Current Issue : January-March Volume : 2015 Issue Number : 1 Articles : 21 Articles
Metronidazole is antiamoebic, antiprotozoal, antibacterial agent belonging to the class of nitroimidazoles. Metronidazole is active against a wide variety of anaerobic Protozoal parasites and anaerobic Bacteria, This compound is directly trichomonacidal. It is also active against protozoaes such as trichomonas vaginalis, entamoeba histolytica, giardia lamblia. Metronidazole used in the treatment of intestinal and extraintestinal amoebiasis. Metronidazole used alone or in combination. Metronidazole was first approved by sanofi-aventis for marketing in France and its International Birth Date (IBD) is 29 July 1959. Since that time it has been registered and marketed worldwide. This review covers most recent analytical methods such as various spectroscopic methods, chromatographic methods and other methods for determination of Metronidazole Benzoate and Related Impurity in various pharmaceutical dosage forms and biological matrix were reported....
A new simple, sensitive HPLC method was developed and validated for the determination of 3-amino phenol in aripiprazole. Amino impurity was separated on xterra C18 analytical column with buffer consists 0.01 m dipotassium hydrogen phosphate and acetonitrile as mobile phase at a flow rate 1.0 ml/min. The effluent was monitored by UV detection at 210 nm. Column temperature maintained at 40°C, injection volume 10 µl. Calibration plots were linear in the range of LOQ to 150% level, LOQ and LOD were 0.0006 and 0.0002. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amino phenol in aripiprazole....
The simple, precise and cost effective spectrophotometric methods have been developed for the estimation of bosentan in bulk and its pharmaceutical formulations. Bosentan shows λmax at 223.0 nm in zero-order derivative spectrum (Method A), 217.13 nm in first-order derivative spectrum (Method B). Method C was based on calculation of area under curve (AUC) for analysis of bosentan in the wavelength range of 218.0 – 228.0 nm. The drug follows the Beer-Lambert’s law in the concentration range of 2 – 16 µg/ml for all the methods. The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization. All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of bosentan in bulk and pharmaceutical dosage forms....
The manuscript describes validated Q-absorbance ratio method for the simultaneous estimation of brimonidine tartrate and timolol maleate in eye drop. Q-absorbance ratio method was based on the estimation of both the drugs at two wavelengths i.e. absorption maxima of one drug and iso-absorptive point. An absorption maximum of timolol maleate was 294.1 nm and iso-absorptive point was 270.0 nm in methanol. The linearity was obtained over the concentration range of 10–70 µg/ml for both the drug with mean recovery of 97.81±1.29% and 97.72±0.63% for brimonidine tartrate and timolol maleate, respectively. The method was found to be simple, sensitive, accurate, precise and economical and applicable for the simultaneous determination of brimonidine tartrate and timolol maleate in combined dosage form....
Ropinirole hydrochloride, an orally administered non-ergoline dopamine agonist, is widely used in treatment of parkinsonism. In present study, a simple, rapid, accurate and economical UV-spectrophotometric method has been developed for the estimation of ropinirole hydrochloride from bulk and pharmaceutical formulation. The developed method was statistically validated in accordance with ICH requirement on the basis of various parameters like linearity, accuracy, precision, sensitivity, repeatability and ruggedness. The drug follows linearity in the concentration range 5-30 μg/ml with a correlation coefficient value of 0.9998 at λmax of 239 nm. The accuracy of the method was checked by recovery experiment performed at three different levels, i.e., 80%, 100% and 120%. The % recovery was found to be in the range of 100.98- 101.54%. The precision of the method was studied as an intraday; interday variations and repeatability. The % RSD value < 2 indicates that the method was precise, reproducible and accurate. Ruggedness of the proposed method was also studied with the help of two analysts. The proposed method was then successfully applied to pharmaceutical formulation. Amount of drug estimated was found to be 99.29-100.52%, which was in good agreement with the label claim. Excipients used in tablet formulation did not interfere in the estimation of ropinirole hydrochloride by developed method. The proposed method can be successfully employed in the routine analysis of drug in pharmaceutical dosage forms....
