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High-throughput on-line solid-phase extraction–liquid chromatography–tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma

Summary A rapid, sensitive and fully automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed and validated for the direct analysis of 14 antidepressants and their metabolites in plasma. Integration of the sample extraction and LC separation into a single system permitted direct injection of the plasma without prior sample pre-treatment. The applied gradient ensured the elution of all the examined drugs within 14 min and produced chromatographic peaks of acceptable symmetry. The total process time was 20 min and only 50 uL of plasma was required. Selectivity of the method was achieved by a combination of retention time and two precursor-product ion transitions for the non-deuterated compounds. The use of SPE was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Extraction was found to be both reproducible and efficient with recoveries >99% for all the analytes. The method showed excellent intra-assay and inter-assay precision (relative standard deviation (RSD) and bias <20%) for quality control (QC) samples spiked at a concentration of 40, 200 and 800 |xg/L and the r2 >0.99 over the range investigated (10-1000 ug/L). Limits of quantification (LOQs) were estimated to be 10 ug/L. Furthermore, the processed samples were demonstrated to be stable for at least 48 h, except for clomipramine and norclomipramine, where a slight negative trend was observed, but did not compromise the quantification. The method was subsequently applied to authentic samples previously screened by a routine HPLC method with diode array detection
Category 3. Symbiosis User Application
These are applications that have been made by Symbiosis customers. They are validated and have been published.
Matrix Plasma
Market Clinical
Cartridge Oasis MCX
Detection MS (Waters Quattro Micro)
Compounds Trazodone, Fluvoxamine, Norflouxetine, Paroxetine, Citalopram, Venlafaxine, Fluoxetine, Desipramine, Nortriptyline, Norclomipramine, Imipramine, Sertraline, Amitriptyline, Clomipramine
Compound Group Antidepressants, selective serotonin reuptake inhibitors (SSRIs), serotonin and noradrenaline reuptake inhibitors (SNaRIs), noradrenergic and specific sero¬tonergic antidepressants (NaSSAs) and noradrenaline reuptake inhibitors (NaRIs)
Sample_volume 50µL
Contact Ana de Castro, Maria del Mar Ramírez Fernandez, Marleen Laloup, Nele Samyn, Gert De Boeck, Michelle Wood, Viviane Maes, Manuel Lopez-Rivadulla
Account Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, Santiago de Compostela, Spain Federal Public Service Justice, National Institute of Criminalistics and Criminology, Brussels, Belgium Waters Corporation, MS Technologies Centre, Manchester, UK
Published Journal of Chromatography A, Volume 1160, Issues 1-2, 10 August 2007, Pages 3-12
Date 10-8-2007
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Remarks Total run time is 20 minutes with a lod of around 1 ng/mL per compound.

Users NICC
Status Published