Method development and alkali degradation study of doxofylline by rp-hplc and lc-ms/ms
response for concentrations in the range of 1-200 ìg/mL using acetonitrile: formic Acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rate of 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, rugge dness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from
recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality
control analysis. The acid degradation product as well as pathway was characterized by LC-MS/MS.
RESULT AND DISCUSSION
A sensitive, selective, precise and accurate high performance liquid chromatographicmethod of analysis of doxofylline in both as bulk drug and in formulation was developed and validated. The mobile phase consisted of acetonitril: 0.05M formic Acid (90: 10v/v); pH-3.0. The detection wavelength was 274nm. This system was found to give the sharp peak for Doxofylline (RT-2.9). The method was validated as per ICH guideline. Stability indicating assay method in which alkali stress condition was used for quantitative estimation of doxofylline in tablet formulation and identification of alkali degradation product The separation of drug from its degradation product were optimized by varying the ratio &/or nature of organic modifier. Finally method was developed using same
mobile phase composed of acetonitrile: formic Acid (90: 10); pH-3.0, in that both drug and degradation product showing good elution RT-2.9 (Doxofylline) and RT-5.1 (Alkali
degradation product) and m/e-262. The acid degradation product and pure drug were identified by LC-MS/MS in order to establish acid degradation pathway(fig.-04, 05and
06).
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Keywords
Method developmentalkali degradationdoxofyllineRP-HPLCRP-HPLC and LC-MS/MSstability indicating assayRP-HPLC methoddegradation productcharacterized by LC-MS/MSSelection of WavelengthMETHOD VALIDATIONAnalytical BiochemistryBiochemistry and Cell Biology not elsewhere classifiedBiogeography and PhylogeographyInfectious DiseasesInfectious AgentsMicrobial GeneticsMicrobial EcologyMicrobiologyMicrobiology not elsewhere classifiedMolecular BiologyMolecular EvolutionPharmacologyPhylogeny and Comparative AnalysisPhysiologySystems BiologySynthetic BiologyToxicologyStructural Biology (incl. Macromolecular Modelling)Analytical Chemistry not elsewhere classifiedAnalytical SpectrometryBiochemistryBioinorganic ChemistryBiologically Active MoleculesBiomolecular Modelling and DesignCharacterisation of Biological MacromoleculesChemical Characterisation of MaterialsChemical Sciences not elsewhere classifiedCatalysis and Mechanisms of ReactionsChemical Thermodynamics and EnergeticsCheminformaticsCheminformatics and Quantitative Structure-Activity RelationshipsComputational ChemistryElectrochemistryEnvironmental ChemistryForensic ChemistryInstrumental Methods (excl. Immunological and Bioassay Methods)Macromolecular and Materials Chemistry not elsewhere classifiedMedicinal and Biomolecular Chemistry not elsewhere classifiedMolecular MedicineMolecular PhysicsNatural Products ChemistryOrganic Chemical SynthesisOrganic ChemistryOrganic Chemistry not elsewhere classifiedOrganic Green ChemistryOrganometallic ChemistryQuality Assurance, Chemometrics, Traceability and Metrological ChemistryRadiation and MatterReaction Kinetics and DynamicsStereochemistrySynthesis of MaterialsTheoretical and Computational Chemistry not elsewhere classifiedTheory and Design of MaterialsAllergyAutoimmunityChemotherapyClinical Chemistry (diagnostics)Clinical MicrobiologyClinical Nursing: Primary (Preventative)Clinical Pharmacology and TherapeuticsClinical Nursing: Tertiary (Rehabilitative)Clinical Nursing: Secondary (Acute Care)Clinical Pharmacy and Pharmacy PracticeClinical Sciences not elsewhere classifiedCommunity Child HealthDiseasesMedical Biochemistry and Metabolomics not elsewhere classifiedMedical BacteriologyMedical Biochemistry: LipidsMedical Infection Agents (incl. Prions)Medical Microbiology not elsewhere classifiedMedical ParasitologyMedical VirologyMetabolic MedicineMolecular TargetsNephrology and UrologyNeurology and Neuromuscular DiseasesNeurosciences not elsewhere classifiedNutritional PhysiologyObstetrics and GynaecologyOncology and Carcinogenesis not elsewhere classifiedOphthalmologyOphthalmology and Optometry not elsewhere classifiedOptical TechnologyOral and Maxillofacial SurgeryOral Medicine and PathologyOrthodontics and Dentofacial OrthopaedicsPharmaceutical SciencesPharmacogenomicsPharmacology and Pharmaceutical Sciences not elsewhere classifiedPhysiotherapyRadiation TherapyRadiology and Organ ImagingRehabilitation and Therapy (excl. Physiotherapy)Respiratory DiseasesSurgeryTraditional Chinese Medicine and TreatmentsToxicology (incl. Clinical Toxicology)Systems Physiology
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