高级搜索

加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃

,  ,  ,  , 

downloadPDF

上一篇

下一篇

陶鑫, 全洗强, 俞建国, 杜文越, 秦愫妮. 加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃[J]. 环境化学, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
引用本文: 陶鑫, 全洗强, 俞建国, 杜文越, 秦愫妮.

加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃

[J]. 环境化学, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
shu
TAO Xin, QUAN Xiqiang, YU Jianguo, DU Wenyue, QIN Suni. Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography[J]. Environmental Chemistry, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
Citation: TAO Xin, QUAN Xiqiang, YU Jianguo, DU Wenyue, QIN Suni.

Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography

[J]. Environmental Chemistry, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
shu

加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃

  • 中国地质科学院岩溶地质研究所, 自然资源部/广西壮族自治区岩溶动力学重点实验室, 桂林, 541004

    • 通讯作者: 全洗强, E-mail: quanxq@karst.ac.cn ; 
  • 基金项目:

    中国地质科学院岩溶地质研究所科研业务费项目（2017027）资助.

Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography

  • Institute of Karst Geology, CAGS/Key Laboratory of Karst Dynamics, MNR & GZAR, Guilin, 541004, China

    • Corresponding author: QUAN Xiqiang, quanxq@karst.ac.cn ; 
  • Fund Project: Support by the Research Fund of CAGS(2017027).

  • 摘要:

    建立了加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤样品中16种多环芳烃（PAHs）的方法.旋蒸定容有效减少了污染物的引入，特别是萘、菲.研究了影响PAHs回收率的主要因素.优化后的条件为：萃取温度110℃，静态萃取时间3 min，冲洗量30%，氮气吹扫时间30 s，正己烷/丙酮（体积比2：1）为萃取液，1次静态萃取循环，弗罗里硅土柱为固相萃取小柱，正己烷/二氯甲烷（体积比7：3）为淋洗液，淋洗液体积10 mL.在20-200 mg·L-1范围内，各目标物线性关系（R2）为0.9994-1.目标物的检出限和定量限分别为0.08-2.50 mg·kg-1和0.25-8.33 mg·kg-1.在优化的实验条件下，加标水平为25 mg·kg-1和100 mg·kg-1时，目标物平均加标回收率分别为73.9%-105%、79.0%-110%，相对标准偏差（n=7）均小于10%.土壤PAHs QC样品的检测中，各目标物检测值均在参考值范围内；土壤PAHs QC样品加标回收率为63.4%-94.8%，适合实际土壤样品中多环芳烃的检测.

    Abstract:

    A method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in soil by high performance liquid chromatography was proposed based on accelerated solvent extraction and rotary evaporation to obtain a constant volume. The introduction of pollutants, especially for naphthalene and phenanthrene, could be effectively reduced by rotary evaporation to obtain a constant volume. The main factors affecting the recoveries of PAHs were investigated. Optimized conditions are:110℃ extraction temperature, three minutes static extraction, 30% rinse volume, 30 s nitrogen purge, a mixture of hexane and acetone (2:1, V/V) for extraction solvent, one static extraction cycle, florisil was used as SPE column, mixture of hexane and dichloromethane (7:3, V/V) as eluent, and 10 mL eluent volume. The correlation coefficients (R2) for PAHs were between 0.9994 and 1 in the range of 20-200 mg·L-1.The limits of detection and quantitation of PAHs were 0.08-2.50 mg·kg-1 and 0.25-8.33 mg·kg-1, respectively. Under the optimized experimental conditions, the recoveries of PAHs, with 25 mg·kg-1and 100 mg·kg-1 standard addition, were in the range of 73.9%-105% and 79.0%-110%, respectively, while the relative standard deviations (n=7) was less than 10%. In the detection of PAHs in soil QC sample, the concentrations of all the values of target analytes were within the reference value ranges and the recoveries were 63.4%-94.8%. Therefore, the present protocol is satisfactory for the detection of PAHs in actual soil samples.

