Search

The pharmaceutical combination of dexpanthenol (DPA), lidocaine hydrochloride (LIH) and mepyramine maleate (MAM) is used for their anti-allergic, anti-inflammatory, anti-pruritic, anesthetic and antiseptic properties. The present study was aimed to develop and validate a new, first and rapid high performance liquid chromatographic method for simultaneous determination of DPA, LIH and MAM in the presence of their stress-induced degradation products in pharmaceutical gel/fluigel formulations. The chromatographic separation was performed on an Inertsil ODS-3 V, 250 × 4.6 mm (5 μm) column using a gradient mobile phase of an aqueous solution of ammonium acetate (0.01 M) and methanol mixture at gradient flow rates of 1.3 mL/min and 1.5 mL/min with detection at 230 nm. The retention times for DPA, LIH and MAM were ~3.28 min, 11.67 min and 12.99 min, respectively. The method was validated in accordance with International Conference on Harmonisation guidelines. Calibration curves were linear in the ranges of 9-54 μg/mL for MAM and LIH and 30-180 μg/mL for DPA with satisfactory correlation coefficients (R2 > 0.999). The mean % recoveries obtained were found to be 99.9% for MAM, 100.3% for LIH and 99.3% for DPA. Precision % RSD was <2. Robustness results were uniform, there were no marked changes, so method is highly validated. All drugs were subjected to stress conditions and degradation products were separated with acceptable peak tailing (T ≤ 2) and good resolution (Rs > 2). The validated method therefore can be adapted for quality control procedures of the drugs in pharmaceutical dosage forms and their stability studies.

An isocratic reversed phase HPLC method for the simultaneous determination of doxorubicine (DOX) and celecoxib (CXB) out of a nanoparticulate fixed dose combination (NanoFDC) was developed and validated. Linearity of the results was demonstrated from 1-11 μg/mL for both components. Lower limits of detection were determined as 7 ng/mL for DOX and 13 ng/mL for CXB. Total run time was approximately 15 min.

New analytical methods have been developed and validated on high performance liquid chromatography (HPLC) to assess the assay, content uniformity and dissolution of immediate release candesartan cilexetil 32 mg tablets. Method development studies were performed on cyano column. Mobile phase of assay and content uniformity test consisted of mixture of 0.05 M phosphate buffer, pH 4.5 and methanol (40 : 60, v/v) adjusted to pH 4.0 with trifluoroacetic acid, whereas mobile phase of dissolution test consisted of mixture of I mM phosphate buffer and acetonitrile (50 : 50, v/v) adjusted to pH 2.0 with trifluoroacetic acid. Mobile phases were pumped at flow rate of 1.0 mL/min, ultraviolet-visible (UV) detector was operated at 254 nm, injection volume was set at 20 μL, column temperature was held at 25⁰C. Dissolution medium was 0.05 M phosphate buffer, pH 6.5 including 0.70% (w/v) polysorbate 20. Validation studies met acceptance criteria of system suitability, specificity, linearity and range, accuracy, precision, detection limit (LOD), quantitation limit (LOQ) and robustness parameters.