气相色谱-串联质谱法测定土壤中的邻苯二甲酸酯

建立了土壤中6种邻苯二甲酸酯的气相色谱-串联质谱(GC-MS/MS)分析方法。土壤样品用超声提取,以二氯甲烷-丙酮(1:1, v/v)混合溶液为提取溶剂,提取液经Florisil小柱净化后,经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,利用MS/MS的多反应监测(MRM)模式进行定性和定量。结果表明本方法可对样品中的邻苯二甲酸酯进行分析,在10～1000 μg/L质量浓度范围内,线性关系良好,相关系数为0.9973～0.9976;6种邻苯二甲酸酯的相对标准偏差(RSD)不大于14.3%, 2 μg/kg和10 μg/kg两个加标水平的回收率为72.9%～106.2%; 6种目标化合物的检出限为0.1～0.5 μg/kg。该方法快速准确、背景干扰较少、分析灵敏度较高,适用于土壤样品中邻苯二甲酸酯的分析。

Determination of phthalic acid esters in soil by gas chromatography-tandem mass spectrometry

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the determination of phthalic acid esters (PAEs) in soil. The soil sample was extracted by dichloromethane-acetone (1: 1, v/v) with an ultrasonic instrument, and the extract was cleaned up with a Florisil column. The identification and quantification of the analytes were carried out in the multiple reaction monitoring (MRM) mode after the GC separation on an HP-5MS column (30 m x 0.25 mm x 0.25 microm). The eight point calibration curves showed a good linearity for all the congeners (0.997 3 - 0.997 6). The limits of detection (LODs) ranged from 0.1 to 0.5 microg/kg. The relative standard deviations (RSDs) were not more than 14.3% and the spiked recoveries were in the range of 72.9% - 106.2%. The developed analytical method is rapid and accurate, and suitable for the determination of PAEs in soil.