Current Issue : July-September Volume : 2014 Issue Number : 3 Articles : 60 Articles
Improvement of life quality is the major important objectives of the global research work. The quality of life is related to a better control of diseases, the quality of our environment and drug and food quality and safety. A continuous, fast, reliable and sensitive monitoring is required to control key parameters and biosensors are very much important for that purpose. Biosensors are composed of two main parts such as a biological recognizing component (enzyme, antibody, cell and tissue) which is connected to a physical transducer (spectro¬photometric, conductometric, voltammetric and amperometric). Various biological systems that can be used as recognizing agents allow specific biosensors for many analytes. Biosensors mainly used due to high sensitivity, specificity, ease of use, fast, cost-effective and repetitive measurements with miniaturized and portable devices for the quality analysis of drugs, medicines and other analytes of interest in the pharmaceutical, biomedical and environmental field. Biosensors allow quantification of the active component in pharmaceutical formulations and also the degradation products and metabolites analysis in biological fluids. Thus, this work presents a brief review of biosensor application in pharmaceutical analysis....
A simple, rapid, precise, sensitive and reproducible high performance liquid chromatographic method was developed for estimation of minoxidil in tablet dosage form. Chromatographic separation of the drug was achieved on a phenomenex kinetex 5µ C-18 100 A column (250 × 4.6 mm) using a mobile phase, methanol and water (60:40% v/v) at a flow rate of 1 ml/min. The drug eluted was monitored at 235 nm. The retention time was 3.3 min. The calibration curve was linear over the range of 10 ng - 200 μg/ml. The performance of the method was validated according to ICH guidelines. The method can be applied for determination of drug in its tablet dosage form without any interference from excipients or degradant substances and also applicable to topical solutions (MINTOP). The proposed method is suitable for routine quality control analysis....
A rapid, simple, precise, accurate and reproducible reverse phase high performance liquid chromatographic method was developed for the estimation of mesoindigo in the bulk by using thermoscientific column (5 µm, 250 mm × 4.6 mm i.d). Combination of methanol: buffer (0.1% ammonium dihydrogen phosphate adjusted to pH-3 using orthophosphoric acid) in the ratio of 90:10 v/v as a mobile phase at a flow rate of 1 ml/min in an isocratic mode at a detection wavelength of 265 nm was used for the analysis. The drug was eluted at a retention time of 7 min. The method was validated as a final verification of method development with respect to precision, linearity, accuracy and robustness. Calibration curve was linear with the correlation coefficient of 0.999 over a concentration range of 50-300 µg/ml. The mean recovery obtained was within the range of 98-102%....
This study describes the development and validation of stability indicating HPLC method for blonanserin in its bulk and tablet dosage forms. Blonanserin was subjected to different stress conditions such as acid, base, oxidation, dry heat and photolytic stress conditions and the stressed samples were analyzed by the proposed method. Chromatographic separation achieved isocratically on a C18 column by utilizing mobile phase acetonitrile: methanol: water: triethylamine (60 : 30 : 10 : 0.1 v/v/v) at the flow rate of 1 ml/min with UV detection at 240 nm. The retention time of blonanserin is 11-12 min. Linearity was established for blonanserin within the range of 2-12 µg/ml with regression coefficient R2 = 0.999.The limit of detection and limit quantification were found to be 0.053448 μg/ml and 0.161962 μg/ml respectively, percentage recoveries were obtained in the range of 99.58 - 100.98%. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation and robustness. The method proved to be specific to the drug and its degradation products. All the results were found to be within the specification limit. The method was validated as per ICH guidelines. The developed method can be applied effectively and successfully for determination of blonanserin in bulk and tablet dosage forms and their force degradation studies....
A simple, selective, rapid, precise and economical reverse phase high-pressure liquid chromatographic method has been developed for the simultaneous estimation of isosorbide dinitrate and hydralazine hydrochloride from pharmaceutical formulation. The method was carried out on a hypersil C18 (250 x 4.6 mm, 5 μm) column, with a mobile phase consisting of acetonitrile: phosphate buffer pH 3.6 (30:70 v/v) at a flow rate of 0.8 ml/min. The retention time of hydralazine hydrochloride and isosorbide dinitrate was 3.59, 6.56 min respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation. The proposed method can be used for estimation of these drugs in combined dosage form for routine analysis....
UV spectrophotometric method has been developed for simultaneous estimation of dyphylline (DYP) and guaifenesin (GUA) in bulk drug and in their combined dosage form by first order derivative. This method utilizes distilled water as a solvent and λmax of dyphylline and guaifenesin selected for analysis was found to be 273 nm (at ZCP of GUA) and 260 nm (at ZCP of DYP) respectively. Linearity was observed in the concentration range of 2-10 μg/ml for DYP (r2 = 0.998) and 20-100 μg/ml for GUA (r2 = 0.996). 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....
