加速溶剂萃取-QuEChERS-气相色谱质谱联用法测定土壤中增塑剂

Detection of Plasticizers in Soil by Accelerated Solvent Extraction-QuEChERS-Gas Chromatography/Mass Spectrometry

建立加速溶剂萃取-QuEChERS-气相色谱质谱联用法对土壤样品中17种增塑剂进行检测.土壤样品以正己烷饱和乙腈萃取,经25 mg乙二胺-N-丙基硅烷和25 mg硅胶净化,气相色谱质谱联用法选择离子监测(SIM)模式下检测,以外标法进行定量分析.17种增塑剂在0.01~2 mg/L质量浓度内线性关系良好,各化合物相关系数均在0.999以上.方法的检出限在0.01~0.05 mg/kg之间,定量限在0.03~0.15 mg/kg之间,17种增塑剂在0.5、1.0、5.0 mg/kg添加水平下,加标回收率和精密度分别为72.8%~116.2%和1.73%~6.15%.方法简易便捷、灵敏度和准确度高,适合于检测土壤中17种增塑剂.

A method for the detection of 17 plasticizers in soil samples by the accelerated solvent extraction(ASE)-QuEChERS-gas chromatography/mass spectrometry(GC/MS)has been established.The soil samples were extracted with hexane saturated acetonitrile,and purified by 25 mg PSA(primary secondary amine)and 25 mg Silica.GC/MS was used for the detection in the selected ion monitoring(SIM)mode,and the matrix-matched external standard calibration curves were used for the quantitative analysis.The standard solution of 17 plasticizers showed a good linearity in the concentration range of 0.01 to 2 mg/L,and the correlation coefficient(r)were above 0.999.The limit of detection was between 0.01 and 0.05 mg/kg,and the limit of quantitation was between 0.03 and 0.15 mg/kg.The spiked recoveries and precisions of 17 plasticizers were ranged from 72.8%to 116.2%and 1.73%to 6.15%at the three spiked concentration levels(0.5,1.0,5.0 mg/kg),respectively.The method is simple,convenient,sensitive and accurate,and is suitable for the detection of 17 plasticizers in soil.