Current Issue : July - September Volume : 2014 Issue Number : 3 Articles : 11 Articles
A simple and sensitive RP-HPLC method for the determination of dabigatran etexilate mesylate in pharmaceutical dosage formulation and in bulk has been developed and validated along with its stress degradation studies as recommended by ICH stress conditions. Degradation of dabigatran etexilate mesylate was observed almost in all stress conditions (hydrolytic, oxidative and thermal). A validated stability-indicating RP-HPLC method was developed for the determination of dabigatran etexilate mesylate in presence of its degradation products. The best separation was achieved using kromasil C18 (250 X 4.6 mm, 5 µm particle size) analytical column at temperature 28°C using a mobile phase composed of HPLC grade methanol and 100 mM ammonium acetate buffer (pH 7.4) (85 : 15% v/v) in low pressure gradient mode. The flow rate was set at 1 ml/min and UV detection wavelength was 226 nm. The method was validated with respect to linearity, sensitivity, accuracy, precision, robustness and solution stability. The method was specific and it was observed that there was no interference with excipients. The validation results obtained from the analysis also reveals that the developed method is specific and selective. The retention time of dabigatran etexilate mesylate was found to be 4.95±0.2 min. The linearity was established over the concentration range of 2-10 µg/ml with correlation coefficients 0.999. The method can be successfully employed for the determination of dabigatran etexilate mesylate in pharmaceutical dosage formulation and in bulk....
A simple, efficient, precise and accurate method have been developed for the estimation of carvedilol and lisinopril in synthetic binary mixture. In this 1st order derivative spectroscopic method UV spectrum of carvedilol and lisinopril have λmax at 283.71 and 205.8 and their ZCP are at 222.83 and 286.8 nm respectively. Methanol is used as a solvent. Both the drugs obeyed beer's law in the concentration range 5–25 μg/ml and 5–25 μg/ml for carvedilol and lisinopril respectively. The accuracy of the method was determined by recovery studies and was found to be 99.53±0.31% and 99.15±0.47% for carvedilol and lisinopril respectively. The method was validated as per ICH guidelines and statically. The method showed good reproducibility and recovery with % RSD less than 2. The method was found to be simple, economic, accurate and reproducible and can be used for routine analysis of Carvedilol and Lisinopril in pure and in fixed dose combination....
A reverse phase liquid chromatography (LC) method was developed and validated for simultaneous estimation of closantel and ivermectin in injection dosage form. The isocratic LC analysis was performed on phenomenex gemini ODS C18 column (200 mm x 4.6 mm, 5 μ) using mobile phase composed of acetonitrile : water pH 3 adjusted by orthophosphoric acid (80:20, v/v) at a flow rate of 1.0 ml/min. Quantitation was performed using UV detector at 240 nm. The retention times were found to be 3.56±0.004 min for closantel and 5.46±0.007 min for ivermectin. The analytical method was validated according to ICH guidelines. The linearity was observed in the range of 25-125 and 1-5 μg/ml with correlation coefficient, r2 = 0.999 and 0.999 for closantel and ivermectin respectively. The accuracy (%recovery) was found to be 99.27 - 100.13 % for closantel and 99.00–100.18 % for ivermectin. The relative standard deviation values for repeatability and intermediate precision studies were less than 2%. The method was successfully applied for market sample analysis and mean percentage assay values were 99.97±0.87 and 99.09±0.22 for closantel and ivermectin respectively. The present method is precise and accurate and can be used for the routine estimation of closantel and ivermectin in injection dosage form....
