Citation: LIANG Jing, ZHUANG Wan'e, LIN Fang, YAO Wensong, WEN Yuyun, OU Yan, GONG Zhenbin. Sample pretreatment for the measurement of phthalate esters in complex matrices[J]. Chinese Journal of Chromatography, ;2014, 32(11): 1242-1250. doi: 10.3724/SP.J.1123.2014.07051 shu

Sample pretreatment for the measurement of phthalate esters in complex matrices

LIANG Jing ^1,3 ,
ZHUANG Wan'e ² ,
LIN Fang ² ,
YAO Wensong ² ,
WEN Yuyun ^1,3 ,
OU Yan ³ ,
GONG Zhenbin ^1,2,,

1.
1. State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361102, China;

Corresponding author: GONG Zhenbin,
Received Date: 30 July 2014
Available Online: 11 August 2014
Fund Project: 环保部环保公益性行业科研专项(201309007) (201309007)福建省自然科学基金重点项目(2012Y0005). (2012Y0005)

Sample pretreatment methods for the measurement of phthalate esters (PAEs) by gas chromatography-mass spectrometry (GC-MS) in various complex matrices, including sediment, soil, suspended particle matter, urban surface dust, Sinonovacula Constricta, cosmetic, leather, plastic and coastal/estuarine seawater, were proposed. The pretreatment which was appropriate for GC-MS detection was focused on the investigation and optimization of operating parameters for the extraction and purification, such as the extraction solvent, the eluant and the adsorbent of solid phase extraction. The results of the study of pretreatment for various complex matrices showed that methylene chloride was the best solvent for the ultrasonic extraction when solid-liquid extraction was used; silica gel was the economical and practical adsorbent for solid-phase extraction for purification; C18 was the most commonly adsorbent for preconcentration of PAE in coastal/estuarine seawater sample; the mixed solution of n-hexane and ethyl acetate with a certain proportion was the suitable SPE eluent. Under the optimized conditions, the spiked recoveries were above 58% and the relative standard deviations (RSDs) were less than 10.5% (n=6). The detection limits (DL, 3σ) were in the range of 0.3 μg/kg (dibutyl phthalate)-5.2 μg/kg (diisononyl phthalate) for sediment, and 6 ng/L (dipropyl phthalate)-67 ng/L (diisodecyl phthalate) for costal/estuarine seawater. The pretreatment method for various complex matrices is prominent for the measurement of the 16 PAEs with GC-MS.
- gas chromatography-mass spectrometry (GC-MS),
- phthalate esters,
- complex matrices,
- sample pretreatment
1. [1]
  [1] Staples C A, Peterson D R, Parkerton T F, et al. Chemosphere, 1997, 35(4): 667
2. [2]
  [2] Wang P, Wang S L, Fan C Q. Chemosphere, 2008, 72(10): 1567
3. [3]
  [3] Fromme H, Küchler T, Otto T, et al. Water Res, 2002, 36(6): 1429
4. [4]
  [4] Zhang L F, Dong L, Ren L J, et al. J Environ Sci, 2012, 24(2): 335
5. [5]
  [5] Langer S, Weschler C J, Fischer A, et al. Atmos Environ, 2010, 44(19): 2294
6. [6]
  [6] Sun J Q, Huang J, Zhang A P, et al. J Hazard Mater, 2013, 248/249(15): 142
7. [7]
  [7] Wormuth M, Scheringer M, Vollenweider M, et al. Risk Anal, 2006, 26(3): 803
8. [8]
  [8] Deng D F, Yan Y L, Xie X J. Freshwater Fisheries (邓冬富, 闫玉莲, 谢小军. 淡水渔业), 2012, 42(2): 55
9. [9]
  [9] Stanley M K, Robillard K A, Staples C A. The Handbook of Environmental Chemistry, 2003, 3: 299
10. [10]
  [10] Wang X Y, Lin X T, Ke H M, et al. Journal of Environment and Health (王小逸, 林兴桃, 客慧明, 等. 环境与健康杂志), 2007, 24(9): 736
11. [11]
  [11] Shen T.[MS Dissertation]. Beijing: Beijing University of Technology (沈婷.[硕士学位论文]. 北京: 北京工业大学), 2009
12. [12]
  [12] Hu X X, Han Z H, Zhou Y K, et al. Environmental Chemistry (胡雄星, 韩中豪, 周亚康, 等. 环境化学), 2007, 26(2): 258
13. [13]
