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Title

Simultaneous determination of six antipsychotics, two of their metabolites and caffeine in human plasma by LC-MS/MS using a phospholipid-removal microelution-solid phase extraction method for sample preparation

AuthorsKoller, Dora; Zubiaur, Pablo; Saiz-Rodríguez, Miriam; Abad-Santos, Francisco; Wojnicz, Aneta
KeywordsAntipsychotics
Caffeine
Liquid chromatography-tandem mass spectrometry
Solid phase extraction
Phospholipids
Therapeutic drug monitoring
Issue Date2019
PublisherElsevier
CitationTalanta 198: 159-168 (2019)
AbstractA simple and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated in human plasma for the simultaneous determination of aripiprazole (ARI) and its metabolite dehydro-aripiprazole (DARI); olanzapine (OLA), risperidone (RIS), paliperidone (PAL), quetiapine (QUE), clozapine (CLO) and caffeine (CAF). CAF is included to the method because it can have an influence on drug metabolism due to competitive inhibition. The above mentioned compounds and their isotope-labeled internal standards were extracted from 200 µL human plasma samples by both, effective phospholipids-eliminating three-step microelution-solid-phase extraction (µ-SPE) and protein precipitation (PPT) for comparison. A combination of formic acid (0.2%)-acetonitrile (pH 3.0; 65:35, v/v) was used as mobile phase and the chromatogram was run under gradient conditions at a flow rate of 0.6 mL/min. Run time lasted 6 min, followed by a re-equilibration time of 3 min. All analytes were monitored by mass spectrometric detection operating in multiple reaction monitoring mode and the method was validated covering the corresponding therapeutic ranges: 0.18–120 ng/mL for ARI, 0.25–80 ng/mL for DARI, 1.00–100 ng/mL for OLA, 0.70–60 ng/mL for RIS, 0.20–30 ng/mL for PAL, 0.50–160 ng/mL for QUE, 0.50–1000 ng/mL for CLO, and finally 1200–3700 ng/mL for CAF. The method was validated based on the recommendations of regulatory agencies through tests of precision, accuracy, extraction recovery, identity confirmation, trueness, matrix effect, process efficiency, stability, selectivity, linearity and carry-over effect fulfilling the guideline requirements. Our µ-SPE method results in the elimination of more than 99% of early eluting and more than 92% of late-eluting phospholipids compared to PPT. Additionally, the method was successfully applied for quantifying ARI and OLA plasma concentrations from healthy volunteers.
Publisher version (URL)https://doi.org/10.1016/j.talanta.2019.01.112
URIhttp://hdl.handle.net/10261/186598
DOIhttp://dx.doi.org/10.1016/j.talanta.2019.01.112
ISSN0039-9140
E-ISSN1873-3573
ReferencesKoller, Dora; Zubiaur, Pablo; Saiz-Rodríguez, Miriam; Abad-Santos, Francisco; Wojnicz, Aneta. (2021) "Dataset related to article: Simultaneous determination of six antipsychotics, two of their metabolites and caffeine in human plasma by LC-MS/MS using a phospholipid-removal microelution-solid phase extraction method for sample preparation [Dataset]", http://dx.doi.org/10.20350/digitalCSIC/13931
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