Tags

Type your tag names separated by a space and hit enter

In situ derivatization/solid-phase microextraction coupled with gas chromatography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood.
Rapid Commun Mass Spectrom. 2008 Apr; 22(7):1023-31.RC

Abstract

An in situ derivatization solid-phase microextraction (SPME) method has been developed for the determination of the trichloroethylene (TCE) metabolites, trichloroacetic acid (TCA), dichloroacetic acid (DCA) and trichloroethanol (TCOH), in rat blood. The analytical procedure involves derivatization of TCA and DCA to their ethyl esters with acidic ethanol, headspace sampling using SPME, and gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS) determination. Parameters affecting both derivatization efficiency and the headspace SPME procedure, such as the concentration of sulfuric acid, amount of ethanol, derivatization-extraction temperature and time, sample preheating time, agitator speed and desorption conditions, were optimized. The method showed good linearity over the range of 1-1000 ng/mL in rat blood for each metabolite with correlation coefficients (R(2)) higher than 0.99. The intra-day and inter-day precision and accuracy were less than 10%. The relative recoveries for all analytes were greater than 84%. Validation results demonstrated that selected ion monitoring of the (35)Cl and (37)Cl isotopes using NCI resulted in reliable and sensitive quantitation of all three TCE metabolites. This validated method was successfully applied to study the toxicokinetic behavior of TCE metabolites following a 1 mg/kg oral dose of TCE.

Links

Publisher Full Text (DOI)

Authors+Show Affiliations

Liu Y
Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USA.
Muralidhara S
No affiliation info available
Bruckner JV
No affiliation info available
Bartlett MG
No affiliation info available

MeSH

AnimalsAnionsBlood Chemical AnalysisEnvironmental PollutantsGas Chromatography-Mass SpectrometryMaleRatsRats, Sprague-DawleyReproducibility of ResultsSensitivity and SpecificitySolid Phase ExtractionSpectrometry, Mass, Electrospray IonizationTrichloroethylene

Pub Type(s)

Evaluation Study
Journal Article
Research Support, U.S. Gov't, Non-P.H.S.

Language

eng

PubMed ID

18320547

Citation

Liu, Yongzhen, et al. "In Situ Derivatization/solid-phase Microextraction Coupled With Gas Chromatography/negative Chemical Ionization Mass Spectrometry for the Determination of Trichloroethylene Metabolites in Rat Blood." Rapid Communications in Mass Spectrometry : RCM, vol. 22, no. 7, 2008, pp. 1023-31.
Liu Y, Muralidhara S, Bruckner JV, et al. In situ derivatization/solid-phase microextraction coupled with gas chromatography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood. Rapid Commun Mass Spectrom. 2008;22(7):1023-31.
Liu, Y., Muralidhara, S., Bruckner, J. V., & Bartlett, M. G. (2008). In situ derivatization/solid-phase microextraction coupled with gas chromatography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood. Rapid Communications in Mass Spectrometry : RCM, 22(7), 1023-31. https://doi.org/10.1002/rcm.3453
Liu Y, et al. In Situ Derivatization/solid-phase Microextraction Coupled With Gas Chromatography/negative Chemical Ionization Mass Spectrometry for the Determination of Trichloroethylene Metabolites in Rat Blood. Rapid Commun Mass Spectrom. 2008;22(7):1023-31. PubMed PMID: 18320547.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - In situ derivatization/solid-phase microextraction coupled with gas chromatography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood. AU - Liu,Yongzhen, AU - Muralidhara,Srinivasa, AU - Bruckner,James V, AU - Bartlett,Michael G, PY - 2008/3/6/pubmed PY - 2008/5/30/medline PY - 2008/3/6/entrez SP - 1023 EP - 31 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 22 IS - 7 N2 - An in situ derivatization solid-phase microextraction (SPME) method has been developed for the determination of the trichloroethylene (TCE) metabolites, trichloroacetic acid (TCA), dichloroacetic acid (DCA) and trichloroethanol (TCOH), in rat blood. The analytical procedure involves derivatization of TCA and DCA to their ethyl esters with acidic ethanol, headspace sampling using SPME, and gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS) determination. Parameters affecting both derivatization efficiency and the headspace SPME procedure, such as the concentration of sulfuric acid, amount of ethanol, derivatization-extraction temperature and time, sample preheating time, agitator speed and desorption conditions, were optimized. The method showed good linearity over the range of 1-1000 ng/mL in rat blood for each metabolite with correlation coefficients (R(2)) higher than 0.99. The intra-day and inter-day precision and accuracy were less than 10%. The relative recoveries for all analytes were greater than 84%. Validation results demonstrated that selected ion monitoring of the (35)Cl and (37)Cl isotopes using NCI resulted in reliable and sensitive quantitation of all three TCE metabolites. This validated method was successfully applied to study the toxicokinetic behavior of TCE metabolites following a 1 mg/kg oral dose of TCE. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/18320547/In_situ_derivatization/solid_phase_microextraction_coupled_with_gas_chromatography/negative_chemical_ionization_mass_spectrometry_for_the_determination_of_trichloroethylene_metabolites_in_rat_blood_ DB - PRIME DP - Unbound Medicine ER -

Related Citations

More