阳离子固相萃取-超高效液相色谱-串联质谱法测定皮革制品中的4种三取代有机锡化合物

建立了超高效液相色谱-串联质谱测定皮革制品中三丁基锡、三苯基锡、双-三苯基锡氧化物、三环锡等4种三取代有机锡化合物(TOT)的方法。采用盐酸溶液提取皮革制品中的有机锡化合物,使其呈阳离子态,经阳离子固相萃取净化,有机锡化合物在超高效C18色谱柱中完成分离,在正离子模式下采用多反应监测模式进行串联质谱测定。三丁基锡、三苯基锡、双-三苯基锡氧化物(以三苯基锡计)的定量限为10 μg/kg,三环锡的定量限为20 μg/kg;分别添加4种待测物于空白皮革样品中,加标回收率为54.1%～101.4%,相对标准偏差为4.3%～9.8%。实验结果表明,该方法简单、灵敏、准确,各项技术指标均满足国内外法规的要求,可用于皮革制品中4种三取代有机锡化合物残留的确证检测。

Determination of four triorganotin residues in leather products by ultra performance liquid chromatography-tandem mass spectrometry and cation solid-phase extraction

A confirmative method was developed for the determination of four triorganotins (TOTs) included tributyltin (TBT), triphenyltin (TPhT), di-triphenyltin oxide (DTPhT), and cyhexatin (CYT) in leather products by cation solid-phase extraction (SPE) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The organotin residues were extracted with HCl solution. The ionized compounds were purified with SPE. The reconstituted sample solution was analyzed by UPLC-MS/MS in positive ion electrospray and multi-reaction monitor (MRM) mode, with a UPLC C18 column as the separation column. The limits of quantification were 10 μg/kg for TBT, TPhT, DTPhT (calculated as TPhT) and 20 μg/kg for CYT. The method was validated at three levels for each compound. The recoveries were from 54.1% to 101.4%, and the relative standard deviations (RSD) were between 4.3% and 9.8%. The method is simple, reliable and accurate. It can meet the requirements of the domestic and international legislations. The method adapts to simultaneously confirm the residues of the four TOTs in leather products.