加速溶剂萃取-硅胶萃取净化-气相色谱/质谱法检测地表水中有机氯农药和多氯联苯

注册 English

加速溶剂萃取-硅胶萃取净化-气相色谱/质谱法检测地表水中有机氯农药和多氯联苯

邵阳 , 杨国胜 , 韩深 , 马玲玲 , 罗敏 , 刘韦华 , 徐殿斗

引用本文: 邵阳, 杨国胜, 韩深, 马玲玲, 罗敏, 刘韦华, 徐殿斗. 加速溶剂萃取-硅胶萃取净化-气相色谱/质谱法检测地表水中有机氯农药和多氯联苯[J]. 分析化学, 2016, 44(5): 698-706. doi: 10.11895/j.issn.0253-3820.150805 shu

shu

Citation: SHAO Yang, YANG Guo-Sheng, HAN Shen, MA Ling-Ling, LUO Min, LIU Wei-Hua, XU Dian-Dou. Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Surface Water Using Accelerate Solvent Extraction Coupling with Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016, 44(5): 698-706. doi: 10.11895/j.issn.0253-3820.150805 shu

shu

加速溶剂萃取-硅胶萃取净化-气相色谱/质谱法检测地表水中有机氯农药和多氯联苯

1.
中国科学院高能物理研究所核技术应用研究中心, 北京 100049;
2.
北京市射线成像技术与装备工程技术研究中心, 北京 100049;
3.
北京出入境检验检疫局技术中心, 北京 100026
基金项目:
本文系国家自然科学基金项目(Nos.11275216,11575210,11435002和21407149)资助

摘要: 建立了加速溶剂萃取-硅胶固相萃取净化-气相色谱/质谱同时检测地表水中15种有机氯农药(OCPs)和82种多氯联苯(PCBs)的方法。对影响OCPs和PCBs回收率的主要因素进行优化,得出最优的萃取条件:3次静态萃取循环,100℃的萃取温度,丙酮/正己烷(1:1,V/V)为萃取液,静态萃取10 min。在最优条件下,15种OCPs和82种PCBs在加标水溶液中的回收率分别为70.9%~130%和52.5%~89.1%。日内和日间相对标准偏差分别为1.7%~16.1%和2.4%~33.3%。OCPs和PCBs混合标样在10~800μg/L范围内线性相关系数(R²)均大于0.995。OCPs和PCBs方法检测限分别为0.13~0.38 ng/L和0.10~0.32 ng/L。相比于传统萃取方法,本方法回收率高、萃取时间短、试剂用量少。应用本方法测得北京城区地表水中OCPs和PCBs的含量范围分别为n.d.~3.45 ng/L和n.d.~4.88 ng/L。

关键词:

English

Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Surface Water Using Accelerate Solvent Extraction Coupling with Gas Chromatography-Mass Spectrometry

1.
Division of Nuclear Technology and Applications, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China;
2.
Beijing Engineering Research Center of Radiographic Techniques and Equipment, Beijing 100049, China;
3.
Beijing Entry-Exit Inspection and Quarantine Bureau Technology Centre, Beijing 100026, China
Received Date: 13 October 2015
Revised Date: 26 December 2015
Fund Project:
This work was supported by the National Natural Science Foundation of China (Nos. 11275216, 11575210, 11435002, 21407149)

