Current Issue : July - September Volume : 2016 Issue Number : 3 Articles : 11 Articles
A new RP-HPLC method was developed for the quantitative determination of acamprosate calcium in human plasma as per US-FDA guidelines. The drug was spiked in the plasma and extracted with the acetonitrile by the precipitation method. The extracted analyte was injected in to a Symmetry C18 (4.6 x 150 mm, 5 µm, Make: Primesil), maintained at 25°C and the effluent was monitored at 215 nm. The mobile phase consisted of acetonitrile:potassium dihydrogen phosphate pH 3.0 (80:20 V/V). The flow rate was maintained at 1.0 ml min-1. The calibration curve for acamprosate calcium was linear from 0.5 to 2.5 µg ml-1 (r2 0.997) and the retention time was 2.2 min. The inter-day and intra-day precision was found to be within the limits. The LOD and LOQ were found to be 0.049 and 0.15 µg ml-1 respectively. The average % recovery was 98.9-101.6 % and the reproducibility was found to be satisfactory and within acceptable range. The proposed method has an adequate sensitivity, reproducibility and specificity for determination of acamprosate acalcium in bulk and pharmaceutical individual dosage forms in human plasma and the method can be applied to monitor plasma concentration of acamprosate calcium in pharmacokinetic studies....
The simple, accurate and precise simultaneous equation method has been developed for the simultaneous estimation of cefuroxime axetil and linezolid in combined tablet dosage form. The method utilizes methanol as solvent and λmax of cefuroxime axetil and linezolid selected for analysis were found to be 281 nm and 250 nm respectively. The method was validated as per international conference on harmonization (ICH) guidelines. The linearity range lies between 2-10 μg/ml (R2 0.9996) for cefuroxime axetil and 2.4-12 μg/ml (R2 0.9998) for linezolid. The accuracy and precision were determined and found to comply with ICH guidelines. The method showed good reproducibility and recovery with % RSD in desired range. The proposed method can be applied for routine analysis of both drugs....
This study was aimed to develop and validate the difference and visible spectrophotometric methods for the quantitative estimation of esomeprazole in pure form and formulations. In difference spectrophotometric method 0.1N HCl and 0.1N NaOH were used as solvents to induce the spectral changes in order to measure the difference in the absorbance. The difference absorbance maximum was observed at 307 nm. Beer-Lambert’s law was obeyed at a concentration range of 5-25 μg/ml with a limit of detection and limit of quantification of 0.872 μg/ml and 2.64 μg/ml respectively. The coefficient of correlation (r2) was found to be 0.998. A visible spectrophotometric method was developed by using 0.05% w/v bromocresol green solution as chromogenic agent. Linearity was found at a concentration range of 5-25 μg/ml at max of 691 nm. The coefficient of correlation (r2) was observed as 0.997. The developed methods were validated as per ICH Q2 (R1) guidelines and all the results obtained were in accordance with those of the official limits. The proposed methods were successfully applied for the analysis of esomeprazole tablets (NEXPRO-40 mg) and the assay values were 100.62% and 99.89% respectively. The difference spectrophotometric method found to be more sensitive than visible spectrophotometric method. Both the methods can be applied for routine quality control analysis of esomeprazole....
A simple, precise, accurate, reproducible and robust HPLC method was developed for the estimation of curcumin whole extract. The method was validated as per ICH guidelines. Analysis of the drug was performed on Phenomenex C18 (250 mm x 4.6 mm, 5 μ) column using 0.1 % citric acid: acetonitrile in a gradient elution system (0.01 – 8.00 min = 2.0 ml/min, 8.00 – 18.00 min = 0.6 ml/min, 18.00 – 45.00 min = 2.0 ml/min). Curcuminoids were detected at 420 nm and turmerone was detected at 257 nm. Retention times for the components were observed as Bis-Demethoxy curcumin: 13.29 min, Desmethoxy curcumin: 14.19 min, Curcumin: 14.99 min and Ar-Turmerone: 24.67 min. Linearity was obtained in the range of 10-50 μg/ml. The % recovery was observed to be 99.72 – 100.30% for Bis-D-curcumin, 100.42 – 101.20% for D-curcumin, 98.85 – 100.57% for Curcumin and 99.04 – 100.19% for Ar-turmerone respectively. The statistical parameters were found within range....
A simple, selective and accurate RP-HPLC method has been developed and validated for the simultaneous estimation of salbutamol sulphate, ambroxol HCl and dextromethorphan HBr in their combined pharmaceutical dosage form. The chromatographic separation was performed on zorbax eclipse plus C18 (100 × 4.6 mm, i.d: 3.5 µm) column. Mobile phase comprised of a mixture of 0.025M phosphate buffer pH 6.4, acetonitrile and triethylamine (70:30:01, v/v/v) at a flow rate 0.8 ml/min. The detection wavelength was set at 224 nm. The calibration curve was linear over the range of 1-5 μg/ml, 5-25 μg/ml, 2-10 μg/ml for salbutamol sulphate, ambroxol HCl and dextromethorphan HBr respectively. The proposed method was validated as per ICH guideline Q2R1 and successfully applied for the estimation of three drugs in combined marketed formulation....
