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Determination of asenapine in presence of its inactive metabolites in human plasma by LC-MS/MS

Journal of Pharmaceutical Analysis 2018年第5期8卷 341-347页

作者： Nirav R Patel Mallika Sanyal Naveen Sharma Dinesh S.Patel Pranav S.Shrivastav Bhavin N.Patel Bioanalytical Laboratory Uiantha Research India Ltd.BodakdevAhmedabad 380054GujaratIndia Kadi Sarva Viswavidyalaya Sector-15Ghandhinagar 382715GujaratIndia Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad 380009GujaratIndia Department of Chemistry School of SciencesGujarat UniversityNavrangpuraAhmedabad 380009GujaratIndia

A highly selective and sensitive liquid chromatography-tandem mass spectrometry （LC-MS/MS） assay has been described for the determination of asenapine （ASE） in presence of its inactive metabolites N-desmethyl asenapine （DMA） and asenapine-N-glucuronide （ASG）. ASE, and ASE 13C-d3, used as internal standard （IS）, were extracted from 300 μL human plasma by a simple and precise liquid-liquid extraction procedure using methyl tert-butyl ether. Baseline separation of ASE from its inactive metabolites was achieved on Chromolith Performance RPse （100 mm ×4.6 mm） column using acetonitrile- 5.0 mM ammonium acetate-10% formic acid （90：10：0.1, v/v/v） within 4.5 min. Quantitation of ASE was done on a triple quadrupole mass spectrometer equipped with electrospray ionization in the positive mode. The protonated precursor to product ion transitions monitored for ASE and ASE 13C-d3 were m/z 286.1 → 166.0 and m/z 290.0 → 166.1, respectively. The limit of detection （LOD） and limit of quantitation （LOQ） of the method were 0.0025 ng/mL and 0.050 ng/mL respectively in a linear concentration range of 0.050-20.0 ng/mL for ASE. The intra-batch and inter-batch precision （% CV） and mean relative recovery across quality control levels were 〈 5.8% and 87.3%, respectively. Matrix effect, evaluated as IS-normalized matrix factor, ranged from 1.03 to 1.05. The stability of ASE under different storage conditions was ascertained in presence of the metabolites. The developed method is much simpler, matrix free, rapid and economical compared to the existing methods. The method was suc- cessfully used for a bioequivalence study of asenapine in healthy Indian subjects for the first time.

关键词： asenapine asenapine 13C-d3 Metabolites LC-MS/MS Bioequivalence study Human plasma

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Simultaneous determination of asenapine and valproic acid in human plasma using LC-MS/MS:Application of the method to support pharmacokinetic study

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Journal of Pharmaceutical Analysis 2013年第6期3卷 394-401页

作者： Ambavaram Vijaya Bhaskar Reddy Nandigam Venugopal Gajulapalle Madhavi Department of Chemistry Sri Venkateswara University

Combination of asenapine with valproic acid received regulatory approval for acute treatment of schizophrenia and maniac episodes of bipolar disorders. A simple LC-MS/MS method was developed and validated for simultaneous quantification of asenapine and valproic acid in human plasma. Internal standards were added to 300 ~L of plasma sample prior to liquid-liquid extraction using methyl tertiary butyl ether （MTBE）. Chromatographic separation was achieved on Phenomenex C18 column （50 mm ~ 4.6 mm, 5 pm） in isocratic mode at 40 ~C. The mobile phase used was 10 mM ammonium formate-acetonitrile （5：95, v/v） at a constant flow rate of 0.8 mL/min monitored on triple quadrupole mass spectrometer, operating in the multiple reaction monitoring （MRM） mode. The injection volume used for LC-MS/MS analysis was 15 taL and the run time was 2.5 min. These low run time and small injection volume suggest the high efficiency of the proposed method. The method was validated over the concentration range of 0.1-10.02ng/mL and 10-20,000ng/mL for asenapine and valproic acid respectively. The method recoveries of asenapine （81.33%）, valproic acid （81.70%）, gliclazide （78.45%） and benzoic acid （79.73） from spiked plasma samples were consistent and reproducible. The application of this method was demonstrated by a pharmacokinetic study in 8 healthy male volunteers with 5 mg asenapine and 250 mg valproic acid administration.

关键词： asenapine Gliclazide PharmacokineticsBipolar disordersSchizophrenia Valproic acid

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