加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂

引用本文: 张玮庭, 宋善军, 卢柏灵, 彭子娟, 李彭辉. 加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂[J]. 分析化学, 2021, 49(4): 571-580. doi: 10.19756/j.issn.0253-3820.211029 shu

Citation: ZHANG Wei-Ting, SONG Shan-Jun, LU Bo-Ling, PENG Zi-Juan, LI Peng-Hui. Simultaneous Determination of Polychlorinated Biphenyls, Polybrominated Diphenyl Ethers and Organophosphate Flame Retardants in Sediments Using Accelerated Solvent Extraction-Column Purification-Solid Phase Extraction method[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 571-580. doi: 10.19756/j.issn.0253-3820.211029 shu

加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂

张玮庭 ^1,2, ,
宋善军 ^{2,
,} ,
卢柏灵 ^1, ,
彭子娟 ^2, ,
李彭辉 ^{1,
,}

1.
天津理工大学, 天津 300384;
2.
中国计量科学研究院, 北京 100029

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 李彭辉,E-mail:lipenghui406@163.com

基金项目:
中国计量科学研究院基本科研业务费（No.AKY1720）、天津市重点研发计划科技支撑重点项目（No.18YFZCSF01400）和天津市高等学校科技发展基金计划项目（No.2017KJ244）资助。

摘要: 建立并优化了对沉积物中多氯联苯（PCBs）、多溴联苯醚（PBDEs）和有机磷酸酯阻燃剂（OPFRs）3种有机污染物同时测定的分析方法。采用加速溶剂萃取（ASE）法对沉积物样品进行萃取，并通过固相萃取与层析柱串联方法对样品进行净化。在优化的分析条件下，PCBs的平均加标回收率为104.1%~121.7%，PBDEs的平均加标回收率为80.7%~101.6%，OPFRs的平均加标回收率为80.7%~132.2%，本方法可有效降低基质效应的影响。应用标准物质SRM-1944进行方法确证，证明本方法准确性良好。对采集于黄河三角洲地区的20个表层沉积物样品进行分析，分别检出了PBDEs和OPFRs等12种化合物，浓度范围为0.01~0.38 ng/g和1.18~21.99 ng/g，该区域有机磷系阻燃剂含量明显高于溴代阻燃剂。实际样品分析结果表明，本方法可满足实际样品分析检测的需求。

关键词:

English

Simultaneous Determination of Polychlorinated Biphenyls, Polybrominated Diphenyl Ethers and Organophosphate Flame Retardants in Sediments Using Accelerated Solvent Extraction-Column Purification-Solid Phase Extraction method

1.
Tianjin University of Technology, Tianjin 300384, China;
2.
National Institute of Metrology, Beijing 100029, China

Corresponding author: SONG Shan-Jun, ; LI Peng-Hui,

Received Date: 13 January 2021
Revised Date: 03 March 2021
Fund Project:
Supported by the Fundamental Research Funds of National Institute of Metrology, China (No.AKY1720), the Key Research and Development Plan of Tianjin (No.18YFZCSF01400) and the Tianjin Municipal Education Commission Research Project (No.2017KJ244).

Abstract: An analytical method for simultaneous determination of three organic pollutants, including polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs) and organic phosphorus flame retardants (OPFRs), in sediments was developed. Accelerated solvent extraction (ASE) was used to extract the targets from sediment samples, and the extracts were purified by solid phase extraction coupled with chromatography column purification. After optimization of the reaction conditions, the recoveries were 104.1%-121.7% for PCBs, 80.7%-101.6% for PBDEs, and 80.7%-132.2% for OPFRs. The developed method effectively eliminated the matrix effects. The method was verified by SRM-1944, showing satisfying accuracy. The method was further applied to detection of 20 surface sediment samples collected from the Yellow River Delta, and 12 compounds including PBDEs and OPFRs were detected with the concentration ranges of 0.01-0.38 ng/g and 1.18-21.99 ng/g. The results showed that the content of organophosphorus flameretardants in this area was higher than that of brominated flame retardants, and the method could be used for the detection of real samples.

