Current Issue : April-June Volume : 2014 Issue Number : 2 Articles : 56 Articles
A simple, specific, accurate and economical uv-spectrophotometric method has been developed for estimation of niacin from bulk and pharmaceutical formulation. The solvent used to develop the method was methanol. The λ max of niacin in methanol was found to be 260 nm. The drug follows linearity in the concentration range of 2-10 µg/ml with correlation coefficient value 0.999. The proposed method was applied to pharmaceutical formulation and % amount of drug estimated 99.99% was found in good agreement with the label claim. The accuracy of the method was checked by recovery experiment performed at three different levels i.e. 25%, 50% and 100%.The % recovery was found to be in the range 98.88%-99.99%. The low values of % R.S.D are indicative of the accuracy and reproducibility of the method. The precision of the method was studied as an intra-day, inter-day variations and repeatability. The % R.S.D value less than 2 indicate that the method is precise. The above method was a rapid and cost-effective quality-control tool for routine analysis of niacin in bulk and in pharmaceutical dosage form....
A simple, rapid, specific, accurate and precise reverse phase high performance liquid chromatographic method was developed for the estimation of methylcobalamin in bulk and solid dosage form. The determination was carried out on a C-8 (250 × 4.6 mm, 5 micron) column using mobile phase 1.0 %w/v solution of sodium dihydrogen phosphate dihydrate and acetonitrile in the ratio of 735:265 adjusts pH 3.50 with 10% ortho phosphoric acid and then added 3.76 gm/liter of sodium 1-hexane sulfonate (hexane-1-sulfonic acid sodium salt). The flow rate and runtime were 1 ml/min and 10 min, respectively. The eluent was monitored at 318 nm. The retention time of methylcobalamin was 2.88 mins. The method was reproducible, the detector response was found to be linear in the concentration range of 16 ppm to 24 ppm....
A stability indicating RP-HPLC method has been developed and validated for quantitative determination of Lamivudine, Emtricitabine, Tenofovir Disoproxil Fumarate and Efavirenz in different Pharmaceutical dosage forms. Chromatographic separation was achieved through gradient elution. Detection wavelength was monitored at 260 nm. The retention times of the Lamivudine, Emtricitabine, Tenofovir disoproxil fumarate and Efavirenz was about 3.2, 5.97, 8.15 and 12.52 min respectively. The developed method was validated as per ICH guidelines. This method is found to be simple, fast and economical. Hence this validated method can be used in routine quality testing of individual dosage forms and combination dosage forms of Lamivudine, Emtricitabine, Tenofovir disoproxil fumarate and Efavirenz....
UV spectrophotometric method has been developed for simultaneous estimation of ciprofloxacin HCl (CIPRO) and bromhexine HCl (BROM) in their combined pharmaceutical dosage form. This method utilizes methanol as a solvent and λmax of ciprofloxacin HCl and bromhexine HCl selected for analysis was found to be 279 nm and 250 nm respectively. Linearity was observed for ciprofloxacin HCl and for bromhexine HCl in the concentration range of 2-12 μg/ml and (r2 = 0.999) and 5-30 μg/ml and (r2 = 0.993). The accuracy and precision were determined and found to comply with ICH guidelines. This method showed good reproducibility and recovery with % RSD in the desired range. The proposed methods can be successfully applied for the routine analysis of both the drugs in combined pharmaceutical dosage form. This method was simple, rapid, accurate and sensitive....
In the present study the simultaneous estimation of isosorbide dinitrate and hydralazine hydrochloride in combined tablet dosage form have been developed using 0.1 N NaOH in methanol as a solvent by absorption correction method. The method is developed at 222 nm and 252 nm which is the maximum absorbance of isosorbide dinitrate and hydralazine hydrochloride respectively. Beer’s law obeyed in concentration range of 40 - 120 µg/ml and 10 - 50 µg/ml for isosorbide dinitrate and hydralazine hydrochloride respectively. The accuracy of the method was assessed by recovery studies was found to be 99.98±0.3175 and 99.88±1.020 for isosorbide dinitrate and hydralazine hydrochloride. These methods are simple, accurate and rapid; those require no preliminary separation and can therefore be used for routine analysis of both drugs in quality control laboratories....
Two simple, sensitive, accurate and precise spectrophotometric methods (method A and method B) have been developed and validated for the determination of hyoscine butylbromide. The first method involved reduction of ferric ions to ferrous ions and in turn formed coloured complex with potassium ferricyanide which showed absorption maxima at 725 nm. In the second method, hyoscine butylbromide in presence of acidic medium reacts with excess amount of chloramine-T and unreacted chloramine-T reacts with crystal violet to produce greenish-blue colour. The absorption maxima was found to be 598 nm. The linearity range was found to be in concentration range 5-25 µg/ml for both the methods. The correlation coefficient was found to be 0.9998 and 0.9996 for method A and method B respectively. The regression equation was found to be y = 0.0371x + 0.0045 and y = 0.1732x - 0.031 for method A and method B respectively. The method was validated according to ICH guidelines....
Two simple, sensitive, accurate and precise spectrophotometric methods (method A and method B) have been developed and validated for the determination of ofloxacin hydrochloride. The first method involved reduction of vanadium (V) to vanadium (IV) and development of greenish-blue colour which shows maximum absorption at 752nm. In the second method, ferric ions directly enters the active carboxylic acid and adjacent keto group in 3- and 4- position respectively and orange-red coloured complex is developed. The absorption maxima was found to be 420nm. The linearity range was found to be in concentration range 5-25�µg/ml for both the methods. The correlation coefficient was found to be 0.9994 and 0.9996 for method A and method B respectively. The regression equation was found to be y=0.056x.0021 and y= 0.0317x-0.0015 for method A and method B respectively. These methods were validated according to USP and ICH guidelines....