A new simple, rapid, accurate, sensitive and precise spectrophotometric method in colorimetric region has been developed for determination of Ezetimibe in bulk and pharmaceutical dosage form by MBTH reagent. The principle involved in this method is iron catalysed coupling reaction of MBTH with the drug in the presence of Fecl3 to form green colored coumpound which exhibited maximum absorbance at 621 nm in methnol. Beer''s law was found to be obeyed in the concentration range 20-100 �µg/mL. Regression equation was found to be 0.009x and coefficient of correlation was 0.9922. The developed method was validated respect to stability, linearity, precision, accuracy. The proposed method is useful for the routine estimation of Ezetimibe in bulk and pharmaceutical dosage form....
Simple, Accurate and rapid HPLC methods for paroxetine hydrochloride tablets and determination of drug release in modified dosage form were developed. USP type-II, paddle apparatus was selected to determine the % drug release. 0.1 N HCl, 6.8 pH phosphate buffer and 7.4 pH Phosphate buffer were used as dissolution media. Column eluent was detected at 295 nm. Methods were validated according to the present ICH guidelines for linearity, accuracy, precision, LOD, LOQ, robustness and results were found satisfactory. Method shows linearity in the range of 0.4-1.2 µg/ml (0.1 N HCl), 2-10 µg/ml (6.8 pH phosphate buffer) and 0.2-1 µg/ml (7.4 pH phosphate buffer) with correlation coefficient 0.9980, 0.9968 and 0.9983 respectively. Accuracy was found in the range of 98.42%-101.25% (0.1 N HCl), 98.85%-100.09% (6.8 pH phosphate buffer) and 98.84%-101.06% (7.4 pH phosphate buffer). LOD and LOQ were found to be 0.772 µg/ml and 1.0906 µg/ml (0.1 N HCl), 2.274 µg/ml and 6.80 µg/ml (6.8 pH phosphate buffer), 0.738 µg/ml and 0.923 µg/ml (7.4 pH phosphate buffer). %Assay was found to be 93.87% (0.1 N HCl), 97.78% (6.8 pH phosphate buffer) and 96.27% (7.4 pH phosphate buffer). The dissolution profile of marketed brands of controlled release paroxetine hydrochloride tablets were compared with reference brand. The results were subjected to statistical evaluation of similarity factor and difference factor. There was no significant difference found between dissolution profiles of different brands of paroxetine hydrochloride controlled release tablets. Comparison study shows that there was similarity in dissolution profile of all brands....
UV spectrophotometric absorption correction method has been developed for simultaneous estimation of mefenamic acid and tranexamic acid. Wavelength selected for TRA was 402.6nm and for MAA corrected absorbance was measured by deducing the absorbance of TRA at 402.6 nm from absorbance of mixture at 297.2 nm. Overlay spectra for both the drug and selected wavelengths are shown in Figure 2. Beer’s law obeyed in concentration range of 4-20 μg/ ml MAA and 8-40 μg/ ml in methanol for both the drugs. Limit of detection was found to 0.173 and 0.346 μg/ ml and limit of quantitation 0.524 and 1.048 μg/ml of mefenamic acid and tranexamic acid respectively. The proposed methods are simple, sensitive, accurate and precise since they are recommended for routine analysis....
A rapid, specific and economic simple UV spectrophotometric method has been developed using water and methanol (50:50, v/v) as a solvent to determine the alogliptin benzoate in bulk and pharmaceutical dosage formulation. At a predetermined λmax of 223 nm, it was proved linear in the range of 2.0 to 12.0 μg/ml and exhibited good correlation coefficient (r2 = 0.999) and excellent mean recovery (99.25-99.83%). This method was successfully applied to the determination of alogliptin benzoate content in the marketed brand and the results were in good agreement with the label claim. The method was validated statistically and by recovery studies for linearity, precision, repeatability and reproducibility. The obtained results proved that the method can be employed for the routine analysis of alogliptin benzoate in bulk as well as in the pharmaceutical dosage formulation....
A simple, fast and precise reverse phase high performance liquid chromatographic method has been developed for the estimation of spironolactone in oral suspension. The chromatographic separation was achieved on zorbax RX-C18 (150 x 4.6) mm; 5 µm column with an isocratic mixture of methanol: water (60:40). The mobile phase at a flow rate of 1 ml/min, injection volume 20 μl and wavelength of detection was kept at 240 nm with column temperature at 25°C. The retention times for spironolactone, methyl paraben and propyl paraben were 6.61±0.04 min, 2.25±0.04 min and 4.67±0.04 min respectively. Here methyl paraben and propyl paraben is a major excipient of oral solution. The linearity was obtained in the range of 250-600 μg/ml, 50-120 μg/ml and 5-12 μg/ml for spironolactone, methyl paraben and propyl paraben respectively with correlation coefficient 0.998, 0.999 and 0.999 for spironolactone, methyl paraben and propyl paraben respectively. The proposed methods were validated as per ICH guidelines and successfully applied for the determination of investigated drugs in oral suspension....