A simple isocratic RP-HPLC method was developed and validated for the determination of pirfenidone in bulk drug. The method was developed using C18 column with 0.5% triethylamine as aqueous phase (pH adjusted to 4.5 with orthophoshoric acid) and organic phase as acetonitrile: methanol (90:10) as mobile phase (55:45). The flow rate was maintained at 1 ml/min and detected at a wavelength of 315 nm using PDA detector. Pirfenidone was completely resolved and the retention time of pirfenidone was found to be 3.3 min. Regression analysis of the calibration data for pirfenidone showed that the dependent variable (peak area) and the independent variable (concentration) were represented by the equation Y=29654x + (-8619.9). The correlation of coefficient (R2) obtained for pirfenidone was 0.9998. Thus a good linear relationship was observed in the concentration range of 10 to 50 µg/ml of pirfenidone. The good percentage recovery clearly confirmed the reproducibility and accuracy of the developed method. The %RSD value for precision was also within the acceptable limit. The robustness studies were performed by changing the pH, wavelength and flow rate by chemometric method. The robustness factors were evaluated with the aid of full factorial design and the optimum chromatographic conditions were established by central composite design (CCD). Satisfactory data was obtained for all the method validation parameters tested. Stress degradation studies performed for pirfenidone by acid and base hydrolysis, oxidative degradation, dry heat degradation and photolysis, complied the ICH guidelines. The results of the study showed that the developed RP-HPLC method was found to be simple, rapid, precise, accurate, robust and stability indicating which can be used for routine analysis of pirfenidone....
A simple, sensitive, linear, precise and accurate RP-HPLC method for the simultaneous estimation of olmesartan medomoxil and cilindipine in bulk and tablet formulation was developed and validated. The chromatographic separation of the two drugs was achieved on eclipse XBD, C18 column (150 mm 4.6 mm i.d; particle size-5 micron) in a gradient mode. The mobile phase consisting of 0.01 M KH2PO4 buffer whose pH was adjusted to 3.0 using dilute ortho phosphoric acid (solvent A): acetonitrile (solvent B) was set with gradient programming for 15 min and was delivered at a flow rate of 1 ml/ min and effluents were monitored at 240 nm. The retention time of olmesartan medomoxil and cilindipine was found to be 5.32 and 7.16 min, respectively. Calibration curves were linear with a correlation coefficient of 0.9999 for both the drugs over the concentration range of 600-1800 µg/ml for OLM and 300-900 µg/ml for CIL and precise with (%RSD<2). The method was validated as per the ICH guidelines and can be employed for routine quality control analysis....
A stability indicating RP-UFLC method was developed and validated for the determination of alogliptin in tablet dosage form using Waters XSelectTM HSS PFP (150 X 4.6 mm, 2.5 µm particle size) analytical column with mobile phase consisting of acetonitrile-0.1%TEA in milli q water pH adjusted to 7.5, 60:40 v/v, at a flow rate of 1 ml / min with PDA detector at 276 nm. Linearity was observed over the concentration range 10.0-120.0 μg/ml and exhibited good correlation coefficient (r2 = 0.999) and excellent mean recovery (98.4-101.34%). The limit of detection and limit of quantification was found to be 0.0468 and 0.1418 respectively, which proved the adequate sensitivity of the method. Alogliptin was subjected to stress conditions including acidic, alkaline, oxidation and thermal degradation. The method was validated statistically as per ICH Q2 R1 guideline and the results were found to be satisfactory. The obtained results proved that the method can be employed for the routine analysis of alogliptin in bulk as well as in commercial formulation....
A simple, sensitive HPTLC method has been developed and validated for the quantitative estimation of andrographolide in callus extracts of Andrographis paniculata. The stationary phase used was precoated silica gel 60F 254 plate. The mobile phase used was a mixture of chloroform: toluene: methanol (6:2.5:1.5 v/v/v). The detection of spots was carried out densitometrically using a UV detector at 310 nm in absorbance mode. Andrographolide showed mean Rf value of 0.59 with λmax at 231 nm. The method was validated in terms of linearity (100 – 700 ng), precision and accuracy (99.52% recovery). Limit of detection and limit of quantification were found to be 30 ng and 100 ng respectively. The calibration curve was found to be linear between 100 to 700 ng/spot for andrographolide. The validated method was applied for quantification of andrographolide in methanolic extracts of Andrographis paniculata samples obtained from various callus tissues. The proposed method is simple, sensitive and precise; it can be used for routine analysis....
