Mast cell stabilizer and histamine receptor antagonist olopatadine hydrochloride (OPT) assay method predicated on LC have been established for the analysis in multiple formulations. The current method dealt with ophthalmic solution, nasal spray, and tablet formulation products. The isocratic chromatography method was optimized and validated with a Boston green C8 column (150 Â 4.6 mm, 5 μm i.d.). Sodium dihydrogen phosphate buffer (pH 3.5) with acetonitrile in the ratio of 75:25 (v/v) was used as a mobile phase at a flow rate of 1.0 mL min À1 and at the column temperature of 30 C, and the detection was done at 299 nm. The method was validated as per International Council for Harmonisation (ICH) guidelines and United States Pharmacopoeia (USP). The accuracy results ranged from 99.9 to 100.7%, % relative standard deviation (RSD) from the precision was 0.5, and correlation coefficient from the linearity experiment was > 0.999. Solution stability was established for 24 h at room temperature and refrigerator conditions, and it was found that the solutions were stable. Using quality by design-based experiment designs, critical quality attributes were studied and it was found that the method was robust. In all the forced degradation studies peak purity was passed, and no interference was found at the retention time of the active component. The method validation data demonstrated that the developed method is linear, precise, accurate, specific, robust, and stable for the determination of OPT from multiple formulations. Analytical eco-scale tool, Green Analytical Procedure Index (GAPI) tool, and the National Environmental Method Index (NEMI) were used to evaluate the greenness of the method, and the analytical eco-score of 77 for the presented method was found to be excellent.
The current study is to develop a simple high-performance liquid chromatography method for Carbidopa and Levodopa impurities' simultaneous determination with the combination of Entacapone in solid oral dosage forms. The estimation of impurities are critical in a combination product due to the more number of impurities. The presence of impurities in drug products affects quality and bio-efficacy. The quality by design approach allows the assessment of various analytical parameters and their effects with the minimum number of experiments. The current high-performance liquid chromatography method was developed using a kromasil column with gradient mobile phase. The detection was made 220 nm; the flow rate was 1.0 mL/min, and the column's temperature was 25 • C. The analytical curves presented a coefficient of correlation of >0.99, and detection and quantification limits were evaluated for all impurities. Excellent precision and accuracy were obtained for carbidopa and levodopa impurities. Intra-and interday precisions RSD were lower than 10.0, and recoveries of impurities varied between 91.2 and 108.2%. The results reveal the method's successful applicability for estimating Carbidopa and Levodopa with their process and degradation impurities from its marketed formulation.
Midostaurin (MTN), designated as an orphan medicinal product, is emerging as an important drug for treating acute myeloid leukemia and advanced systematic mastocytosis. The proposed method was developed and validated to evaluate the related impurities of MTN. The impurities were separated using a YMC Trait C18 ExRS column (150 Â 4.6 mm, 3 μm). Mobile phase A consisted of a 10-mM concentration of phosphate buffer adjusted to pH 3.0 with diluted orthophosphoric acid, and mobile phase B consisted of 90% acetonitrile and 10% water. The optimized chromatographic conditions were as follows: flow rate, 0.5 mL min À1 ; injection volume, 10 μL;UV detection, 290 nm; and linear gradient program, up to 65 min. The method was developed using an analytical quality by design approach. A systematic flow chart shows the evaluation, control, and life cycle management method. As part of method evaluation, risk assessment was conducted. The method has been validated per current guidelines of the International Conference on Harmonization. The recovery study and linearity ranges were established from the limit of quantification to 150% optimal concentrations. The recovery was found to be between 95.5 and 102.5%, and linearity (r 2 ) was 0.9998-0.9999 for all the identified impurities. The method precision results were achieved below 10% of relative standard deviation. Forced degradation studies were performed under chemical and physical stress conditions. The compound was sensitive to chemical stress conditions. During the study, the analyte degraded and was converted into the identified degradation impurities, and its molecular mass was found using the LC-MS technique.
A simple, precise, linear, robust, accurate, and stability‐indicating liquid chromatography method was developed and validated to determine Ibrutinib in finished solid dosage forms by reversed‐phase high‐performance liquid chromatography/photodiode array detector. Separation was achieved using a Luna C18 150 mm × 4.6 mm × 3.0 μm with a suitable mobile phase. The mobile phase: A consists of a 10 mM phosphate buffer concentration and 1 mL triethylamine, adjusted to pH 5.6 with a diluted orthophosphoric acid solution and acetonitrile in the ratio of 95:5 v/v to enhance the results. Moreover, mobile phase ‐ B contains 85% of acetonitrile. The optimized chromatographic conditions such as flow rate 1.0 mL/min, injection volume 10 μL, column temperature 40°C, and wavelength 258 nm. The proposed method is significant because it was developed by the Quality by Design approach. All impurities were identified, such as degradation and placebo impurities without interference at principle peak retention time. After development, it has been validated as per current regulatory guidelines. Obtained recovery between 98 and 102% at 50–200% level; linearity found (r2) = 0.9999 from 20 to 200% level; precision results achieved <2.0% relative standard deviation; and the robustness study results are found satisfactory. It's beneficial.
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