Candesartan is an angiotensin II Receptor antagonist, widely used in treatment of various disorders like hypertension, heart failure and myocardial infarction. Hydrochlorthiazide belongs to thiazide class of diuretics. It reduces blood volume. Since many years, varied analytical methods were developed both in dosage forms as well as biological fluids in order to estimate their desired pharmacological action. Candesartan variable oral bioavailability is due to its high lipophilic nature. Its estimation for therapeutic efficacy in biological fluids is very critical. A few UV spectrophotometric methodshave been reported to estimate candesartan in bulk formulations. Additionally, capillary electrophoresis methods provided qualitative and quantitative estimation of candesartan. Ultimately, different HPLC and LC-MS/MS methods explained the importance of the methods while estimating candesartan in various biological fluids (e.g. plasma, urine, etc.) as well as in routine drug analysis. This review providesclear and short notes on the various analytical techniquesemployed for determination of candesartan in both in vitro and in vivo conditions...
Two precise, simple, accurate, reproducible, rapid and economical UV spectrophotometric methods have been developed for simultaneous estimation of montelukast and doxofylline in tablet dosage form by using distilled water as solvent. Method I is based on formation and solving of simultaneous equation method, known as vierodt’s method. Montelukast and doxofylline show absorbance maxima at 283 nm and 274 nm respectively, so absorbance was measured at the same wavelength for the estimation of montelukast and doxofylline in tablet combination. Method II is based on principle of Q-analysis, known as absorbance ratio method. Absorbance was measured at 285 nm (isobestic point) and 274 nm (λmax of doxofylline). Montelukast and doxofylline obeys beer’s law in the concentration range of 5 to 30 µg/ml. Percentage estimation of montelukast and doxofylline in tablet dosage form by method I is 99 and 99.85 and by method II is 99 and 99.89 respectively with standard deviation ≤2. Methods are validated according to ICH guidelines and can be applied for routine analysis of drugs in tablet dosage form....
Lornoxicam is and Diclofenac sodium is analgesic, antipyretic drugs both are NSAID class. The combination of this two drug is used for the treatment of rheumatoid arthritis. Two new ,simple,accurate and precise uv spectrophotometric methods have been developed amd validated for the simultaneous determination of Lornoxicam (LOR) and Diclofenac sodium (DIC) in their combine dosage forms. The first derivative spectroscopy method (Method A) in which first derivative amplitudes were measured at selected wavelengths. The amplitudes at 251 nm and 263 nm in the first derivative spectra were selected to determine LOR and DIC, respectively. Beer’s law is obeyed in the concentration ranges of 4-24 and 3-18 μg/ml for LOR and DIC respectively in methanol for both the methods. The second method is Q-absorbance method. For Q-absorbance method the absorbances of the standard solutions were taken at two wavelengths 281.2 nm (λmax of lornoxicam) and 260.6 nm (Isobestic point), in methanol. Beer’s law is obeyed in the concentration ranges of 4-40 and 3-18 μg/ml for LOR and DIC respectively in methanol for both the methods. Both methods were validated statistically and recovery studies carry out.The suitability of this method for the quantitative determination of Lornoxicam and Diclofenac sodium was proved by validation. The proposed method was found to be simple and sensitive for the routine quality control application of Lornoxicam and Diclofenac sodium in combination. The results of analysis have been validated statistically and by recovery studies.The validation study is statistically significant as all statistical parameter are within the acceptance range (% RSD<2.0 and S.D.<2.0) for both accuracy and precision....
A simple, sensitive, accurate and rapid reverse phase HPLC method is developed for the determination of aspirin and esomeprazole in bulk and in synthetic mixture. Chromatography was carried out on C18 column (250 mm×4.6mm×5µm particle size, make: kromasil 1005) using a mixture of 0.05% tetrahydrofuran and methanol and water in the ratio (70:30 v/v) as a mobile phase at a flow rate of 1.0 ml/min. Detection was carried out at 237 nm. The retention time of the drug aspirin and esomeprazole was 1.82 and 4.90 min. The method produced linear responses in the concentration range of 20-120 µg/ml and 5-30 µg/ml of aspirin and esomeprazole respectively. The LOD values for HPLC method for aspirin and esomeprazole were found to be 1.9585 µg/ml and 0.1181 µg/ml. The LOQ values for aspirin and esomeprazole were found to be 5.9348 µg/ml and 0.3597 µg/ml respectively. The proposed method can be used for the estimation of these drugs in bulk and in synthetic mixture....
The current method describes the derivative spectrophotometry with absorbance correction method for the estimation of tramadol hydrochloride (TRM), diclofenac sodium (DIC) and chlorzoxazone (CHL) from their combined tablet dosage form by using 0.1 N NaOH as a solvent. The first derivative absorption at 243.75 nm, 265.08 nm and 272.25 nm were used for the estimation of diclofenac sodium, tramadol hydrochloride and chlorzoxazone. The method follows beer’s linearity in the range of 5-45 µg/ml for tramadol hydrochloride, 10-50 µg/ml for diclofenac sodium and 10-50 µg/ml for chlorzoxazone. The % recovery was found to be 99.33 - 99.77 % for TRM, 99.5 – 100.3% for DIC and 99.63 - 99.79 % for CHL. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of TRM, DIC and CHL from their combined Tablet dosage form....
A new simple, accurate, precise and reproducible reverse phase liquid chromatographic method developed and validated for the quantification of diosmin in pharmaceutical dosage form. Separation was achieved under optimized chromatographic condition on inertsil C18 column (250× 4.6 mm, 5 µm), the mobile phase consisting of methanol: water (60:40 v/v). An isocratic elution was achieved at a flow rate 1.0 ml/min at an ambient temperature. The detection was carried out at 255 nm. The calibration curve was linear in concentration range 5-25 μg/ml (r2 0.999) for diosmin. The recovery studies were performed and the percentage recoveries were found to be 98.36% diosmin. So, proposed method was found to be simple, accurate, specific, linear and rugged....
