Determination of nicousamide in human plasma by liquid chromatography–tandem mass spectrometry

A sensitive and specific ultra-performance liquid chromatography tandem mass spectrometry (LC–MS/MS) method has been developed for the determination of nicousamide in human plasma. This method has also been validated in terms of selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, stability, matrix effect and recovery. Chromatography was carried out on an Acquity UPLC CSH C18 column and mass spectrometric analysis was performed using an QTrap5500 mass spectrometer coupled with electro-spray ionization (ESI) source in the Negative ion mode. The MRM transition of m/z 399 → 353 was used to quantify nicousamide. The assay was validated from 1 to 1000 ng/mL for nicousamide. Intra- and Inter-day precision for nicousamide was <13.1%, method accuracy (RE%) was between −7.5 and 8.8%. This method was used to support a clinical study where a single oral dose was administered by Chinese healthy volunteers to investigate the pharmacokinetics of nicousamide.

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► A sensitive LC–MS/MS method for quantify nicousamide in human plasma was developed and fully validated.
► Only 100 μL plasma was required for the sample pretreatment procedures.
► The overall run time was 1.5 min, that allow to analyze large sample in a short time.
► The method had been successfully applied in the clinical study of nicousamide.