基于四通道色谱分离仪净化-GC-MS法测定土壤中邻苯二甲酸酯类残留

Determination of phthalate acid esters in soil by GC-MS based on four-channel purification chromatograph

建立了四通道色谱分离仪净化-气相色谱-质谱（GC-MS）法同时检测土壤中6种邻苯二甲酸酯（PAEs）类化合物的分析方法。样品经正己烷-丙酮（1：1,V：V）超声提取、四通道色谱分离仪净化（以正己烷-丙酮（1：1,V：V）洗脱）、GC-MS选择SIM模式测定。结果表明：6种PAEs类化合物在0.02-10 mg/L范围内定量离子的峰面积与质量浓度具有良好的线性关系（r〉0.9988）,仪器检出限（LOD）为0.51-3.52μg/L,在3个浓度水平的加标回收率为83.7%-108.8%,相对标准偏差（RSD）为3.4%-11%。该方法可满足土壤中邻苯二甲酸酯类残留物的分析检测。

A method for the simultaneous determination of six phthalate acid esters （PAEs） in soil by gas chromatography-mass spectrometry （GC-MS）based on four-channel purification chromatograph was established and evaluated. The soil samples were extracted by the method of ultrasonic extraction with hexane-acetone （ 1 ： 1,V： V）and purified by an instrument called four-channel purification chromatography. The eluent were determined by GC-MS in SIM mode . The results indicated the calibration curves of 6 PAEs had a good linear relationshipat the concentration from 0. 02 to 10 mg/L. The correlation coefficients（r） were larger than 0. 9988. The detection of limits （LODs）were 0. 51 - 3.52μg/L. The recoveries at three concentration levels were 83.7% - 108.8% and the relative standard deviations （RSDs） were 3.4% - 11%. The method is very quick, convenient, and easy to operate, with high repeatability and strong practicability. This method is suitable for the determination of PAEs in soil.