Key words:

1. [1]
  WANG Bing-Hua, LI Xin-Ji. News Environ. Sci., 1994, (4):16-18. 王炳华, 李新纪. 环境科学动态, 1994, (4):16-18.
2. [2]
  MU Ya-Nan, WANG Jin-Ye, ZHANG Yan, GE Wei, WANG Ji-Fang, CHAI Chao. Environ. Chem., 2019, 38(1):131-141. 牟亚南, 王金叶, 张艳, 葛蔚, 王继芳, 柴超. 环境化学, 2019, 38(1):131-141.
3. [3]
  XIANG Y Z, LIANG X, QIONG P H, YI L, JIAN F H, WEI S L, ZHI Q Y. Mar. Pollut. Bull., 2020, 151:110843.
4. [4]
  WEI Jin-Fei, ZHAO Xia, JING Ling-Yun, LI Qing-Wei, ZHANG Rui. Appl. Chem. Indust., 2019, 48(8):1908-1913. 魏晋飞, 赵霞, 景凌云, 李庆维, 张瑞. 应用化工, 2019, 48(8):1908-1913.
5. [5]
  HAN Shan-Long, WANG Bao-Sheng, RUAN Ting, WANG Ya-Wei, FU Jian-Jie, HU Jing-Tian, JIANG Gui-Bin. Environ. Chem., 2012, 31(7):958-965. 韩善龙, 王宝盛, 阮挺, 王亚韡, 傅建捷, 胡敬田, 江桂斌. 环境化学, 2012, 31(7):958-965.
6. [6]
  WANG Ya-Wei, CAI Ya-Qi, JIANG Gui-Bin. Sci. Chin. Chem., 2010, 40(2):99-123. 王亚韡, 蔡亚岐, 江桂斌. 中国科学-化学, 2010, 40(2):99-123.
7. [7]
  SHAN Yue, WANG Shi-Yu, GU Lei-Yan, CHEN Su, LUO Qing. Environ. Sci. Manag., 2019, 44(6):15-18. 单岳, 王诗雨, 谷雷严, 陈苏, 罗庆. 环境科学与管理, 2019, 44(6):15-18.
8. [8]
  WU Di, YIN Hong-Ling, LI Shi-Ping, WANG Zeng-Wu, DENG Xu, LUO Yi, LUO Lin. Environ. Sci., 2019, 40(3):1245-1251. 吴迪, 印红玲, 李世平, 王增武, 邓旭, 罗怡, 罗林. 环境科学, 2019, 40(3):1245-1251.
9. [9]
  YU H Y, LIU Y F, SHU X Q, MA L M, PAN Y W. Chemosphere, 2020, 243:125392.
10. [10]
  WANG Sen, YUAN Qi, HAN Rui-Xia, QIAN Ya-Li, DING Liu-Yi. Environ. Chem., 2017, 36(12):2584-2599. 王森, 袁琪, 韩瑞霞, 钱亚利, 丁柳屹. 环境化学, 2017, 36(12):2584-2599.
11. [11]
  ZENG X Y, XU L, HU Q P, LIU Y, HU J F, LIAO W S, YU Z Q. Mar. Pollut. Bull., 2020, 151:110843.
12. [12]
  ZHU Yun, LI Shi-Gang, ZHOU Yuan, YU Ya-Dong. Environ. Monit. Early Warning, 2019, 11(3):30-35. 朱芸, 李世刚, 周圆, 于雅东. 环境监控与预警, 2019, 11(3):30-35.
13. [13]
  ZHANG Fu-Hai, CHEN Xin, TIAN Bing-Zheng, ZHAO Bin, ZHANG Min. China Environ. Monit., 2019, 35(4):141-148. 张付海, 陈鑫, 田丙正, 赵彬, 张敏. 中国环境监测, 2019, 35(4):141-148.
14. [14]
  GAO Li-Hong, LI Wen-Hui, SHI Ya-Li, LIU Jie-Min, CAI Ya-Qi. Environ. Chem., 2014, 33(10):1750-1761. 高立红, 厉文辉, 史亚利, 刘杰民, 蔡亚岐. 环境化学, 2014, 33(10):1750-1761.
15. [15]
  CHRISTIA C, TANG B, YIN S S, LUO X J, MAI B X, POMA G, COVACI A. Anal. Bioanal. Chem., 2019, 411(26):7015-7025.
16. [16]
  GENG Cun-Zhen, DUAN Yu-Shuang, WANG Yi-Xuan, HU Fei, YANG Yong-Liang, XIA Yan-Zhi. J. Ecotoxicol., 2016, 11(2):124-133. 耿存珍, 段玉双, 王艺璇, 胡飞, 杨永亮, 夏延致. 生态毒理学报, 2016, 11(2):124-133.
17. [17]
  WANG Shi-Yu, LUO Qing, SUN Li-Na, SHAN Yue. Environ. Engineer., 2018:353-356. 王诗雨, 罗庆, 孙丽娜, 单岳. 环境工程, 2018:353-356.
18. [18]
