Current Issue : January - March Volume : 2013 Issue Number : 1 Articles : 14 Articles
A rapid, simple, precise stability indicating RP-HPLC method has been developed for the estimation of Naftopidil on Phenomenex Luna C8 (4.6x150mm,5μ) .A mobile phase consisiting of Methanol : water (90:10 %v/v) was used. The flow rate was 0.8 ml/min with UV detection at 232 nm. Naftopidil was subjected to stress conditions of hydrolysis (acid, base), oxidation, photolysis and thermal degradations. Beer’s law was obeyed in the concentration range of 1-5 µg/ml and correlation coefficient as 0.9999. This method can be used for the routine analysis of naftopidil in tablet dosage form....
Pharmaceutical industry is moving towards quality. Many pharmaceutical companies have used several Quality Management System (QMS) for instance ISO 9001. Design process has one of the most important factors that contributing in pharmaceutical product quality. The pharmaceutical industry is used the concept of Quality by Design (QbD) to apply science-based manufacturing principles for new and existing products to assure quality of the formulation. In a first step, the QbD-methodology is systematically used to establish the critical quality attribute identifies potentially critical input factor and these factors to define activities for process characterization. A process DOE was used to evaluate effects of the design factors on manufacturability and final product CQAs, and establish design space to ensure desired CQAs. Critical material and process parameters are linked to the critical quality attributes of the product. Experiments were designed with focus on critical material and process attributes. Quality by design is an essential part of the modern approach to pharmaceutical quality. The purpose of this article is to discuss the use of Quality by Design (QbD) in pharmaceuticals and describe how it can be used to ensure pharmaceutical quality. Process parameters and quality attributes were identified for each unit operation. The design space was established by the combined use of DOE, optimization and multivariate analysis to ensure desired CQAs. Multivariate analysis of all variables from the DOE batches was conducted to study relationships between the variables and to evaluate the impact of material attributes/process parameters on manufacturability and final product CQAs....
International Conference on Harmonization requires a quality concept for impurities during the drug development process is proposed based on the requirements featured in the impurity guidelines. Because of the particular nature of the drug development process, one crucial element is qualification. Once an impurity profile is qualified by the first toxicological studies, attention is then focused on the comparison made, by means of comprehensive analytical monitoring, between qualified impurities and those of new batches. The clear assignment of impurities to toxicologically-qualified impurities can be addressed using multidimensional information, such as retention times, molecular mass or spectral properties. The advantages of use of the hyphenated LC–MS technique in performing this ‘impurity inventory’ are discussed by the authors using the example of peptide drugs. As part of an integrated quality concept for impurities during drug development, the multidimensional evaluation of impurity profiles by LC–MS coupling is presented using peptide drugs as an example. This quality concept can be regarded as an adaptation of the ICH-requirements to the special situation during the drug development process. The primary goal is to obtain qualitative molecular weight information for impurity peaks detected at the same UV wavelength as for the impurity test procedure. The approach is focused on the investigation, if the impurities in a clinical batch were also present in the toxicologically qualified batch(es). Depending on the relevance of individual impurities in further batches or as degradation products, the molecular weight can be used as a starting point for further characterization and identification. Often, eluents with volatile buffers required for MS result in different selectivities and/or inferior chromatographic separation and sensitivity compared with nonvolatile buffers (e.g. phosphates). In these cases, peak ‘tracking’ especially for small peaks can become critical. A procedure is presented for on-line coupling of LC methods with non-volatile eluents to mass spectrometry. Impurity profile of an active pharmaceutical ingredient (API) is a very important task for all stages of drug development. A systematic approach for tracking impurity profile of API is described. Various real pharmaceutical applications are presented through successful examples of impurity profile tracking for novel APIs A general strategy including selection of a reversed phase high performance liquid chromatographic (RP-HPLC) impurity profile method based on screening various stationary phases and changing the pH of the mobile phase and elucidation of impurity structures through the utilization of LC–MS, preparative-LC and NMR is demonstrated. A series of studies were conducted on the peak purity check by using the LC-UV diode-array and LC–MS detections. The advantages and disadvantages of each technique in the evaluation of peak purity are discussed....