Abstract: A rapid and sensitive analytical method for the simultaneous determination of 15 organochlorine pesticides (OCPs) and 82 polychlorinated biphenyls (PCBs) in water using accelerate solvent extraction (ASE) and silica gel solid phase extraction (SPE) cleanup followed by gas chromatography-mass spectrometry (GC-MS) analysis was developed. The main potential influence parameters which affected the recoveries of OCPs and PCBs were investigated for the optimum ASE efficiency. Finally, 3 static extraction cycles, 100℃ of extraction temperature, mixture of acetone and hexane (1:1, V/V) as extraction solvent, and 10 min of static extraction time were used. Under the optimized conditions, the recoveries of 15 OCPs and 82 PCBs in spiked water were 70.9%-130% and 52.5%-89.1%, respectively. The intra-day and inter-day relative standard deviation was 1.7%-16.1% and 2.4%-33.3%, respectively. The correlation coefficients (R²) for OCPs and PCBs were above 0.995 in the range of 10-800 μg/L. And the method detection limits were characterized as 0.13-0.38 ng/L for OCPs and 0.10-0.32 ng/L for PCBs. Compared to the traditional methods, the developed method had the advantages of higher recoveries and less consumption of extraction time and toxic solvent. Subsequently, the developed method was applied to measure the concentrations of OCPs and PCBs in the surface water of Beijing. The concentrations of OCPs and PCBs were in the range of not detected (n.d.)-3.45 ng/L and n.d.-4.88 ng/L, respectively.

Key words:

