Environmental Analysis Health and Toxicology

The Korean Society of Environmental Health and Toxicology (환경독성보건학회)
권호 표지

Part-Per-Trillion Level Determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water Samples

GC/MS-SIM 방법에 의한 수돗물 중 알킬페놀, 플로로페놀과 비스페놀 A의 ppt 정량

  • Kim, Hyub (Technology Innovation Center, Sangju National University)
  • 김협 (국립상주대학교, TIC)
  • Published : 2003.09.01
Download PDF
⟨ Previous Next ⟩

Abstract

A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the CC/MS SIM mode. The recoveries were 86.6 ∼ 105.2％ (isoBOC derivatization) and 97.6∼484.5％ (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol h for SIM were 0.001∼0.050 $\mu\textrm{g}$/1 (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/1 (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). When these methods were applied to tap water samples, the range of concentrations were 22.8∼31.3 ng/1 in 2,4-dichlorophenol, 28.6∼70.3 ng/1 in pentachlorophenol, 15.2∼17.4 ng/1 in t-butylphenol, 10.8∼13.2 ng/1 in t-octylphenol and 17.6∼36.3 ng/l in bisphenol A, respectively.

Keywords

References

  1. 김 협, 홍종기, 김용화, 김경례, 기체 크로마토그래피/질량 분석기를 이용한 field-screening 적용을 위한 알킬페놀류, 클로로페놀류 및 비스페놀 A의 isoBOC 유도체, TBDMS 유도체와 US EPA 방법의 비교, 분석과학회지 2002; 15(3): 196-213
  2. 김 협, 김진호. 기체 크로마토그래피/질량분석기를 이용한 종이류 중 알킬페놀류, 클로로페놀류 및 비스페놀 A 정량, 환경독성학회지 2003; 18(1): 45-55
  3. Achilli G, Celrino GP, d'Eril GM and Bird S. Simultaneous determination of 27 phenols and herbicides in water by high-performance liquid chromatography with muti-electrode electrochemical detection, J. Chromatogr. A 1995; 697: 357-362 https://doi.org/10.1016/0021-9673(94)00791-7
  4. Boyd ThJ. Indentification and quantification of mono-, di- and trihydroxybenzenes(phenols) at trace concentrations in seawater by aqueous acetylation and gas chromatographic-mass spectrometric analysis, J. Chromatogr. 1994; 662: 281-292 https://doi.org/10.1016/0021-9673(94)80516-4
  5. EPA method 625, Base/neutrals and acids; http://www.epa.gov/epaoswer/hazwaste/test
  6. Heberer T and Stan HJ. Detection of more than 50 substituted phenols as their t-butyldimethylsilyl derivatives using gas chromatography-mass spectrometry, Analytica Chemica Acta 1997; 341: 21-34 https://doi.org/10.1016/S0003-2670(96)00557-0
  7. Helaleh MIH, Takabayashi Y, Fujii Sand Korenaga T. Gas chromatographic-mass spectrometric method for separation and detection of endorcrine disruptors from environmental water samples, Analytica Chemica Acta 2001; 428: 227-234 https://doi.org/10.1016/S0003-2670(00)01251-4
  8. Illinois EPA Endocrine Disruptors Strategy; http://www.nihs.go.jp/hse/environ/illiepatable.html
  9. John AF. Accelerated solvent extraction: An evaluation for screening of soils for selected U.S. EPA semivolatile organic priority pollutants, Environ. Sci. Technol. 1997; 31: 1120-1127 https://doi.org/10.1021/es9606283
  10. Kim K-R and Kim H. Gas chromatographic profiling and screening for phenols as isobutoxycarbonyl derivatives in aqueous samples, J. Chromatogr. A 2000; 866: 87 -96 https://doi.org/10.1016/S0021-9673(99)01068-7
  11. Lee HB, You RLH and Fowlie PJA. Chemical derivatization Analysis of Phenols. Part VI. Determination of chlorinated phenolics in Pulp and paper effluents, J. Assoc. Off. Anal. Chem. 1989; 72(6): 979-984
  12. Lee HB, Stokker YD and Chau ASY, Analysis of Phenols by Chemical Derivatization. V. Determination of Penta-chlorophenol and 19 Other Chlorinated Phenols in Sediments, J. Assoc. Off. Anal. Chem. 1987; 70(6): 1003-1008
  13. Lee HB, Weng LD and Chau ASY, Chemical Derivatization Analysis of Pesticide Residues. IX. Analysis of Phenol and 21 Chlorinated Phenols in Natural Waters by Formation of Pentafluorobenzyl Ether Derivatives, J. Assoc. Off. Anal. Chem. 1984; 67(6): 1086-1091
  14. Masque N, Pocurull E, Marce RM and Borrull F. Determination of eleven priority EPA phenolics at ng L-l levels by on-line solid-phase extraction and liquid chromatography with UV and electrochemical detection, Chromatographia 1998; 47: 176-182 https://doi.org/10.1007/BF02466578
  15. Moder M, Schrader S, Franck U and Popp P. Determination of phenolic compounds in water by solid-phase micro extraction, Fresenius J. Anal Chem. 1997; 357: 326-332 https://doi.org/10.1007/s002160050162
  16. Penalver A, Pocurull E, Borrull F and Marce RM. Solid-phase microextraction coupled to high-performance liquid chromatography to determine phenolic compounds in water samples, J. Chromatogr. A 2002; 976: 382-390
  17. Rodriguez I, Mejuto MC, Bollain MH and Cela R. Evaluation of two solid-phase extraction procedures for the preconcentration of chlorophenols in drinking water, J. Chromatogr. A 1997; 786: 285-292 https://doi.org/10.1016/S0021-9673(97)00579-7
  18. Shin H-S, Park C-H, Park S-J and Pyo H-S. Sensitive determination of bisphenol A in environmental water by gas chromatography with nitrogen-phosphorus detection after cyanomethylation, J. Chromatogr. A 2001; 912: 119-125 https://doi.org/10.1016/S0021-9673(01)00570-2
  19. SPEED 98/JEA; http://www.eic.or.jp/eanet/e/end/sp98.html. Validation Requirements; http://www.aoac.org
  20. Vom Saal FS, Cooke PS, Buchanan DL, Palanza P, Thayer KA, Nagel SC, Parmigiani S and Weshons WV. Texicol. Ind. Health 1998; 14: 239 https://doi.org/10.1177/074823379801400115
  21. Wissiack R and Rosenberg E. Universal screening method for the determination of US environmental protection agency phenols at the lower ng $l^{-1}$ level in water samples by on-line solid-phase extraction-high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry within a single run, J. Chromatogr. A 2002; 963: 149-157 https://doi.org/10.1016/S0021-9673(02)00546-0
  22. Yergey AL, Edmonds CG, Lewis IAS and Vestal ML. Liquid Chromatography/Mass Spectrometry, Plenum Press, New York 1990