固相萃取-气相色谱/质谱法检测纺织品中的邻苯二甲酸酯

摘要

A method was developed by solid phase extraction (SPE)-gas chromatography (GC)/mass (MS) to solve the difficult problem of PAEs enrichment in textile.The best solid phase extraction column was selected by comparing the extraction results of 3 different kinds of solid phase extraction agents,and then the main factors affecting the extraction efficiency were discussed.The result showed that the optimum extraction conditions were as follows:the C18 was selected as the solid phase extraction column,the 5 mL methanol activation,the sample flow rate 1 mL/min,the ethyl acetate elution of 5 mL,and the elution rate 3 mL/min.This method has a good linear relationship,and the correlation coefficient is 0.997 8～ 0.999 7.The recoveries of spiked samples ranged from 86.3％ to 101.9％,and the relative standard deviations were less than 4％.The detection limit of the method was 1 ～ 3 μg/L.This method is effective and convenient to detect trace amounts of phthalate esters in textiles.%针对纺织品中邻苯二甲酸酯类(PAEs)环境激素富集困难的问题,建立了固相萃取-气相色谱/质谱法测定纺织品中PAEs的方法.通过比较3种性质不同固相萃取剂的萃取效果,筛选最优固相萃取柱,再探讨影响萃取效果的主要因素.结果表明,最优萃取条件为:选取C18为固相萃取柱,5 mL甲醇活化,上样流速1 mL/min,5 mL的乙酸乙酯洗脱,洗脱速率3 mL/min.该方法线性关系良好,相关系数为0.997 8～0.999 7,样品的加标回收率为86.3％～ 101.9％,含量检测的相对标准偏差小于4％,方法的检出限为1～3μg/L.对实际样品检测结果表明,该方法能够有效、便捷地检测出纺织品中痕量的邻苯二甲酸酯类物质.