  • 加载中
  • [1] 邓绍坡, 吴运金, 龙涛, 等. 我国表层土壤多环芳烃(PAHs)污染状况及来源浅析[J]. 生态与农村环境学报, 2015, 31(6):866-875.

    DENG S P, WU Y J, LONG T, et al. PAHs Contamination in the surface soil of china and its sources[J]. Journal of Ecology and Rural Environment, 2015, 31(6):866-875(in Chinese).

    [2] 熊丽君, 吴杰, 王敏, 等. 交通道路沿线土壤多环芳烃污染及风险防控综述[J]. 生态环境学报, 2018, 27(5):974-982.

    XIONG L J, WU J, WANG M, et al. Characteristics and risk prevention of polycyclic aromatic hydrocarbons (PAHs) in farmland soil along traffic road:A review[J]. Ecology and Environmental Sciences, 2018, 27(5):974-982(in Chinese).

    [3] 潘栋宇, 侯梅芳, 刘超男, 等. 多环芳烃污染土壤化学修复技术的研究进展[J]. 安全与环境工程, 2018, 25(3):54-60

    , 66. PAN D Y, HOU M F, LIU C N, et al. Review of chemical remediation technology of polycyclic aromatic hydrocarbons contaminated soil[J]. Safety and Environmental Engineering, 2018, 25(3):54-60, 66(in Chinese).

    [4] 张俊叶, 俞菲, 俞元春. 中国主要地区表层土壤多环芳烃含量及来源解析[J]. 生态环境学报, 2017, 26(6):1059-1067.

    ZHANG J Y, YU F, YU Y C. Content and source apportionment of polycyclic aromatic hydrocarbons in surface soil in major areas of China[J]. Ecology and Environmental Sciences, 2017, 26(6):1059-1067(in Chinese).

    [5] 赵涵, 赵军, 徐晓晔, 等. 快速城市化地区土壤多环芳烃的空间分布及来源:以深圳市为例[J]. 生态与农村环境学报, 2019, 35(1):38-45.

    ZHAO H, ZHAO J, XU X Y, et al. Spatial distribution, sources and risk assessment of polycyclic aromatic hydrocarbons in a rapid urbanization city:Shenzhen[J]. Journal of Ecology and Rural Environment, 2019, 35(1):38-45(in Chinese).

    [6] 龙明华, 龙彪, 梁勇生, 等. 南宁市蔬菜基地土壤多环芳烃含量及来源分析[J]. 中国蔬菜, 2017, 30(3):52-57.

    LONG M H, LONG B, LIANG Y S, et al. Analysis of contents and sources of polycyclic aromatic hydrocarbons in vegetable production base of Nanning city[J]. China Vegetables, 2017, 30(3):52-57(in Chinese).

    [7] 张娟, 吴建芝,刘燕. 北京市绿地土壤多环芳烃分布及健康风险评价[J]. 中国环境科学, 2017, 37(3):1146-1153.

    ZHANG J, WU J Z, LIU Y. Polycyclic aromatic hydrocarbons in urban green space of Beijing:Distribution and potential risk[J]. China Environmental Science, 2017, 37(3):1146-1153(in Chinese).

    [8] 杨靖宇, 俞元春, 王小龙. 南京市不同功能区林业土壤多环芳烃含量与来源分析[J]. 生态环境学报, 2016, 25(2):314-319.

    YANG J Y, YU Y C, WANG X L. Characterization and sources of polycyclic aromatic hydrocarbons in urban forestry soil from different functional areas of Nanjing City[J]. Ecology and Environmental Sciences, 2016, 25(2):314-319(in Chinese).

    [9] 张永兵, 陈军, 张钧, 等. 固相萃取-高效液相色谱法快速测定土壤中多环芳烃[J]. 环境工程, 2013, 31(S1):608-610.

    ZHANG Y B, CHEN J, ZHANG J, et al. Rapid determination of polycyclic aromatic hydrocarbons in soil by SPE-HPLC[J]. Environmental Engineering, 2013, 31(S1):608-610(in Chinese).

