作者：苏趋, 张小芳, 陈丽鸣, 王亚静, 李苇苇, 向罗京
作者单位：湖北省环境科学研究院, 湖北 武汉 430000
关键词：气相色谱质谱;全国土壤污染状况详查;多环芳烃;加速溶剂萃取
摘要：
建立加速溶剂萃取-固相柱净化-气相色谱-质谱法测定《全国土壤污染状况详查》项目中多环芳烃的方法。对加速溶剂萃取以及分析仪器的参数条件进行优化，考察了氮吹体积的影响，有效地保证16种多环芳烃较高的回收率。结果表明，16种多环芳烃在10 ~500 μg/L范围内线性良好，该方法检出限在0.019~0.046 mg/kg之间。用新鲜土壤配置低、中、高加标水平分别为0.1，0.4，1.0 mg/kg的加标样品，16种多环芳烃的加标回收率在61.6%~115.6%之间，平行分析（n=6）得到的相对标准偏差（RSD）均小于19%，方法具有较高的准确度和精密度，利用生态环境部标样所提供的多环芳烃标准样品作为质控样，目标物质含量均在有效范围内。该方法能够为测定土壤中多环芳烃的含量提供技术支撑。
Determination of polycyclic aromatic hydrocarbons in the national soil pollution survey with chromatography-mass spectrometry
SU Qu, ZHANG Xiaofang, CHEN Liming, WANG Yajing, LI Weiwei, XIANG Luojing
Hubei Academy of Environmental Sciences, Wuhan 430000, China
Abstract: In this paper, a method for the determination of polycyclic aromatic hydrocarbons (PAHs) in the national soil pollution survey by accelerated solvent extraction-solid phase column purification-gas chromatography mass spectrometry was established. The parameters of accelerated solvent extraction and analytical instruments were optimized.The influence of nitrogen blowing volume was investigated, which effectively ensured the high recovery rate of 16 PAHs. The results showed that PAHs has good linearity in the range of 10 -500 μg/L, and the detection limit was 0.019 -0.046 mg/kg. The spiked samples with low, medium and high spiked levels of 0.1, 0.4, 1.0 mg/kg were prepared with fresh soil. The spiked recoveries of PAHs were between 61.6% and 115.6%, and the parallel analysis (n=6) was obtained. The relative standard deviation (RSD) is less than 19%. The method has high accuracy and precision. The PAHs standard samples provided by the institute for environmental reference materials were used as quality control sample, and the contents of target substance were within the valid range.The method can provide technical support for the determination of PAHs in soil.
Keywords: chromatography-mass spectrometry;national soil pollution survey;polycyclic aromatic hydrocarbons;accelerated solvent extraction
2020, 46(4):58-64 收稿日期: 2019-08-19;收到修改稿日期: 2019-10-21
基金项目: 中央土壤污染防治专项资金（2018年度）
作者简介: 苏趋(1991-),男,湖北武汉市人,工程师,硕士,主要从事土壤污染状况调查与环境污染损害司法鉴定工作
参考文献
[1] CHEN S C, LIAO CHUANGMIN. Health risk assessment on human exposed to environmental Polycyclic Aromatic Hydrocarbons pollution sources[J]. The science of The Total Environment, 2006, 366(1):112-123
[2] WANG C H, WU S H, ZHOU S L, et al. Polycyclic aromatic hydrocarbons in soils from urban to rural areas in Nanjing:Concentration, source, spatial distribution, and potential human health risk[J]. Science of the Total Environment, 2015(527-528):375-383
[3] ZHANG L L, YANG L, ZHOU Q Y, et al. Size distribution of particulate? polycyclic aromatic hydrocarbons? in fresh combustion smoke and ambient air:A review[J]. Journal of Environmental Sciences, 2020(3):370-384
[4] TADEO J L, SANCHEZ-BRUNETE C, ALBERO B, et al. Application of ultrasound-assisted extraction to the determination of contaminants in food and soil samples[J]. Journal of Chromatography A, 2010, 1217(16):2415-2440
[5] 李军, 张干, 祁士华. 广州市大气中多环芳烃分布特征、季节变化及其影响因素[J]. 环境科学, 2004, 25(3):7-13
[6] 张琳, 陈勇, 孔利锋, 等. 新疆准东煤矿开采区域中多环芳烃的污染特征分析[J]. 环境化学, 2017, 36(3):677-684
[7] WANG Z, CHEN J W, QIAO X L, et al. Distribution and sources of polycyclic aromatic hydrocarbons from urban to rural soils:A case study in Dalian, China[J]. Chemosphere, 2007, 68(5):965-971
[8] 张权, 陈文生, 洪亮, 等. 基质固相分散-加压溶剂萃取法测定土壤中多环芳烃[J]. 环境化学, 2014, 33(3):470-476
[9] 吕爱娟, 时磊, 蔡小虎, 等. QuEChERS-高效液相色谱法快速测定稻谷和土壤中16种多环芳烃[J]. 理化检验-化学分册, 2016, 52(9):470-476
[10] 张旭, 卢双, 裴晋, 等. 长江湖北段表层土中多环芳烃分布、来源及风险评价[J]. 环境科学学报, 2016, 36(12):4531-4536
[11] 陆继龙, 陈玉岩, 郝立波, 等. 吉林省中部农业土壤中PAHs的分布及风险评价[J]. 吉林大学学报, 2010, 40(3):683-688
[12] 李爱民, 刘彬, 贺小敏, 等. 湖北省典型水体半挥发性有机物分布及来源分析[J]. 环境科学与技术, 2015, 38(6P):391-397
[13] 杜芳芳, 杨毅, 刘敏, 等. 上海市表层土壤中多环芳烃的分布特征与源解析[J]. 中国环境科学, 2014, 34(4):989-995
[14] 王娜. 加速溶剂萃取-固相萃取净化-色谱法测定土壤中的多环芳烃和有机氯[J]. 环境化学, 2013, 32(3):524-525
[15] 张茜, 刘潇威, 罗铭, 等. 快速溶剂(ASE)提取、凝胶渗透色谱联合固相萃取净化,高效液相色谱法测定土壤中的多环芳烃[J]. 环境化学, 2011, 30(4):771-777
[16] 环境保护部. 环境监测分析方法标准制修订技术导则:HJ168-2010[S].北京:中国环境科学出版社, 2010.
