固相萃取-气相色谱/质谱法检测纺织品中的邻苯二甲酸酯

Determination of phthalic esters in textiles by solid phase extraction-gas chromatography/mass spectrom

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 m L甲醇活化,上样流速1 m L/min,5 m L的乙酸乙酯洗脱,洗脱速率3 m L/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。

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 （μL. This method is effective and convenient to detect trace amounts of phthalate esters in textiles.