    [10] 宋盼盼, 黄满红, 陈东辉, 等. 高效液相色谱-DAD检测法分离测定土壤中的多环芳烃[J]. 环境工程, 2014, 32(S1):988-991.

    SONG P P, HUANG M H, CHEN D H, et al. Separation and determination of PAHs in soil by HPLC-DAD detection[J]. Environmental Engineering, 2014, 32(S1):988-991(in Chinese).

    [11]
    [12]
    [13] 徐林林, 张立中. 公园地表土中多环芳烃的分离提取及含量分析[J]. 中国环境监测, 2016, 32(2):104-108.

    XU L L, ZHANG L Z. Extraction and analysis of polycyclic aromatic hydrocarbons from the surface soil of park[J]. Environmental Monitoring in China, 2016, 32(2):104-108(in Chinese).

    [14] 张亚楠, 杨兴伦, 卞永荣, 等. 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[J]. 分析化学, 2016, 44(10):1514-1520.

    ZHANG Y N, YANG X L, BIAN Y R, et al. An accelerated solvent extraction-solid phase extraction-high performance liquid chromatographic method for determination of polycyclic aromatic hydrocarbons in soil and earthworm samples[J].Chinese Journal of Analytical Chemistry, 2016, 44(10):1514-1520(in Chinese).

    [15] 张茜, 刘潇威, 罗铭, 等. 快速溶剂(ASE)提取、凝胶渗透色谱(GPC)联合固相萃取(SPE)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.

    ZHANG X, LIU X W, LUO M, et al. Determination of polycyclic aromatic hydrocarbons in soil by ASE-GPC-SPE purification and detection[J]. Environmental Chemistry, 2011, 30(4):771-777(in Chinese).

    [16] 王伟. 基质固相分散-快速溶剂萃取-GC/MS法同时测定土壤中有机氯农药和多环芳烃[J]. 中国环境监测, 2019, 35(1):135-141.

    WANG W. Simultaneous Determination of organochlorine pesticides and polycyclic aromatic hydrocarbons in soil by matrix solid-phase dispersion-accelerated solvent extraction and gas chromatography-mass spectrometry[J]. Environmental Monitoring in China, 2019, 35(1):135-141(in Chinese).

    [17] 陈海英, 沈加林, 吕爱娟, 等. 液相色谱法测定地下水中多环芳烃的准确度控制[J]. 安全与环境学报, 2014, 14(3):312-316.

    CHEN H Y, SHEN J L, LV A J, et al. Accuracy assurance of PAHs in the groundwater by way of using liquid-liquid extraction of HPLC[J]. Journal of Safety and Environment, 2014, 14(3):312-316(in Chinese).

    [18] 魏峰, 吕爱娟, 陈海英, 等. 水中多环芳烃前处理过程中的污染来源及去除方法[J]. 岩矿测试, 2011, 30(2):169-173.

    WEI F, LV A J, CHEN H Y, et al. The source of some contaminants during pretreatment of polycyclic aromatic hydrocarbons in water and the purification method[J]. Rock and Mineral Analysis, 2011, 30(2):169-173(in Chinese).

    [19] 贺行良, 夏宁, 张媛媛,等.ASE/GC-MS法同时测定海洋沉积物中65种多氯联苯、多环芳烃与有机氯农药[J].分析测试学报,2011,30(2):152-160.

    HE X L, XIA N, ZHANG Y Y, et al. Simultaneous determination of 65 polychlorinated biphenyls, polycyclic aromatic hydrocarbons and organochlorine pesticides in marine sediments by GC-MS with accelerated solvent extraction[J]. Journal of Instrumental Analysis, 2011,30(2):152-160(in Chinese).

    [20] 宋晓娟, 李海燕, 尹明明, 等. 快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃[J]. 色谱, 2018, 36(1):51-58.

    SONG X J, LI H Y, YIN M M, et al. Determination of 16 polycyclic aromatic hydrocarbons in marine sediments by gas chromatography-tandem mass spectrometry with accelerated solvent extraction[J]. Chinese Journal of Chromatography, 2018, 36(1):51-58(in Chinese).

