微波辅助萃取-UPLC-MS/MS法测定纺织品中有机锡化合物

Determination of organotin compounds in textiles by ultra performance liquid chromatography tandem mass spectrometry with microwave-assisted extraction

建立了微波辅助萃取-UPLC-MS/MS同时检测纺织品中3种三取代有机锡化合物的方法。该方法以甲酸-甲醇(体积比5∶95)溶液为萃取溶剂,微波辅助萃取,流动相A为甲醇溶液,B为0.01 mol/L甲酸-甲酸胺(pH=3.0)缓冲盐溶液,梯度洗脱,采用串联质谱ESI正模式电离,选择反应监测(SRM)模式检测。结果表明,该方法能有效分离3种有机锡化合物,在选定的浓度范围内线性关系良好,线性相关系数均在0.9991以上,方法的检出限为0.005~0.010 mg/kg,三个水平的加标回收率为85.2%~98.8%,精密度为0.9%~6.2%(n=7)。方法前处理简单,免衍生化,适用于纺织品中有机锡化合物的检测分析。

A method of simultaneous determination of tri-substituted organotin compounds in textiles by ultra performance liquid chromatography trandem mass spectrometry with microwave-assisted extraction is developed.In this method,formicethanol(volume ratio 5∶95)solution is used as extraction solvent,microwaveassisted extraction is carried out,mobile phase A is methanol solution,mobile phase B is 0.01 mol/L formic acid-ammonium formate buffer salt solution(pH=3.0),gradient elution is performed,Electrospray ionization mass is operated in the positive mode(ESI+)using selected reaction monitoring(SRM).The results show that it can effectively separate the 3 kinds of organotin compounds.Organotin compounds represent good linearity in the selected concentration range,with correlation coefficients higher than 0.9991,the detection limits varies from 0.005 to 0.010 mg/kg,the average recoveries of three concentration levels are 85.2%to 98.8%,with RSD of 0.9%to 6.2%(n=7).The method is accurate,derivatization-free and suitable for the determination of organotin compounds in textiles.