The simple, specific, accurate, precise and reproducible RP-HPLC method have been developed and validated for the simultaneous estimation of dicyclomine HCl and diclofenac sodium. RP – HPLC method was developed using mobile phase:-acetonitrile and 0.050 M potassium dihydrogen phosphate buffer adjusted to pH 7.0 with 0.1N NaOH (65:35 v/v) and stationary phase hypersil BDS C18 column (250 mm x 4.6 mm, 5.0 μm) at wavelength 218 nm and 1 ml/min flow rate. The calibration plot shown r2 0.998 and 0.999, in the concentration range of 10-45 µg/ml and 25 – 112.5 µg/ml for dicyclomine HCl and diclofenac sodium respectively. Accuracy was found to be 99.58% – 101.00% and 99.83% –100.11% respectively. LOD was found to be 1.97 and 1.51 µg/ml for dicyclomine HCl and diclofenac sodium respectively. Retention time was found to be 6.0 min and 4.2 min for dicyclomine HCl and diclofenac sodium respectively. These methods were statistically validated for accuracy, precision, linearity, LOD, LOQ and robustness according to ICH guidelines and can be used for analysis of combined dosage form....
A RP-HPLC method was developed for the simultaneous estimation of metoprolol succinate and chlorthalidone in their combined dosage form. The separation was achieved by BDS hypersil C18 (250 x 4.6 mm) 5 μm column and phosphate buffer (pH 3.5 using O-phosphoric acid): methanol: acetonitrile (50:25:25 v/v/v) as mobile phase, at a flow rate of 1.0 ml/min having injection volume 20 µl. Detection was carried out at 223 nm. Retention time of metoprolol succinate and chlorthalidone was found to be 6.073 min and 3.500 min respectively. The method has been validated for linearity, accuracy and precision. Linearity for metoprolol succinate and chlorthalidone were in the range of 20-60 μg/ml and 6-14 µg/ml respectively. The % recoveries obtained for metoprolol succinate and chlorthalidone were found to be in range of, 99.93-100.02% and 100.18-101.57% respectively. The Stability Indicating RP-HPLC method were found to be accurate, precise, selective and stability indicating. Metoprolol succinate and chlorthalidone showed degradation in acidic, basic, oxidative, photolytic and thermal in appropriate condition....
The simple, precise and accurate first derivative spectroscopic method has been developed for simultaneous estimation of gatifloxacin and flurbiprofen in bulk and eye drops. The solution of both the drugs and eye drops were prepared in methanol. Quantitative determination of the drugs was performed using double beam UV-visible spectrophotometer at 248 nm and 262 nm for gatifloxacin and flurbiprofen respectively. The method was linear in the concentration range of 20-70 μg/ml for gatifloxacin and 2-7 μg/ml for flurbiprofen with correlation coefficients of 0.9994 for both the drugs. The percentage recoveries obtained for gatifloxacin and flurbiprofen ranges from 98.40-101.25% and 98.5-101.60%, respectively. The method was validated and successfully employed for simultaneous estimation of both drugs in commercial products....
A simple and sensitive RP-HPLC method has been developed for the estimation of ilaprazole (ILA) and domperidone (DOM) in their capsule dosage form in the ratio of 1:3. The method was carried on a C18 (250 × 4.6 mm, 5 μm) column with a mobile phase consisting of methanol and water in the ratio (80:20 v/v) and flow rate 0.9 ml min-1. The detection was carried out at 289 nm. The retention time for ILA and DOM were found to be 4.644 and 7.232 min respectively. The ILA and DOM followed linearity in the concentration range of 50 – 150 μg/ml and 150 – 450 μg/ml respectively. The developed method was validated for precision, accuracy, sensitivity and robustness. The developed method can be used for routine analysis of these drugs in combination in the capsule formulations....
Reverse phase-high performance liquid chromatography (RP-HPLC) method have been developed and validated for the estimation of allopurinol and α-lipoic acid in combination tablet. The developed method is rapid, accurate, precise, simple and economical. The separation was achieved on reversed-phase unisphere C18 column (agela tech.), (5 µm, 250 mm x 4.6 mm i.d) column using mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate (60:40, v/v) adjust pH with ortho phosphoric acid to 5.25 which gives greater resolution. Wavelength used for UV detection was 220 nm. Linearity was observed in the concentration range of 50-150 μg/ml for both allopurinol and α-lipoic acid with correlation coefficient 0.9999 and 0.9999 for allopurinol and α-lipoic acid respectively. The proposed method was successfully applied for the simultaneous estimation of both drugs in combination tablet. Assay value of allopurinol was found to be 100.90% and that of α-lipoic acid was found to be 100.11%. Mean recovery were found to be 100.75 % and 100.15 % for allopurinol and α-lipoic acid, respectively. LOD and LOQ were found to be 2.889 μg/ml and 8.755 μg/ml for allopurinol, respectively and 0.084 μg/ml and 0.255 μg/ml for α-lipoic acid, respectively. Proposed method can be successfully applied for the quantitative determination of Allopurinol and α-Lipoic Acid in combination tablet....
