DLLME-GC-MS法测定纺织品中的痕量锡

Determination of trace tin in textiles by DLLME-GC-MS method

基于纺织品水迁移相中有机锡离子首先与四乙基硼化钠生成有机锡化合物，再以四氯乙烯为萃取剂，乙腈为分散剂，建立了分散液液微萃取（DLLME）结合气相色谱-质谱（GC—MS）测定十种有机锡含量的新方法。对影响DLLME萃取效率的因素进行优化试验，萃取条件为：50曲四氯乙烯为萃取剂，0．5mL乙腈为分散剂，超声萃取0．5min，以3000r／min离心3min，取萃取溶液1．0μL直接进行GC-MS分析。该方法线性范围为0．005—1mg／L，线性相关系数（R2）为0．9926—0．9995，检出限为0．1—0．5μg／L，平均回收率为82．6％-113．5％，相对标准偏差为5．45％～13．56％，平均富集倍数达到140。

A new method, dispersive liquid-liquid micro-extraction （DLLME） and gas chromatography-mass spectrometry （GC-MS） has been established for the determination of ten organotins [ Methyltin （ MeT）, Butyltin （ BuT）, Dibutyltin （ DBT）, Tributyltin （TBT）, Tetrabutyltin （TeBT）, Monooctyltin （MOT）, Dioctyltin （DOT）, Dipropyltin （DProT）, Diphenyltin （DPhT）, Triphenyltin （TPhT） ] in aqueous solution from textile products. In this method, the aqueous organotins are derivatized with sodium tetraethylborate firstly, and then extracted by dispersive liquid-liquid micro-extraction with tetrachloroethylene as an extraction solvent and acetonitrile as a dispersing solvent. The experimental parameters exerting influence on extraction recoveries of organotin compounds by DLLME are optimized. The results show that the linearity range is 0. 005 -1 mg/L, the linearity correlation coefficient Re is 0. 992 6 -0. 999 5, the relative standard deviation is 5.45 % N 13.56 %, the average recovery rate is 82.6% -113.5%, the method detection limit is 0. 1 -0.5 μg/L, and the average enrichment factor is 140. This method is suitable for determination of trace ten aqueous organotins in textile products.