GC-MS/MS结合QuEChERS法测定土壤中16种多环芳烃的方法研究
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摘要
建立了三重四级杆气质联用仪(GC-MS/MS)结合QuEChERS法测定土壤中16种多环芳烃(PAHs)含量的方法。土壤样品经二氯甲烷超声提取,用QuEChERS净化试剂净化,离心过膜后GC-MS/MS分析,外标法定量。在10～1 000μg·L-1浓度范围内基质加标,得到16种多环芳烃的相关系数均在0.996 6以上;各参数的检出限(LOD)为0.17～2.35μg·kg~(-1),定量限(LOQ)为0.55～7.84μg·kg~(-1);16种PAHs在低、中、高3种不同浓度水平的平均回收率在62%～119%,RSD值在0.32%～15.60%。此方法操作简单快速,回收率稳定,满足土壤中PAHs的检测要求,可为相关检测研究人员提供理论依据。
The combination of the triple quadrupole GC-MS/MS with QuEChERS was used to measure the contents of 16 Polycyclic Aromatic Hydrocarbons(PAHs) in the soil. The method of ultrasonic extraction with methylene dichloride was used to get the soil samples, and the QuEChERS purification reagent was adopted. After centrifugation and membrane,GC/MS-MS analysis was conducted by external standard method. In the concentration range of 10～1 000μg·L-1 by matrix standard addition, the correlation coefficients of the 16 kinds of PAHs were all above 0.996 6. The limit of detection(LOD) of various parameters was 0.17～2.35 μg·kg~(-1), and the limit of quantification(LOQ) was 0.55～7.84 μg·kg~(-1). The average recovery of the 16 kinds of PAHs was between 62% and 119% with low, middle and high concentration levels, and the value of RSD was between 0.32% and 15.60%. This method has fast and simple operation and stable recovery, which could satisfy the detecting demands of PAHs in soil and provide theoretical basis for related researchers.
The combination of the triple quadrupole GC-MS/MS with QuEChERS was used to measure the contents of 16 Polycyclic Aromatic Hydrocarbons(PAHs) in the soil. The method of ultrasonic extraction with methylene dichloride was used to get the soil samples, and the QuEChERS purification reagent was adopted. After centrifugation and membrane,GC/MS-MS analysis was conducted by external standard method. In the concentration range of 10～1 000μg·L-1 by matrix standard addition, the correlation coefficients of the 16 kinds of PAHs were all above 0.996 6. The limit of detection(LOD) of various parameters was 0.17～2.35 μg·kg~(-1), and the limit of quantification(LOQ) was 0.55～7.84 μg·kg~(-1). The average recovery of the 16 kinds of PAHs was between 62% and 119% with low, middle and high concentration levels, and the value of RSD was between 0.32% and 15.60%. This method has fast and simple operation and stable recovery, which could satisfy the detecting demands of PAHs in soil and provide theoretical basis for related researchers.
引文
[1]李永霞,刘燕,王文刚,等.某钢铁企业表层土壤中多环芳烃含量特征与生态风险评价[J].环境化学,2017,36(6):1320-1327.
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[3]刘庚,牛俊杰,王玲,等.污灌区农田土壤多环芳烃污染及风险评价[J].环境化学,2017,36(7):1622-1629.
[4] WANG J Z,ZHU C Z,CHEN T H. PAHs in Chinese environment:Levels,inventory mass,source and toxic potency assessment[J].Environmental Science Processes and Impacts,2013,15(6):1104-1112.
[5] WILD S R, JO NES K C. Polynuclear aromatic hydrocarbons in the United Kingdom environment:A preliminary source inventory and budget[J]. Environmental Pollution, 1995, 88:91-108.
[6] ANASTASSIAEDS M,LEHO TAY S J,STAJNBAHER D,et al.Fast and easy multi residue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in product[J].JAO AC International,2003,86(2):412-431.
[7]李拥军,黎小鹏,李盛安,等. Q uEChER S前处理-GC-MS法测定土壤中16种多环芳烃[J].广东化工,2017,43(13):269-271.
[8]吕爱娟,沈小明,时磊,等.优化Q uEChER S结合HPLC测定沉积物中14种多环芳烃[J].中国环境监测,2017,33(1):116-120.
[2]胡敏,唐倩,彭剑飞,等.我国大气颗粒物来源及特征分析[J].环境与可持续发展,2011(5):15-18.
[3]刘庚,牛俊杰,王玲,等.污灌区农田土壤多环芳烃污染及风险评价[J].环境化学,2017,36(7):1622-1629.
[4] WANG J Z,ZHU C Z,CHEN T H. PAHs in Chinese environment:Levels,inventory mass,source and toxic potency assessment[J].Environmental Science Processes and Impacts,2013,15(6):1104-1112.
[5] WILD S R, JO NES K C. Polynuclear aromatic hydrocarbons in the United Kingdom environment:A preliminary source inventory and budget[J]. Environmental Pollution, 1995, 88:91-108.
[6] ANASTASSIAEDS M,LEHO TAY S J,STAJNBAHER D,et al.Fast and easy multi residue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in product[J].JAO AC International,2003,86(2):412-431.
[7]李拥军,黎小鹏,李盛安,等. Q uEChER S前处理-GC-MS法测定土壤中16种多环芳烃[J].广东化工,2017,43(13):269-271.
[8]吕爱娟,沈小明,时磊,等.优化Q uEChER S结合HPLC测定沉积物中14种多环芳烃[J].中国环境监测,2017,33(1):116-120.