples were tested, and three kinds of butyl tin were detected. The recoveries of spiked samples were 84.14% ~ 111.71% with relative standard deviations less than 10%. The results show that this method is simple, sensitive and can be applied to the determination of organotin in PVC products.