超临界CO_2萃取/气相色谱-质谱联用测定纺织品中邻苯二甲酸酯

Determination of the phthalate in textiles by SFE CO_2/GC-MS

采用超临界CO_2萃取技术(SFE-CO_2)从纺织品中萃取了邻苯二甲酸酯类增塑剂。探讨了不同萃取条件(萃取压力、萃取温度、萃取时间、共溶剂种类、收集溶剂种类)对邻苯二甲酸酯萃取率的影响,建立了超临界CO_2流体萃取/气相色谱-质谱联用(SFE-CO_2/GC-M S)法测定纺织品中13种邻苯二甲酸酯的检测方法。研究表明:采用正己烷为共溶剂和接收剂,萃取温度60℃、压力35 M Pa,萃取时间60 min的条件最佳,萃取物经GC-M S测定,邻苯二甲酸二异癸酯在10~1000μg/m L范围内线性关系良好,其余12种邻苯二甲酸酯在1~500μg/m L范围内线性关系良好,相关系数为0.9917~0.9994,加标回收率在80.0%~117.2%之间,RSD在1.1%~7.2%之间。

The phthalate in textiles was extracted by means of supercritical CO2 extraction technology （SFE-CO2）. The effects of different extraction conditions （the pressure, temperature and time of extraction, the variety of co-solvent and trapping solvent） on the extraction yield of the phthalate were discussed. A method was established for the determination of thirteen phthalate in textiles by using supercritical CO2 fluid extraction and gas chromatography （SFE CO2/GC-MS）. The results showed the optimum extraction conditions wereas following： both co-solvent and trapping solvent were n-hexane, respectively, the temperature was 60℃, the pressure was 35 MPa, the dynamic extraction time was 60 min. The calibration eurveof Di-iso-decylphthalate （DIDP） was linear in the range of 10 ~ 1000 μg/mL, and 1 ~ 500 μg/mL for the others 12 kinds of PAEs, with correlation coefficients of 0. 9917-0. 9994. The average recoveries of target compounds in sample were in the range of 80.0% - 117.2% , and the relative standard deviations were between 1.1% and 7.2%.