唐会智, 宋冬梅. 加速溶剂萃取-QuEChERS-气相色谱质谱联用法测定土壤中增塑剂[J]. 分析测试技术与仪器, 2023, 29(1): 105-110. DOI: 10.16495/j.1006-3757.2023.01.016
引用本文: 唐会智, 宋冬梅. 加速溶剂萃取-QuEChERS-气相色谱质谱联用法测定土壤中增塑剂[J]. 分析测试技术与仪器, 2023, 29(1): 105-110. DOI: 10.16495/j.1006-3757.2023.01.016
TANG Huizhi, SONG Dongmei. Detection of Plasticizers in Soil by Accelerated Solvent Extraction-QuEChERS-Gas Chromatography/Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 105-110. DOI: 10.16495/j.1006-3757.2023.01.016
Citation: TANG Huizhi, SONG Dongmei. Detection of Plasticizers in Soil by Accelerated Solvent Extraction-QuEChERS-Gas Chromatography/Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 105-110. DOI: 10.16495/j.1006-3757.2023.01.016

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

  • 摘要: 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.

     

    Abstract: 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.

     

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