ABSTRACT
The objective of this study was to demonstrate the possibility to use deuterated compounds as internal standards for the quantitative analysis of morphine by gas chromatography with mass-selective detection for the purpose of doping control. The paper is focused on the problems associated with the use of deuterated morphine-D3 as the internal standard. Quantitative characteristics of the calibration dependence thus documented are presented along with uncertainty values obtained in the measurements with the use of deuterated morphine-D6. An approach to the assessment of method bias associated with the application of morphine-D6 as the deuterated internal standard is described.
Subject(s)
Analgesics, Opioid/analysis , Deuterium/analysis , Doping in Sports/prevention & control , Gas Chromatography-Mass Spectrometry/methods , Morphine/analysis , Deuterium/chemistry , Humans , Reference StandardsABSTRACT
An HPLC-ESI-MS method has been developed for determining 2-ethyl-6-methyl-3-oxypyridine (EMO) in human urine upon peroral administration of this substance in form ofmexidol. Various sample preparation (extraction) procedures were tested and compared for evaluating the recovery and matrix effect. Solid-phase extraction procedure followed by derivation with dansyl chloride is proposed as a method of choice. The recovery of analyte was 48.1 +/- 3.4%, and the matrix effect was 99.4 +/- 4.1%. The MS and MS/MS spectra of EMO and its dansyl derivatives are presented and interpreted. The analyses were performed using a mass spectrometer of the ion trap type with electrospray ionization at atmospheric pressure, operating in the regime of positive ion detection.
Subject(s)
Picolines/urine , Psychotropic Drugs/urine , Chromatography, High Pressure Liquid , Humans , Picolines/pharmacokinetics , Psychotropic Drugs/pharmacokinetics , Spectrometry, Mass, Electrospray Ionization , Tandem Mass SpectrometryABSTRACT
3'-Hydroxystanosolol detection in biological fluids at pg levels by gas chromatography/tandem mass spectrometry is described. Gas chromatography/high resolution mass spectrometry results can be confirmed with gas chromatography/tandem mass-spectrometry.