Citation: LAO Wenjian. Analysis of toxaphene and its eight congeners in sediment and fish tissue by gas chromatography-negative ion mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(7): 667-673. doi: 10.3724/SP.J.1123.2013.06030 shu

Analysis of toxaphene and its eight congeners in sediment and fish tissue by gas chromatography-negative ion mass spectrometry

LAO Wenjian ^,

1.
Southern California Coast Water Research Project, Costa Mesa 92626, CA, USA

Corresponding author: LAO Wenjian,
Received Date: 17 June 2013

Toxaphene quantification incorporating gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS) offers improved sensitivity and specificity. The U.S. Environmental Protection Agency (USEPA) recently released a GC/NCI-MS method (Method 8276) for the measurement of technical toxaphene and eight specific congeners (Hx-Sed, Hp-Sed, P26, P41, P40, P44, P50 and P62). However, there is still lack of a practical and complete analytical method including sample extraction, clean up, instrumental analysis, and data analysis. The goal of this work was to develop a ready-to-use method for the quantification of total toxaphene and the eight congeners. Sediment and salmon fish tissue were selected as sample matrices and extracted with methylene chloride using an accelerated solvent extraction system. The sample extracts were cleaned up with active copper powder or gel permeation chromatography, and finally silica/alumina combination column. Separation was performed on a DB-XLB column. GC/NCI-MS was operated under selected ion monitoring mode with an identical set of confirmation and quantitation ions for total toxaphene and the eight congeners. Oxygen reaction of polychlorinated biphenyls (PCB) was monitored by PCB204, an internal calibration standard, and the reaction level was kept below 1%. Average relative response factors were used in quantitation. Quantitation of total toxaphene employed the sum of all detectable (S/N ≥ 3) 6-Cl to 10-Cl homolog peak areas, while the individual congeners were quantified followed the standard procedures for single analytes. Multi-point calibration solutions ranged from 0.5 (5 for P62) to 500 μ g/L for the individual congeners, and 50 to 500 μ g/L for technical toxaphene, with the lowest calibration levels as lower limits of quantitation. Average congener recovery was (90.8±17.4)% (n=10) in spiked sediment with relative standard deviations of 5.4%-12.8% (n=10), underscoring an excellently accurate and precise method. The method was applied to analyze sediment and fish tissue samples.
- gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS),
- toxaphene,
- toxaphene congener,
- sediment,
- fish tissue
1. [1]
  [1] Voldner E C, Li Y F, Chemosphere, 1993, 27(10): 2073
2. [2]
  [2] de Geus H J, Besselink H, Brouwer A, et al. Environ Health Perspect, 1999, 107: 115
3. [3]
  [3] Wong F, Alegria H A, Bidleman T F. Environ Pollut, 2010, 158(3): 749
4. [4]
  [4] Kucklick J R, Helm P A. Anal Bioanal Chem, 2006, 386(4): 819
5. [5]
  [5] Korytar P, van Stee L L P, Leonards P E G, et al. J Chromatogr A, 2003, 994(1/2): 179
6. [6]
  [6] Vetter W. Chemosphere, 1993, 26(6): 1079
7. [7]
  [7] Maruya K A, Francendese L, Manning R O. Estuaries, 2005, 28(5): 786
8. [8]