Two simple, accurate, precise and economical spectrophotometric methods have been developed for the estimation of amlodipine besylate (AML) and clopedogrel bisulphate (CLP) simultaneously in tablet dosage form. Simultaneous method (Method 1) and Absorb (Absorbance) method (Method 2) were used. Beer’s law is obeyed in the concentration ranges of 3-15 μg/ml and amlodipine besylate (AML) and clopedogrel bisulphate (CLP) for simultaneous method as well as absorbance ratio method. The wavelength ranges 279 nm and 289 nm in simultaneous method were selected to determine amlodipine besylate (AML) and clopedogrel bisulphate (CLP), respectively. Wavelength ranges 317 nm (iso-absorptive point) and 230.27 nm (λmax) of (amlodipine besylate) were selected for absorbance ratio (Q absorbance) method. The percent assay for commercial formulation was found to be in the range 99.92% – 100.07% for simultaneous method and 99.85–100.04% for absorbance ratio methods. Recovery was found in the range of for amlodipine besylate (AML) and 98.66-101% for clopedogrel bisulphate (CLP) by simultaneous spectroscopic method and 98.33-100.75% for amlodipine besylate (AML) and clopedogrel bisulphate (CLP) by absorbance ratio method for both the formulations. The results of analysis have been validated statistically and recovery studies confirmed the accuracy and reproducibility of the proposed methods which were carried out according to ICH guidelines....
A simple, rapid, accurate and precise, spectrophotometric method was developed for determination of mebeverine hydrochloride and its formulations i.e., Meb Sr and Colospa. In this method mebeverine hydrochloride shows absorbance maximum at different wavelength in different solvents, so absorbance was measured and the same wavelengths used for the estimation of mebeverine hydrochloride in respective solvents. Mebeverine hydrochloride obeys the beer lamberts’ law. Method was validated according to ICH guideline and carried out for analysis of mebeverine hydrochloride....
The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric area under curve method for estimation of olmesartan medoxomil. This area under curve of UV spectrum between 250 to 260 nm was validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 5-35 μg/ml. The value of correlation coefficient was 0.998. Satisfactory values of Percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. Results of the recovery studies (99.12% to 99.87%) showed accuracy of the method. LOD and LOQ were calculated as 3.271 μg/ml and 9.913 μg/ml, respectively. The developed method can be used for routine estimation of olmesartan medoxomil in bulk and tablet dosage forms....
The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric area under curve method for estimation of pioglitazone hydrochloride. This area under curve of UV spectrum between 221 to 231 nm was validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 10-50 μg/ml. The value of correlation coefficient was 0.999. Satisfactory values of percent relative standard deviation for the intra-day and inter-day precision indicated that method was precise. Results of the recovery studies (96.62% to 108.84%) showed accuracy of the method. LOD and LOQ were calculated as 0.16596 μg/ml and 0.50292 μg/ml, respectively. The developed method can be used for routine estimation of pioglitazone hydrochloride in bulk and tablet dosage forms....
The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric area under curve method for estimation of tramadol hydrochloride. This Area under Curve of UV spectrum between 266 to 276 nm was validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 30-150 μg/ml. The value of correlation coefficient was 1. Satisfactory values of Percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. Results of the recovery studies (97.94% to 106.98%) showed accuracy of the method. LOD and LOQ were calculated as 0.8937 μg/ml and 2.70 μg/ml respectively. The developed method can be used for routine estimation of tramadol hydrochloride in bulk and capsule dosage forms....
A simple, precise, accurate and economical UV visible spectrophotometric method has been developed for estimation of quinapril hydrochloride drug by AUC method. The standard and sample solutions were prepared by using double distilled water as a solvent. Quantitative determination of the drug was performed at wavelength range 206-216 nm. The linearity was established over the concentration range of 15-25 µg/ml for quinapril hydrochloride with correlation coefficient value of 0.999. Precision studies showed that % relative standard deviation was within range of acceptable limits. The mean percentage recovery was found to be 98.96%. The proposed method has been validated as per ICH guidelines....
