Quantitative Analysis of Selegiline and Three Metabolites (N-Desmethylselegiline, Methamphetamine, and Amphetamine) in Human Plasma by High-Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Tandem Mass Spectrometry

Abstract

This report describes a sensitive and specific high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry method for the detection of subnanogram concentrations of selegiline and its three principle metabolites, N-desmethylselegiline, methamphetamine, and amphetamine, in human plasma. The assay has a dynamic range of 0.1-20 ng/mL for selegiline and N-desmethylselegiline (norselegiline) and 0.2-20 ng/mL for methamphetamine and amphetamine. The inter- and intra-assay precision and accuracy varied by less than 11% for all analytes at 0.3, 2.5, and 15 ng/mL and less than 16% at the lower limit of quantitation (0.1 ng/mL for selegiline and norselegiline; and 0.2 ng/mL for methamphetamine and amphetamine). Selegiline and its metabolites showed no significant loss in quantitative accuracy after three freeze/thaw cycles or after up to 6 h at room temperature prior to extraction. Extracted plasma samples retained quantitative accuracy after storage for at least 7 days at -20 degrees C or up to 70 h at room temperature. Methanolic stock solutions were stable for at least 6 h when kept at room temperature or at least 90 days when kept at -20 degrees C.

Development of a liquid chromatography–tandem mass spectrometric method for the determination of methamphetamine and amphetamine using small volumes of rat serum

“…2A and B, respectively. These product ion spectra are similar to those recently presented by Slawson et al for the collision-induced dissociation of METH and AMP [10]. Slawson et al successfully quantitated METH and AMP concentrations from extracted human plasma in the MRM mode using m/z 150 → 91 and 136 → 91, respectively.…”

“…Liquid chromatography coupled to atmospheric pressure ionization mass spectrometry has become the method of choice for the determination of small molecules in biological matrices, including amphetamine-like compounds [9][10][11][12]. A recent review by Marquet lists several LC/MS methods for the quantitation of AMP and METH for clinical and forensic toxicology studies [13].…”

Electrochemical behavior and assay of anti-Parkinson drug selegiline using cathodic adsorptive stripping square wave voltammetry in bulk form

“…[6][7][8] There has been no electrochemical study published on quantitative determination of selegiline in bulk form as well as pharmaceutical formulations. The widespread use of submit your manuscript | www.dovepress.com…”

Simultaneous determination of selegiline and desmethylselegiline in human body fluids by headspace solid-phase microextraction and gas chromatography–mass spectrometry

“…Many methods have been reported for determining selegiline and desmethylselegiline concentrations in human plasma, serum, urine and hair using gas chromatography (GC)-mass spectrometry (MS) [5,6,[10][11][12], GC with electron capture detection (ECD) [13], GC with nitrogen phosphorus detection [9,14], high-performance liquid chromatography (HPLC) with fluorescence detection [15,16], and HPLC-MS [17][18][19]. Most of these methodologies employ extraction methods, such as liquid-liquid extraction (LLE) [6,11,13,[15][16][17]19] or solid-phase extraction (SPE) [7,10,12,18] in order to remove impurities contained in various matrices.…”

“…Most of these methodologies employ extraction methods, such as liquid-liquid extraction (LLE) [6,11,13,[15][16][17]19] or solid-phase extraction (SPE) [7,10,12,18] in order to remove impurities contained in various matrices. Although LLE and SPE methods may successfully extract selegiline and desmethylselegiline from biological samples, the large amounts of organic solvent used in the extraction procedure can cause health and environmental problems.…”