A simple, efficient and reproducible RP-HPLC method for the simultaneous determination of cilnidipine and metoprolol succinate in pharmaceutical dosage form has been developed and validated. The separation was carried out on hyperchrom ODS-BP (4.6 mm X 200 mm, 5 μm) column using acetonitrile: 0.05 M potassium dihydrogen phosphate buffer (adjusted to pH 3 with 10% OPA) in the ratio of 50:50 v/v as eluent. The flow rate was 1 ml/min and effluent was detected at 280 nm. The retention time of cilnidipine and metoprolol succinate was 3.36 and 6.25 min. respectively. The linear dynamic range was 2-10 μg/ml for cilnidipine and 10-50 μg/ml metorolol succinate, respectively. Percentage recoveries for cilnidipine and metoprolol succinate were 99.95 – 100.05% and 99.29 – 99.76% respectively. All the analytical validation parameters were determined and found in the limit as per ICH guidelines, which indicates the validity of the method. The developed method is also found to be precise and robust for the simultaneous determination of cilnidipine and metoprolol in tablet dosage forms....
A specific, accurate, precise and reproducible RP-HPLC method has been developed and subsequently validated for the simultaneous determination of ketorolac tromethamine and fluorometholone in ophthalmic formulation. The proposed HPLC method utilizes hypersil (thermo scientific) C18 column (250 mm × 4.6 mm id, 5 μm particle size) and mobile phase consisting of phosphate buffer: methanol (70:30) and pH adjusted to 3.0 with orthophosphoric acid at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 260 nm based on peak area with linear calibration curves at concentration ranges 2.5-7.5 μg/ml for fluorometholone and 12.5-37.5 μg/ml for ketorolac tromethamine. The retention time of fluorometholone and ketorolac tromethamine were found to be 3.69 min and 6.303 min respectively. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation and robustness. This method has been successively applied to ophthalmic formulation and no interference from the formulation excipients was found....
The article describes a simple, sensitive, rapid, accurate, precise and specific RP-HPLC method for the simultaneous estimation of ofloxacin and ornidazole with their related impurities in the i.v. infusion dosage form. The chromatography is carried out using merck purospher STAR RP C18® (250 mm x 4.6 mm, 5 µm particle size) column and mixture of phosphate buffer and acetonitrile in the ratio (85:15 v/v) at flow rate of 0.9 ml/min as mobile phase. Detection was carried out at 300 nm using PDA detector. The retention time of ofloxacin and ornidazole were found to be 8.72 min and 14.67 min respectively while for ofloxacin related compound A and 2- methyl-5- nitro imidazole, retention time were 8.20 min and 4.80 min respectively. The LOD value for ofloxacin, ornidazole, ofloxacin related compound A and 2- methyl-5-nitro imidazole were found to be 0.26 µg/ml, 0.41 µg/ml, 0.055 µg/m and 0.05 µg/ml respectively. The LOQ value for ofloxacin, ornidazole, ofloxacin related compound A and 2-methyl-5-nitro imidazole were found to be 0.79 µg/ml, 1.41 µg/ml, 0.18 µg/ml and 0.18 µg/ml respectively. The developed method can be applied effectively and successfully for determination of ofloxacin, ornidazole, ofloxacin related compound A and 2- methyl-5-nitro imidazole in the intravenous infusion dosage form....
A specific, accurate, precise and reproducible HPLC method has been developed and subsequently validated for the simultaneous determination of timolol maleate and pilocarpine nitrate in ophthalmic formulation. The proposed HPLC method utilizes BDS hypersil (thermo scientific) C18 column (250 mm × 4.6 mm id, 5 μm particle size) and mobile phase consisting of methanol: 0.02 M phosphate buffer [60: 40, v/v] and pH adjusted to 5.0 with NaOH at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 230 nm based on peak area with linear calibration curves at concentration ranges 5-15 μg/ml for timolol maleate and 20-60 μg/ml for pilocarpine nitrate. The retention time of timolol maleate and pilocarpine nitrate were found to be 3.467 min and 6.08 min respectively. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation and robustness. This method has been successively applied to ophthalmic formulation and no interference from the formulation excipients was found....
The spectroscopic method (in methanol – second derivative zero crossing method) has been developed, which were novel, simple, accurate, reproducible, economical and validated for the determination of clobetasol propionate and miconazole nitrate in cream. The drug is extracted from cream by sonication, heating, cooling. Absorbance of miconazole nitrate and clobetasol propionate were measured at 266 nm (zero crossing point of clobetasol propionate) and 282 nm (zero crossing point of miconazole nitrate), respectively and show linearity over the range of 4-24 μg/ml for clobetasol propionate and 160-960 μg/ml for miconazole nitrate with correlation coefficient 0.9996 and 0.9994 for clobetasol propionate and miconazole nitrate in respectively. LOD and LOQ were found to be 0.20 μg/ml and 0.60 μg/ml for clobetasol propionate respectively and 6.17 μg/ml and 18.17 μg/ml for miconazole nitrate, respectively....
A rapid, specific, easy and economic UV spectrophotometric method has been developed using methanol as a solvent to determine the oxcarbazepine content in bulk and pharmaceutical dosage forms. At a pre-determined λmax of 306 nm, it was proved linear in the range of 20-100 µg/ml and exhibited good correlation coefficient (R2 = 0.9997) and excellent mean recovery (99.166%). This method was successfully applied to the determination of oxcarbazepine content in two marketed brands from India and the results were in good agreement with the label claims. The method was validated statistically and by recovery studies for linearity, precision, repeatability and reproducibility. The obtained results proved that the method can be employed for the routine analysis of oxcarbazepine in bulks as well as in the commercial formulations....
