固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂

引用本文: 严小菊, 何欢, 彭英, 王晓萌, 高占啟, 杨绍贵, 孙成, 固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂[J]. 分析化学, 2012, 40(11): 1693-1697. doi: 10.3724/SP.J.1096.2012.20298 shu

Citation: YAN Xiao-Ju, HE Huan, PENG Ying, WANG Xiao-Meng, GAO Zhan-Qi, YANG Shao-Gui, CHEN Hong-Zhe, SUN Cheng. Determination of Organophosphorus Flame Retardants in Surface Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(11): 1693-1697. doi: 10.3724/SP.J.1096.2012.20298 shu

固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂

通讯作者: 孙成; 孙成

基金项目:
本文系国家自然科学基金(No.2127061) (No.2127061)

江苏省环境监测科研基金项目(No.1115) (No.1115)

江苏省研究生创新计划(No.CXZZ11-0050)资助 (No.CXZZ11-0050)

摘要: 建立了固相萃取(SPE)与气相色谱质谱(GC-MS)联用测定自然水体中8种有机磷酸酯阻燃剂(OPFRs)OPFRs的分析方法。通过对GC-MS条件与SPE萃取条件的优化, 采用Poly-Sery PSD固相萃取小柱对水样进行富集浓缩, 用4 mL乙酸乙酯洗脱, 以选择离子扫描方式对目标物进行定性和定量分析, 并采用内标法定量。本方法在对应OPFRs线性范围内的线性相关系数为0.9937-0.9995;检出限为0.006-0.850 ng/L;定量限为0.015-2.0 ng/L。除磷酸三(2-乙基)己基酯(TEHP)外, 其它OPFRs的加标回收率为70.3%-114.3%。TEHP加标10和50 ng/L时,回收率为64.0%-69.3%;加标100 ng/L时回收率为34.3%。将本方法应用于太湖梅梁湾水体中OPFRs分析, 其总浓度值为1000-2700 ng/L。

关键词:

English

Determination of Organophosphorus Flame Retardants in Surface Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

1.
School of the Environment, Nanjing University, State Key Laboratory of Pollution Control and Resources Reuse, Nanjing 210046, China

Corresponding author: 孙成; 孙成

Received Date: 23 March 2012
Fund Project:
本文系国家自然科学基金(No.2127061)

江苏省环境监测科研基金项目(No.1115)

江苏省研究生创新计划(No.CXZZ11-0050)资助

Abstract: Organophosphorus flame retardants (OPFRs), as their increasing production and consumption, are almost ubiquitous in environmental compartments. In this study, a solid phase extraction (SPE) coupled with gas chromatography-mass spectrometric (SPE-GC-MS) method was developed for the determination of 8 typical OPFRs. The targets in water samples were concentrated by Poly-Sery PSD SPE cartridge, and then eluted by 4 mL ethyl acetate. The OPFRs were qualified and quantified by GC-MS in selective ion scan monitoring method (SIM). Good linearity was observed in the range of 2 to 200 ng/L OPFRs with correlation coefficients varing between 0.9937 and 0.9995. The limits of detection and limits of quantification ranged from 0.006 to 0.850 ng/L and 0.015 to 2.000 ng/L, respectively. Spiked recoveries of pure water and river water samples ranged from 70.3% to 114.3%, with the relative standard deviations less than 15%, except for tri(2-ethylhexyl)phosphate(TEHP). The satisfied recovery of TEHP was achieved when the spiked concentration was less than 50 ng/L. The results showed that the SPE-GC-MS analytical method established was sensitive and accurate for the determination of OPFRs in surface water samples. Then the method was applied to analyze OPFRs in the water collected in Meiliang Bay of Taihu Lake, and it was found that the total concentration of OPFRs was ranging from 1000 to 2700 ng/L.

Key words:

