Determination of seven phenols in soil by gas chromatography-mass spectrometry after ultrasonic extraction
HU Zu-guo1,CAO Ban2,LI Zi-yi3
1. Hangzhou Iron&Steel Group Company Technology Center,Hangzhou 310022,China; 2. Zhejiang Institute of Geological & Mineral Resources,Hangzhou 310007,China; 3. China University of Geosciences,Wuhan 430074,China
Abstract：The content of phenols in soil was low. Moreover, their chemical properties were active. As a result, the extraction and analysis of phenols in soil were relatively difficult. The organic components in soil were extracted by ultrasonic for 20 min using dichloromethane and n-hexane (V/V=2) as mixed solvent. The strongly alkaline aqueous solution (pH>12) was added into extracting solution. The phenols could react with alkali to form corresponding water-soluble slats due to the weak acidity of phenolic hydroxyl groups. Therefore, the phenols could be separated from the organic phase. The dichloromethane and n-hexane (V/V=2) mixed solvent was added into water phase after separation for purification. The interference organic components in alkaline aqueous solution were further removed. Then, the solution was adjusted to acid (pH<3). The phenolic compounds were extracted with dichloromethane/n-hexane (V/V=4) mixed solvent. Finally, seven types of phenols (including phenol, 2-chlorophenol, 2-nitrophenol, 2,4-dimethylolphenol, 2,4-dichlorophen, 4-chlor-3-methylolphenol and 2,4,6-trichlorophenol) in sample were determined by gas chromatography-mass spectrometry (GC-MS). The detection limit of method was 0.03-0.48 mg/kg. The proposed method was applied to the detection of seven phenols in actual samples. The relative standard deviations (RSD,n=7) were between 1.6% and 7.9%, and the recoveries were between 82% and 111%.
胡祖国,曹攽,李紫艺. 超声波萃取—气相色谱-质谱法测定土壤中7种酚类化合物[J]. 冶金分析, 2016, 36(2): 27-32.
HU Zu-guo,CAO Ban,LI Zi-yi. Determination of seven phenols in soil by gas chromatography-mass spectrometry after ultrasonic extraction. , 2016, 36(2): 27-32.
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