Spectrofluorometric method has been developed for estimation of gatifloxacin and flurbiprofen sodium. (Simultaneous method) The method involves measurement of fluorescence intensity of both drug at wavelength (λmax) of each other (gatifloxacin at 495.96 nm and 312.68 nm, flurbiprofen at 312.68 nm and 495.96 nm). The method has linear response in the range of 40-120 ng/ml and 5-45 ng/ml with co-efficient of correlation, (R2) = 0.9992 for GATI and (R2) =0.9993 for FLURBI The limit of detection and limit of quantification was 12.90 and 39.10 for GATI and 1.5 and 4.7 for FLURBI respectively. Accuracy of the method was performed by % recovery studies. Based on results, proposed spectrofluorometric method was found to be simple, sensitive, accurate and precise for determination of GATI and FLURBI in Ophthalmic dosage form....
The article describes a simple, sensitive, rapid, accurate and precise spectrophotometric method for the estimation of alfuzosin hydrochloride in bulk and in pharmaceutical dosage forms. The wavelength maximum for alfuzosin hydrochloride was found to be 245 nm. The different analytical parameters were determined according to ICH Q2 (R1). Beer’s law was obeyed in the concentration range of 2-10 µg/ml. Limit of detection and limit of quantitation were found to be 0.0196 µg/ml and 0.0593 µg/ml respectively. The % recovery of drug for proposed method was 101.5760% indicating no interference of excipients. The precision of method was found within the limits....
UV Spectrophotometric method has been developed for simultaneous estimation of dyphylline (DYP) and guaifenesin (GUA) in bulk drug and in pharmaceutical dosage form. This method utilizes distilled water as a solvent and λmax of dyphylline and guaifenesin selected for analysis was found to be 273 nm and 290 nm respectively. Linearity was observed in the concentration range of 4-12 μg/ml (DYP) (r2 = 0.9998) and 20-100 μg/ml (GUA) (r2 = 0.9997) 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 and sensitive first order derivative spectrophotometric method has been developed for the estimation of ilaprazole (ILA) and domperidone (DOM) in their capsule dosage form in the ratio of 1:3. The estimation of ILA and DOM was carried out on a UV/VIS spectrophotometer using 1 cm quartz cell. The method was performed at 282 nm and 285 nm as a zero crossing point for ILA and DOM respectively. ILA and DOM obeyed beer’s law in a concentration range of 5 – 25 (0.9990) μg/ml and 15 – 75 μg/ml (0.9991) respectively. The average percentage recovery of ILA and DOM was found to be 100.10% and 100.71 % respectively. The LOD and LOQ value were found to be 0.78 and 2.38 ppm for ilaprazole and 1.25 and 3.79 ppm for domperidone respectively. The developed and validated method was successfully used for the quantitative analysis of commercially available dosage form....
A simple, sensitive, specific, accurate and stability‑indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of ebastine and phenylephrine hydrochloride, using a pursuit C18 (300 x 3.9 ) mm; 10 µm (particle size) column as a stationary phase and a mobile phase composed of methanol: 0.02 M ammonium acetate (60:40 v/v), pH 6.7. The retention times of phenylephrine hydrochloride and ebastine were found to be 5.11 min and 7.09 min, respectively. Linearity was established for ebastine and phenylephrine hydrochloride in the range of 4-34 μg/ml. The percentage recoveries of ebastine and phenylephrine hydrochloride were found to be in the range of 99.34-100.32% and 98.92-102.09%, respectively. Both the drugs were subjected to acid, alkali and neutral hydrolysis, oxidation, dry heat and UV degradation. The degradation studies indicated ebastine and phenylephrine hydrochloride to be more susceptible to oxidative hydrolysis. This method can be successfully employed for simultaneous quantitative analysis of ebastine and phenylephrine hydrochloride and in bulk drugs and formulations....
A simple, sensitive, precise, accurate, economic and rapid spectrophotometric method has been developed and validated for estimation of levonorgestrel using UV spectrophotometer. Maximum absorbance was observed at 241 nm using methanol as a solvent. Linearity was found in the concentration range of 2-20 μg/ml for levonorgestrel. The method was validated for linearity, precision, accuracy, limit of detection and limit of quantification as per ICH guidelines. The %RSD values were <2%. The average % recovery was found to be 99.91±0.26% for proposed method. The assay result obtained was 102.53±0.35% for levonorgestrel using proposed method. A stability indicating UV spectrophotometric method was developed for analysis of the drug in various degradation conditions. It involved acidic, alkaline, oxidative, thermal, UV and sunlight degradation conditions in which methanol were used as solvent. The amount of degraded drug was calculated by taking absorbance at 241 nm. The proposed method was found to be simple, economic and sensitive, hence can be used for the routine analysis and quality control checking of levonorgestrel in pharmaceutical dosage form....