  [13] The European Parliament and the Council of the European Union. Directive 2005/84/EC of the European parliament and of the council of 14 December 2005. (2005-12-27). http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2005:344:0040:0043:EN:PDF
14. [14]
  [14] Ministry of Health of the Peoples Republic of China. Hygienic Standard for Cosmetics. Beijing: Ministry of Health of the Peoples Republic of China (中华人民共和国卫生部. 化妆品卫生规范. 北京: 中华人民共和国卫生部), 2007: 14
15. [15]
  [15] Zhang J, Chen H M. Modern Chemical Industry (张静, 陈会明. 现代化工), 2011, 31(12): 1
16. [16]
  [16] Ranjbari E, Golbabanezhad A, Aliasghar H, et al. Talanta, 2012, 100(15): 447
17. [17]
  [17] Chen H M, Wang C, Wang X, et al. Journal of Instrumental Analysis (陈会明, 王超, 王星, 等. 分析测试学报), 2004, 23(4): 61
18. [18]
  [18] Yan H Y, Liu B M, Du J J, et al. Analyst, 2010, 135(10): 2585
19. [19]
  [19] Fan J C, Wang S T, Huang X H, et al. Chinese Journal of Health Laboratory Technology (樊继彩, 王姝婷, 黄希汇, 等. 中国卫生检验杂志), 2013, 23(5): 1063
20. [20]
  [20] Blair J D, Ikonomou M G, Kelly B C, et al. Environ Sci Technol, 2009, 43(16): 6262
21. [21]
  [21] Gong S G, Kong B, Tuo S X, et al. Chinese Journal of Chromatography (龚淑果, 孔波, 庹苏行, 等. 色谱), 2013, 31(10): 989
22. [22]
  [22] Liu H C, Den W, Chan S F, et al. J Chromatogr A, 2008, 1188(2): 286
23. [23]
  [23] Shen H Y. Talanta, 2005, 66(3): 734
24. [24]
  [24] Liang J, Zhuang W E, Wei D Q, et al. Chinese Journal of Chromatography (梁婧, 庄婉娥, 魏丹琦, 等. 色谱), 2012, 30(3): 273
25. [25]
  [25] Lin F, Wen Y Y, Hong X Y, et al. Analytical Instrumentation (林芳, 温裕云, 洪小燕, 等. 分析仪器), 45(2): 15
26. [26]
  [26] Zhuang W E, Liang J, Huang D R, et al. Journal of Applied Oceanograph (庄婉娥, 梁婧, 黄东仁, 等. 应用海洋学学报), 2013, 32(2): 288
27. [27]
  [27] Yao W S, Zhuang W E, Lin F, et al. Journal of Xiamen University: Natural Science (姚文松, 庄婉娥, 林芳, 等. 厦门大学学报: 自然科学版), 2011, 50(4): 783
28. [28]
  [28] Yao W S.[MS Dissertation]. Xiamen: Xiamen University (姚文松.[硕士学位论文]. 厦门: 厦门大学), 2010
29. [29]
  [29] Zhuang W E.[PhD Dissertation]. Xiamen: Xiamen University (庄婉娥.[博士学位论文]. 厦门: 厦门大学), 2012
30. [30]
  [30] Liang J.[PhD Dissertation]. Xiamen: Xiamen University (梁婧.[博士学位论文]. 厦门: 厦门大学), 2014
31. [31]
  [31] Meng J R, Bu J, Deng C H, et al. J Chromatogr A, 2011, 1218(12): 1585
32. [32]
  [32] Cao B, Ma J, Li Y M Z, et al. Journal of Geology (曹攽, 马军, 李云木子, 等. 地质学刊), 2011, 35(1): 73
33. [33]
  [33] Llompart M, Celeiro M, Pablo Lamas J, et al. J Chromatogr A, 2013, 1293: 10
34. [34]
  [34] Pu D L, Sang J L, Ren K L, et al. Guangdong Trace Elements Science (蒲德岚, 桑佳陆, 任凯莉, 等. 广东微量元素科学), 2014, 21(1): 1
35. [35]
  [35] Lin Z P, Ikonomou M G, Jing H W, et al. Environ Sci Technol, 2003, 37(10): 2100
36. [36]
  [36] Zeng F, Chen L X, Cui K X, et al. Chinese Journal of Analytical Chemistry (曾锋, 陈丽旋, 崔昆鑫, 等. 分析化学), 2008, 33(8): 1063
37. [37]
  [37] Fu S L, Ding L, Zhu S H, et al. Chinese Journal of Chromatography (付善良, 丁利, 朱邵华, 等. 色谱), 2011, 29(8): 737
38. [38]
  [38] Farajzadeh M A, Mogaddam M R A. Anal Chim Acta, 2012, 728: 31
39. [39]
  [39] Liu P Y, Gao L, Shen J, et al. Chinese Journal of Chromatography (刘芃岩, 高丽, 申杰, 等. 色谱), 2010, 28(5): 517
40. [40]
  [40] Wu H Q, Zhu Z X, Huang X L, et al. Journal of Instrumental Analysis (吴惠勤, 朱志鑫, 黄晓兰, 等. 分析测试学报), 2011, 30(10): 1079
41. [41]
  [41] Xu D M, Deng X J, Fang E H, et al. J Chromatogr A, 2014, 1324: 49
42. [42]
  [42] Zheng H H, Li J, Wu D N, et al. Chinese Journal of Analysis Laboratory (郑和辉, 李洁, 吴大南, 等. 分析试验室), 2008, 27(7): 75
43. [43]
  [43] Li X J, Zeng Z R, Chen Y, et al. Talanta, 2004, 63(5): 1013
44. [44]
  [44] Huang Y H. Plastics Science and Technology (黄永辉. 塑料科技), 2011, 39(1): 94
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