A simple, rapid, precise and accurate High-Performance Thin Layer Chromatography (HPTLC) method was developed and validated for the estimation of Nintedanib, a novel tyrosine kinase inhibitor used in idiopathic pulmonary fibrosis, in bulk drug. Chromatography was carried out using silica gel 60 F254 Thin Layer Chromatography (TLC) plate and mobile phase Chloroform: Methanol in the ratio 7:3 v/v. The densitometric determination was done at 386 nm. Regression analysis data for the calibration plot were indicative of a good linear relationship between response and concentration over the range of 800–3200 ng/band. The variance (r) was found to be 0.999. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found to be 83.357 ng/band and 252.599 ng/band respectively. The method was validated according to the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use [ICH Q2(R1)] guideline. The method was precise and accurate with %RSD 0.5323 (intraday) and 0.6939 (interday) respectively and percentage recoveries in the range 99.65–101.43%.
The whole plant of bhringaraj (Eclipta alba) was dried and pulverized. The phytoconstituents of the pulverized plant material were extracted separately with two different solvents namely petroleum ether (hot percolation) and methanol (cold maceration) to carry out a comparative extraction efficiency of the above two solvents. β-sitosterol reported to have antiandrogenic, anticancer, antiinflammatory, antiprostatitic, antitumor, etc. activity, was selected as the active biomarker for quantification of the aforementioned plant material.HPTLC was carried out for quantification of the biomarker and obtained data was compared with HPLC data. Petroleum ether was found to be an effective extracting solvent for β sitosterol from E. alba as compared to methanol. The percentage content of β-sitosterol in E. alba methanolic and petroleum ether extract was found to be 0.10% and 4.65% w/w respectively by HPTLC whereas the percentage content of β-sitosterol in Eclipta alba petroleum ether extract was found to be 4.67 % w/w by HPLC. AAS data revealed the presence of the metals (ppm ± SEM) are within safety limits, copper (1.151 ± 0.031), chromium (0.528 ± 0.012), cadmium (0.021 ± 0.035), lead (0.860 ± 0.009), arsenic (0.081 ± 0.007), mercury (0.036 ± 0.010).
A simple and rapid stability-indicating method for determination of nintedanib (NTB) in bulk drug using HPTLC and LC-MS n was developed and validated. Stress degradation studies were carried out by hydrolysis, oxidation, thermal and photolytic. Drug was found to be stable in thermal whereas one degradant was found in acid hydrolysis, three in basic hydrolysis, five in oxidative and two in photolytic stress. The probable structures of the degradation products were predicted & the degradation pathway was also established. Chromatography was carried out using silica gel 60 F254 TLC plate and mobile phase of Chloroform : Methanol in the ratio 7:3 v/v. The densitometric determination was done at 386 nm. The degradants were not detectable when stressed as per ICH recommended conditions but on increasing the strength of acid, base and peroxide, the degradants were very much prominent and were easily detectable in HPTLC. The LC system consisted of a Zorbax Bonus C18 (150 mm×4.6 mm, 3.5 µ). A gradient mobile phase consisting of mobile phase A: 10mM Ammonium formate (0.05% formic acid): ACN (pH 3.9) (90:10) and mobile phase B: 10mM Ammonium formate (0.05% formic acid): ACN (pH 3.9) (10:90) with a flow rate of 0.7mL/min was used to separate the degradants up to a total retention time of 15 min. Mass spectrometric detection was performed using Thermo Scientific LCQ fleet Ion Trap LC/MS n .
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