气相色谱-质谱联用法测定土壤中邻苯二甲酸酯类增塑剂

Determination of Phthalate Ester Plasticizer in Soils by Gas Chromatography-Mass Spectrometry

应用加速溶剂萃取,气相色谱-质谱联用法测定土壤中6种邻苯二甲酸酯类有机污染物。对邻苯二甲酸酯类污染物的提取溶剂进行了优化选择,确定二氯甲烷作为最佳提取溶剂。对色谱柱升温程序进行了优化,以使两个出峰时间较接近的目标物邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)能够达到基线分离。方法标准曲线的线性范围为0.50～20.0mg/L,线性相关系数均大于0.9970,方法检出限为67μg/kg,加标回收率为81.9%～111.4%。方法检出限较低,精密度好,简便快速,可满足大批量样品分析对质量和进度的要求。

A method for the determination of 6 phthalate esters （PAEs） by gas chromatography-mass spectrometry （GC-MS） with accelerated solvent extraction （ASE） sample preparation was developed.Methylene chloride was selected as the optimum extraction solvent through the experiments and the programmed temperature condition of the chromatograph column was optimized in order to obtain the baseline separation between adjacent spectra from the targets of dimethyl （o-） phthalate （DMP） and diethyl （o-） phthalate（DEP）.The linear range of the calibration curve was from 0.50 to 20 mg/L with correlation coefficient 0.997.The detection limit of the method for the PAEs was 0.067 mg/L and the recoveries were 81.9% ～ 111.4%.The method provides the advantages of low detection limits,good precision,high efficiency and is suitable for routine analysis of PAEs in soil samples.