Two methods for simultaneous estimation of camylofin dihydrochloride (CFD) and paracetamol (PCM) in combined tablet dosage form have been developed after derivatizing with potassium permanganate as a solvent. KMnO4 used as a derivatizing agent for increasing absorbtivity of CFD in UV spectroscopic methods. The first method is based on first order derivative method and second method is based on dual wavelength method. For the method I, the estimation of CFD was carried out at max 273 nm (ZCP of PCM) and of PCM at 374.5 nm (ZCP of CFD). For method II, estimation of CFD was carried out at max 259.5 nm and 382 nm (difference is zero for PCM) and of PCM at 254 nm and 270 nm (difference is zero for CFD). The methods obey beer’s law in concentration ranges employed for the estimation. The developed methods were validated in terms of linearity, LOD, LOQ, accuracy, precision and robustness as per ICH Q2 (R1) guidelines. The proposed methods have been applied successfully for the analysis of the drug in pure and in its pharmaceutical dosage forms. The results obtained from both methods were statistically compared using paired t test....
Without resolving mixtures of formoterol fumarate dihydrate and beclomethasone dipropionate, by application of various UV methods for simultaneous estimation of combined pharmaceutical formulation were developed as follows: in UV spectroscopic methods, estimation of formoterol fumarate dihydrate and beclomethasone dipropionate were carried out using methanol as solvent at max 214 nm and 239 nm for simultaneous equation method, 284 nm and 239 nm for absorption correction method, absorbance difference of 229 nm – 247 nm (difference is zero for FFD) and 208 nm – 218.40 nm (difference is zero for BD) for dual wavelength method and 267.20 nm (ZCP of FFD) and 306 nm (ZCP of BD) for first order derivative spectroscopic method respectively for FFD and BD. The methods obey beer’s law in concentration ranges employed for the estimation. The developed methods were validated in terms of linearity, LOD, LOQ, accuracy, precision and robustness as per ICH Q2 (R1) guidelines. Comparison of all developed and validated methods were carried out by using statistical tools. The method is successfully applied to pharmaceutical formulation, with no interference from excipients. Developed method was simple, accurate for routine simultaneous estimation of formoterol fumarate dihydrate and beclomethasone dipropionate....
Novel combination of flurbiprofen sodium (FLB) and gatifloxacin (GATI) is available as eye drops form in the ratio of 1:10 and no spectrophotometric 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 first order derivative spectroscopy, using methanol as a solvent. The method was performed at 247.60 nm (zero crossing point of FLB) and 262 nm (zero crossing point of GATI) for GATI and FLB sodium respectively. The regression analysis data for the calibration plot showed good linear relationship in the concentration range of 0.5-2.5 μg/ml (R2 = 0.9996) for FLB and 5-25 μg/ml (R2 = 0.9988) for GATI. The average percentage recovery of FLB and GATI combination was found to be 100.05% and 99.74% respectively. The LODs for FLB and GATI were 0.1057μg/ml and 0.4408 μg/ml and LOQs were found to be 0.3204 μg/ml and 1.3359 μg/ml respectively. Statistical analysis proves that the method is reproducible and selective for the simultaneous determination of FLB and GATI. The Results were found to be within acceptance criteria according to ICH Q2 R1 guidelines....
A simple, sensitive, rapid and accurate extractive visible spectrophotometric method has been developed for determination of enalapril maleate in API and in pharmaceutical formulations. The method developed was based on formation of pale yellow colour dichloromethane extractable ion-pair complex between the basic nitrogen of the drug and acidic dye bromocresol green in the presence of 0.1M HCl, at absorption maxima of 417 nm. The test solutions were found to follow beer’s law in concentration range of 5-25 µg/ml. The method was successfully developed. The data was subjected to statistical treatment. The method offers advantages of simplicity, sensitivity, accuracy and reproducibility....
A simple, precise and accurate UV spectrophotometric method has been developed for estimation of saroglitazar in bulk and tablet dosage form. In this method saroglitazar shows λmax at 294 nm using ethanol as a solvent. The responses were linear in the range of 10-70 μg/ml. The regression equation of the calibration graph and correlation coefficient were found to be y = 0.016x - 0.005 and 0.9998 respectively. The recovery of the drug from the sample was ranged between 99.10% and 101.23%. The proposed method was validated as per ICH Q2 (R1) guidelines for precision, linearity, accuracy and recovery. The %RSD values for both intraday and interday precision were less than 2.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.186 μg/ml and 0.563 μg/ml respectively by simple UV spectroscopy....
Dosulepin HCl is chemically (E,Z)-3-(dibenzo[b,e]thiepin-11(6H)-ylidene)-N,Ndimethylpropan-1-amine is used to treat depression. The drug is commercially available as tablets for oral administration. In the present work a simple, rapid, accurate, precise, sensitive and economical UV spectrophotometric method has been developed for estimation of dosulepin HCl in tablet dosage form. The λmax of dosulepin HCl was found to be 229 nm. The linearity was observed in concentration range 2-10 µg/ml with correlation coefficient value 0.9996. The proposed method was applied to pharmaceutical formulation and % amount of drug estimated 98.8% 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., 50%, 100% and 150%. The % recovery was found to be in the range 98.46 – 100.10%. The precision of the method was studied as an intra-day, inter-day variations and repeatability and the % R.S.D value was found to be less than 2 indicate that the method is precise. The above method was a cost-effective quality-control tool for routine analysis of dosulepin HCl in bulk and in pharmaceutical dosage form....
