title: The ICH guidance in practice: stress degradation studies on stavudine and development of a validated specific stability-indicating HPTLC assay method.
abstract: A sensitive, selective, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for the analysis of stavudine both as a bulk drug and in formulations is developed and validated. The solvent system consisted of toluene-methanol-chloroform-acetone (7.0:3.0:1.0:1.0, v/v/v/v). Densitometric analysis of stavudine is carried out in the absorbance mode at 270 nm. This system is found to give compact spots for stavudine (retention factor value of 0.45 +/- 0.05) following development of chromatoplates with the mobile phase. Stavudine is subjected to acid and alkali hydrolysis, oxidation, dry-heat and wet-heat treatment, and photo and UV degradation. The drug undergoes degradation under acidic and basic conditions, oxidation, and wet-heat degradation. Linearity is found to be in the range of 30-1000 ng/spot with a significantly high value of correlation coefficient. The linear regression analysis data for the calibration plots show a good linear relationship with r2 = 0.9997 +/- 0.05 in the working concentration range of 300 to 1000 ng/spot. The mean value of slope and intercept are 0.10 +/- 0.06 and 22.12 +/- 1.08, respectively. The method is validated for precision, robustness, and recovery. The limits of detection and quantitation are 10 and 30 ng/spot, respectively. The proposed HPTLC method is utilized to investigate the kinetics of the acid degradation process. Arrhenius plot is constructed and activation energy is calculated.
authors.affiliation: Department of Quality Assurance Techniques, Bharati Vidyapeeth Deemed University, Poona College of Pharmacy, Erandwane, Pune-411038, India.
authors.forename: Neeraj
authors.initials: N
authors.lastname: Kaul
authors.forename: Himani
authors.initials: H
authors.lastname: Agrawal
authors.forename: Anant R
authors.initials: AR
authors.lastname: Paradkar
authors.forename: Kakasaheb Ramoo
authors.initials: KR
authors.lastname: Mahadik
mesh_terms: D002855:Chromatography, Thin Layer / Q000379:methods*; D004355:Drug Stability; D017408:Guidelines as Topic; D015203:Reproducibility of Results; D018894:Reverse Transcriptase Inhibitors / Q000737:chemistry*; D012680:Sensitivity and Specificity; D018119:Stavudine / Q000737:chemistry*
chemical_list: D018894:Reverse Transcriptase Inhibitors; D018119:Stavudine