快速溶剂萃取-GC-MS/MS测定土壤中邻苯二甲酸酯类化合物

Determination of Phthalate Esters in Soil by ASE-GC-MS/MS

采用气相色谱和质谱联用法(GC-MS/MS),创建土壤中邻苯二甲酸酯类化合物的便捷有效测试方法,从而为沉积物和土壤中邻苯二甲酸酯类化合物在土壤中的残留测定提供一定参考。选择试样中的6种碳酸酯类化合物,经过正己烷和丙酮(1:1,V:V)的萃取,过PSA/Silica净化小柱,除水干燥浓缩后,经GC-MS/MS上机分析,定量结果采用外标方法。相关试验结果显示,这6种碳酸酯类化合物的测定回收效果较好,在84.6%~98.3%之间,实验室内精密度较高,相对标准偏差在2.7%~12%之间,检出限在0.2~0.8μg/kg之间,相关性R为0.9968~0.9995。该方法准确可靠、高效便捷、精密度高,具有显著节约人力和财力的特点,适宜于土壤中邻苯二甲酸酯类化合物的测定分析。

To provide reference for determining the residues of phthalate esters in soil and solids,we used the gas chromatography-tandem mass spectrometry(GC-MS/MS)to build the purified determination method of 6 phthalate esters in soil.The extract was determined for phthalate esters by acetone and n-hexane(1:1,V:V),PSA/Silica composite packing glass column,purification,drying and concentrating,and analyzed by GC-MS/MS with ASE,and external standard method was applied to quantitative analysis.The results of the 6 phthalate esters showed good linearity,with correlation coefficients(R)of 0.9968-0.9995.The recoveries of the 6 phthalate esters were 84.6%-98.3%,the detection limit of the method was 0.2-0.8μg/kg,and the relative standard deviation(n=6)was 2.7%-12%.This method is accurate,stable,simple,efficient and convenient,and it could save the cost and meet the test requirements of phthalate esters in soil.