Tags

Type your tag names separated by a space and hit enter

Detection of gamma-hydroxybutyrate in hair: validation of GC-MS and LC-MS/MS methods and application to a real case.

Abstract

A gas chromatography-mass spectrometry (GC-MS) and a liquid chromatography tandem mass spectrometry (LC-MS/MS) method were validated for quantifying endogenous and exogenous hair concentrations of gamma-hydroxybutyrate (GHB). The GC-MS method is based on overnight extraction of 25 mg hair in NaOH at 56 °C, liquid/liquid extraction in ethylacetate and trimethylsylil derivatization; analysis is by electron ionization and single ion monitoring of three ions. The LC-MS/MS method entails a rapid digestion of 25 mg hair with NaOH at 75 °C for 40 min, liquid/liquid extraction in ethylacetate and reconstitution of the extract in the LC mobile phase; negative ion electrospray ionization and multiple reaction monitoring (MRM) analysis are employed for the LC-MS/MS detection. In both cases, GHB-d6 is used as an internal standard. The endogenous amount in "blank" hair are estimated by the standard addition method. Limits of detection are 0.4 and 0.5 ng/mg for GC-MS and LC-MS/MS respectively, while the limit of quantification (LOQ) is 0.6 ng/mg for both methods; the GC-MS method proved to be linear in the range 1-50 ng/mg whereas linearity was demonstrated from 0.6 to 50 ng/mg for the LC-MS/MS; imprecision and inaccuracy were always lower than 23% for quality controls samples. The two methods were applied to a real case of a man addicted to GHB; the drug concentration in segments from 17 cm hair strand well correlated with self-reported use of GHB in different periods of his life. Performances of the two methods were similar.

Links

  • Publisher Full Text
  • Authors+Show Affiliations

    ,

    Forensic Toxicology Division, Institute of Legal Medicine, University of Florence, Italy. elisabetta.bertol@unifi.it

    , , , , ,

    Source

    MeSH

    Acetates
    Adult
    Calibration
    Chromatography, Liquid
    Crime
    Forensic Toxicology
    Gas Chromatography-Mass Spectrometry
    Hair
    Humans
    Limit of Detection
    Linear Models
    Liquid-Liquid Extraction
    Male
    Quality Control
    Reference Standards
    Reproducibility of Results
    Sodium Hydroxide
    Sodium Oxybate
    Spectrometry, Mass, Electrospray Ionization
    Street Drugs
    Substance Abuse Detection
    Substance-Related Disorders
    Tandem Mass Spectrometry
    Temperature

    Pub Type(s)

    Case Reports
    Journal Article
    Validation Studies

    Language

    eng

    PubMed ID

    22884787

    Citation

    Bertol, Elisabetta, et al. "Detection of Gamma-hydroxybutyrate in Hair: Validation of GC-MS and LC-MS/MS Methods and Application to a Real Case." Journal of Pharmaceutical and Biomedical Analysis, vol. 70, 2012, pp. 518-22.
    Bertol E, Argo A, Procaccianti P, et al. Detection of gamma-hydroxybutyrate in hair: validation of GC-MS and LC-MS/MS methods and application to a real case. J Pharm Biomed Anal. 2012;70:518-22.
    Bertol, E., Argo, A., Procaccianti, P., Vaiano, F., Di Milia, M. G., Furlanetto, S., & Mari, F. (2012). Detection of gamma-hydroxybutyrate in hair: validation of GC-MS and LC-MS/MS methods and application to a real case. Journal of Pharmaceutical and Biomedical Analysis, 70, pp. 518-22. doi:10.1016/j.jpba.2012.07.009.
    Bertol E, et al. Detection of Gamma-hydroxybutyrate in Hair: Validation of GC-MS and LC-MS/MS Methods and Application to a Real Case. J Pharm Biomed Anal. 2012;70:518-22. PubMed PMID: 22884787.
    * Article titles in AMA citation format should be in sentence-case
    TY - JOUR T1 - Detection of gamma-hydroxybutyrate in hair: validation of GC-MS and LC-MS/MS methods and application to a real case. AU - Bertol,Elisabetta, AU - Argo,Antonina, AU - Procaccianti,Paolo, AU - Vaiano,Fabio, AU - Di Milia,Maria Grazia, AU - Furlanetto,Sandra, AU - Mari,Francesco, Y1 - 2012/07/25/ PY - 2012/05/21/received PY - 2012/07/10/revised PY - 2012/07/12/accepted PY - 2012/8/14/entrez PY - 2012/8/14/pubmed PY - 2013/2/8/medline SP - 518 EP - 22 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 70 N2 - A gas chromatography-mass spectrometry (GC-MS) and a liquid chromatography tandem mass spectrometry (LC-MS/MS) method were validated for quantifying endogenous and exogenous hair concentrations of gamma-hydroxybutyrate (GHB). The GC-MS method is based on overnight extraction of 25 mg hair in NaOH at 56 °C, liquid/liquid extraction in ethylacetate and trimethylsylil derivatization; analysis is by electron ionization and single ion monitoring of three ions. The LC-MS/MS method entails a rapid digestion of 25 mg hair with NaOH at 75 °C for 40 min, liquid/liquid extraction in ethylacetate and reconstitution of the extract in the LC mobile phase; negative ion electrospray ionization and multiple reaction monitoring (MRM) analysis are employed for the LC-MS/MS detection. In both cases, GHB-d6 is used as an internal standard. The endogenous amount in "blank" hair are estimated by the standard addition method. Limits of detection are 0.4 and 0.5 ng/mg for GC-MS and LC-MS/MS respectively, while the limit of quantification (LOQ) is 0.6 ng/mg for both methods; the GC-MS method proved to be linear in the range 1-50 ng/mg whereas linearity was demonstrated from 0.6 to 50 ng/mg for the LC-MS/MS; imprecision and inaccuracy were always lower than 23% for quality controls samples. The two methods were applied to a real case of a man addicted to GHB; the drug concentration in segments from 17 cm hair strand well correlated with self-reported use of GHB in different periods of his life. Performances of the two methods were similar. SN - 1873-264X UR - https://www.unboundmedicine.com/medline/citation/22884787/Detection_of_gamma_hydroxybutyrate_in_hair:_validation_of_GC_MS_and_LC_MS/MS_methods_and_application_to_a_real_case_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(12)00410-4 DB - PRIME DP - Unbound Medicine ER -