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建立了一种可同时测定聚氯乙烯(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。利用三水合二乙基二硫代氨基甲酸钠(NaDDTC)与有机锡的螯合作用,以甲醇-NaDDTC水溶液(2%,m/v)的混合溶液浸取PVC样品中的有机锡,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。对样品前处理过程、衍生化条件、色谱条件等进行了优化,并考察了方法的线性关系、检出限、回收率和精密度等。方法的线性范围为0.1～50.0 mg/L,线性相关系数为0.999 0～0.999 8。有机锡化合物的检出限为0.005～0.025 mg/L,样品加标回收率为87.64%～110.16%,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制品中微量有机锡的测定。
A GC-MS method was developed for the simultaneous determination of seven organotin compounds, such as monobutyltin, dibutyltin, tributyltin, tetrabutyltin, monooctyltin, diphenyltin and triphenyltin in polyvinyl chloride (PVC) Mass spectrometry (GC-MS) detection method. The organotin in PVC samples was extracted by the chelating action of NaDDTC and organic tin and the mixed solution of methanol-NaDDTC aqueous solution (2%, m / v) NaBEt4 aqueous solution was derivatized with n-hexane extraction and separation, followed by qualitative and quantitative analysis of GC-MS. The sample pretreatment, derivatization conditions and chromatographic conditions were optimized. The linear relationship, detection limit, recovery and precision of the method were also investigated. The linear range of the method is 0.1 ~ 50.0 mg / L, and the linear correlation coefficient is 0.999 0 ~ 0.999 8. The detection limits of organotin compounds ranged from 0.005 to 0.025 mg / L. The recoveries of spiked samples ranged from 87.64% to 110.16% with relative standard deviations less than 10%. The results show that the method is simple, sensitive and can be applied to the determination of trace organotin in PVC products.