Reverse phase-high performance liquid chromatography (RP-HPLC) method have been developed and validated for the estimation of edaravone and citicoline sodium in bulk drug and synthetic mixture. The developed method is rapid, accurate, precise, simple and economical. The separation was carried out using luna C18 100A° (250 mm×4.6 mm i.d.) 5 µm reverse phase column (phenomenex, luna®) in gradient mode, with mobile phase containing Acetonitrile: Water (70:30, v/v). The flow rate is 0.8 ml/min and effluents are monitored at 244 nm. Chromatogram showed peak at a retention time of 3.667±0.008 min for edaravone and 2.258±0.008 min for citicoline sodium. The method is validated for system suitability, linearity, precision, accuracy specificity, ruggedness, robustness, LOD and LOQ. Recovery of edaravone and citicoline sodium is found to be in the range of 99.94 - 100.19 %. The LOD and LOQ for estimation of edaravone and citicoline sodium are found to be 0.078 µg/ml, 0.237µg/ml and 1.223µg/ml, 3.707 µg/ml respectively. Proposed method can be successfully applied for the quantitative determination of edaravone and citicoline sodium in bulk drug and in synthetic mixture....
A simple, sensitive, accurate, precise and economical visible spectrophotometric method was developed and validated for the estimation of blonanserin in synthetic mixture. The method is based on the reaction of blonanserin with bromothymol blue dye in dichloromethane giving yellow color chromogen, which shows maximum absorbance at 409 nm against reagent blank. The chromogen obeyed Beer’s law in the concentration range of 1-8 µg/ml for blonanserin. The results of the analysis have been validated statistically and by recovery studies....
Camptothecin (CPT) a monoterpene indole alkaloid was extracted from stem bark of Nothapodytes nimmoniana using ultrasonic and microwave assisted extraction technology under different conditions such as surfactant concentration (SC), temperature and exposure time. The optimum parameters for ultrasonic extraction were determined as SC 0.2%, temperature 60 degree for 1 hour. While in microwave extraction, exposure time was reduced up to 2 min at 350 W. By using the optimized parameters, CPT was obtained at 1.645% w/w and 1.654 % w/w for ultrasonic and microwave extraction respectively. The yield of CPT extracted by using surfactant were found to be maximum than those by other solvents and this method was found to be simple, economic, time saving and with high yield....
The aim of this work was to exercise concurrent process validation of Modafinil 200 mg Tablets. All the instruments were qualified as per standard operating procedures. In-process quality monitoring of all critical processing steps like granulation, compression, and packaging was done for three production batches. End product testing of current production batches was done to provide documented evidence that manufacturing process is in state of control. Assay for drug content was within the acceptable limit for the samples which were collected after dry mixing and lubrication stage, indicating blend uniformity. LOD for the granules after dry mixing and lubrication was within 0.8-2.5%. Physical parameters like average weight of tablet was found to be 448.0 to 451.0mg, thickness was between 3.8 mm-3.9mm, hardness was within the acceptable limit, disintegration time was 1min-2min, assay of tablets was within 90.0%-110.0% for all the three batches of compressed tablets. Dissolution occurred in 0.1N HCL for up to 30min. at 50 rpm, drug release was within the limit of NLT 75% in 30min. During blister packing operation each pack size was checked for physical appearance and sealing quality and found satisfactory. All the tests were found to have satisfactory results and there was no significant variation between batch to batch. Thus process validation of Modafinil 200mg uncoated tablets was successfully completed and found within the specifications....
Validation is one of the important steps in achieving and maintaining the quality of the final product. If each step of production process is validated we can assure that the final product is of the best quality. This paper presents an introduction and general overview on process validation of sterile liquid products. Main objective is to maintain the sterility of a product, assembled from sterile components Validation of aseptic processing should include a process simulation test using a nutrient medium (media fill). Validation of aseptic processes relies upon prospective, concurrent and retrospective validation as well as re-validation....
The purpose of the research investigation was to study prospective process validation of Enalapril Maleate 10 mg tablet dosage form. Quality cannot be adequately assured by in-process and finished inspections and testing but it should be built in to the manufacturing process. These processes should be controlled in order that the finished product meets all quality specifications. Therefore building of quality requires careful attention to a number of factors, such as the selection of materials, product and process design, control variables, in process control and finished product testing. The critical process parameters were identified with the help of process capability and evaluated by challenging its lower and upper release specifications. Three initial process validation batches of same size, method, equipment and validation criteria were taken. The critical parameter involved in sifting, dry mixing, preparation of granulating agent, wet mixing, wet milling, drying, sizing, lubrication & compression stages were identified and evaluated as per validation plan. The outcome indicated that this process validation data provides high degree of assurance that manufacturing process produces product meeting its predetermined specifications and quality attributes....