1. [1]
  Zhang K, Wei Y L, Zeng E Y. Sci. Total Environ., 2013,463-464:1093-1110
2. [2]
  Mrema E J, Rubino F M, Brambilla G, Moretto A, Tsatsakis A M, Colosio C. Toxicology, 2013,307:74-88
3. [3]
  DING Li-Ping, CAI Chun-Ping, WANG Dan-Hong. Journal of Instrumental Analysis, 2014,33(10):1178-1183 丁立平, 蔡春平, 王丹红.分析测试学报,2014,33(10):1178-1183
4. [4]
  Nozar S L M, Ismail W R, Zakaria M P. Hum. Ecol. Risk Assess., 2014, 20(6):1507-1520
5. [5]
  Sharma B M, Bharat G K, Tayal S, Nizzetto L, Cupr P, Larssen T. Environ. Int., 2014,66:48-64
6. [6]
  HUA Xiao-Mei, SHAN Zheng-Jun. Advances in Environmental Science, 1996,4(2):33-45 华小梅, 单正军.环境科学进展,1996,4(2):33-45
7. [7]
  China SEPA. GEF Project Brief (GF/CPR/02/010)2003
8. [8]
  Zhang W, Ye Y B, Hu D, Ou L B, Wang X J. J. Environ. Monit., 2010,12(11):2153-2160
9. [9]
  Zhang Y F, Fu S, Dong Y, Nie H F, Li Z, Liu X C. Bull. Environ. Contam. Toxicol., 2014,92(4):466-471
10. [10]
  Li Y M, Zhang Q H, Ji D S, Wang T, Wang Y W, Wang P, Ding L, Jiang G B. Environ. Sci. Technol., 2009,43(4):1030-1035
11. [11]
  XU Peng-Jun, TAO Bu, LI Nan, ZHENG Sen, ZHAO Hu, FAN Shuang, ZHOU Zhi-Guang, REN Yue, QI Li, CHEN Ji-Ping. Chinese J. Anal.Chem., 2015,43(3):356-365 许鹏军, 陶晡, 李楠, 郑森, 赵虎, 范爽, 周志广, 任玥, 齐丽, 陈吉平.分析化学,2015,43(3):356-365
12. [12]
  Yang G S, Ma L L, Xu D D, Liu L Y, Jia H L, Chen Y, Zhang Y B, Chai Z F. Atmos. Environ., 2012,56:222-227
13. [13]
  Zhang Z L, Huang J, Yu G, Hong H S. Environ. Pollut., 2004,130(2):249-261
14. [14]
  Shi Y, Meng F, Guo F, Lu Y, Wang T, Zhang H. Arch. Environ. Contam. Toxicol., 2005,49(1):37-44
15. [15]
  Li J, Huang Y, Ye R, Yuan G L, Wu H Z, Han P, Fu S. J. Geochem. Explor., 2015,158:177-185
16. [16]
  Jaward F M, Zhang G, Nam J J, Sweetman A J, Obbard J P, Kobara Y, Jones K C. Environ. Sci. Technol., 2005,39(22):8638-8645
17. [17]
  HONG Wei-Zhe, LI Ying-Ming, ZHANG Lin-Nan, BAO Jia, WANG Pu, ZHU Chao-Fei, ZHANG Qing-Hua. Environmental Chemistry, 2015,34(3):410-416 洪维哲, 李英明, 张林楠, 鲍佳, 王璞, 朱超飞, 张庆华.环境化学,2015,34(3):410-416
18. [18]
  Li X M, Zhang Q H, Dai J Y, Gan Y P, Zhou J, Yang X P, Cao H, Jiang G B, Xu M.Q. Chemosphere, 2008, 72(8):1145-1151
19. [19]
  Yu Y, Li Y X, Shen Z Y, Yang Z F, Mo L, Kong Y H, Lou I. Chemosphere, 2014,114:136-143
20. [20]
  Yang G S, Ma L L, Xu D D, Liu L Y, Jia H L, Chen Y, Zhang Y B, Chai Z F. Atmos. Environ., 2012,61:614-619
21. [21]
  Herbert B M J, Halsall C J, Villa S, Jones K C, Kallenborn R. Environ. Sci. Technol., 2005,39(9):2998-3005
22. [22]
  Xu D D, Dan M, Song Y, Chai Z F, Zhuang G S. Atmos. Environ., 2005,39(22):4119-4128
23. [23]
  EPA Method 3545A. Pressurized Fluid Extraction (PFE). United States Environmental Protection Agency, 1996
24. [24]
  Ottonello G, Ferrari A, Magi E. Food Chem., 2014,142:327-333
25. [25]
  Mercier F, Gilles E, Saramito G, Glorennec P, Bot B. J. Chromatogr. A, 2014,1336:101-111
26. [26]
  WANG Dao-Wei, ZHAO Shi-Min, JIN Wei, SHEN Qiu-Ying, HU Ping, HUANG Bin, PAN Xue-Jun. Chinese J. Anal. Chem., 2013,41(6):861-868 王道玮, 赵世民, 金伟, 沈秋莹, 胡平, 黄斌, 潘学军.分析化学,2013,41(6):861-868
27. [27]
  Klees M, Hiester E, Bruckrnann P, Schmidt T C. J. Chromatogr. A, 2013,1300:17-23
28. [28]
  Raeppel C, Fabritius M, Nief M, Appenzeller B M R, Millet M. Talanta, 2014,121:24-29
29. [29]
  YAN Rui, SHAO Ming-Yuan, JU Fu-Long, SONG Da-Qian, ZHANG Han-Qi, YU Ai-Min. Chinese J. Anal. Chem., 2013,41(2):315-316 闫蕊, 邵名媛, 鞠福龙, 宋大千, 张寒琦, 于爱民.分析化学,2013,41(2):315-316
30. [30]
  Lv J G, Shi R G, Chai Y M, Liu Y, Wang Z H, Feng J M, Zhang M. Bull. Environ. Contam. Toxicol., 2010,85(2):137-141
31. [31]
  Wu C F, Luo Y M, Gui T, Huang Y J. Sci. Total Environ., 2014,470:1047-1055
32. [32]
  Zhi H, Zhao Z H, Zhang L. Chemosphere, 2015, 119:1134-1140
33. [33]
  Tang Z W, Huang Q F, Yang Y F, Zhu X H, Fu H H. Ecotox. Environ. Safe, 2013,87:89-97
34. [34]
  GAI Nan, PAN Jing, CHEN Da-Zhou, YANG Yong-Liang. China Environmenalt Science, 2014,34(4):996-1003 盖楠, 潘静, 陈大舟, 杨永亮.中国环境科学,2014,34(4):996-1003

WeChat

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 1119
HTML全文浏览量: 55

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

/

下载: 全尺寸图片幻灯片

分享

用微信扫码二维码

分享至好友和朋友圈