凝胶过滤色谱-串联质谱法测定纺织品中的烷基酚聚氧乙烯醚

建立了纺织品中烷基酚聚氧乙烯醚的凝胶过滤色谱-串联质谱(GFC-MS/MS)分析方法。纺织品样品采用加速溶剂萃取法,以无水乙醇为提取溶剂进行提取,提取液经Sep-Pak Carbon/NH2石墨化碳黑/氨基复合型固相萃取柱净化。烷基酚聚氧乙烯醚经Shodex MSpak GF-310 2D色谱柱(150×2.0 mm)分离后,在多反应监测(MRM)模式下进行串联质谱定性及定量分析。方法对壬基酚聚氧乙烯醚(NPnEO)和辛基酚聚氧乙烯醚(OPnEO)的定量限均为0.2 mg/kg,在0.2～5 mg/kg的3个添加水平范围内,NPnEO的平均回收率为84.2%～93.5%,相对标准偏差(RSD)为3.9%～7.5%;OPnEO的平均回收率为85.5%～96.1%,RSD为3.4%～8.1%。该方法能够满足纺织品中烷基酚聚氧乙烯醚的检测要求。

Determination of Alkylphenol Ethoxylates in Textiles by GelFiltration Chromatography-Tandem Mass Spectrometry

A comprehensive analytical method based on gel filtration chromatography-tandem quadrupole mass spectrometry has been developed for the determination of alkylphenol ethoxylates in textiles.The textile samples were extracted with ethanol by accelerated solvent extraction method.The extract was cleaned by a Sep-Pak Carbon/NH2 solid phase extraction cartridge.Qualitative and quantitative analyses were carried out for alkylphenol ethoxylates under the multiple reaction monitoring(MRM) mode after the chromatographic separation on Shodex MSpak GF-310 2D column(150×2.0 mm).The limits of quantitation(LOQs) for nonylphenol ethoxylates and octylphenol ethoxylates were 0.2 mg/kg.At the spiked levels of 0.2~5 mg/kg,the mean recoveries for nonylphenol ethoxylates were 84.2%~93.5% with the relative standard deviations(RSDs) of 3.9%~7.5%,and the mean recoveries for octylphenol ethoxylates were 85.5%~96.1% with the relative standard deviations(RSDs) of 3.4%~8.1%.The method is suitable for the determination of alkylphenol ethoxylates in textiles.