A simple, accurate, precise and specific spectrophotometric method has been developed for simultaneous determination of piroxicam and paracetamol in their combined tablet dosage form by using 0.1M HCl as a solvent. The method is first order derivative method in which absorption at 313.12 nm (zero cross point of paracetamol) was used for quantification of piroxicam and 259.24 nm (zero cross point of piroxicam) for quantification of paracetamol. The method follows Beer’s linearity in the range of 0.8-10 μg/ml for piroxicam and 8-32 μg/ml for paracetamol. The mean % recoveries were found to be in the range of 98.33–101.38% and 99.55–100.28% for piroxicam and paracetamol respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of piroxicam and paracetamol in their combined Tablet dosage form....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical first order derivative spectrophotometry method for the determination of chlorhexidine gluconate in mouthwash. The Absorbance value at 272 nm of first derivative spectrum was used for the estimation of chlorhexidine gluconate using methanol as a solvent. This method was found to be linear (r2 > 0.9982) in the range of 10-70 µg/ml at 272 nm. The limit of detection (LOD) was 0.0733 µg/ml. The limit of quantification (LOQ) was 0.2222 µg/ml. This method was successfully applied for the determination of chlorhexidine gluconate in mouthwash. No interference was observed from excipients present in the mouthwash. The suitability of this method for the quantitative determination of chlorhexidine gluconate was proved by validation. The proposed method was found to be simple and sensitive for the routine analysis of chlorhexidine gluconate in mouthwash. The results of analysis have been validated statistically and by recovery studies....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical first order derivative spectrophotometry method for the determination of ketoconazole in tablet dosage form. The absorbance value at 256.514 nm of first derivative spectrum was used for the estimation of ketoconazole using methanol as a solvent. This method was found to be linear (r2>0.9989) in the range of 5-35 µg/ml at 256.514 nm. The Limit of detection (LOD) was 0.047 µg/ml. The Limit of quantification (LOQ) was 0.1428 µg/ml. This method was successfully applied for the determination of ketoconazole in tablet dosage form. No interference was observed from excipients present in the tablet. The suitability of this method for the quantitative determination of was ketoconazole proved by validation. The proposed method was found to be simple and sensitive for the routine analysis of ketoconazole in tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
A new simple, sensitive, rapid, accurate, precise and economical first derivative Spectrophotometric method for the simultaneous determination of cilnidipine (CIL) and metoprolol succinate (METO) in combined pharmaceutical formulation was developed. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectrums were obtained in methanol and the determinations were made at 241.13 nm (ZCP of CIL) for quantification of METO and 275.22 nm (ZCP of METO) for quantification of CIL. The linearity was obtained in the concentration range of 2-10 μg/ml for CIL and 10-50 μg/ml for METO. The mean recovery was 99.58% – 100.83% and 98.66% – 99.66% for CIL and METO respectively. The results of analysis have been validated statistically as per ICH guidelines....
Clotrimazole (CLZ) and dexamethasone (DEX) is available as cream formulation and no any method have been reported yet. So aim of present research work is to develop a simple, sensitive and reproducible method for simultaneous estimation of both drugs by first order derivative spectrophotometric method. Methanol was used as a solvent for analysis. The method used has been tested for accuracy and precision for the estimation of both the drugs. In this method 239.00 nm, the zero crossing point of DEX was selected for determination of CLZ and 252.80 nm, the zero crossing point of CLZ was selected for determination of DEX. The regression analysis data for the calibration plot showed good linearity in the range 100-500 µg/ml (R2 = 0.9985) for CLZ and 4-20 µg/ml (R2 = 0.9987) for DEX. The LOD for CLZ and DXM were 8.66 µg/ml and 0.49 µg/ml and LOQ were found to be 26.28 µg/ml and 1.45 µg/ml respectively. These methods were applied to the assay of the drugs in marketed formulation, which were found in the range of 98% to 100% for both CLZ and DEX. Statistical analysis proves that the method is reproducible and selective for the simultaneous estimation of CLZ and DEX. The results were found to be within acceptance criteria according to ICH Q2 R1 guidelines....
A new simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of levosulpiride (LEVO) and esomeprazole magnesium trihydarte (ESO) in combined pharmaceutical formulation was developed. The spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectrums were obtained in methanol and the determinations were made at 302.58 nm (ZCP of esomeprazole) for quantification of levosulpiride and 320.17 nm (ZCP of levosulpiride) for quantification of esomeprazole. The linearity was obtained in the concentration range of 10-40 μg/ml for levosulpiride and 4-24 μg/ml for esomeprazole. The mean recovery was 100% – 101.7% and 98.33% – 99.2% for levosulpiride and esomeprazole respectively. The results of analysis have been validated statistically as per ICH guidelines....
