ABSTRACT
A new stability-indicating RP-HPLC assay method was developed and validated for quantitative determination of loteprednol etabonate in bulk drugs and in ophthalmic suspensions in the presence of degradation products generated from forced degradation studies. The system consisted of Agilent Technologies Zorbax Eclipse XDB-Phenyl 5 µm 4.6 × 250 mm, and detection was performed at 244 nm. The mobile phase consisted of water-acetonitrile-acetic acid (34.5:65.0:0.5, v/v/v) run at a flow rate of 1 mL/min and maintained at room temperature. The calibration curve was linear from 30 to 70 µg/mL with r > 0.999. Accuracy (mean recovery 100.78%) and precision were found to be satisfactory. Stress conditions including acid and alkali hydrolysis, water stress, oxidation, photolysis and heat were applied. The degradation products did not interfere with the detection of loteprednol etabonate, thus the method can be considered as a stability-indicating method. The proposed method can be used for quality control assay of loteprednol etabonate in bulk drug and in ophthalmic suspensions and for stability studies as a result of the ability of the method to separate loteprednol etabonate from its degradation products and excipients.
Subject(s)
Androstadienes/chemistry , Chromatography, High Pressure Liquid/methods , Ophthalmic Solutions/chemistry , Chromatography, Reverse-Phase/methods , Drug Stability , Loteprednol Etabonate , Quality ControlABSTRACT
During preformulation studies of cosmetic/pharmaceutical products, thermal analysis techniques are very useful to detect physical or chemical incompatibilities between the active and the excipients of interest that might interfere with safety and/or efficacy of the final product. Differential scanning calorimetry (DSC) was used as a screening technique for assessing the compatibility of avobenzone with some currently used cosmetic excipients. In the first phase of the study, DSC was used as a tool to detect any interaction. Based on the DSC results alone, cetearyl alcohol, isopropyl myristate, propylparaben, diethylhexyl syringylidene malonate, caprylic capric triglyceride, butylated hydroxytoluene (BHT), glycerin, cetearyl alcohol/ceteareth 20, cetearyl alcohol/sodium lauryl sulfate/sodium cetearyl sulfate, and paraffinum liquidum exhibit interaction with avobenzone. Stressed binary mixtures (stored at 50°C for 15 days) of avobenzone and excipients were evaluated by high-performance liquid chromatography. Binary mixtures were further investigated by infrared (IR) spectroscopy. Based on DSC, isothermal stress testing, and fourier transform infrared results; avobenzone is incompatible with caprylic capric triglyceride, propylparaben, and BHT.