Gene is a building block of body and through knowledge about gene and genetically derived products is called as Genetic engineering. Genetic Engineering is a part of Biotechnology. Biotechnology has been defined as the application of biological organisms, system or processes to manufacturing and service industries. Genetic Engineering is defined as genetic modification; it is the direct manipulation of any organisms, genome using modern DNA technology. Biotechnology having wide application in field of Pharmaceutical, Agriculture Industry, Beverages, Dairy products, Environmental science, Medical & Health sciences, Amino acid production. Both Qualitative and quantitative methods are now available for identification and quantification of gene. Various analytical methods like Protein Content Analysis, Amino Acid Analysis, Protein sequence, Peptide Mapping, Immunoassay, Electrophoresis, Chromatography, DNA determinations, Quantitative Assay, Biomimetic Assay, Carbohydrate determination, Adventitious and endogenous protein detections used for identification of gene and genetic materials. Other methods like Uv spectrophotometry, Kjeldahl nitrogen analysis, Biuret assay, Lowry protein, Bradford assay, Bicinchoninic acid assay, Fluoroscent methods used for protein analysis. Protein content assays are among the most important of all the methods used for biotechnology derived products because the results of other types of assays, such as potency, are also dependent on them....
A simple, economical, precise and reproducible visible spectrophotometric method have been developed for the estimation of Gemifloxacin mesylate(GEM) and Ambroxol hydrochloride(AMB) from its tablet dosage form. First order derivative spectroscopy methods adopted to eliminate spectral interference. Beer’s law was obeyed in the range of 2 to 12 μg/ml for AMB and 10-60 μg/ml for GEM; wavelengths selected for Quantitation are 291nm and 244 nm respectively which are the λmax of both the drugs. The proposed methods was validated statistically and applied successfully to determination of Gemifloxacin mesylate and Ambroxol hydrochloride in bulk and tablet formulation....
A simple, sensitive, rapid and accurate spectrophotometric method has been developed and validated for the estimation of voglibose in bulk and pharmaceutical dosage forms. The method was based on the combination of Sodium periodate and Taurine, showing the absorption about 280 nm in water and methanol. The proposed method has permitted the quantification of voglibose over linearity in the range of 10-70µg/mL (r2 =0.997). The method was validated as per ICH guidelines....
Novel, sensitive and accurate spectrofluorimetric method has been developed and validated for estimation of tapentadol hydrochloride in bulk and in laboratory tablet dosage form. The method is based on measurement of native fluorescence of tapentadol in distilled water at 298 nm after its excitation at 273 nm. The fluorescence intensity-concentration plot was linear in the concentration range of 1- 10 μg/ml with good correlation coefficient 0.9990. The developed method was successfully applied for determination of tapentadol hydrochloride in laboratory sample of tablet dosage form. Furthermore developed method was successfully validated as per ICH guidelines in terms of, linearity (1 - 10 μg/ml), repeatability (RSD 0.39 %), precision (intra-day variation, RSD, 0.17 to 0.63 % and inter-day variation, RSD, 0.34 to 0.63 %) and accuracy (99.44 to 99.62 %). The limit of detection and quantification was found to be 0.011 and 0.034 μg/ml respectively. The developed method proved to be simple, economic and precise. Therefore proposed method can be employed for the routine quality assessment of the tapentadol hydrochloride in bulk as well as in pharmaceutical dosage forms....
The aim of this present work was to develop and validate a simple, rapid, accurate RP-HPLC method for the simultaneous estimation of Alfuzosin hydrochloride (ALH) and Dutasteride (DUT) in bulk drug and pharmaceutical dosage form. The chromatographic separation was carried out in an isocratic mode using an Kromasil C18 column (150mm×4.6mm,5µm particle size) with a mobile phase of mixed phosphate buffer:acetonitrile(30:70%v/v) and the eluents were monitored at 242nm.The retention times of ALH and DUT were 2.2 and 7.2min respectively. The method was found to be linear over the concentration range of 5-30µg/ml for ALH and 0.25-1.5µg/ml for DUT with a correlation coefficient of 0.999. The proposed RP-HPLC method was validated according to ICH guidelines and was successfully employed for routine quality control analysis in bulk and combined dosage forms....
A simple, rapid, cost-effective, sensitive, precise and specific reverse phase high performance liquid chromatographic method was developed and validated for the determination of prasugrel and aspirin in bulk and tablet dosage form. It was found that the excipient in the tablet dosage form does not interfere in the quantification of active drug by proposed method. The HPLC separation was carried out by reverse phase chromatography on phenomenex C8 column( 250×4.6 mm, 5µ) with a mobile phase composed methanol: water 80:20 v/v in isocratic mode of separation at flow rate 1ml/min. The detection was monitored at 236nm. The calibration curve for aspirin and prasugrel was found to be linear from 2 to 18 µg/ml and 15 to 135 µg/ml respectively. The interday and intraday precision was found to be within limits. The proposed method validated according to the ICH guidelines and has adequate sensitivity, reproducibility and specificity for the determination of prasugrel and aspirin in bulk and its tablet dosage forms. LOD and LOQ for prasugrel were found to be 30 ng/ml and 100 ng/ml respectively. LOD and LOQ for aspirin were found to be 10 g/ml and 30 ng/ml respectively. Accuracy for prasugrel were found to be 98.13-101.98 and for aspirin 99.92-100.26 respectively. The Robustness study and percentage of assay of the formulation were found within limit as per ICH guidelines....