The method for the development and validation of First order derivative spectrometric method was developed for the simultaneous estimation of Budesonide and Salbutamol sulphate in their combined dosage form was developed. For this both the drugs were determined based on the derivative spectroscopic method at their respective zero crossing point (ZCP). The first order derivative spectra were obtained in methanol and determinations were made at 243 nm (ZCP of Budesonide) for Salbutamol sulphate and at 251 nm (ZCP of Salbutamol sulphate) for Budesonide. The linearity was obtained in the concentration range of 12-28 μg/ml for Budesonide and 30-70 μg/ml for Salbutamol sulphate. The mean recovery was 99.13±0.01 for Budesonide and 99.8±0.005 for Salbutamol sulphate and LOD and LOQ values for Budesonide were 0.214 μg/ml and 0.514 μg/ml respectively and for Salbutamol sulphate were 0.564 μg/ml and 2.3 μg/ml respectively. The recovery studies confirmed accuracy of proposed methods and low values of standard deviation confirmed precision of method. Thus a simple, sensitive, rapid, accurate, precise and economical first order derivative spectrometric method has been developed for the simultaneous estimation of Budesonide and Salbutamol sulphate....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous determination of cefixime and dicloxacillin sodium in tablet dosage form. In absorbance ratio method, the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point and other being the λ-max of one of the two components. Cefixime and dicloxacillin sodium show an isoabsorptive point at 224.7 nm in methanol. The second wavelength used is 289 nm, which is the λ-max of cefixime in methanol. The linearity was obtained in the concentration range of 3-16 μg/ml for both the drugs. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λ-max of cefixime. The method was successfully applied for the determination of these two drugs in tablet dosage form. No interference was observed from excipients present in the tablet. The suitability of this method for the quantitative determination of cefixime and dicloxacillin sodium was proved by validation. The proposed method was found to be simple and sensitive for the routine analysis of these two drugs in tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous determination of chlorzoxazone and paracetamol in tablet dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one of which is an isoabsorptive point and other being the λ-max of one of the two components. Chlorzoxazone and paracetamol shows an isoabsorptive point at 269.40 nm in distilled water. The second wavelength used is 280 nm, which is the λ-max of chlorzoxazone in distilled water. The linearity was obtained in the concentration range of 5-40 μg/ml for both chlorzoxazone and paracetamol. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λ-max of chlorzoxazone. The method was successfully applied for the determination of these two drugs in tablet dosage form. No interference was observed from excipients present in the tablet. The suitability of this method for the quantitative determination of chlorzoxazone and paracetamol was proved by validation. The proposed method was found to be simple and sensitive for the routine analysis of these two drugs in tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
The present research works aims to develop a simple, sensitive, accurate and reproducible Q-absorbance ratio method for the simultaneous estimation of cilnidipine (CILN) and metoprolol succinate (METO) in their combined dosage form. Q-absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an Isobestic point at 230 nm in methanol. The second wavelength is used 240 nm, which is λmax of CILN in methanol. The regression analysis data for the calibration plot showedgood linear relationship in the concentration range of 4-8 μg/ml for CILN and 20-40 μg/ml for METO with R2 value greater than 0.998. Accuracy of this method was determined by recovery studies and showed % recovery between 99 to 103%. Intraday and interday precision was checked for all methods and mean %RSD was found to be less than 2. This method was successfully applied for estimation of cilnidipine and metoprolol succinate in marketed formulation. The results were found to be within acceptance criteria according to ICH Q2 R1 guidelines....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical ratio spectra derivative method for the simultaneous determination of paracetamol and tramadol HCl in tablet dosage form. The method is based on use of the first derivative of the ratio of spectra. The absorption spectrum of the mixture is obtained and the amplitudes at appropriate wavelengths are divided by the corresponding amplitudes in the absorption spectrum of a standard solution of one of the components and the first derivative of the ratio spectrum is obtained. The concentration of the other component is then determined from a calibration graph. The amplitude in first derivative of ratio spectra at 236.20 nm and 266.40 nm were selected to determine paracetamol and tramadol HCl, respectively in distilled water. The linearity was obtained in the concentration range of 2-14 μg/ml for paracetamol and 10-22 μg/ml for tramadol HCl. The method was successfully applied for the determination of these two drugs in tablet. No interference was observed from excipients present in the tablet dosage form. The suitability of this method for the quantitative determination of paracetamol and tramadol HCl was proved by validation. The proposed method was found to be simple and sensitive for the routine analysis of these two drugs in tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
Novel combination of flurbiprofen sodium (FLB) and gatifloxacin (GATI) is available as eye drops form in the ratio of 1:10 and no HPLC method has been reported yet. The present research work aims to develop a simple, sensitive, accurate and reproducible method for the simultaneous estimation of both drugs by the RP-HPLC method, on a C18 column (250×4.6×5 μm) of spinco tech pvt. ltd column was used with a mobile phase containing a mixture methanol: 0.05M phosphate buffer pH-4.2 (50: 50 % v/v). The flow rate was 0.8 ml/min and peaks were monitored at 254 nm and eluted at 5.34 min and 7.94 min for GATI and FLB respectively without interference of blank. The linearity range from 30-70 μg/ml and 30-700 μg/ml for FLB and GATI respectively. The linear regression analysis data for calibration plots shows good linear relationship with R2 value is 0.9999 and 0.9997 and mean % recovery is 99.79% and 99.90 % with the LOD of 0.8831 μg/ml and 2.6990 μg/ml and LOQ is 0.2735 μg/ml and 8.1807 μg/ml for FLB and GATI respectively. Precision (% RSD) is less than 2%. Statistical analysis proves that the method is reproducible and selective for the simultaneous determination of flurbiprofen sodium and gatifloxacin. The results were found to be within acceptance criteria according to ICH Q2 R1 guidelines....
Simple and reliable second order derivative spectrophotometric method was developed and validated for the simultaneous estimation of beclomethasone dipropionate and ketoconazole in combined dosage form. The quantitative determination of the drugs was carried out using the second derivative values measured at 287 nm and 265 nm for beclomethasone dipropionate and ketoconazole respectively. The solutions of standard and the sample were prepared in methanol. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of 5-35 μg/ml for both beclomethasone dipropionate and ketoconazole. The low relative standard deviation values indicate good precision and high recovery values indicate accuracy of the proposed method. Developed second derivative spectrophotometric method was simple, accurate, precise, specific, sensitive and reproducible which can be directly and easily applied to pharmaceutical dosage forms....
A simple, precise and accurate method was developed for the estimation of amlodipine besylate (AMLO) and irbesartan (IRBE) in synthetic mixture using second order derivative spectrophotometry. Wavelengths selected for quantitation were 233.2 nm for amlodipine besylate (zero crossing point of irbesartan) and 221 nm for irbesartan (zero crossing point of amlodipine besylate). The method was validated with respect to linearity, accuracy, precision, limit of detection and limit of quantitation in accordance with the international conference on harmonization (ICH) guidelines. Linearity was observed in concentration range of 8-48 μg/ml for amlodipine besylate and 2-14 μg/ml for irbesartan. The limit of detection and limit of quantitation were found to be 0.275 μg/ml and 0.883 μg/ml for amlodipine besylate and 0.126 μg/ml and 0.384 μg/ml for irbesartan. The percentage recovery of amlodipine besylate and irbrsartan was found to be 99.53% and 99.39%, respectively. The % R.S.D. values for intra-day and inter-day precision study were <2.0%, confirming that the method was precise. The method can be successfully employed for the simultaneous estimation of amlodipine besylate and irbesartan in synthetic mixture....