  XIONG Wen-Ming, XIE Cai-Ling, HUANG Yong, XIE Lin. Guangdong Chem. Indust., 2018, 45(2):190-191. 熊文明, 谢彩玲, 黄勇, 谢琳. 广东化工, 2018, 45(2):190-191.
19. [19]
  XIANG Lei-Lei, SONG Yang, BIAN Yong-Rong, SHENG Hong-Jie, LIU Guang-Xia, JIANG Xin, LI Guo-Hua, WANG Fang. Chin. J. Anal. Chem., 2016, 44(5):671-677. 相雷雷, 宋洋, 卞永荣, 生弘杰, 柳广霞, 蒋新, 李国华, 王芳. 分析化学, 2016, 44(5):671-677.
20. [20]
  NEUGEBAUER F, DREYER A, LOHMANN N, KOSCHORRECK J. Anal. Bioanal. Chem., 2018, 410(4):1375-1387.
21. [21]
  RUAN Wei, TAN Xiao-Xin, LUO Xiao-Jun, MAI Bi-Xian. Chin. Environ. Sci., 2014, 34(9):2394-2400. 阮伟, 谭晓欣, 罗孝俊, 麦碧娴. 中国环境科学, 2014, 34(9):2394-2400.
22. [22]
  SUNDKVIST A M, OLOFSSON U, HAGLUND P. J. Environ. Monit., 2010, 12(4):943.
23. [23]
  WEN Yu-Yun, CHEN Zhi-Hua, OU Yan, GONG Zhen-Bin. Chin. J. Anal. Chem., 2015, 43(9):95-101. 温裕云, 陈志华, 欧延, 弓振斌. 分析化学, 2015, 43(9):1342-1348.
24. [24]
  MA Qiang, BAI Hua, WANG Chao, XI Hai-Wei, MA Wei, ZHOU Xin, DONG Yi-Yang, WANG Bao-Lin. Chem. J. Chin. Univ., 2010, 31(3):473-478. 马强, 白桦, 王超, 席海为, 马微, 周新, 董益阳, 王宝麟. 高等学校化学学报, 2010, 31(3):473-478.
25. [25]
  HE C, WANG X Y, THAI P, MUELLER J F, GALLEN C, LI Y, BADUEL C. Talanta, 2017, 164:503-510.
26. [26]
  IWEGBUE C M A, TESI G O, OVERAH L C, EMOYAN O O, NWAJEI G E, MARTINCIGH B S. Polycycl. Aromat. Comp., 2020, 40(2):228-244.
27. [27]
  SUN J, LIU J, LIU Q, QU G B, RUAN T, JIANG G B. Talanta, 2012, 88(1):669-676.
28. [28]
  JU Ting, GE Wei, CHAI Chao. Environ. Chem., 2017, 36(4):839-848. 鞠婷, 葛蔚, 柴超. 环境化学, 2017, 36(4):839-848.
29. [29]
  WANG X, ZHU Q, YAN X, WANG Y, LIAO C, JIANG G. Sci. Total Environ., 2020, 731:139071.

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沈阳化工大学材料科学与工程学院沈阳 110142

加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 李彭辉,E-mail:lipenghui406@163.com

English

Simultaneous Determination of Polychlorinated Biphenyls, Polybrominated Diphenyl Ethers and Organophosphate Flame Retardants in Sediments Using Accelerated Solvent Extraction-Column Purification-Solid Phase Extraction method

Corresponding author: SONG Shan-Jun, ; LI Peng-Hui,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

加速溶剂萃取-固相萃取-层析柱净化法同时测定 沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 李彭辉,E-mail:lipenghui406@163.com

English

Simultaneous Determination of Polychlorinated Biphenyls, Polybrominated Diphenyl Ethers and Organophosphate Flame Retardants in Sediments Using Accelerated Solvent Extraction-Column Purification-Solid Phase Extraction method

Corresponding author: SONG Shan-Jun, ; LI Peng-Hui,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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