Validation of a Manual Headspace Gas Chromatography Method for Determining Volatile Compounds in Biological Fluids

Background We report the validation of a method for the determination of acetaldehyde, acetone, methanol, and ethanol in biological fluids using manual headspace sample introduction and an acetonitrile internal standard. Methods This method uses a capillary column ( l = 30 m, I.D. = 0.25 mm, d F = 0.25 μm) installed in a gas chromatography–flame ionization detector (GC-FID) apparatus with a run time of 7.5 minutes. Results Analysis of the retention times and the resolution of the analyte peaks demonstrated excellent separation without widening of the peaks. Precision and accuracy were good (interassay precision <15% and recovery between 85% and 115%) in both blood and urine. Conclusion The method was linear (r >0.99) over the analytical measurement range (AMR) of each analyte.

[1]  N. A. Al katheeri,et al.  Rapid and sensitive static headspace gas chromatography-mass spectrometry method for the analysis of ethanol and abused inhalants in blood. , 2004, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[2]  Lúcio Flávio,et al.  Validação em métodos cromatográficos e eletroforéticos , 2004 .

[3]  Michael Zilly,et al.  Highly sensitive gas chromatographic determination of ethanol in human urine samples. , 2003, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[4]  B. D. de Martinis,et al.  Automated headspace solid-phase microextraction and capillary gas chromatography analysis of ethanol in postmortem specimens. , 2002, Forensic science international.

[5]  A. Parczewski,et al.  Optimization of solid-phase microextraction conditions for gas chromatographic determination of ethanol and other volatile compounds in blood. , 2002, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[6]  N. Sakura,et al.  Determination of acrolein by headspace solid-phase microextraction gas chromatography and mass spectrometry. , 2001, Journal of chromatography. B, Biomedical sciences and applications.

[7]  Philippe Hubert,et al.  The SFSTP guide on the validation of chromatographic methods for drug bioanalysis: from the Washington Conference to the laboratory , 1999 .

[8]  T. Kumazawa,et al.  Ultra-sensitive method for determination of ethanol in whole blood by headspace capillary gas chromatography with cryogenic oven trapping. , 1999, Journal of chromatography. B, Biomedical sciences and applications.

[9]  F. Taggi,et al.  Ethanol in biological fluids: headspace GC measurement. , 1995, Journal of analytical toxicology.

[10]  F. Tagliaro,et al.  Chromatographic methods for blood alcohol determination. , 1992, Journal of chromatography.

[11]  K. Dubowski Alcohol determination in the clinical laboratory. , 1980, American journal of clinical pathology.

[12]  A. Parczewski,et al.  Concentration of ethanol and other volatile compounds in the blood of acutely poisoned alcoholics. , 2002, Alcohol.