UV Spectrophotometric method has been developed for simultaneous estimation of amlodipine besylate (AB) and candesartan cilexetil (CC) in bulk drug and in laboratory mixture. This method utilizes methanol as a solvent and λ max of amlodipine besylate and candesartan cilexetil selected for analysis was found to be 238 nm and 255 nm respectively. Linearity was observed in the concentration range of 5-25 μg/ml and (r2 = 0.999) of both drugs. The accuracy and precision were determined and found to comply with ICH guidelines. This method showed good reproducibility and recovery with % RSD in the desired range. The proposed methods can be successfully applied for the routine analysis of both the drugs in Synthetic mixture. This method was simple, rapid, accurate and sensitive....
A simple, precise, accurate and reproducible uv-spectrophotometric method has been developed for the simultaneous estimation of bromhexine hydrochloride (BH) and phenylephrine hydrochloride (PL) in their combined pharmaceutical dosage form. This method utilizes methanol as a solvent and λmax of bromhexine hydrochloride and phenylephrine hydrochloride selected for analysis was found to be 250 nm and 275 nm respectively. Linearity was observed in the concentration range of 5-30 μg/ml for bromhexine HCl (r2 = 0.998) and 10-60 μg/ml for phenylephrine HCl (r2 = 0.999). The method was validated by statistically and by recovery study. The mean % recovery was 98.5-101.66% and 98.87-101.46% for bromhexine HCl and phenylephrine HCl respectively. Developed method was applied to marketed formulation. The results were found to be within acceptance criteria according to ICH guideline....
UV Spectrophotometric method has been developed for simultaneous estimation of olmesartan medoxomil (OM) and cilnidipine (CIL) in bulk drug and in laboratory mixture. This method utilizes methanol as a solvent and λmax of olmesartan medoxomil and cilnidipine selected for analysis was found to be 241 nm and 253 nm respectively. Linearity was observed in the olmesartan medoxomil concentration range of 4-20 μg/ml and cilnidipine concentration range 2-10 µg/ml (r2 = 0.998 and r2 = 0.999) of both drugs. The accuracy and precision were determined and found to comply with ICH guidelines. This method showed good reproducibility and recovery with % RSD in the desired range. The proposed methods can be successfully applied for the routine analysis of both the drugs. This method was simple, rapid, accurate and sensitive....
UV spectrophotometric method has been developed and validated for simultaneous estimation of tolperisone hydrochloride and aceclofenac in synthetic mixture by absorbance ratio method. Absorbance ratio method involves formation of Q-absorbance equation at 239 nm (isoabsorptive point) and also at 275 nm (λmax of aceclofenac). The different analytical parameters were determined according to ICH Q2 (R1) guideline. The method was found to be linear between the range of 3-15 µg/ml for tolperisone hydrochloride and 2-10 µg/ml for aceclofenac using methanol as solvent. The mean percentage recovery was found to be 100.255% and 99.865% for tolperisone hydrochloride and aceclofenac respectively, at three different levels of standard additions. The precision of method was found within the limits (RSD < 2%). It could be concluded from the results obtained in the present investigation for simultaneous estimation of tolperisone hydrochloride and aceclofenac in synthetic mixture are simple, rapid, accurate, precise, economical and robust....
UV spectrophotometric method has been developed for simultaneous estimation of tramadol hydrochloride (TRM) and chlorzoxazone (CHZ) in bulk drug and in pharmaceutical dosage form. This method utilizes 0.1 N NaOH as a solvent and λmax of tramadol hydrochloride and chlorzoxazone selected for analysis was found to be 271 nm and 245 nm respectively. Linearity was observed in the concentration range of 30-90 μg/ml (TRM) (r2 = 0.998) and 6-14 μg/ml (CHZ) (r2 = 0.999) of both drugs. The accuracy and precision were determined and found to comply with ICH guidelines. This method showed good reproducibility and recovery with % RSD in the desired range. The proposed methods can be successfully applied for the routine analysis of both the drugs in marketed formulation. This method was simple, rapid, accurate and sensitive....
A simple, accurate, rapid sensitive, specific and cost effective spectrophotometric method has been developed for the estimation of rebamipide (REB) in its tablet dosage form. The relative absorbance of rebamipide was measured in methanol at wave length (λmax 229 nm). The method is calibration graph method. This method follows Beer’s linearity in the range of 2-64 μg/ml. The mean % recovery was found to be in the range of 99.59–99.84 % for REB. The result demonstrates that the developed method is accurate, precise and reproducible. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of REB in its tablet dosage form....
The present work discusses the development of a spectrophotometric method for rivaroxaban. A simple, accurate, precise and specific spectrophotometric method has been developed for the estimation of rivaroxaban in its tablet dosage form by using methanol as a solvent. The method is calibration graph method which involves estimation of rivaroxaban by taking absorbance at 249 nm. This method follows beer’s linearity in the range of 0.5-30 μg/ml. The mean % recovery was found to be in the range of 100.07–101.83% for rivaroxaban. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of rivaroxaban in its tablet dosage form....
Two simple, accurate, precise and specific spectrophotometric methods have been developed for simultaneous determination of Ceftriaxone Sodium (CFS) and Tazobactam Sodium (TAZO) in its combined Pharmaceutical formulation by using NaOH as a solvent. The first method is dual-wavelength method which involves estimation of CFS by absorbance difference at 248.48 nm and 265.78 nm, and TAZO by absorbance difference at 239.41 nm and 255.83 nm. The second method is first order derivative method in which absorption at 302.8 nm (zero cross point of TAZO) was used for quantification of CFS and 247.8 nm (zero cross point of CFS) for quantification of TAZO. Two methods follow Beer’s linearity in the range of 5-50μg/ml for CFS and 2.5-15 μg/ml for TAZO. The mean % recoveries were found to be in the range of 99.21 – 100.2 % and 99.52 – 100.26 % for CFS and TAZO respectively for dual-wavelength method and in the range of 98.84 – 99.69% and 100.08 – 100.73% CFS and TAZO respectively for first order derivative method. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of CFS and TAZO in their combined Pharmaceutical formulation....
