Current Issue : April - June Volume : 2013 Issue Number : 2 Articles : 12 Articles
Analysis of beta blockers in formulated and unformulated samples demand a highly specific and rapid method as many beta blockers have serious stability problems. HPLC techniques can provide a valuable tool for generating highly pure preparations for characterizing and identification of the beta blockers and its combined dosage form. In the present review article, column and mobile phase conditions for the various Beta Blockers viz. Atenolol, Bisoprolol, Carvedilol, Metoprolol, Nebivolol, Propranolol, etc. have been presented. A brief discussion on chemical structure, spectrum of activity and action mechanism of each beta blocker has also been given....
The current study aimed to develop a simple, accurate, precise and rapid RP- HPLC method and subsequent validation as per ICH guidelines for the determination of tapentadol hydrochloride in pure form and synthetic mixture. The method was performed using HPLC system with a sunfire TM C18 5 µm column (4.6 mm i.d.× 150 mm) at ambient temperature. The optimum mobile phase consisted of acetonitrile: distilled water (85:15 v/v) containing triethylamine 10-5 %V/V and glacial acetic acid 3x10-4% V/V. The pH of the mobile phase was adjusted to pH 3.5. The mobile phase was delivered isocratically at a flow rate of 1.0 mL/min with UV detection at 271 nm. Tapentadol hydrochloride was eluted at 2.1 min. The calibration plots constructed using the optimized chromatographic conditions displayed good linear relationship in the concentration range of (1-45) μg/mL with r=0.9998; the % recovery of the drug was found to be 100.96±0.6 %; the LOD was (0.22) µg/mL; the LOQ was (0.66) µg/ml. The recovery of tapentadol from the bulk drug & synthetic mixture was 100.96 & 100.3 % respectively. The method has been successfully applied for analysis of bulk drug & synthetic mixture and is suitable for the routine quality control analysis....
Two simple, rapid, precise and accurate spectrophotometric methods have been developed for simultaneous analysis of Cinitapride Hydrogen Tartrate (CNT) and Rabeprazole Sodium (RAB) in their combined dosage form. Method A, Ratio derivative spectrophotometry, involves division of spectra of Cinitapride Hydrogen Tartrate by one selected standard spectrum of Rabeprazole sodium and then measuring absorbance at 277.70 nm in ratio derivative spectra for estimation of Cinitapride Hydrogen Tartrate. Similarly, spectra of Rabeprazole Sodium are divided by one selected standard spectrum of Cinitapride Hydrogen Tartrate and then measuring absorbance at 281.40 nm in ratio derivative spectra for estimation of Rabeprazole Sodium. Method B, 1st Derivative Q-method, It involves formation of Q-absorbance equation at 289.80 nm (isoabsorptive point) and 255.80 nm (λ max of Cinitapride Hydrogen Tartrate) in 1st derivative spectra. Developed methods were validated according to ICH guidelines. The calibration graph follows Beer’s law in the range of 4.0 to 20.0 μg/ml for Cinitapride Hydrogen Tartrate and 4.0 to 20.0 μg/ml for Rabeprazole Sodium in Distilled water as a solvent with R square value greater than 0.999. Accuracy of all methods was determined by recovery studies and showed % recovery between 98 to 102 %. Intraday and inter day precision was checked for all methods and mean %RSD was found to be less than 2 for all the methods. The methods were successfully applied for estimation of Cinitapride Hydrogen Tartrate and Rabeprazole Sodium in marketed formulation....
A simple, precise, accurate and rapid high performance thin layer chromatographic method has been developed and validated for the simultaneous estimation of Risedronate Sodium Hemi-pentahydrate (RSHPH). The stationary phase used was precoated silica gel 60F (254). The mobile phase used was a mixture of Water: Methanol: 25 % Ammonia (100:15:15) v/v/v). The detection of spots was carried out at 266 nm. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 3 to 6 µg/spot for RSHPH. The limit of detection and the limit of quantification for the RSHPH were found to be 0.6945 and 2.1046 respectively. The proposed method can be successfully used to determine the drug content of marketed formulation....
A sensitive, selective, precise and stability indicating high performance thin layer chromatographic method of analysis of valacyclovir hydrochloride in bulk drug and in formulations was developed and validated in pharmaceutical dosage form. The method employed TLC aluminium plates precoated with silica gel 60F-254 as stationary phase. The solvent system consisted of toluene: methanol: diethylamine (8:1:1 v/v/v). This system was found to give compact spots for Valacyclovir hydrochloride (retention factor value of 0.39). Densitometric analysis of valacyclovir hydrochloride was carried out in the absorbance mode at 252 nm. The linear regression data for the calibration plots showed good linear relationship with r2=/0.997/in the concentration range of 100-500 ng/band. The method was validated for precision, accuracy, robustness and specificity. The limits of detection and limits of quantitation were 33.3 ng/spot and 100 ng/spot respectively. The drug undergoes acidic, alkaline, neutral, oxidation, dry heat and photo degradation treatment. Statistical analysis proved the method is an economic, reproducible, accurate and selective for estimation of valacyclovir hydrochloride. Because the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method....
A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the determination of Piracetam, using C18 column and a mobile phase composed of Phosphate Buffer: Acetonitrile (95:5, v/v), pH 7.0. The retention time of Piracetam was found to be 7.8 min. Linearity was established for Piracetam in the range of 100-200 μg/ml. The percentage recovery of Piracetam was found to be in the range of 98.02-98.70%. The drug was subjected to acid, alkali, oxidation, dry heat and UV degradation. The degradation studies indicated Piracetam showed degradation in base. The degradation product of Piracetam in basic condition was well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for quantitative analysis of Piracetam in bulk drug and formulation....