The present research work aims to develop a simple, sensitive, accurate and reproducible method for the simultaneous estimation of Avanafil and Dapoxetine hydrochloride by two different spectroscopic method viz, Simultaneous equation Method (Vierodt's method) (Method-A) and Q-Absorption method (Method-B). Absorbance maxima for Avanafil and Dapoxetine hydrochloride were found to be at 247 nm and 211 nm respectively for method-A, and Iso-absorptive point for both drugs was found to be 226.6 nm for method-B by using 0.1 N HCl as a solvent. Absorption maxima of avanafil at 247nm, was taken as second wavelength for determination by method-B. Linearity for both the methods was observed in concentration range of 2.5-15 μg/ml for Avanafil and 1.5-9 μg/ml for Dapoxetine hydrochloride. The correlation coefficients for both the methods obtained were near to 1. The accuracy of both methods was evaluated by recovery studies and recovery results were obtained from 98 % to 102% for both the methods and the relative standard deviations below 2% were achieved. Validation was done as per ICH guidelines. Proposed methods can estimate Avanafil and Dapoxetine hydrochloride simultaneously in combined dosage form without the interference of common excipients....
The aim of present study to develop methods for estimation of gabapentin in pharmaceutical dosage forms. Distil water is used as a solvent so methods are called green analytical methods. Absorption minima in first order derivative spectra was found to be 220 nm (method-A) and area under curve was measured from 200-210 nm (method-B) and 200-280 nm (method-C), the drug followed a linear relationship in the range of 100-600 μg/ml while the correlation coefficient was at 1.0, 0.999 and 1.0 respectively. The recovery was 99.52% ±0.56(method-A) and the coefficient of variance for intraday and interday was found to be less than 2%, LOD and LOQ for this method was found 25 μg/ml and 83 μg/ml(method-C) respectively. This method is found suitable for day to day analysis of GBP in tablet dosage form....
A simple and sensitive colorimetric method has been developed for the quantitative estimation of Moxifloxacin from Pharmaceutical liquid dosage form. Developed method is based on formation of ion pair coloured complex of drug with Eosin Blue dye. The complex formed showed absorbance maxima at 534.0 nm. Linearity was observed in concentration range of 100-400 μgm/ml of Moxifloxacin. The results of analysis were validated statistically and by recovery studies....
In the present study, two different chemometric methods – partial least squares (PLS) and principal component regression (PCR) for simultaneous determination of cefixime and ornidazole in pharmaceuticals are described. These two approaches were successfully applied to resolve the overlapped data and quantify the two components in the studied mixture using the calibrations constructed with the absorption data matrix corresponding to the concentration data matrix with measurements in the range of 205-400 nm (Δλ = 1 nm) of the zero order spectra. The calibration range was found to be 0.8-4 µg mL-1 for cefixime and 2-10 µg mL-1 for ornidazole, respectively. The PLS and PCR methods neither require any separation step, nor any prior graphical treatment of the overlapping spectra of the two drugs in a mixture. The calibration of the chemometric models were evaluated by internal validation (prediction of components in its own designed training set of calibration) and by external validation over synthetic and pharmaceutical preparations. Both studied methods can be considered acceptable for the pharmaceutical quality assurance of cefixime and ornidazole in combined dosage forms....
Pramipexole Hydrochloride is a nonergot dopamine agonist, indicated for the treatment of the Parkinson''s disease. An attempt was done to develop simple precise, accurate and validated HPTLC method for the estimation of Pramipexole Hydrochloride bulk and in pharmaceutical dosage form. The compounds were separated on aluminium-backed silica gel 60 F254 plates with toluene, acetonitrile, methanol, ammonia, 5.5:3:1.5:0.2 (% v/v/v/v) as mobile phase. These system was found to give compact spots for the drug with the RF value of 0.50. Densitometric analysis of Pramipexole Hydrochloride was done at 268 nm. Regression analysis for the calibration plots was indicative of good linearity between response and concentration over the range 2000-6000 ng per spot with the correlation coefficient (r2) 0.9991. Pramipexole Hydrochloride was subjected to acid, base, peroxide, dry heat and photo degradation. It was susceptible to acid and base hydrolysis, oxidation, dry heat and photodegradation. Statistical analysis proved the method is repeatable, selective, and accurate for estimation of Pramipexole Hydrochloride. Because the method could effectively separate the drugs from their degradation products, it can be used as a stability-indicating method....
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