Two simple, accurate, precise procedures have been developed for the simultaneous estimation of tapentadol hydrochloride (TAP) and lornoxicam (LOR) in combined synthetic mixture. The first method was based on employing simultaneous equation method for analysis of both drugs. Tapentadol hydrochloride and lornoxicam have shown absorbance maxima at 217 and 265 nm in methanol, respectively. The second method was based on derivative spectrophotometric method involving the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectrum was obtained in methanol and the determinations were made at 267.4 nm (ZCP of lornoxicam) for tapentadol hydrochloride and 343.0 nm (ZCP of tapentadol hydrochloride) for lornoxicam. The linearity was obeyed in the concentration range of 8-36 μg/ml for tapentadol hydrochloride and 4-28 μg/ml for lornoxicam. Both methods were validated statistically and recovery studies were carried out. The methods were successfully applied to synthetic mixture because no interference from the mixture excipients was found. The suitability of this method for the quantitative determination of tapentadol hydrochloride and lornoxicam was proved by validation. The proposed method was found to be simple and sensitive for the routine quality control application of tapentadol hydrochloride and lornoxicam in combination. The results of analysis have been validated statistically and by recovery studies. The validation study is statistically significant as all statistical parameter are within the acceptance range (% RSD < 2.0 and S.D. < 2.0) for both accuracy and precision....
In the present work, a simple, sensitive, specific and validated colorimetric method has been developed for the quantitative estimation of losartan potassium in bulk and pharmaceutical dosage form. Losartan potassium in the presence of an acidic medium reacts with excess amount of chloramine-T and remaining chloramine-T reacts with crystal violet to produce greenish blue colour. The final stock solution was made to produce 100 µg/ml with distilled water. The λmax was found to be 618 nm for assay. The linearity was found in concentration range of 10-50 μg/ml. The correlation coefficient was found to be 0.9982. The regression equation was found as y=0.0181x +0.0091. The method was validated as per ICH Guidelines....
In the present work, a simple, sensitive, specific and validated colorimetric method has been developed for the quantitative estimation of salbutamol sulphate in bulk and pharmaceutical dosage form. Salbutamol sulphate forms a blue coloured chromogen with gibbs reagent in alkaline conditions by electrophilic aromatic substitution. The final stock solution was made to produce 100 μg/ml with distilled water. The λmax was found to be 600 nm for assay. The linearity was found in concentration range of 5-30 μg/ml. The correlation coefficient was found to be 0.9991. The regression equation was found as y=0.0316x-0.0081. The method was validated as per ICH Guidelines....
Two simple sensitive and accurate spectrophotometric methods for the determination of ciprofloxacin hydrochloride have been developed and validated. Method A engross the addition of a known excess of bromate-bromide mixture to ciprofloxacin hydrochloride in hydrochloric acid medium followed by determination of residual bromine by reacting with a fixed amount of thymol blue and measuring the absorbance at 545 nm. In method B ciprofloxacin hydrochloride, in presence of acidic medium reacts with excess amount of ceric ammonium sulphate and remaining reacts with crystal violet to produce coloured complex and the absorbance measured at 619 nm. The final stock solution was made to produce 25 µg/ml and 100 µg/ml with distilled water in method A and method B respectively. The linearity was found in concentration range of 2.5-12.5 µg/ml and 5-25 µg/ml for method A and method B respectively. The correlation coefficient was found 0.9994 and 0.9993 for method A and method B respectively. The regression equation was found as y=0.0672x-0.0035 and y= 0.0312x-0.0042 for method A and method B respectively. The method was validated according to USP and ICH Guidelines....
Two simple, sensitive and accurate spectrophotometric methods for the determination of norfloxacin hydrochloride have been developed and validated. The methods are based on the oxidative coupling reaction of norfloxacin hydrochloride with MBTH in the presence of Ce (IV) as an oxidant, to form a bluish green coloured product (method A), while norfloxacin hydrochloride in presence of acidic medium reacts with excess amount of chloramine-T and the unreacted chloramine-T reacts with crystal violet to produce greenish blue colour (method B). The final stock solution was made to produce 100 µg/ml with methanol for both method A and method B. The λmax was found to be 667 nm and 625 nm, for method A and method B respectively. The linearity was found in concentration range of 5-30 µg/ml and 10-50 µg/ml respectively for method A and method B. The correlation coefficient was found 0.999 and 0.9994 for method A and method B respectively. The regression equation was found as Y=0.0249x+0.0106 and Y=0.0153x+0.0086 respectively for method A and method B. The methods were validated according to ICH and USP guidelines....
Two simple, sensitive and accurate spectrophotometric methods for the determination of pantoprazole sodium have been developed and validated. The methods are based on oxidation of pantoprazole sodium with ferric ammonium sulphate followed by complex formation of resulting ferrous ion (Fe2+) with 1, 10-phenanthroline to form orange red coloured chromogen (method A), while pantoprazole sodium in presence of acidic medium reacts with excess amount of chloramine-T and the unreacted chloramine-T reacts with crystal violet to produce greenish blue coloured chromogen (method B). The final stock solution was made to produce 100 µg/ml with distilled water for both methods A and method B respectively. The λmax was found to be 507 nm and 620 nm for method A and method B respectively. The linearity was found in concentration range of 10-50 µg/ml and 5-30 µg/ml respectively, for method A and method B. The correlation coefficient was found 0.9986 and 0.9991 for method A and method B respectively. The regression equation was found as Y = 0.0198x + 0.0202 and Y = 0.0251x + 0.0022 respectively for method A and method B. The methods were validated according to ICH and USP guidelines....
