DLLME-ESI-MS/MS快速筛查轻纺消费品中有机锡

Rapid screening of organotins in light and textile consuming products by DLLME-ESI-MS/MS

轻纺消费品水迁移相中有机锡离子,首先与二乙基二硫代甲酸钠(Na-DDTC)络合剂,在p H值3~7条件下,形成有机锡金属络合物,再以四氯乙烯为萃取剂,丙酮为分散剂,建立了基于分散液液微萃取(DLLME)结合电喷雾-串联质谱仪(ESI-MS/MS)直接筛查八种有机锡[一甲基锡(Me T)、一丁基锡(Bu T)、二丁基锡(DBT)、三正丁基锡(TBT)、一正辛基锡(MOT)、二苯基锡(DPh T)、二辛基锡(DOT)和三苯基锡(TPh T)]的检测方法,整个分析过程不超过5 min。重点考察了不同种类有机锡离子与DDTC络合产物的特征规律,确定ESIMS/MS条件下产物的分子离子峰和特征子离子峰;再对影响DLLME萃取效率的因素进行优化,平均富集倍数达到100倍。采用外标法定量,在0.1~2.0 mg/L有机锡离子质量浓度范围内的线性相关系数均高于0.95,精密度(RSD,n=7)为10.5%~19.3%。DLLME-ESI-MS/MS方法简便,速度快,灵敏度高,定性准确,适用于轻纺消费品中有机锡化合物的快速筛查分析。

A rapid screening method, dispersive liquid-liquid micro-extraction （DLLME） and electrospraytandem mass spectrometry （ESI-MS/MS） has been established for determination of eight organotins [Methyltin （MET）, Butyltin （BUT）, Dibutyltin （DBT）, Tributyltin （TBT）, Monooctyltin （MOT）, Dioctyltin （DOT）, Diphenyltin （DPhT）, Triphenyltin （TPhT）] in aqueous solution from light and textile consuming products. The analytical process can be done in 5 minutes. The characteristics of different kinds of organic tin ions and DDTC complex products are investigated, and the molecular ion peaks and characteristic ion peaks of ESI-MS/MS are determined. The experimental parameters affecting extraction recover- ies of organotin compounds by DLLME are optimized, and the average enrichment factor is 100. Using external standard method, the results show that the linearity range is O. IN2.0 mg/L, the linearity correlation coefficient is above 0.95; the relative standard deviation （RSD, n=7） is 10.5%N19.3%. The method of DLLME-ESI-MS/MS is simple, rapid, sensitive and accurate, and it is suitable for rapid screening analysis of organotin compounds in light and textile consuming products.