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J Chromatogr B Analyt Technol Biomed Life Sci ; 1130-1131: 121809, 2019 Nov 01.
Artículo en Inglés | MEDLINE | ID: mdl-31669634

RESUMEN

This work describes the development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry method that uses disposable pipette extraction (DPX-UHPLC-MS/MS) to determine the endocannabinoid anandamide (AEA) in cerebrospinal fluid samples (CSF). The DPX parameters sorption equilibrium time, sample volume, number of draw-eject cycles, washing solvent volume, and elution solvent volume were optimized by design of experiments (DOE) techniques. The simple DPX protocol proposed herein required a reduced amount of CSF sample and organic solvent. The DPX-UHPLC-MS/MS method presented linear range from 0.10 ng mL-1 (LLOQ) to 3.0 ng mL-1, inter- and intra-assay accuracy with EPR values varying from -8.2% to 9.6%, inter- and intra-assay precision with CV values ranging from 1.3% to 14.8% (except for the LLOQ), and no significant matrix effect. The innovative DPX-UHPLC-MS/MS method was successfully applied to determine AEA in CSF samples from Parkinson's disease (PD) patients and should therefore be used in clinical studies.


Asunto(s)
Ácidos Araquidónicos/líquido cefalorraquídeo , Cromatografía Líquida de Alta Presión/métodos , Endocannabinoides/líquido cefalorraquídeo , Alcamidas Poliinsaturadas/líquido cefalorraquídeo , Espectrometría de Masas en Tándem/métodos , Ácidos Araquidónicos/aislamiento & purificación , Endocannabinoides/aislamiento & purificación , Humanos , Modelos Lineales , Alcamidas Poliinsaturadas/aislamiento & purificación , Reproducibilidad de los Resultados , Sensibilidad y Especificidad
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