建立了气相色谱-质谱法(GC-MS)测定南疆特色林果土壤中22种邻苯二甲酸酯类化合物残留的分析方法。样品经超声提取,离心分离,Al2O3小柱净化,进气相色谱-质谱检测。在该条件下,采用内标法定量,EI模式下,22种邻苯二甲酸酯在0.05~5mg/L范围内呈现良好的线性,检测限为0.4~10μg/kg,回收率为78.5%~108.2%。经过对南疆三个林果区的90个土壤样品分析,得出最主要的邻苯二甲酸酯类污染物为邻苯二甲酸二异丁酯,邻苯二甲酸二丁酯和邻苯二甲酸(2-乙基己)酯,部分达到了严重污染。所建立的方法准确度高,灵敏度好,适合土壤样品中邻苯二甲酸酯类物质的测定。
A gas chromatography-mass spectrometry(GC-MS)based method for simultaneous determination of 22 kinds of phthalates in Southern Xinjiang characteristic soils was developed.The samples were extracted by ultrasonic assisted extraction,separated by centrifuge and then purified by alumina column.Under the EI mode,pyrimethanil was selected as the internal standard.The method has good linearity in the range of 0.05-5mg/L,the limit of detection(LOD)was 0.4-10μg/kg.The average recovery were between 78.5%-108.2%.Accoding to the analysis of 90 soil samples,it was found that the most serious soil pollutants were DIBP,DBP and DEHP.The analytical method in the present study has been well validated by systematically searching for satisfactory conditions using experimental designs including precision,repeatability and spiked recovery.It is suitable for analysis of phthalates in soils.