1. [1]
  1 Reemtsma T, Quintana J B, Rodil R, Garcia-Lopez M, Rodriguez I. Trac-Trend Anal. Chem., 2008, 27(9): 727-7371 Reemtsma T, Quintana J B, Rodil R, Garcia-Lopez M, Rodriguez I. Trac-Trend Anal. Chem., 2008, 27(9): 727-737
2. [2]
  2 Weil E D, Levchik S V. J. Fire Sci., 2008, 26(3): 243-2812 Weil E D, Levchik S V. J. Fire Sci., 2008, 26(3): 243-281
3. [3]
  3 Marklund A, Andersson B; Haglund P. Chemosphere, 2003, 53(9): 1137-11463 Marklund A, Andersson B; Haglund P. Chemosphere, 2003, 53(9): 1137-1146
4. [4]
  4 Andresen J A, Grundmann A, Bester K. Sci. Total Environ., 2004, 332(1-3): 155-1664 Andresen J A, Grundmann A, Bester K. Sci. Total Environ., 2004, 332(1-3): 155-166
5. [5]
  5 Marklund A, Andersson B; Haglund P. Environ. Sci. Technol., 2005, 39(10): 3555-35625 Marklund A, Andersson B; Haglund P. Environ. Sci. Technol., 2005, 39(10): 3555-3562
6. [6]
  6 Kim S D, Cho J,Kim I S,Vanderford B J; Snyder S A. Water Res., 2007, 41(5): 1013-10216 Kim S D, Cho J,Kim I S,Vanderford B J; Snyder S A. Water Res., 2007, 41(5): 1013-1021
7. [7]
  7 Bacaloni A, Cucci F,Guarino C, Nazzari M, Samperi R, Lagana A. Environ. Sci. Technol., 2008, 42(6): 1898-19037 Bacaloni A, Cucci F,Guarino C, Nazzari M, Samperi R, Lagana A. Environ. Sci. Technol., 2008, 42(6): 1898-1903
8. [8]
  8 Stapleton H M, Klosterhaus S, Eagle S, Fuh J, Meeker J D, Blum A, Webster T F. Environ. Sci. Technol., 2009, 43(19): 7490-74958 Stapleton H M, Klosterhaus S, Eagle S, Fuh J, Meeker J D, Blum A, Webster T F. Environ. Sci. Technol., 2009, 43(19): 7490-7495
9. [9]
  9 Fries E, Mihajlovic I. J. Environ. Monitor., 2011, 13(10): 2692-26949 Fries E, Mihajlovic I. J. Environ. Monitor., 2011, 13(10): 2692-2694
10. [10]
  10 Kim J W, Isobe T, Chang K H, Amano A, Maneja R H, Zamora P B, Siringan F P, Tanabe S. Environ. Pollut., 2011, 159(12): 3653-365910 Kim J W, Isobe T, Chang K H, Amano A, Maneja R H, Zamora P B, Siringan F P, Tanabe S. Environ. Pollut., 2011, 159(12): 3653-3659
11. [11]
  11 Wang X W, J-f L, Yin Y G. J. Chromatogr. A, 2011, 1218(38): 6705-671111 Wang X W, J-f L, Yin Y G. J. Chromatogr. A, 2011, 1218(38): 6705-6711
12. [12]
  12 Ingerowski G, Friedle A, Thumulla J. Indoor Air., 2001, 11(3): 145-14912 Ingerowski G, Friedle A, Thumulla J. Indoor Air., 2001, 11(3): 145-149
13. [13]
  13 Follmann W, Wober J. Toxicol. Lett., 2006, 161(2): 124-13413 Follmann W, Wober J. Toxicol. Lett., 2006, 161(2): 124-134
14. [14]
  14 Lin K. Environ. Chem. Lett., 2009, 7 (4): 309-31214 Lin K. Environ. Chem. Lett., 2009, 7 (4): 309-312
15. [15]
  15 Makinen M S E, Makinen M R A, Koistinen J T B, Pasanen A L, Pasanen P O, Kalliokoski P I, Korpi A M.Environ. Sci. Technol., 2009, 43(3): 941-94715 Makinen M S E, Makinen M R A, Koistinen J T B, Pasanen A L, Pasanen P O, Kalliokoski P I, Korpi A M.Environ. Sci. Technol., 2009, 43(3): 941-947
16. [16]
  16 Andresen J, Bester K. Water Res., 2006, 40(3): 621-62916 Andresen J, Bester K. Water Res., 2006, 40(3): 621-629
17. [17]
  17 Mihajlovic I, Miloradov M V, Fries E. Environ. Sci. Technol., 2011, 45(6): 2264-226917 Mihajlovic I, Miloradov M V, Fries E. Environ. Sci. Technol., 2011, 45(6): 2264-2269
18. [18]
  18 Martinez-Carballo E, Gonzalez-Barreiro C, Sitka A, Scharf S, Gans O. Environ. Sci. Technol., 2007, 388(1-3): 290-29918 Martinez-Carballo E, Gonzalez-Barreiro C, Sitka A, Scharf S, Gans O. Environ. Sci. Technol., 2007, 388(1-3): 290-299

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂

通讯作者: 孙成; 孙成

English

Determination of Organophosphorus Flame Retardants in Surface Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

Corresponding author: 孙成; 孙成

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂

通讯作者: 孙成; 孙成

English

Determination of Organophosphorus Flame Retardants in Surface Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

Corresponding author: 孙成; 孙成

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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