Simultaneous Determination of 36 Kinds of Polycyclic Aromatic Hydrocarbons and Their Derivatives in Groundwater by Gas Chromatography-Mass Spectrometry
摘 要
按DD 2008-01规定采集浅层地下水样品并于4℃保温箱中保存。取水样1.000 0 L置于分液漏斗中,依次加入氯化钠20.0 g,1.0 mg·L-1替代物混合标准溶液100 μL和正己烷-二氯甲烷(1+1)混合萃取液60 mL,萃取10 min,分层后,取有机相并保留,再用正己烷萃取2次,每次用30 mL。合并3次萃取液,旋转蒸发至体积约为2~3 mL,随即改用吹氮蒸发至约剩0.8 mL,加入2.0 mg·L-1内标混合标准溶液100 μL,用正己烷定容至1.0 mL。用Rxi-5Sil MS毛细管色谱柱选择初始温度为65℃,按程序升温条件进行气相色谱分离;质谱分析采用电子轰击离子源,全扫描模式定性和选择离子模式定量。结果表明:36种多环芳烃及其衍生物的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)在1.3~8.8 ng·L-1之间。以空白水样为基体进行加标回收试验,回收率在71.1%~120%之间,测定值的相对标准偏差(n=5)在1.2%~9.7%之间。
Abstract
Samples of shallow groundwater were collected and stored at 4℃ in a refrigerator according to DD 2008-01. 1.000 0 L of the water sample was taken, and extracted for 10 min with 60 mL of a mixed extracting solvent of n-hexane and dichloromethane (1+1), after successive addition of 20.0 g of NaCl and 100 μL of 1.0 mg·L-1 standard solution of mixed substitutes. After the 2 phases were separated, the organic phase was separated and preserved, and the water phase was extracted twice further with 30 mL of n-hexane for each extraction. The 3 extracts were combined and evaporated under swirling until its volume was concentrated to 2-3 mL, the evaporation was continued by N2-blowing to concentrate the solution to a volume ca. 0.8 mL. 100 μL of the 2.0 mg·L-1 mixed internal standard solution was added and the volume of the solution was made up to 1.0 mL with n-hexane. Rxi-5Sil MS capillary chromatographic column was selected for GC separation, under temperature elevation program by choosing 65℃ as the initial temperature. In MS analysis, EI ionization source was used, and mode of full-scanning was adopted for qualification while the mode of SIM for quantification. As shown by the results, linear relationships between values of peak area and mass concentration of the 36 polycyclic aromatic hydrocarbons and their derivatives were found in definite ranges, with detection limits (3S/N) in the range of 1.3-8.8 ng·L-1. Test for recovery by standard addition method was made on the base of blank water sample, giving results in the range of 71.1%-120%, and RSDs (n=5) ranged from 1.2% to 9.7%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201901006
所属栏目 工作简报
基金项目 中国地质调查项目(DD20160312,DD20160323,1212011120283,12120123500016000902)
收稿日期 2018/3/26
修改稿日期
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联系人作者饶竹(raozhu@126.com)
备注许丹丹,硕士研究生,研究方向为环境地球化学
引用该论文: XU Dandan,RAO Zhu,LIANG Handong. Simultaneous Determination of 36 Kinds of Polycyclic Aromatic Hydrocarbons and Their Derivatives in Groundwater by Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(1): 31~38
许丹丹,饶竹,梁汉东. 气相色谱-质谱法同时测定地下水中36种多环芳烃及其衍生物[J]. 理化检验-化学分册, 2019, 55(1): 31~38
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【5】董淑萍,金祖亮,李玉琴,等.北京地区大气颗粒物中硝基多环芳烃与多环芳烃的研究[J].环境科学学报, 1989,9(3):308-317.
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【7】QIAO M, QI W X, LIU H J, et al. Simultaneous determination of typical substituted and parent polycyclic aromatic hydrocarbons in water and solid matrix by gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2013,1291:129-136.
【8】DASGUPTA S, CAO A, MAUER B, et al. Genotoxicity of oxy-PAHs to Japanese medaka (Oryzias latipes) embryos assessed using the comet assay[J]. Environmental Science and Pollution Research, 2014,21(24):13867-13876.
【9】AHMED T M, AHMED B, AZIZ B K, et al. Native and oxygenated polycyclic aromatic hydrocarbons in ambient air particulate matter from the city of Sulaimaniyah in Iraq[J]. Atmospheric Environment, 2015,116:44-50.
【10】LI J, YU H, LUAN Y. Meta-analysis of the copper, zinc, and cadmium absorption capacities of aquatic plants in heavy metal-polluted water[J]. International Journal of Environmental Research and Public Health, 2015,12(12):14958-14973.
【11】曹攽,胡祖国,郑存江,等.超声萃取-气相色谱法测定土壤中石油烃[J].理化检验-化学分册, 2018,54(3):275-279.
【12】BANDOWE B A M, MEUSEL H, Huang R J, et al. PM2. 5-bound oxygenated PAHs, nitro-PAHs and parent-PAHs from the atmosphere of a Chinese megacity:Seasonal variation, sources and cancer risk assessment[J]. Science of the Total Environment, 2014,473/474:77-87.
【13】ALBINET A, LEOZ-GARZIANDIA E, BUDZINSKI H, et al. Nitrated and oxygenated derivatives of polycyclic aromatic hydrocarbons in the ambient air of two French alpine valleys:Part 1:Concentrations, sources and gas/particle partitioning[J]. Atmospheric Environment, 2008,42(1):43-54.
【14】高冉,饶竹,郭晓辰,等.气相色谱-质谱法同时测定地下水中42种半挥发性有机污染物[J].分析测试学报, 2014,33(5):539-544.
【15】张红庆,饶竹,王晓春,等.全二维气相色谱-飞行时间质谱测定地下水中低环多环芳烃及其衍生物[J].分析测试学报, 2017,36(10):1197-1202.
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