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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%。
A method for determination of 12 phenolic compounds residues in solid wastes by gas chromatography-mass spectrometry was proposed. The sample was extracted with an acetone-dichloromethane (2 + 3) mixture and extracted with an accelerated solvent extractor. The sample was concentrated to 1 mL on a KD concentrator and purified on a silica gel column with acetone-dichloromethane +9) mixture, and then concentrated to 1 mL by KD, separated by HP-5 MS quartz capillary column (30 m × 0.25 mm, 0.25 μm) and selected by ion bombardment ion mass spectrometry. The detection limits (3S / N) of the 12 phenolic compounds ranged from 9.60 to 18.5 μg.kg-1. The blank soil samples were taken as the base for recovery test. The recoveries were between 74.7% and 108.4%. The relative standard deviations (n = 7) of the measured values were less than 7.5%.