A simple, accurate, sensitive, precise and economical spectroscopic method has been developed and validated for the determination of asenapine maleate in bulk and tablet dosage formulation. The solvent used was double distilled water and methanol (for solubility purpose) to determine the asenapine maleate in bulk and tablet dosage formulation. The wavelength corresponding to maximum absorbance of the asenapine maleate was found at 268.60. The method obeys Beer’s law in the concentration range of 40-200 µg/ml and exhibited good correlation coefficient (R2=0.9994) and the regression of the curve was found y=0.0041x-0.0052 with excellent mean recovery (100.7-103.5 %). The limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.054 µg/ml and 0.163 µg/ml respectively. The method was validated for several parameters like accuracy, precision as per ICH guidelines. The values of relative standard deviation and percentage recovery were found to be satisfactory; indicating that the proposed method is precise, accurate and economical hence can be used for the routine analysis....
Easy, sensitive and consistent uv-spectroscopic method has been developed for simultaneous estimation and validation of the resveratrol and quercetin in topical gel formulation. The in-house RES-QUE hydrogel was formulated by using carbopol as gelling agent. Resveratrol and quercetin has absorption maxima of 306 nm and 376 nm respectively. The developed method shows linearity range of 1-6 μg/ml for resveratrol and 3-8 μg/ml for quercetin. The correlation coefficient was 0.9992 for resveratrol and 0.998 for quercetin. LOD and LOQ were found to be 0.183 and 0.555 for resveratrol and 0.323 and 0.979 for quercetin. The % recovery was found to be 99% -101% for both resveratrol and quercetin indicating proposed method is accurate and precise for simultaneous estimation of resveratrol and quercetin in gel....
Standardization is an important aspect to ensure quality and composition of herbal formulations which also confirm optimum levels of active principles, along with traditional approaches there are various analytical techniques also available for the standardization of herbal products like HPLC, HPTLC and UV-Visible Spectroscopy etc. As per herbal analysis concern HPTLC has recently emerged as an important analytical technique for fingerprints and quantification of marker compounds. The present study involves development of fingerprinting HPTLC methods for the quantification of an ayurvedic formulation takrarishta using piperine as standard. The HPTLC method was found to be simple, precise and accurate for the routine laboratory analysis of ayurvedic formulation takrarishta. Analysis represents separated spot of piperine over HPTLC plate and densitometry chromatogram of piperine represented in Figure 2. The results showed linearity and correlation coefficient within the range of concentration (2 μg/ml-10 μg/ml). From the results it can be observed that the piperine can be easily detected as marker compound in formulation....
A reverse phase liquid chromatography (LC) method was developed and validated for simultaneous estimation of cefuroxime axetil and linezolid in pharmaceutical dosage form. The isocratic LC analysis was performed on phenomenex gemini ODS C18 column (200 mm x 4.6 mm, 5μ) using mobile phase composed of buffer pH 4.5:acetonitrile (55:45, v/v) at a flow rate of 1.0 ml/min. Quantitation was performed using UV detector at 225 nm. The retention times were found to be 4.17 min for cefuroxime axetil and 6.87 min for linezolid. The analytical method was validated according to ICH guidelines. The linearity was observed in the range of 15-45 and 12.5-37.5 μg/ml with correlation coefficient, r2=0.997 and 0.995 for cefuroxime axetil and linezolid respectively. The accuracy (%recovery) was found to be 99.88-101.81% for cefuroxime axetil and 99.79-101.89% for linezolid. 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 98.99±0.491 and 98.636±1.379 for cefuroxime axetil and linezolid respectively. The present method is precise and accurate and can be used for the routine estimation cefuroxime axetil and linezolid in pharmaceutical dosage form....
A simple, efficient, precise and accurate spectroscopic method has been developed and validated for quantitative estimation of embelin in bulk and churna formulation. Embelin standard solution was scanned in the UV range (400-200 nm) in a 1 cm quartz cell in a double beam UV spectrophotometer. The max of embelin was 303 nm. The method obeys beers law in the concentration range from 5-17.5 μg/ml. The correlation coefficient was found to be 0.999 and regression of the curve was found y = 0.036x - 0.056 with excellent recovery 99-101%. Limit of detection and limit of quantitation were found to be 2.65 μg/ml and 4.03 μg/ml respectively. The method was validated for several parameters like accuracy, precision as per ICH guidelines. Value of % RSD and % recovery was found satisfactory, hence the proposed method is precise, accurate and economical hence can be used for routine analysis....
In the present work two simple, precise, rapid and accurate UV spectrophotometric methods has been developed for the estimation of warfarin sodium clathrate from tablet dosage form. First method A was area under curve method in which areain the range of 300.00 - 320.00 nm was selected for the analysis. Second method B was first order derivative spectrophotometric methodin which absorbanceat λmin = 282.6 nm, λmax = 328.8 nm and zero cross = 310.41 nm was measured. The standard and sample solutions of warfarin sodium clathrate were prepared in methanol. The accuracy and precision of the methods were determined and validated statically. Both the methods showed good recovery and reproducibility with % RSD less than 2. The methods were found to be rapid, specific, precise and accurate andhence can be employed for routine analysis of warfarin sodium clathrate in bulk and its pharmaceutical dosage form....
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