PMID- 23245230
OWN - NLM
STAT- MEDLINE
DCOM- 20130927
LR  - 20131121
IS  - 1873-264X (Electronic)
IS  - 0731-7085 (Linking)
VI  - 74
DP  - 2013 Feb 23
TI  - Determination of GHB and its precursors (GBL and 1,4-BD) in dietary supplements 
      through the synthesis of their isotopologues and analysis by GC-MS method.
PG  - 31-8
LID - S0731-7085(12)00546-8 [pii]
LID - 10.1016/j.jpba.2012.10.006 [doi]
AB  - Gamma-hydroxybutyric acid (GHB) and its "pro-drugs", gamma-butyrolactone (GBL) 
      and 1,4 butanediol (1,4-BD), are drugs of abuse with depressant effects on the 
      central nervous system. Many analytical methods have been proposed for the 
      quantitative determination of these compounds mainly in biological matrices but 
      only few have been addressed to dietary supplements and foods. Facile synthesis 
      of the GBL and 1,4-BD isotopologues are available by "one pot" Ru-catalyzed 
      homogeneous deuteration of dicarboxylic acids. In this work we propose a new 
      method for determination of GHB, GBL and 1,4-BD in commercially available dietary 
      supplements, based on isotope dilution mass spectrometry (ID-MS). The procedure 
      involves a simple extraction of sample with acidic acetonitrile and direct 
      analysis by GC-ID-MS method without any purification or derivatization. Indeed, 
      the proposed method takes advantage of the complete conversion of GHB (free acid 
      or its salts) to GBL, allowing the quantification of GHB and its pro-drugs. Five 
      levels for each calibration curve have been prepared by diluting working 
      solutions of the analytes to obtain concentrations ranging from 1 to 20mg/mL. The 
      validation procedures have shown an accuracy between 88% and 99% and a precision 
      between 7.3% and 2.9% of each analyte in the sample matrix. Positive ions 
      chemical ionization (PICI) have been employed to preserve the information on 
      molecular ions and to improve specificity and sensitivity of quantitative 
      determination.
CI  - Copyright (c) 2012 Elsevier B.V. All rights reserved.
FAU - Rosi, Luca
AU  - Rosi L
AD  - Dipartimento di Chimica "Ugo Schiff", Universita di Firenze, Via della Lastruccia 
      3-13, I-50019 Sesto Fiorentino, FI, Italy.
FAU - Frediani, Piero
AU  - Frediani P
FAU - Bartolucci, Gianluca
AU  - Bartolucci G
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20121023
PL  - England
TA  - J Pharm Biomed Anal
JT  - Journal of pharmaceutical and biomedical analysis
JID - 8309336
RN  - 0 (Butylene Glycols)
RN  - 0 (Hydroxybutyrates)
RN  - 0 (Prodrugs)
RN  - 30IW36W5B2 (4-hydroxybutyric acid)
RN  - 7XOO2LE6G3 (1,4-butanediol)
RN  - OL659KIY4X (4-Butyrolactone)
SB  - IM
MH  - 4-Butyrolactone/*analysis/chemical synthesis
MH  - Butylene Glycols/*analysis/chemical synthesis
MH  - Dietary Supplements/*analysis
MH  - Gas Chromatography-Mass Spectrometry/*methods/standards
MH  - Hydroxybutyrates/*analysis/chemical synthesis
MH  - Prodrugs/*analysis/chemical synthesis
MH  - Reproducibility of Results
EDAT- 2012/12/19 06:00
MHDA- 2013/09/28 06:00
CRDT- 2012/12/19 06:00
PHST- 2012/06/25 00:00 [received]
PHST- 2012/10/04 00:00 [revised]
PHST- 2012/10/06 00:00 [accepted]
PHST- 2012/12/19 06:00 [entrez]
PHST- 2012/12/19 06:00 [pubmed]
PHST- 2013/09/28 06:00 [medline]
AID - S0731-7085(12)00546-8 [pii]
AID - 10.1016/j.jpba.2012.10.006 [doi]
PST - ppublish
SO  - J Pharm Biomed Anal. 2013 Feb 23;74:31-8. doi: 10.1016/j.jpba.2012.10.006. Epub 
      2012 Oct 23.