Two simple sensitive and accurate spectrophotometric methods for the determination of pravastatin sodium have been developed and validated. Method A involves oxidative coupling of pravastatin sodium with 3-methyl-2-benzothiazolinone hydrazone (MBTH) in presence of ferric chloride dissolved in HCl and green chromogen is formed and exhibits absorption maxima at 627nm. Method B is an indirect method. This method is based on the bromination of pravastatin sodium by a measured excess of in situ bromine in acid medium followed by the determination of unreacted bromine by reacting with o-dianisidine (ODA) and measuring the absorbance at 440 nm.The final stock solution was made to produce 100�µg/ml and 40�µg/ml with distilled water in method A and method B respectively. The linearity was found in concentration range of 10-50�µg/ml and 2-12�µg/ml for method A and method B respectively. The correlation coefficient was found 0.9991 and 0.9986 for method A and method B respectively. The regression equation was found as y= 0.0175x-0.0015 and y= -0.0x-0.0015for method A and method B respectively. The method was validated according to USP and ICH Guidelines....
The present work describes a simple reverse phase HPLC method for the determination of omeprazole and domperidone from capsule formulations. The determination was carried out on a C-18 (250× 4.6 mm, 5 micron) column using mobile phase contains 35 volumes of acetonitrile and 65 volume a solution of 0.1M ammonium acetate (anhydrous). The flow rate and runtime were 1 ml/min and 20 min, respectively. The eluent was monitored at 286 nm. The method was reproducible, with good resolution between omeprazole and domperidone. The detector response was found to be linear in the concentration range of 10-30 μg/ml for omeprazole and 5-15 μg/ml for domperidone....
Nebivolol hydrochloride in the presence of acidic medium reacts with excess amount of potassium bromide-bromate and remaining potassium bromide-bromate reacts with safranin to produce a pink colour. The final stock solution was made to produce 100 µg/ml with methanol. The λmax was found to be 534 nm for assay. The linearity was found in the concentration range of 10-50 µg/ml. The correlation coefficient was found 0.999. The regression equation was found as Y = 0.018x+0.008. The method has been validated according to ICH guidelines....
The present study describes a simple, accurate, precise and cost effective visible-spectrophotometric method for the estimation of atazanavir sulphate, an anti-HIV drug, in bulk and pharmaceutical dosage form. The stock solution of atazanavir sulphate was prepared by using methanol as solvent. This method based on the complex formation when the atazanavir sulphate was treated with FC (folin ciocalteu) reagent diluted with water (1:3) in presence 20% Na2CO3 solution. The complex is bluish green in colour and has the maximum absorbance at 734 nm. The developed method obeys the beer’s law in the concentration range of 15-75 μg/ml. The method was validated for different parameters as per the ICH (International Conference for harmonization) guidelines. This method can be used for the determination of atazanavir sulphate in quality control of formulation without interference of the excipients....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical Q-absorbance method for the simultaneous determination of ciprofloxacin HCl and bromhexine HCl in their combined pharmaceutical dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point at 256 nm in methanol. The second wavelength is used 279 nm, which is λmax of ciprofloxacin HCl in Methanol. Linearity was observed for ciprofloxacin HCl and for bromhexine HCl in the concentration range of 2-12 μg/ml and (r2 = 0.999) and 5-30 μg/ml and (r2 = 0.993). The concentration of drugs was determined by using ratio of absorbance at isoabsorptive point and at the λmax of ciprofloxacin HCl. The method was successfully applied to pharmaceutical dosage form because of no interference. The result of analysis has been validated by recovery studies....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical Q-absorbance method for the simultaneous determination of olmesartan medoxomil (OLME) and cilnidipine (CILNI) in their combined pharmaceutical dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point at 270 nm in methanol. The second wavelength is used 241 nm, which is λmax of olmesartan medoxomil in Methanol. Linearity was observed for olmesartan medoxomil and for cilnidipine in the concentration range of 4-20 μg/ml and (r2 = 0.996) and 2-10 μg/ml and (r2 = 0.999). The concentration of drugs was determined by using ratio of absorbance at isoabsorptive point and at the λmax of cilnidipine. The method was successfully applied to pharmaceutical dosage form because of no interference. The result of analysis has been validated by recovery studies....
High‐performance liquid chromatography (HPLC), particularly Reversed Phase HPLC (RP‐HPLC), is the most important analytical technique in the pharmaceutical industry. In method development, during validation, transfer or out of specification studies, a traditional approach may fail. This article describes how statistically QbD principles can be used for each phase of LC instrument method development. A Quality by Design (QbD) approach to method development make the use of Statistical design of experiments (DoE) for the development of a robust method ‘design space’. To understand the factors and their interaction effects by a desired set of experiments is an important component in QbD. In this approach, first the requirement for a method is defined. There will be understanding of what the method has to measure and requirement for the method Based on the critical material, process and product attributes. The previous knowledge can be helpful in identifying initial conditions. A design space is identified followed by a screening study. The resulting data are utilised for analysis to generate a resolution response surface to identify potential optimum chromatographic conditions....
Carbamazepine is an anticonvulsant drug. In the present work, a simple, sensitive, specific and validated method has been developed for the quantitative estimation of carbamazepine in bulk and pharmaceutical dosage form. Carbamazepine in the presence of acidic medium reacts with excess amount of chloramine-T and remaining chloramine-T reacts with crystal violet to produce a colour complex which shows absorption maxima at 596 nm. The linearity was found in concentration range of 10-50 μg/ml. The correlation coefficient was found to be 0.999. The method was validated as per USP and ICH guidelines....
