加速溶剂萃取-气相色谱-质谱法测定固体废物中酚类化合物

GC-MS Determination of Phenols in Solid Wastes with Accelerated Solvent Extraction of Sample

提出了气相色谱-质谱法测定固体废物中12种酚类化合物残留量的方法。样品以丙酮-二氯甲烷(2+3)混合液为萃取剂,经加速溶剂萃取仪提取后,在K-D浓缩装置上浓缩至1 mL,经硅胶柱净化后,用丙酮-二氯甲烷(1+9)混合液淋洗后再经K-D浓缩至1 mL,通过HP-5 MS石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,采用电子轰击离子源选择离子监测模式进行质谱测定。12种酚类化合物的检出限(3S/N)在9.60～18.5μg.kg-1之间。以空白土壤样品为基体进行回收试验,测得回收率在74.7%～108.4%之间,测定值的相对标准偏差(n=7)均小于7.5%。

GCMS was applied to the determination of residual amounts of 12 phenols in solid wastes. Sample was extracted with a mixture of acetone and dichloromethane （2＋ 3） by accelerated solvent extraction, and the extract was concentrated to 1 mL by K-D concentrator and purified on silica-gel column. The 12 phenols were eluted from the silica-gel column with mixture of acetone and dichloromethane （1＋ 9）, and concentrated to 1 mL, which was used for GCMS analysis. HP-5MS （30 m × 0. 25 mm, 0. 25/2μm） quartz capillary chromatographic column was used for separation, and the selected ion monitoring （SIM） with electron impact ionization source was adopted in MS. Values of detection limit of 12 phenols were found in the range of 9. 60-18. 5 μg.kg^-1. On the base of blank sample of soil, test for recovery was made by standard addition method, values of recovery found were in the range of 74. 7%-108. 4%, with RSD＇s （n=7） less than 7. 50%.