Two precise, simple, accurate, reproducible, rapid and economic UV Spectrophotometric methods have been developed for simultaneous estimation of amlodipine and losartan in tablet dosage form by using distilled water as a solvent. Method I was based on formation and solving of simultaneous equation, known as Vierodt’s method. Losartan potassium and amlodipine besylate shows absorbance maximas at 250 nm and 240 nm respectively, so absorbance was measured at the same wavelength for the estimation of losartan potassium and amlodipine besylate in tablet combination. Method II was based on principle of Q-analysis, known as absorbance ratio method. Absorbance was measured at 254 nm (Isobestic point) and 250 nm (λmax of losartan). Losartan potassium and amlodipine besylate obeys Beer’s law in the concentration range of 0 to 30 µg/ml. Methods are validated according to ICH guidelines and can be applied for routine analysis of drugs in tablet dosage form....
A simple, selective, rapid, precise and economical UV spectrophotometric method and reverse phase high performance liquid chromatography method has been developed for the simultaneous estimation of paracetamol and chlorxazone from pharmaceutical formulation. The primary method was based on UV-spectrophotometric determination of paracetamol and chlorzoxazone, using simultaneous equation method. Its absorbance measurement at 282.5 nm (λmax of chlorzoxazone) and 248.0 nm (λmax of paracetamol) in methanol and the linearity was obtained in the range of 5 – 25 μg/ml for paracetamol and chlorzoxazone. The secondary method was based on RP- HPLC separation of the paracetamol and chlorzoxazone in reverse phase mode. Linearity was obtained in the concentration range of 100-500 μg/ml for paracetamol and 50-250 for the chlorzoxazone. Both these methods have been successively applied to pharmaceutical formulation and were validated according to ICH guidelines. The developed methods are validated in terms of specificity, selectivity, accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability....
Simple, accurate, precise, reproducible, requiring no prior separation and economical procedures for simultaneous estimation of trifluperazine HCl (TPZ) and isopropramide iodide (ISO) in tablet dosage form have been developed. The method was simultaneous equation method; in this method 226.0 nm and 257.0 nm were selected to measure the absorbance of both the drugs at mentioned wavelengths. TPZ shows linearity at 2.5-20 μg/ml and ISO shows linearity in a concentration range of 5-40 μg/ml. Recovery studies range from >99.41% for ISO and >98.93% for ISO in mentioned analytical method i.e. simultaneous equation method. The proposed methods are recommended for routine analysis since it was rapid, simple, accurate and also sensitive and specific (no heating and no organic solvent extraction was required)....
The USFDA guidelines now stress the pharmaceutical companies to file an ANDA which is QbD compliant. So, the pharmaceutical companies show a keen interest in leaning the principles of QbD. QbD refers to the achievement of certain predictable quality with desired and predetermined specifications. The present study describes the development and subsequent validation of an RP-HPLC method for the separation of paracetamol (PCM), tapentadol (TAP) and aceclofenac (ACE) in combination dosage form by application of QbD approach. A 33 full factorial design based on systematic scouting of three factors of RP- HPLC method (pH, mobile phase ratio and flow rate) was presented to study the effects on dependant variables, namely, peak area, number of theoretical plates and tailing factor. A pilot study was performed for obtaining the working range of 3 variable parameters. The statistical evaluation of the results was carried out by design Expert software. Contour and 3D surface plots were obtained and an overlay plot was generated, which showed a wide majority of yellow region indicative of a wide area of design space. Thus one can conclude that the selected range gave robust results. The optimized chromatographic condition was achieved on Enable C18 analytical column with phosphate buffer pH 6.3: methanol (35:65) as the mobile phase and flow rate of 1 ml min-1. The validation of the proposed method was carried as per ICH Q2 (R1) guideline. The calibration graphs ranged from 75- 450 μg ml-1 for PCM, 5 - 30 μg ml-1 for TAP and 20-120 μg ml-1 for ACE....
