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《化学分析计量》 2021年第03期
DOI:10.3969/j.issn.1008-6145.2021.03.011
快速溶剂萃取-气相色谱-质谱法同时测定土壤中多环芳烃、六六六和滴滴涕
岳中慧,吴亮,张皓
核工业二三0 研究所分析测试中心,长沙 410000 
Simultaneous determination of PAHs, BHC and DDT in soil by using accelerated solvent extraction and GC-MS
Yue Zhonghui, Wu Liang, Zhang Hao
No. 230 Research Institute of Nuclear Industry Analysis and Testing Center, Changsha 410000, China 
摘要:建立快速溶剂萃取-气相色谱-质谱法同时测定土壤中多环芳烃、六六六和滴滴涕。优化了提取溶剂 和洗脱溶剂,采用加速溶剂萃取法处理土壤样品,萃取溶剂为二氯甲烷-正己烷(1∶1)。提取液用氮吹仪浓缩、硅酸镁固相萃取小柱净化,用二氯甲烷-正己烷(3∶7)混合溶剂对固相萃取小柱进行活化和洗脱,流出液净化后氮吹浓缩至1 mL,利用气相色谱-质谱内标法进行分析定量。16 种多环芳烃、8 种有机氯农药及3 种替代物在5.0~500 μg/L 范围内线性良好,方法检出限为0.000 55~0.000 77 mg/kg,加标回收率为68.2%~112.7%,相对标准偏差为4.3%~10.1%(n=5)。该方法可用于同时测定土壤中多环芳烃、六六六、滴滴涕的含量。 
Abstract:A method of accelerated solvent extraction and GC-MS for the simultaneous determination of PAHs, BHC and DDT in soil was established. The extraction solvent and elution solvent were optimized, accelerated solvent extraction was used to extract soil sample, and the extraction solvent was dichloromethane-n-hexane(1∶1). The collected extraction liquid was concentrated by nitrogen blowing instrument, purified with magnesium silicate solid phase extraction column, and then, the magnesium silicate solid phase extraction column was activated and eluted with dichloromethane-n-hexane (3∶7). The purified effluent liquid concentrated to 1 mL, and analyzed by GC-MS after adding internal standard. 16 kinds of PAHs, 8 kinds of OCPs and 3 kinds of substitutes showed good linearity in the range of 5.0-500 μg/L. The detection limit of the method was 0.000 55-0.000 77 mg/kg, the recovery of standard addition was 68.2%-112.7%, and the relative standard deviation was 4.3%-10.1%(n=5). The method can be used to simultaneously determine the content of PAHs, BHC and DDT in soil. 
关键词:多环芳烃;六六六;滴滴涕;快速溶剂萃取;气相色谱-质谱法 
Keywords:polycyclic aromatic hydrocarbons; benzene hexachloride; dichlorodiphenyl trichloroethane; accelerated solvent extraction; gas chromatography-mass spectrometry 
本文引用格式:
岳中慧,吴亮,张皓. 快速溶剂萃取- 气相色谱- 质谱法同时测定土壤中多环芳烃、六六六和滴滴涕[J]. 化学分析计量,2021,30(3):49. 

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