A validated stability indicating HPLC method for the determination of process-related impurities in pantoprazole bulk drug and formulations

Abstract

A stability-indicating high-performance liquid chromatographic (HPLC) method was developed with short run time and validated for the assay of process related impurities of pantoprazole in bulk form. Resolution of drug, its potential impurities and degradation products were achieved on a Hypersil ODS column utilizing a gradient with 0.01 M phosphate buffer of pH 7 and acetonitrile as eluent, at the detection wavelength of 290 nm. Flow rate was set at 1 mL min -1 . The procedure was found to be specific, linear (r=0.999), recovery (97.9-103%), LOD (0.043-0.047 µgmL -1 ), LOQ (0.13-0.14 µgmL -1 ) and robust. Acceptable robustness indicates that the assay method remains unaffected by small but deliberate variations. Pantoprazole was found to degrade in acidic, oxidative and under photolytic stress conditions. The drug was stable to alkaline and dry heat conditions. This method has been successively applied to pharmaceutical formulation and no interference from the excipients was found.Uniterms: High performance liquid chromatography/qualitative analysis. High performance liquid chromatography/method development. Pantoprazole/forced degradation.Desenvolveu-se método indicador de estabilidade por Cromatografia a Líquido de Alta Eficiência (CLAE) com pequeno tempo de corrida e validado para o ensaio de impurezas relacionadas ao processo de produção de pantoprazol em batelada. A determinação do fármaco, de suas impurezas potenciais e dos produtos de degradação foi realizada com coluna de ODS Hypersil, utilizando gradiente com tampão de fosfato 0,01 M pH 7 e acetonitrila como eluente, no comprimento de onda de detecção de 290 nm. A velocidade de fluxo foi fixada em 1 mLmin -1 . O procedimento se mostrou específico, linear (r=0,999), com recuperação (97,9-103%), LOD (0,043-0,047 mgmL -1 ), LOQ (0,13-0,14 mg mL -1 ) e robusto. Robustez aceitável indica que o método de ensaio não é afetado por variações pequenas, exceto as planejadas. O pantoprazole degradou em condições ácidas, oxidativas e sob condições de estresse fotolítico. O fármaco foi estável em condições alcalinas e de calor seco. Este método tem sido sucessivamente aplicado à formulação farmacêutica e não se encontrou interferência de excipientes.Unitermos: Cromatografia Líquido de Alta Eficiência/análise qualitativa. Cromatografia Líquido de Alta Eficiência/desenvolvimento de método. Pantoprazol/degradação forçada.

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Determination of Pantoprazole in Bulk and Pharmaceutical Formulations by Validated Rp-HPLC Method

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