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A Novel Bioanalytical Method for the Determination of Opioids in Blood and Pericardial Fluid

A Novel Bioanalytical Method for the Determination of Opioids in Blood and Pericardial Fluid

Elisa Ferreira, Francisco Corte Real, Teresa Pinho E Melo, Cláudia Margalho

J Anal Toxicol. 2020 Jun 9;bkaa064.

PMID: 32518955

Abstract:

Opioids are the drugs most commonly detected in overdose deaths and the second most consumed worldwide. An analytical methodology has been optimized and fully validated for the determination of codeine, morphine, 6-acetylmorphine, 6-acetylcodeine, oxycodone, oxymorphone and fentanyl in whole blood and pericardial fluid. The internal standards used were codeine-d3, morphine-d3, 6-acetylmorphine-d3 and fentanyl-d5. Before solid phase extraction, volumes of 250 μL of blood and pericardial fluid were subjected to a protein precipitation (with 750 μL of ice-cold acetonitrile) and a microwave induced oximation was performed using a solution of 1% aqueous hydroxylamine hydrochloride in PBS (1:2, v/v). Finally, the dried extracts were further derivatized with a solution of MSTFA+5% TMCS under microwave irradiation. The chromatographic analysis was carried out using gas chromatography-mass spectrometry operating in electron impact and selected ion monitoring mode. For all analytes the method was linear between 5 and 1000 ng/mL with determination coefficients (r2) higher than 0.99. Depending on the analyte and matrix the limit of detection varies between 3 and 4 ng/mL. Intra- and intermediate precision (<20%) and bias (±20%) were acceptable for all analytes in both matrices. The stability of the substances in the studied matrices was guaranteed, at least, 24 h in the autosampler, 4 h at room temperature and 30 days after three freeze/thaw cycles. This methodology was applied to real samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.

Chemicals Related in the Paper:

Catalog Number	Product Name	CAS Number	Price
AP136765258	6-Acetylmorphine-d3 solution	136765-25-8	Price
AP67293883	Morphine-D3 solution	67293-88-3	Price
AP70420712-A	Codeine-D3 solution	70420-71-2	Price

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