Validation of a stability-indicating RP-HPLC method for the determination of entecavir in tablet dosage form.
An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 x 4.6 mm id) maintained at 30 degrees C. The mobile phase consisted of acetonitrile-water (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5-200 microg/mL (r2 = 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19%, with bias lower than 1.81%. The LOD and LOQ were 0.39 and 0.5 microg/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.
Dalmora
Sérgio Luiz
SL
Federal University of Santa Maria, Department of Industrial Pharmacy, 97105-900 Santa Maria-RS, Brazil. sdalmora@terra.com.br
Sangoi
Maximiliano da Silva
Mda S
Nogueira
Daniele Rubert
DR
da Silva
Lucélia Magalhães
LM
D000998:Antiviral Agents / Q000032:analysis* / Q000737:chemistry*; D002021:Buffers; D002626:Chemistry, Pharmaceutical / Q000379:methods; D002845:Chromatography / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006147:Guanine / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D006868:Hydrolysis; D013058:Mass Spectrometry / Q000379:methods; D008956:Models, Chemical; D010710:Phosphates / Q000737:chemistry; D017680:Potassium Compounds / Q000737:chemistry; D012016:Reference Values; D015203:Reproducibility of Results; D013607:Tablets / Q000032:analysis*; D013678:Technology, Pharmaceutical / Q000379:methods*; D014867:Water / Q000737:chemistry
D000998:Antiviral Agents; D002021:Buffers; D010710:Phosphates; D017680:Potassium Compounds; D013607:Tablets; D014867:Water; C413685:entecavir; D006147:Guanine; C013216:potassium phosphate