Posted by admin on May 31, 2018 in |
A simple, highly sensitive, precise and accurate liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the rapid quantification of clobazam in human plasma samples. The chromatographic separation was achieved with a reverse phase column Reprosil Gold XBD C18 (100 × 3mm, 3µm) and the mobile phase consisted of 10 mM ammonium acetate buffer and 0.1% acetic acid in methanol (15:85, v/v) as eluent by running a linear gradient method. The effluence was ionized by positive electrospray ionization and measured by mass spectrometry. The method was validated with linear calibration curve over a wide dynamic concentration range of 0.501-499.995 ng/mL and the lower limit of quantification was 0.501 ng/mL with good accuracy and precision. The mean extraction recovery of the method was higher than 96.4% and 103.3% for clobazam and IS, respectively. The method was successfully demonstrated for evaluation of bioequivalence study of 10 mg clobazam tablet formulation in 28 healthy Indian male subjects under fasting...
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Posted by admin on May 31, 2018 in |
A novel stability-indicating mass compatible gradient Reverse Phase Ultra-Performance Liquid Chromatographic (RP-UPLC) method was developed for the quantitative determination of purity of brivaracetam drug substance samples in the presence of its impurities and degradation products. The method was developed using waters acquity UPLC BEH SHIELD RP18 (100 mm x 2.1 mm, 1.7 µm) column with mobile phase containing a gradient mixture of solvents A and B. The eluted compounds were monitored at 230 nm, the run time was 10 min within which brivaracetam and its four impurities were well separated. Brivaracetam was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Brivaracetam was found to degrade significantly in acidic and slightly in oxidative stress conditions and stable in base, hydrolytic, and photolytic degradation conditions. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy,...
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Posted by admin on May 31, 2018 in |
Selenium nanoparticles are attracting more and more attention due to their excellent photoelectrical characteristics and high biological activity. Selenium is also found to be effective against cancer. ZnO nanoparticles are reported to inhibit the growth of a wide range of pathogenic bacteria under normal visible lighting conditions. In this research work, we report the preparation of a set of Selenium doped ZnO nanoparticles (Zn1-xSexO1-δ; where x = 0.05, 0.10, 0.15 and 0.20) by simple chemical synthesis method. The materials were characterized systematically by X-ray Diffraction method, FT-IR spectroscopy, particle size analysis, SEM, EDAX analysis and TEM. The physical characterization studies have revealed the presence of fine particles in the prepared crystalline materials. The prepared materials were also subjected to antimicrobial assay by agar well diffusion method against both Gram positive (Staphylococcus aureus and Bacillus subtilis) and Gram negative bacteria (Escherichia coli and Klebsiella pneumoniae). Among studied, the material with the composition the materials Zn0.80Se0.20O1-δ have exhibited excellent antibacterial activity against the bacteria such as, Bacillus subtilis and Staphylococcus aureus....
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Posted by admin on May 31, 2018 in |
The Pharma market is getting flooded with fixed dose combination drugs due to better patient compliance, has but created a challenging situation for analytical chemists. The objective of study was developing an analytical method for simultaneously estimating aliskiren and amlodipine in combination with their forced degradation products obtained by treating the sample under tress conditions like acid and base hydrolysis (0.01N HCl, and 0.01 NaOH, oxidation(3% H2O2), photolytic and thermal degradation(80oC). The linearity ranging was 2.5-25μg/ml and 10-100μg/ml of Amlodipine and Aliskiren and regression coefficient was found to be 0.998 and 0.996 respectively. The chromatographic separation of analyte was carried out using JASCO HPLC system with HiQ Sil C8 (4.6mmØ × 250mm, 5 ?) column. The mobile phase consists of acetronitrile and pH was adjusted to 4 with orthophosphoric acid solution. The analyte were detected at 210nm using UV detector with flow rate of...
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Posted by admin on May 31, 2018 in |
Dipyrone (sodium noramidopyrine methanesulfate), a member of the pyrazolone group, is a drug that possesses analgesic, antipyretic, anti-inflammatory, and spasmolytic properties. Traditionally, iodimetric methods have been recommended for the quantitative determination of dipyrone in all its pharmaceutical forms. This work describes the development of zero order and fourth order (∆λ = 10) derivative spectrophotometric methods for the determination of dipyrone in different pharmaceutical formulations, using water as solvent. The analytical curves presented correlation coefficients greater than 0.999, limits of detection varying from 0.23 to 0.49 mg L-1, and limits of quantification varying from 0.78 to 1.63 mg L-1. The average recoveries ranged from 98 to 103 % for the zero order method and from 96 to 104 % for third and fourth order derivative methods. Intra and inter-day precisions, expressed as relative standard deviations, were below 4.2 %. The excipients present in dipyrone tablets and solutions did not interfere in the analyses. The method was shown to be linear, reproducible, specific, sensitive and...
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