Ciclopirox belongs to a class of anti fungal. It is used to treat skin infections caused by fungus, such as ringworm, athlete’s foot or dandruff. The method is based on the oxidation reduction reaction involving the formation of a green colored complex between ciclopirox and ammonium molybdate in the presence of 2M HCl giving absorption maxima at 677 nm. The linearity was found in the concentration range of 10-50 µg/ml. the correlation coefficient was found 0.999. The regression equation was found as Y=0.016x+0.010. The method has been validated as per ICH guidelines....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical derivative spectroscopic method for the simultaneous determination of nifedipine and lidocaine in cream. Derivative spectroscopy offers a useful approach for the analysis of drugs in cream. In this study a second derivative spectroscopic method was used for simultaneous determination of nifedipine and lidocaine using the zero-crossing technique. The measurements were carried out at wavelengths of 259.2 nm and 245.2 nm for nifedipine and lidocaine respectively. The method was found to be linear (r2 = 0.997) in the range of 4-20 μg/ml for nifedipine at 259.2 nm. The linear correlation was obtained (r2 = 0.999) in the range of 20-100 μg/ml for lidocaine at 245.2 nm. The limit of detection was found and 0.77 μg/ml for nifedipine and lidocaine respectively. The limit of quantification was found to be 1.19 and 2.34 μg/ml respectively. The method was successfully applied for simultaneous determination of nifedipine and lidocaine in cream....
Roflumilast, which is an anti-inflammatory medicine called phosphodiestarase 4 inhibitor. Roflumilast reduces the activity of phosphodiestarase 4, a protein occurring naturally in body cells. In the present work three simple, economical, precise and accurate UV spectrophotometric methods have been developed for the estimation of roflumilast in bulk and pharmaceutical formulation. Method A is absorption maxima method in which λ max was found to be 250 nm. Method B is area under the curve (AUC) in which area in the wavelength range of 241 nm-259 nm was selected for analysis of roflumilast. Linearity was observed in the concentration range 5-30 μg/ml (r2 =0.997) for two methods. The % assay for the marketed formulation for absorption maxima and area under the curve method was found to be 99.25 % and 99.3434 % respectively. The methods were validated with respect to linearity, precision and accuracy studies. Recovery studies for absorption maxima and area under the curve was found to be 99.32%-100.69% respectively. The methods were found to be simple, precise and accurate and can be employed for routine quality control analysis of roflumilast in bulk as well as from its dosage form....
Spectroscopic method for degradation study of Glibenclamide was described. Force degradation study is a process in which natural degradation rate of pharmaceutical product is increased by application of an additional stress. Glibenclamide is second generation sulphonyl urea derivative and used as Antidiabetic agent. To develop and validate a simple and precise stability indicating UV spectroscopic method for the estimation of Glibenclamide in bulk and tablet dosage form. Force degradation study of Glibenclamide was done by High performance liquid chromatography method but not still done by UV Spectroscopy. Separation of Glibenclamide from its degradation product were achieved by UV spectroscopic method using ethanol. Glibenclamide was subjected to stress condition such as hydrolysis (acid and base), oxidation, photolysis. The maximum absorbance was found to be at 230.6 nm and found to be linear over the range 5-25 ug/ml with good correlation coefficient ( r2) 0.9980. The limit of detection and quantification were 1.1041 and 3.3460 ug/ml respectively. Major degradation was observed in acid, alkaline and oxidative conditions. Glibenclamide was quietly stable under thermal condition. Thus the proposed method was found to be economical, selective and sensitive for desirable range....
New, simple, cost effective, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of nadifloxacin in bulk and pharmaceutical ingredient. Nadifloxacin was estimated at 237 nm in phosphate buffer (pH 6.8). Beer’s law was obeyed in the concentration range of 1–18 µg/ml (r2 = 0.9989) in phosphate buffer (pH 6.8). This method was tested and validated for various parameters according to ICH guidelines. The proposed method was successfully applied for the determination of nadifloxacin in bulk and pharmaceutical formulation. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 2%). At the same time method being simple, cheap and less time consuming, can be suitably applied for the estimation of nadifloxacin in different dosage forms and dissolution studies....
A simple, precise and accurate method was developed for the estimation of chlorzoxazone (CHL) and paracetamol (PCM) in tablet dosage form using second order derivative spectrophotometry. Wavelengths selected for quantitation were 279.18 nm for chlorzoxazone (zero crossing point of PCM) and 270.43 nm for paracetamol (zero crossing point of CHL). The method was validated with respect to linearity, accuracy, precision, limit of detection and limit of quantitation in accordance with the international conference on harmonisation (ICH) guidelines. Linearity was observed in concentration range of 5-40 μg/ml for each chlorzoxazone and paracetamol. The limit of detection and limit of quantitation were found to be 0.16 μg/ml and 0.51 μg/ml for chlorzoxazone and 0.59 μg/ml and 1.83 μg/ml for paracetamol. The percentage recovery of chlorzoxazone and paracetamol was found to be 99.95±0.66 and 99.66±0.62 respectively. The % R.S.D. values for intra-day and inter-day precision study were < 2.0%, confirming that the method was precise. The method can be successfully employed for the simultaneous estimation of chlorzoxazone and paracetamol in tablet dosage form....
A simple, precise and accurate method was developed for the estimation of sildenafil (SIL) and aspirin (ASP) in synthetic mixture using first order derivative spectrophotometry. Wavelengths selected for quantitation were 255.4 nm for sildenafil (zero crossing point of aspirin) and 265 nm for aspirin (zero crossing point of sildenafil). The method was validated with respect to linearity, accuracy, precision, limit of detection and limit of quantitation in accordance with the international conference on harmonization (ICH) guidelines. Linearity was observed in concentration range of 5-35 μg/ml for sildenafil and 20-80 μg/ml for aspirin. The limit of detection and limit of quantitation were found to be 0.15 μg/ml and 0.44 μg/ml for sildenafil and 1.94 μg/ml and 5.87 μg/ml for aspirin. The percentage recovery of sildenafil and aspirin was found to be 100.75% and 100.11%, respectively. The % R.S.D. values for intra-day and inter-day precision study were <2.0%, confirming that the method was precise. The method can be successfully employed for the simultaneous estimation of sildenafil and aspirin in synthetic mixture....
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