A simple, sensitive, specific and accurate spectrofluorometric method was developed for the simultaneous determination of ebastine and phenylephrine hydrochloride using direct and indirect method. In which phenylephrine hydrochloride gives inherent fluorescence in 0.1 M HCl which was measured at 304.0 nm after excitation at 275.0 nm (direct method) and ebastine is converted to its fluorescence derivative. This involves condensation of the drug with mixed anhydrides (citric and acetic anhydrides) producing a product with intense fluorescence, which was measured at 477 nm after excitation at 376 nm (Indirect method). Linearity was established for ebastine and phenylephrine hydrochloride in the range of 0.2-1.0 μg/ml. The precision of the methods were satisfactory; the values of relative standard deviation did not exceed 2%. This method can be successfully employed for simultaneous quantitative analysis of ebastine and phenylephrine hydrochloride and in bulk drugs and formulations....
Ayurveda is a traditional Indian medicinal system being serving the public health by using plants and plant products in various ayurvedic formulations. Arishtas are weakly alcoholic ayurvedic formulations prepared by fermenting the decoction of medicinal plants in an air tight sealed vessels. Fermentation of decoction of medicinal plants is brought about by addition of a source of sugar with flowers of Woodfordia fruticosa. The presence of woodfordia flowers is essential to initiate the fermentation process. The present study was designed with the objective to understand the impact of fermentation on the chemical profile of Woodfordia fruticosa by RP-HPLC studies. The decoction of woodfordia flowers was prepared and some quantity of decoction was kept for fermentation in a closed vessel for 45 days. RP-HPLC analysis of pre-fermented and post-fermented decoction was done after filtration and their comparison was made. It was observed that the chromatogram of post fermented W. fruticosa showed comparatively very few peaks as compared to the chromatogram of pre fermented W. fruticosa. This is probably due to the fact that the large molecular weight polyphenolics particularly ellagitannin are hydrolyzed during fermentation and degraded into small molecules of phenolics or phenolic acids. It means there is a quantitative decrease in the concentration of ellagitannin and quantitative increase in concentration of small molecular weight phenolics, ellagic acid and its derivatives during fermentation of W. fruticosa. This change will modify significantly the biological activity of the fermented extracts and the final ayurvedic formulation, particulary fermented biomedicine like arishtas. By controlling each step of the fermentation process, particularly the incubation time, it should be possible to predict the final content and composition of formulation, but also to prevent the degradation of pharmacolgically important phytoconstituents, thus maintaining the therapeutic potential of the final product....
Cleaning validation is a process of providing documented evidence that the cleaning methods employed within a facility consistently controls carryover of product. The aim of the present study was to validate simple analytical method for verification of residual terazosinin equipment’s used in the production area and to confirm effectiveness of cleaning procedure. UV spectrophotometric method was developed and the detection was made at 245 nm. A cleaning verification assay was validated by using rinsing sampling technique. Recovery studies were carried out on stainless steel surface. The calibration curve was linear over a concentration range from 2 to 10 µg/ml with a correlation coefficient of 0.9992. Detection limit and quantitation limit was detected by UV visible spectroscopy as 0.01547 µg/ml and 0.0469 µg/ml. The developed UV spectroscopic method can be used successfully for routine analysis of terazosin residues on cleaned surface in production area....
A simple, precise, accurate, reproducible and economical stability-indicating reverse phase liquid chromatography method is developed and validated for the quantitative simultaneous estimation of flucloxacillin (fluc) and ampicillin (amp) in combined pharmaceutical dosage form. A chromatographic separation of the two drugs was achieved with a thermosil C18 (4.6 x 250 mm, 5 m) analytical column using buffer – sodium phosphate buffer pH (4.5): methanol (60:40% v/v) in isocratic mode at a flow rate of 1.2 ml/min and column at ambient temperature. The detection was monitored at 238 nm using a PDA detector. The stressed samples were analyzed and this proposed method was found to be specific and stability indicating as no interfering peaks of degradation compounds and excipients were noticed. The described method shows excellent linearity over a range of 10-50 μg/ml for both the drugs. The correlation coefficient for both drugs was 0.9999. The mean recovery values for fluc and amp were 100.22 and 100.83 respectively. The limit of detection for fluc and amp were 0.012 and 0.006 μg/ml respectively. The limit of quantification was 0.042 and 0.020 μg/ml, respectively. The robustness study and percentage of assay of the formulation were found within limit as per ICH guidelines....
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