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A hydrophilic interaction liquid chromatography electrospray tandem mass spectrometry method for the simultaneous determination of γ-hydroxybutyrate and its precursors in forensic whole blood.
Forensic Sci Int. 2012 Oct 10; 222(1-3):352-9.FS

Abstract

A liquid-chromatography-tandem-mass-spectrometry method using pneumatically assisted electrospray ionisation (LC-ESI-MS/MS) was developed for the simultaneous determination of γ-hydroxybutyric acid (GHB), γ-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.

Authors+Show Affiliations

Section for Toxicology and Drug Analysis, Department of Forensic Medicine, Aarhus University, Brendstrupgaardsvej 100, 8200 Aarhus N, Denmark. lks@forensic.au.dkNo affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

22917943

Citation

Sørensen, Lambert K., and Jørgen B. Hasselstrøm. "A Hydrophilic Interaction Liquid Chromatography Electrospray Tandem Mass Spectrometry Method for the Simultaneous Determination of Γ-hydroxybutyrate and Its Precursors in Forensic Whole Blood." Forensic Science International, vol. 222, no. 1-3, 2012, pp. 352-9.
Sørensen LK, Hasselstrøm JB. A hydrophilic interaction liquid chromatography electrospray tandem mass spectrometry method for the simultaneous determination of γ-hydroxybutyrate and its precursors in forensic whole blood. Forensic Sci Int. 2012;222(1-3):352-9.
Sørensen, L. K., & Hasselstrøm, J. B. (2012). A hydrophilic interaction liquid chromatography electrospray tandem mass spectrometry method for the simultaneous determination of γ-hydroxybutyrate and its precursors in forensic whole blood. Forensic Science International, 222(1-3), 352-9. https://doi.org/10.1016/j.forsciint.2012.07.017
Sørensen LK, Hasselstrøm JB. A Hydrophilic Interaction Liquid Chromatography Electrospray Tandem Mass Spectrometry Method for the Simultaneous Determination of Γ-hydroxybutyrate and Its Precursors in Forensic Whole Blood. Forensic Sci Int. 2012 Oct 10;222(1-3):352-9. PubMed PMID: 22917943.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A hydrophilic interaction liquid chromatography electrospray tandem mass spectrometry method for the simultaneous determination of γ-hydroxybutyrate and its precursors in forensic whole blood. AU - Sørensen,Lambert K, AU - Hasselstrøm,Jørgen B, Y1 - 2012/08/20/ PY - 2012/04/20/received PY - 2012/07/17/revised PY - 2012/07/28/accepted PY - 2012/8/25/entrez PY - 2012/8/25/pubmed PY - 2013/2/13/medline SP - 352 EP - 9 JF - Forensic science international JO - Forensic Sci Int VL - 222 IS - 1-3 N2 - A liquid-chromatography-tandem-mass-spectrometry method using pneumatically assisted electrospray ionisation (LC-ESI-MS/MS) was developed for the simultaneous determination of γ-hydroxybutyric acid (GHB), γ-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. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/22917943/A_hydrophilic_interaction_liquid_chromatography_electrospray_tandem_mass_spectrometry_method_for_the_simultaneous_determination_of_γ_hydroxybutyrate_and_its_precursors_in_forensic_whole_blood_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(12)00359-3 DB - PRIME DP - Unbound Medicine ER -