The present research work discusses the development of a simple, accurate and cost effective UV spectroscopic method for the estimation of aprepitant in bulk as well as capsule formulation. The optimum conditions for the analysis of the drug were established. The maximum wavelength (λmax) was found to be 264 nm. The validation was performed as per ICH guidelines for linearity, accuracy, precision, LOD and LOQ. The method shows high sensitivity with linearity in the range of 10‐120 µg/ml. The calibration curve shows a linear relationship between the absorbance and concentration with coefficient of correlation 0.999053. The regression of curve was y = 0.00441x + 0.00333. The precision of method was found to be good. The percentage recovery was found to be 100% ± SD. The optimized method showed good reproducibility and recovery. The standard error in case of recovery studies are satisfactorily low and allow estimation of aprepitant in concentration range employed in the assay of bulk drugs and capsules. The sample solution was observed to be stable upto 48 hours. It is thus concluded that the proposed method is new, simple, cost‐effective, safe, accurate, environmental friendly and can be used as quality control method for bulk as well as pharmaceutical formulations....
Simple spectrophotometric method has been developed for estimation of benzoate salt as preservatives in food. In this method systematic extraction of the benzoate salt from different food products is employed and the concentration of benzoate salt is determined by standard addition method using methanol as a solvent. The wavelength which is λmax 226 nm was selected for estimation of benzoic acid, unionized form of all benzoates salts. The systems obey Beer’s law in the range of 1.5-40 mcg/ml with correlation coefficient of 0.998. Inter-day, intra-day precision and accuracy studies were done as per ICH guidelines. No interference was observed from other food product components....
Quality is the most important attribute of any pharmaceutical product. The source of pharmaceutical products varies greatly, from plants/ marine sources (natural resources), synthetic methods or recombinant DNA methods or a combination of any of these. This necessitates regulatory aspects as defining the standards for a quality product belonging to each of these categories would be a difficult task. Impurity profiling is the common name of a group of analytical activities, the aim of which is the detection, identification/structure elucidation and quantitative determination of organic and inorganic impurities, as well as residual solvents in bulk drugs and pharmaceutical formulations. Impurity profiling is very important during the synthesis of drug substances and manufacture of dosage forms, as it can provide crucial data regarding the toxicity, safety, various limits of detection, and limits of quantitation, of several organic and inorganic impurities, usually accompany with bulk drugs and finished products....
A simple and sensitive spectrophotometric method has been developed for simultaneous determination of Betaxolol Hydrochloride and Chlorthalidone in a binary mixture. In the proposed method, the absorbance was measured at 282.0 nm and 250.0 nm corresponding to the absorbance maxima of Betaxolol and Chlorthalidone in methanol, respectively. Linearity range was observed in the concentration range of 4-14 μg/ml for Betaxolol HCl and 10-60 μg/ml for Chlorthalidone. Concentration of each drug was obtained by using the absorptivity values calculated for both drugs at two wavelengths, 282.0 nm and 250.0 nm and solving the simultaneous equation. Developed method was applied to laboratory mixture. The method was validated statistically and recovery study was performed to confirm the accuracy of the method. The method was found to be rapid, simple, accurate and precise....
A simple, rapid and stability indicating RP-UPLC method was developed for the Simultaneous quantitative determination of chlorthalidone, Amlodipine besylate and Telmisartan HCl from their innovative combined tablet Formulation. The separation was acheived by using 100 mm x 2.1 mm, 1.7 µm RP-Sheild C-18 column with a simple gradient method at 235 nm wavelength. The mobile phase A containes a mixture of ammonium formate buffer 40 mM (PH 5.5±0.05 adjusted with formic acid ) : Acotonitrile in the ratio of 80:20 and Mobile phase B containes a mixture of ammonium formate buffer 40 mM (PH 5.5±0.05 adjusted with formic acid) : acotonitrile in the ratio of 20:80. The flow rate is 0.35 mL/min and the column temperature is maintained at 40°C. The gradient prograrmme time % of B -0/10, 0.5/10, 1.0/30, 2.8/30, 3.0/10, 3.2/10. Injection volume 1.0 µl. The total runtime for the separation of the three active compounds and their degradation products is 3.2 minutes. The method was statistically validated for precision, Linearity, Ruggedness, Robustness & Specificity. Method was showed a linear response in the concentration range of 50-150 % of three components with respect to test concentration. Quantitative and recovery studies of dosage form were also carried out and analysed, the % RSD from recovery studies was found to be less than 1. Due to simple, rapid and accuracy of the method, will be useful for routine quality control analysis....
A simple precise reliable and sensitive isocratic stability indicating RP-UPLC assay method of Linezolid in tablets and for determination of content uniformity has been developed and validated for reducing analysis time and maintaining good efficiency, An isocratic separation of Linezolid was achieved on Waters Acquity BEH C18, 50 × 2.1 mm id, 1.7 μm particle size column with a flow rate of 0.25 ml/min and using photodiode array detector to monitor the elute at 245nm. Mobile phase consisting of methanol: water (50:50 v/v) to achieve good resolution and retention. The detector linearity was established by concentrations range of 1.5-80μg/ml (r2=0.999) with a limit of detection and quantification of 0.4 and 1.5 μg/ml respectively. Recovery of drug was achieved between 99 to 101%. The method was subjected to oxidation, hydrolysis, photolysis and thermal degradation. Stress studies did not interface with the detection of Linezolid and the assay in thus stability-indicating....
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