加速溶剂-固相萃取-高效液相色谱法测定土壤及蚯蚓样品中多环芳烃  

An Accelerated Solvent Extraction-Solid Phase Extraction-High Performance Liquid Chromatographic Method for Determination of Polycyclic Aromatic Hydrocarbons in Soil and Earthworm Samples

作　　者：张亚楠[1,2] 杨兴伦[1] 卞永荣[1] 谷成刚[1] 王代长[3] 蒋新[1] ZHANG Ya-Nan YANG Xing-Lun BIAN Yong-Rong GU Cheng-Gang WANG Dai-Zhang JIANG Xin(Key Laboratory of Soil Environment and Pollution Remediation, Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210008, China University of Chinese Academy of Sciences, Beijing 100049, China College of Resources and Environment, Henan Agricultural University, Zhengzhou 450002, China)

机构地区：[1]中国科学院土壤环境与污染修复重点实验室,南京210008 [2]中国科学院大学,北京100049 [3]河南农业大学资源与环境学院,郑州450002

出　　处：《分析化学》2016年第10期1514-1520,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.41271327;41271464;21377138);中国科学院南京土壤研究所一三五领域前沿项目(Nos.ISSASIP1621;ISSASIP1618)资助~~

摘　　要：研究了加速溶剂萃取（ASE）、固相萃取柱净化（SPE）、高效液相色谱（HPLC）联合（ASE-SPE-HPLC）测定土壤及蚯蚓样品中7种多环芳烃（PAHs）的分析方法,确定了以正己烷-丙酮（4∶1,V/V）作为萃取剂,用ASE对土壤及蚯蚓进行萃取,提取液经SPE柱净化（土壤样品用硅胶柱净化,蚯蚓样品用Al_2O_3-硅胶柱净化）,正己烷-二氯甲烷（9∶1,V/V）进行洗脱,洗脱体积为10 m L,旋转浓缩蒸干后,乙腈定容,过0.22μm有机滤膜,最后用HPLC对提取液中7种PAHs进行定量的分析方法。土壤样品方法回收率在83.5%~110.2%之间,相对标准偏差为1.0%~4.6%;蚯蚓样品回收率在81.2%~97.1%之间,相对标准偏差为1.6%~4.2%。方法检出限为0.15~0.85μg/kg,且重现性好。可满足样品分析的质量控制要求,表明本分析方法具有良好的准确性与可靠性。A high performance liquid chromatographic（ HPLC） method was extablished for determination of the content of 7 polycyclic aromatic hydrocarbons（ PAHs） in soil and earthworm samples based on accelerated solvent extraction（ ASE） for extraction and solid phase extraction（ SPE） column for sample purification. In this method,the samples were first extracted by the mixed solution of n-hexane and acetone extraction（ 4∶ 1,V / V）,and then purified by SPE column（ silica gel column for soil sample purification and Al_2O_3-silica gel column for earthworm sample purification）,eluted by 10 m L of elution of n-hexane and dichloromethane（ 9 ∶ 1,V/V）,and evaporated to dryness with rotary evaporator. After that,the pretreated samples were re-dissolved with acetonitrile to a constant volume,followed by a filtration with a 0.22-μm organic filter membrane for the quantification by HPLC. The recoveries of the method for 7 PAHs were 83.5%-110.2% in soil samples and 81.2%-97.1% in earthworm samples. The detection limits of the method for 7 PAHs were 0.15- 0. 85 μg / kg. The method had good reproducibility and met the quality control requirements of sample analysis.

关 键 词：加速溶剂提取 固相萃取 高效液相色谱 土壤 蚯蚓 多环芳烃 

分 类 号：X830[环境科学与工程—环境工程] O657.72[理学—分析化学]