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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; 70:518-22JP

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.

Authors+Show Affiliations

Forensic Toxicology Division, Institute of Legal Medicine, University of Florence, Italy. elisabetta.bertol@unifi.itNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

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 -