The present study was designed to develop a simple and validated liquid chromatographic method for the analysis metformin hydrochloride and amlodipine besylate in synthetic mixture using ultraviolet detector. Mobile phase was optimized to obtain a fast and selective separation of drug. Flow rate was o.6 ml/min, wavelength was set at 238 nm and the volume of injection was 20 μl. Mobile phase used for better separation and resolution is acetonitrile:methanol:water at the ratio of 40:15:45 v/v/v pH 3.2 was adjusted by using ortho-phosphoric acid. The retention time for metformine hydrochloride and amlodipine besylate was found to be 3.61 and 7.25 min respectively....
One simple, sensitive and accurate spectrophotometric method for the determination of sildenafil citrate has been developed and validated. This method was based on oxidation of sildenafil citrate with excess amount of ceric ammonium sulfate in presence of an acidic medium and unreacted ceric ammonium sulfate reacts with malachite green to produce yellowish green colour. The final solution was made to produce 100 µg/ml with distilled water. The λmax was found to be at 455 nm. The linearity was found in concentration range of 5-30 μg/ml. The correlation coefficient was found to be 0.9996. The regression equation was found as Y = 0.0274x.0.0011. The method was validated as per USP and ICH guidelines....
The main aim and focus of present study was to develop RP-HPLC method and validation in stability indicating manner as per ICH guidelines for the quantification of ibuprofen in pharmaceutical formulations. Ibuprofen is commonly used as non steroidal anti inflammatory drug (NSAID) to achieve higher pharmacological activity. The optimized chromatographic conditions includes a C-18 RP-HPLC column as stationary phase and the mobile phase pumped with the flow rate of 1.0 ml/min and the eluent was monitored at 220 nm were established. The mobile phase contains a combination of buffer and acetonitrile in the ratio of 40:60% (v/v). The developed method is a simple, rapid, precise, specific and accurate for the determination of ibuprofen in the range of 20% to 200% of working concentrations....
Water is the most widely used substance, raw material or starting material in the production, processing and formulation of pharmaceutical products. These include contaminants that may represent hazards in themselves or that may be able to react with intended product substances, resulting in hazards to health. Different grades of water quality are required depending on the route of administration of the pharmaceutical products. Control of the quality of water throughout the production, storage and distribution processes, including microbiological and chemical quality, is a major concern. Therefore validation of pharmaceutical water system is a major pre-requisite for any organization as validation ensures the continuous performance of the same. The research work was performed to validate the Water System. The parameters recorded for the validation were based on phase-1, phase-2 and phase-3 studies and inculcated pH, ammonia, heavy metals, chlorides, sulphates, nitrates, oxidisable substances, residue on evaporation and pathogen content etc. The results were found to be within the standard specification range....
Two simple, sensitive and accurate spectrophotometric methods for the determination of furosemide have been developed. The methods are based on diazotization reaction of furosemide with sodium nitrite for a specific time and later this diazotized product was coupled with aniline through heating which gives red coloured azo dye - method A, while in method B, colorimetric method was based on oxidation-reduction reaction. In this method ceric ammonium sulphate was made to react with furosemide in excess amount, in presence of sulphuric acid. The λmax was found to be at 490 nm and 454 nm and the linearity was found in concentration range of 10-50 μg/ml and 5-25 μg/ml respectively for method A and method B. The correlation coefficient was found to be 0.9991 and 0.9989 respectively for method A and method B. The methods were validated as per USP and ICH guidelines....
Two simple, sensitive and accurate spectrophotometric methods for the determination of glibenclamide have been developed. The methods are based on diazotization reaction of glibenclamide with sodium nitrite for a specific time and later this diazotized product was coupled with aniline through heating which gives red coloured azo dye - method A, while in method B - colorimetric method was based on oxidation-reduction reaction. In this method ceric ammonium sulphate was made to react with glibenclamide in excess amount, in presence of sulphuric acid. The λmax was found to be at 485 nm and 570 nm and the linearity was found in concentration range of 10-50 μg/ml and 5-25 μg/ml respectively for method A and method B. The correlation coefficient was found to be 0.9986 and 0.9993 respectively for method A and method B. The methods were validated as per USP and ICH guidelines....
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