SPE-UPLC-MS/MS测定纺织品中8种有机磷酸酯阻燃剂

摘要

建立了固相萃取-超高效液相-串联质谱联用法(SPE-UPLC-MS/MS)同时测定纺织品中8种有机磷酸酯阻燃剂(OPEs)的分析方法.样品用甲醇超声提取30min后,经弗罗里硅土固相萃取小柱净化后,采用Aglient Eclipse Plus C18色谱柱(3.0×100mm,1.8μm),5mmol/mL乙酸铵水溶液(0.1%的甲酸水溶液)-乙腈作为流动相梯度洗脱电喷雾正离子(ESI+)模式离子化,选择多反应检测(MRM)方式监测,串联质谱测定,外标法定量.结果显示,各目标物方法检出限在0.003~0.500mg/kg,相关系数≥0.9991,回收率为81.7%~93.5%,RSD%为1.5%~3.4%.结果表明,本方法满足测定纺织品中有机磷酸酯阻燃剂的需要.%Analytes in textile samples were extracted with methanol by ultrasonic extraction for 30 min, then were purified by solid phase extraction (SPE) using florisil cartridges.The separation was performed on an Aglient Eclipse Plus C18 (3.0×100mm,1.8μm) column with a gradient mobile mixture composed of 5mmol/mL ammonium acetate solution containing 0.1% formic acid and acetonitrile, and the electrospray ionization(ESI)source in positive ion mode was used for the analysis in the multiple reaction monitoring(MRM), then tandem MS was used for the measurement, and the external standard method was used for the quantification.The measurement results showed that the detection limit was in the range of 0.003-0.500mg/kg, and the correlation coefficient was ≥0.9991.The average recovery rates of eight OPEs were 81.7%-93.5% with relative standard deviation (RSD%) of 1.5%-3.4%.The method can be used for the determination of OPEs in textile.