A hydrophilic interaction liquid chromatography electrospray tandem mass spectrometry method for the simultaneous determination of gamma-hydroxybutyrate and its precursors in forensic whole blood

作者：Sorensen Lambert K^*; Hasselstrom Jorgen B

来源：Forensic Science International, 2012, 222(1-3): 352-359.

DOI：10.1016/j.forsciint.2012.07.017

• Gamma-hydroxybutyrate (GHB)
• Gamma-butyrolactone (GBL)
• 1,4-Butanediol
• Whole blood
• LC-MS/MS

A liquid-chromatography-tandem-mass-spectrometry method using pneumatically assisted electrospray ionisation (LC-ESI-MS/MS) was developed for the simultaneous determination of gamma-hydroxybutyric acid (GHB), gamma-butyrolactone (GBL) and 1,4-butanediol (1,4-BD) in human ante-mortem and post-mortem whole blood. The blood proteins were precipitated using a mixture of methanol and acetonitrile, and the extract was cleaned-up by passage through a polymeric strong cation exchange sorbent. Separation of the analytes and their structural isomers was obtained using a column with a zwitterionic stationary phase. Matrix-matched calibrants, combined with isotope dilution, were used for quantitative analysis. GHB was determined in both positive and negative ion modes. The relative intra-laboratory reproducibility standard deviations were better than 10% and 6% for blood samples at concentrations of 2 mg/L and 20-150 mg/L, respectively. The mean true extraction recoveries were 80% for GHB and greater than 90% for GBL and 1,4-BD at concentration levels of 20-50 mg/L. The limits of detection were approximately 0.5 mg/L for GHB and GBL, and 0.02 mg/L for 1,4-BD in ante-mortem blood. The corresponding lower limits of quantification were less than 1 mg/L for GHB and GBL, and less than 0.1 mg/L for 1,4-BD. GBL was unstable in whole blood freshly preserved with a sodium fluoride oxalate mixture, but the stability could be improved significantly by preservation with a sodium fluoride citrate EDTA mixture.

• 出版日期2012-10-10