Validated method for the quantification of buprenorphine in postmortem blood using solid-phase extraction and two-dimensional gas chromatography–mass spectrometry
File(s)
Accepted version
Author(s)
Nahar, Limon Khatun
Andrews, Rebecca
Paterson, Sue
Type
Journal Article
Abstract
A highly sensitive and fully validated method was developed for the quantification of buprenorphine in postmortem blood. After a two-step protein precipitation process using acetonitrile, buprenorphine was purified using mixed-mode (C8/cation exchange) solid-phase extraction cartridges. Endogenous water-soluble compounds and lipids were removed from the cartridges before the samples were eluted, concentrated and derivatized using N-methyl-N-trimethylsilyltrifluoroacetamide. The samples were analyzed using two-dimensional gas chromatography–mass spectrometry (2D GC–MS) in selective ion-monitoring mode. A low polarity Rxi®-5MS (30 m × 0.25 mm I.D. × 0.25 µm) was used as the primary column and the secondary column was a mid-polarity Rxi® -17Sil MS (15 m × 0.32 mm I.D. × 0.25 µm). The assay was linear from 1.0 to 50.0 ng/mL (r2 > 0.99; n = 6). Intraday (n = 6) and interday (n = 9) imprecisions (percentage relative standard deviation, % RSD) were <5% and the average recovery was 60%. The limit of detection (LOD) of the method was 0.5 ng/mL and limit of quantification was 1.0 ng/mL. 2D GC–MS improved the LOD of buprenorphine by 20-fold compared with analysis on a conventional GC–MS. The method was highly selective with no interference from endogenous compounds or from 62 commonly encountered drugs. To prove method applicability to forensic postmortem cases, 14 authentic postmortem blood samples were analyzed.
Date Issued
2015-05-10
Date Acceptance
2015-05-01
Citation
Journal of Analytical Toxicology, 2015, 39 (7), pp.519-525
ISSN
0146-4760
Publisher
Oxford University Press (OUP)
Start Page
519
End Page
525
Journal / Book Title
Journal of Analytical Toxicology
Volume
39
Issue
7
Copyright Statement
© The Author 2015. Published by Oxford University Press. This is a pre-copy-editing, author-produced version of an article accepted for publication in the Journal of Analytical Toxicology following peer review. The definitive publisher-authenticated version is available online at: https://doi.org/10.1093/jat/bkv051
Subjects
0301 Analytical Chemistry
1115 Pharmacology And Pharmaceutical Sciences
Analytical Chemistry
Publication Status
Published
Date Publish Online
2015-05-10