    [21] 王道玮, 赵世民, 金伟, 等. 加速溶剂萃取-固相萃取净化-气相色谱/质谱法测定沉积物中多氯联苯和多环芳烃[J]. 分析化学, 2013, 41(6):861-868.

    WANG D W, ZHAO S M, JIN W, et al. Simultaneous determination of 28 polychlorinated biphenyls and 16 polycyclic aromatic hydrocarbons in sediments using ASE-SPE-GC-QqQ-MS/MS[J]. Chinese Journal of Analytical Chemistry, 2013, 41(6):861-868(in Chinese).

    [22] 王新成, 赵金, 赵汝松, 等. 加速溶剂提取气-质联用分析土壤中的多环芳烃[J]. 中国环境监测, 2014, 30(3):144-148.

    WANG X C, ZHAO J, ZHAO R S, et al. Determination of polycyclic aromatic hydrocarbons in soils using accelerated solvent extraction and gas chromatography-mass spectrometry[J]. Environmental Monitoring in China, 2014, 30(3):144-148(in Chinese).

    [23] 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.

    ZHANG Q, CHEN W S, HONG L, et al. Determination of polycyclic aromatic hydrocarbons in soil by matrix solid phase dispersion-pressurized liquid extraction[J]. Environmental Chemistry, 2014, 33(3):470-476(in Chinese).

  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  2184
  • HTML全文浏览数:  2184
  • PDF下载数:  49
  • 施引文献:  0
出版历程
  • 收稿日期:  2019-04-17
  • 刊出日期:  2019-12-10
陶鑫, 全洗强, 俞建国, 杜文越, 秦愫妮. 加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃[J]. 环境化学, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
引用本文: 陶鑫, 全洗强, 俞建国, 杜文越, 秦愫妮.

加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃

[J]. 环境化学, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
shu
TAO Xin, QUAN Xiqiang, YU Jianguo, DU Wenyue, QIN Suni. Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography[J]. Environmental Chemistry, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
Citation: TAO Xin, QUAN Xiqiang, YU Jianguo, DU Wenyue, QIN Suni.

Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography

[J]. Environmental Chemistry, 2019, (12): 2797-2807. doi: 10.7524/j.issn.0254-6108.2019041705
shu

加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃

    通讯作者: 全洗强, E-mail: quanxq@karst.ac.cn ; 
  • 中国地质科学院岩溶地质研究所, 自然资源部/广西壮族自治区岩溶动力学重点实验室, 桂林, 541004
  • 收稿日期:  2019-04-17
  • 网络出版日期:  2019-12-10
基金项目:

中国地质科学院岩溶地质研究所科研业务费项目（2017027）资助.

摘要: 

建立了加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤样品中16种多环芳烃（PAHs）的方法.旋蒸定容有效减少了污染物的引入，特别是萘、菲.研究了影响PAHs回收率的主要因素.优化后的条件为：萃取温度110℃，静态萃取时间3 min，冲洗量30%，氮气吹扫时间30 s，正己烷/丙酮（体积比2：1）为萃取液，1次静态萃取循环，弗罗里硅土柱为固相萃取小柱，正己烷/二氯甲烷（体积比7：3）为淋洗液，淋洗液体积10 mL.在20-200 mg·L-1范围内，各目标物线性关系（R2）为0.9994-1.目标物的检出限和定量限分别为0.08-2.50 mg·kg-1和0.25-8.33 mg·kg-1.在优化的实验条件下，加标水平为25 mg·kg-1和100 mg·kg-1时，目标物平均加标回收率分别为73.9%-105%、79.0%-110%，相对标准偏差（n=7）均小于10%.土壤PAHs QC样品的检测中，各目标物检测值均在参考值范围内；土壤PAHs QC样品加标回收率为63.4%-94.8%，适合实际土壤样品中多环芳烃的检测.

English Abstract

    全文HTML

参考文献 (23)

返回顶部

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心