Stability Study of Doxycycline Hyclate and Validation of its UV. Spectrophotometeric Quantification Method

Abstract

Stability assessment of samples of doxycyline hyclate ( raw material / finished products) was carried out through stability testing protocols , which define clearly temperature, humidity , storage time , and suitable light challenge . Details of assay and a comparative study for samples of raw material and finished products, manufactured by various companies were described. A simple, rapid, accurate and economical UV. Spectrophotometric method was carried out according to a validation master plan (VMP). Identification tests and assay for stability study of doxycyline hyclate were applied according to BP(2009) and USP(2007) guides . The wavelength at maximum absorption (λmax) of doxycyline hyclate was found to be 275 nm in water. Absorbance measurements were found to be linear at the concentrations of 1.0 to 4.0 mg/ml. The results of stability studies were satisfactory and agreed with labeled claim .The proposed method was applied to pharmaceutical formulation, and percentage amount of the drug was found to be 98.90% which is in good agreement with the labeled claim. The accuracy of the method was checked by recovery experiment performed at five different levels (50%, 80%, 100%, 120% and 150%). The percentage recovery was found to be almost 100%. The low values of RSD(s) are indicative of accuracy and reproducibility of the method. The precision of the method as an intra- day; inter day variations and its repeatability were studied. The percentages of RSD Values were less than 2 indicating that the method was precise.

V

Ruggedness of the proposed method was studied with the help of two analysts; moreover, the robustness study was carried out to confirm the system suitability. In the present work, comprehensive stability studies were carried out for doxycyline hyclate and the results agreed with the labeled claim. The proposed method showed a rapid and cost – effective quality control tool for routine analysis of doxycycline hyclate in bulk and in pharmaceutical dosage forms.