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Gas chromatographic-mass spectrometric identification and quantitation of urinary phenols after derivatization with 4-carbethoxyhexafluorobutyryl chloride, a novel derivative.
J Chromatogr B Biomed Sci Appl. 1997 Feb 21; 689(2):415-21.JC

Abstract

Urinary phenol is analyzed widely to determine benzene exposure in humans. Most methods utilize direct measurements of phenols after extraction from urine using gas chromatography or high-performance liquid chromatography. We describe a novel derivatization of urinary phenols using 4-carbethoxyhexafluorobutyryl chloride after extraction from urine and subsequent analysis by gas chromatography-mass spectrometry. The derivative elutes at significantly higher temperature than phenol and the method is free from interferences from more volatile components in urine. We also observed excellent chromatographic properties of these derivatives. In addition, we observed strong molecular ions for the 4-carbethoxyhexafluorobutyryl derivative of phenol (m/z 344), p-cresol (m/z 358) and the internal standard 3,4-dimethylphenol (m/z 372) and other characteristic ions in the electron ionization, thus aiding in unambiguous identification of these compounds. The protonated molecular ions (m/z 373 for derivatized phenol, m/z 359 for derivatized p-cresol and m/z 373 for the internal standard) were the base peaks (relative abundance 100%) in the chemical ionization, although other secondary peaks were less abundant. The assay is linear for phenol concentration of 1-100 mg/l. The within-run and between-run precisions were 4.8% (mean = 52.4, S.D. = 2.5 mg/l) and 8.1% (mean = 53.0, S.D. = 4.3 mg/l) respectively, and the detection limit was 0.5 mg/l.

Authors+Show Affiliations

Department of Pathology, University of New Mexico Health Sciences Center, Albuquerque 87106, USA.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

9080331

Citation

Dasgupta, A, et al. "Gas Chromatographic-mass Spectrometric Identification and Quantitation of Urinary Phenols After Derivatization With 4-carbethoxyhexafluorobutyryl Chloride, a Novel Derivative." Journal of Chromatography. B, Biomedical Sciences and Applications, vol. 689, no. 2, 1997, pp. 415-21.
Dasgupta A, Blackwell W, Burns E. Gas chromatographic-mass spectrometric identification and quantitation of urinary phenols after derivatization with 4-carbethoxyhexafluorobutyryl chloride, a novel derivative. J Chromatogr B Biomed Sci Appl. 1997;689(2):415-21.
Dasgupta, A., Blackwell, W., & Burns, E. (1997). Gas chromatographic-mass spectrometric identification and quantitation of urinary phenols after derivatization with 4-carbethoxyhexafluorobutyryl chloride, a novel derivative. Journal of Chromatography. B, Biomedical Sciences and Applications, 689(2), 415-21.
Dasgupta A, Blackwell W, Burns E. Gas Chromatographic-mass Spectrometric Identification and Quantitation of Urinary Phenols After Derivatization With 4-carbethoxyhexafluorobutyryl Chloride, a Novel Derivative. J Chromatogr B Biomed Sci Appl. 1997 Feb 21;689(2):415-21. PubMed PMID: 9080331.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Gas chromatographic-mass spectrometric identification and quantitation of urinary phenols after derivatization with 4-carbethoxyhexafluorobutyryl chloride, a novel derivative. AU - Dasgupta,A, AU - Blackwell,W, AU - Burns,E, PY - 1997/2/21/pubmed PY - 1997/2/21/medline PY - 1997/2/21/entrez SP - 415 EP - 21 JF - Journal of chromatography. B, Biomedical sciences and applications JO - J. Chromatogr. B Biomed. Sci. Appl. VL - 689 IS - 2 N2 - Urinary phenol is analyzed widely to determine benzene exposure in humans. Most methods utilize direct measurements of phenols after extraction from urine using gas chromatography or high-performance liquid chromatography. We describe a novel derivatization of urinary phenols using 4-carbethoxyhexafluorobutyryl chloride after extraction from urine and subsequent analysis by gas chromatography-mass spectrometry. The derivative elutes at significantly higher temperature than phenol and the method is free from interferences from more volatile components in urine. We also observed excellent chromatographic properties of these derivatives. In addition, we observed strong molecular ions for the 4-carbethoxyhexafluorobutyryl derivative of phenol (m/z 344), p-cresol (m/z 358) and the internal standard 3,4-dimethylphenol (m/z 372) and other characteristic ions in the electron ionization, thus aiding in unambiguous identification of these compounds. The protonated molecular ions (m/z 373 for derivatized phenol, m/z 359 for derivatized p-cresol and m/z 373 for the internal standard) were the base peaks (relative abundance 100%) in the chemical ionization, although other secondary peaks were less abundant. The assay is linear for phenol concentration of 1-100 mg/l. The within-run and between-run precisions were 4.8% (mean = 52.4, S.D. = 2.5 mg/l) and 8.1% (mean = 53.0, S.D. = 4.3 mg/l) respectively, and the detection limit was 0.5 mg/l. SN - 1387-2273 UR - https://www.unboundmedicine.com/medline/citation/9080331/Gas_chromatographic_mass_spectrometric_identification_and_quantitation_of_urinary_phenols_after_derivatization_with_4_carbethoxyhexafluorobutyryl_chloride_a_novel_derivative_ DB - PRIME DP - Unbound Medicine ER -