  [8] Krock B, Vetter W, Luckas B. Chemosphere, 1997, 35(7): 1519
9. [9]
  [9] Maruya K A, Walters T L, Manning R O. Estuaries, 2001, 24(4): 585
10. [10]
  [10] Smalling K L, Maruya K A. J Sep Sci, 2001, 24(2): 104
11. [11]
  [11] Bordajandi L R, Ramos J J, Sanz J, et al. J Chromatogr A, 2008, 1186(1/2): 312
12. [12]
  [12] de Geus H J, Baycan-Keller R, Oehme M, et al. J High Resolut Chromatogr, 1998, 21(1): 39
13. [13]
  [13] Zhang B, Zheng M H, Liu G R, et al. Chinese Journal of Analytical Chemistry (张兵, 郑明辉, 刘国瑞, 等. 分析化学), 2012, 40(8): 1213http://wuxizazhi.cnki.net/Magazine/FXHX201208.html
14. [14]
  [14] Swackhamer D L, Charles M J, Hites R A. Anal Chem, 1987, 59(6): 913
15. [15]
  [15] Xia X Y, Crimmins B S, Hopke P K, et al. Anal Bioanal Chem, 2009, 395(2): 457
16. [16]
  [16] Skopp S, Oehme M, Chu F L, et al. Environ Sci Technol, 2002, 36(12): 2729
17. [17]
  [17] Gouteux B, Lebeuf M, Trottier S, et al. Chemosphere, 2002, 49(2): 183
18. [18]
  [18] Chan H M, Yeboah F. Chemosphere, 2000, 41(4): 507
19. [19]
  [19] Veyrand B, Venisseau A, Marchand P, et al. J Chromatogr B, 2008, 865(1/2): 121
20. [20]
  [20] Fowler B. Chemosphere, 2000, 41(4): 487
21. [21]
  [21] Santos F J, Galceran M T, Caixach J, et al. Rapid Commun Mass Spectrom, 1997, 11(4): 341
22. [22]
  [22] Lao W J, Tsukada D, Maruya K A. J Chromatogr A, 2012, 1270: 262
23. [23]
  [23] SN 0502-95
24. [24]
  [24] YC/T 180-2004
25. [25]
  [25] Wang M T, Liu Z Y, Mu J, et al. Dyeing and Finishing (王明泰, 刘志研, 牟峻, 等. 印染), 2006(6): 37http://www.redlib.cn/qikan/4919/200606.htm
26. [26]
  [26] Xie Y L, Rao Z, Wang X H, et al. Journal of Instrumental Analysis (谢原利, 饶竹, 王晓华, 等. 分析测试学报), 2009, 28(7): 804http://wuxizazhi.cnki.net/Search/TEST200907009.html
27. [27]
  [27] Zhang B, Wu J J, Liu G R, et al. Chinese Journal of Chromatography (张兵, 吴嘉嘉, 刘国瑞, 等. 色谱), 2010, 28(5): 456
28. [28]
  [28] Tian S Q, Mao X H, Miao S, et al. Chinese Journal of Chromatography (田绍琼, 毛秀红, 苗水, 等. 色谱), 2012, 30(1): 14
29. [29]
  [29] Xie Y L, Rao Z, Wang M, et al. Rock and Mineral Analysis (谢原利, 饶竹, 王沫, 等. 岩矿测试), 2008, 27(5): 363http://wuxizazhi.cnki.net/Search/YKCS200805011.html
30. [30]
  [30] Liu J S, Liu H Y, Zhang H, et al. Chinese Journal of Environmental Science and Technology (刘婕丝, 刘红玉, 张慧, 等. 环境科学与技术), 2007, 30(10): 90http://www.cnki.com.cn/Article/CJFDTotal-YZZK200601007.htm
31. [31]
  [31] Carlin F J, Revells H L, Reed D L. Chemosphere, 2000, 41(4): 481
32. [32]
  [32] USEPA. Method 8276-2012. [2013-06-10]. http://www.epa.gov/osw/hazard/testmethods/pdfs/8276.pdf
33. [33]
  [33] Meng X Z, Blasius M E, Gossett R W, et al. Environ Pollut, 2009, 157: 2731
34. [34]
  [34] Lao W, Tsukada D, Greensteint D J, et al. Environ Toxicol Chem, 2010, 29(4): 843
35. [35]
  [35] Maruya K A, Wakeham S G, Vetter W, et al. Environ Toxicol Chem, 2000, 19(9): 2198
36. [36]
  [36] Li Y F. J Geophys Res-Atmosphere, 2001, 106(D16): 17919
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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

Analysis of toxaphene and its eight congeners in sediment and fish tissue by gas chromatography-negative ion mass spectrometry

南开大学师唯/华北电力大学（保定）刘景维：二维配位聚合物中有序的亲锂冠醚位点用于无枝晶锂沉积

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通讯作者: 陈斌, bchen63@163.com