Oxcarbazepine (OXB) is a newer antiepileptic drug indicated for the treatment of partial seizures as both monotherapy and combination therapy in adults and children with epilepsy. At present, determinations of OXB have been established by the use of HPLC-UV spectrometry, [1][2][3] or LC-APCI-MS mass-spectrometry. 4) However, none of these methods achieved the quick quantification and identification of OXB in a single run. Although methods for simultaneous determination of OXB and some of antiepileptic drugs has been described, 5-11) they were not particular interest since it takes too long chromatographic run time especially when applied to OXB, and had low sensitivity; it appeared that no assay existed for determination of the OXB using HPLC-MS/MS. The assay described here requires small mobile phase and sample volume, short chromatographic run and is sensitive, specific and fully validated.Optimization of an MS response includes methods to improve the abundance of a specific precursor or product ion, or yielding as comprehensive or selective measurements as possible (Table 1). Maximization of the signal or the signal-tonoise ratio (S/N) of a particular ion can be used for quantitative optimization, but choosing qualitative optimization criteria are less trivial.Optimization techniques of particular interest are factorial design and central composite design, for screening of the important parameters Placket-Burman design can be useful. Chemometric approaches for optimization of ESI or MS/MS parameters also occur in literature. 12,13) In this present study Plackett-Burman and factorial designs are employed for screening of essential parameters and optimization respectively. ExperimentalChemicals and Reagents OXB, and imipramine (Internal standard), were kindly provided by Glenmark Pharmaceuticals (Mumbai, India). HPLC-grade acetonitrile, methanol, formic acid and diethyl ether were purchased from Qualigens (Mumbai, India). Blank human plasma was harvested after 5 min centrifugation at 4000ϫg and stored at Ϫ20°C until use.Instrumentation The HPLC system consisted of an HP1100 binary pump, auto sampler, column oven, and online degasser (Agilent Technologies, Palo Alto, CA, U.S.A.). The analytical column used was reversedphase symmetry C18 (75 mmϫ4.6 mm i.d. 3.5 mm). A mobile phase of 10 mM ammonium formate/ACN (10 : 90, v/v) was pumped at a flow rate of 0.3 ml/min and the injected sample volume to whole over the method is 10 ml. The LC elute was introduced directly into an Applied Biosystems triple quadrupole mass spectrometer API 4000 (MDS-Sciex, Toronto Canada, software: Analyst 1.4.1) equipped with an electrospray ionization source. The triple quadrupole mass spectrometer was operated in the positive ion mode and the multiple reaction monitoring (MRM) chromatograms obtained were used for quantification. MRM transitions of m/z 253→208, m/z and 281→86 were respectively optimized for OXB and Imipramine. The 28Vol. 56, No. 1 A rapid tandem mass spectrometric (MS-MS) method for the quantification of Oxcarbazepine (O...
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