Thin layer chromatography and Bioautography: The seed extract with a concentration of 1mg/ml was spotted on the TLC plates.The solvent system used was acetone and hexane with various ratios. The spots were identified in long UV, short UV and also in the iodine chamber. Then RF value was calculated to find the active metabolites. The developed TLC plates were sprayed with DPPH to study the zone of inhibition. The compounds having antioxidant property will exhibit a clear zone over the plates .
Total flavonoid content To determine the total flavonoid content (TFC), the aluminium chloride method was followed (Zhang et al., 2011). The method is based on the formation of flavonoid-aluminium complex, which shows absorption at 510 nm. Quercitrin hydrate (1 mg/ml in ethanol) was used as standard. 2.6. Free radical scavenging activity (FRSA) Free radicals scavenging activity was assessed by the method of Mellors and Tappel (1966).
The residue was reconstitute for LCMS/MS analysis, were chromatographic separation was carried on a HyPurity Advance, 50X4.6mm column with a mobile phase 10mM Ammonium formate ( pH=8) and Acetonitrile. The flow rate was 0.8 ml/min throughout the process. The liquid Chromatography, Agilent 1290 coupled to electrospray ion (ESI) Mass Spectrometer (MS QQQ). The developed method was validated for specificity, accuracy, precision, stability, linearity, sensitivity and recovery. The method was linear and found to be acceptable over the range of 50–1000 ng/ml.
Highest overall desirability was obtained from the optimized formulation comprising at 0.0 level of polymer: drug ratio and 1.0 level of phase volume ratio. In vitro gefitinib release data showed burst release (5.93 ± 0.28% in 1 h) followed by sustained release (17.95 ±0.95%) for 276 h. Best fitted Higuchi’s model assured the potential controlled gefitinib release form the microcapsules.SEM image of microcapsules was spherical. This preliminary study indicated controlled release of drug for prolong period of time. However, this study could be substantiated by the performance of in vivo. Keywords: gefitinib, poly-e-caprolactone, microcapsules, desirability, controlled release.
A simple, accurate and precise high-performance thin layer chromatographic method for analysis of pirfenidone both as a bulk drug and in tablet formulation was developed and validated in pharmaceutical dosage form. The method employed aluminum-backed silica gel 60GF-254 TLC plates as the stationary phase. The solvent system consisted of toluene:methanol in the ratio of 8:2 vv at 25±0.2 ºC of ambient temperature was found to give compact spots for pirfenidone with R value of 0.49 ± 0.01. Densitometric analysis of pirfenidone was carried out in absorbance mode at 315 nm. The linearity study was carried out in the concentration range of 800-1600 ng spot-1 showed good linear regression with r2 > 0.996 and 0.995 by area and height respectively.
The ﬂow rate was 0.3 ml/min and UV detection was performed at 215 nm. A System Suitability Test (SST) was developed to govern the quality of the separation. The developed method has been validated further with respect to linearity, accuracy, precision, selectivity, LOD, LOQ and robustness. Different batches of samples were examined using this method, the method proved to be successful when applied to analyze a commercial magnesium valproate formulation. KEYWORDS Magnesium Valproate,Ultra Performance Liquid Chromatography, Process Related Impurities, Method Validation, Isocratic Elution.
Human Defensins (1-5) are small, cationically charged, cysteine-rich endogenous antibiotic peptides with antimicrobial and cytotoxic properties that contain 29-35 amino acid residues, including six invariant disulphide linked cysteines moiety having a molecular weight of 4-5 kDa. The novel trend in drug development is the design and development of biopharmaceuticals, thus, the pharmaceutical industry has focused on bio molecules method development and validation (8-9). HPLC is a widely used technique for proteins and peptides because of its ease of usage, higher selectivity and faster analysis. In this study one of the antim... ... middle of paper ... ...Table 2). The results for intraday (0.30 – 0.80%) & interday precision (0.34 – 0.62%) study performed on 3 concentrations (20, 30 & 40 μg/ml) of standard solution of BSA & Defensin indicate that the purported method being precise (Table 2).
Thus, the aim of this work was to develop, optimize and validate a specific, accurate, precise and sensitive a new spectrophotometric method based on the oxidation reaction between iodide and iodate in the presence of carboxylic acid form of LP yielding a yellow-colored product (λmax=286 nm) to determine LP in pharmaceutical tablets. The optimization of the reaction conditions was performed by applying a response surface methodology based on the central composite design which can save the time and effort by the estimation of the optimum conditions. In addition, the kinetic study of reaction was executed for avoid theinterference of colored and/or turbidity background of samples.
The deionized water with a conductivity of 6.1-6.4 μScm-1 was double distilled over KMnO4 and used throughout the experiments. 8-anilino-1-napthalenesulfonic acid (ANS) (used as Chromoform) was obtained from Aldrich and used as received. Stock solutions of ILs and Chromoform (1mM) were prepared using distilled water. Aqueous solutions of calculated amount of ILs were prepared by weight using an analytical balance with a precision... ... middle of paper ... ...tant temperature control bath. Dynamic light scattering measurements were performed at 298.15 ± 0.1 K using NaBiTec SpectroSize300 light scattering apparatus (NaBiTec, Germany) with a He−Ne laser (633 nm, 4 Mw).
35(1): 9–40  Krishna, M.V., & Sankar, D.G. 2007, Adaptation of Color Reactions for Spectrophotometric Determination of Pitavastatin Calcium in Bulk Drugs and in Pharmaceutical Formulations, E-J. of Chemistry,. 4(2), 272–278  Satheesh, N.K., & Baghyalakshmi J., 2007, Determination and Quantification of pitavastatin calcium in tablet dosage formulation by HPTLC Method, Anal. Letters 40 (14), 2625–2632  Panchal HJ, Suhagia BN, Patel NJ, Patel BH, 2008, A Simple and Sensitive HPTLC method For Estimation of Pitavastatin Calcium in Tablet Dosage J. Planar Chromatography Modern TLC, 21(4): 267-270.