Validation is the one of the most important step in achieving and maintaining the quality of the final product. Validation is defined as the collection and evaluation of the data from process design stages through production which establishes scientific evidence that a process is capable of consistently delivering quality product. If each step of the production process is validated than one can assure the final product is of the best quality. Validation of individual step is called as process validation. The purpose of the research was to study Prospective process validation of Piroxicam Dispersible tablet 20mg. In this article three batches of Piroxicam Dispersible Tablets were taken. They have same size, quantity, equipment, method and validation criteria. The critical parameters involved in sifting, milling, blending, lubrication and compression were identified and evaluated as per Validation Master Plan. All batches fulfill the requirement of given criteria. The outcome states that this Process Validation gives a higher degree of quality assurance....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous estimation of bromhexine HCl (BHX) and phenylephrine HCl (PLE) in their combined pharmaceutical dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point and other being the λmax of one of the two components. BHX and PLE show an isoabsorptive point at 266 nm (λ1). The second wavelength used is 250 nm (λ2), which is the λmax of BHX in methanol. The linearity was obtained in the concentration range of 5-30 μg/ml for BHX and 10-60 μg/ml for PLE. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λmax of BHX. The developed method was successfully applied to pharmaceutical dosage form. The results were found to be within acceptance criteria according to ICH guideline....
To develop simple, accurate and precise reversed phase high performance liquid chromatography method for the estimation of ketorolac and fluorometholone in the combined ophthalmic dosage form available in the market for conjunctivitis and refractive eye Surgery. Both drugs ketorolac and fluorometholone are present in ratio of 5:1. The separation was made in a hyperchrome ODS-BP (250×4.6 mm, 5 µm C18) using a methanol: water (pH 4.0) (70:30, v/v) as mobile phase at 240 nm. The mobile-phase flow rate and the sample volume injected were 1.0 ml/min and 20 μl, respectively. Retention time of ketorolac and fluorometholone was found to be 5.17 and 3.66 minutes. The correlation coefficient of both drugs was found to be 0.999. Percent recoveries obtained for both the drugs were 99.73-99.89% and 100.430-100.581%. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. Over all % RSD was found to be less than 2%. The developed method can be used for routine analysis of ketorolac and fluorometholone in their pharmaceutical dosage forms....
Metronidazole (METRONIDAZOLE) and mupirocinpirocin (MUPIROCIN) both are anti-microbial type of antibiotics. This combination of drugs will be used to treat infections and are applied directly on the wounds. In RP-HPLC method, a mobile phase of phosphate buffer (pH 4): methanol (30:70 v/v) was used to resolve metronidazole and mupirocinpirocin from a mixture. Phenomex C18 column was used and flow rate was selected as 1 ml/min. Detection was carried out at 242 nm which is isosbestic point of metronidazole and mupirocinpirocin. The linearity range obtained for the RP-HPLC method were 5-15 μg/ml and 10 - 30 μg/ml with corresponding correlation coefficient of 0.999 and 0.999 for metronidazole and mupirocinpirocin respectively. First derivative spectrophotometry method that involves estimation of metronidazole at 330.0 nm and mupirocinpirocin at 232.0 nm. In this method linearity evaluated is 2.5 - 12.5 μg/ml for metronidazole and 5 - 25 μg/ml for mupirocinpirocin and correlation coefficients found 0.999 and 0.999 for both the drugs respectively. The method was found to be rapid, accurate and precise. This method was validated according to ICH guidelines....
A simple, specific, precise and accurate method development and validation of amiloride hydrochloride and torsemide tablet formulation by RP-HPLC was developed. The method employed BDS hypersil C18, 250 mm × 4.6 mm, 5µ (particle size), column as stationary phase. The mobile phase consisted of phosphate buffer and methanol (50:50 v/v) pH 4.0 adjusted by orthophosphoric acid, at a flow rate of 1 ml/min. Detection was carried out at wavelength 327 nm. The retention time of amiloride hydrochloride and torsemide were found to be 3.5 and 5.27 minutes respectively. Linearity was established by over the concentration range of 5 to 15 μg/ml for amiloride hydrochloride with correlation coefficients (r2) 0.997 and 10 to 30 μg/ml for torsemide with correlation coefficients (r2) 0.999. The percentage recovery obtained for amiloride hydrochloride and torsemide were 99.66% and 100% respectively. The method has been validated as per ICH guideline and successfully applied to estimation of amiloride hydrochloride and torsemide in tablet dosage form....
The present work describes a simple, rapid and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of clindamycin phosphate (CLINDA) and nicotinamide (NICO). The separation was achieved on a hypersil BDS C18 (250 mm X 4.6 mm i.d., 5 μm particle size) with an isocratic system of Phosphate buffer (pH-3.5): methanol in the ratio of 60:40 v/v. The mobile phase at a flow rate of 1.0 ml/min, injection volume 20 μl and wavelength of detection used was 210 nm. The retention time for nicotinamide and clindamycin phosphate were obtained as 4.053±0.11 min and 5.730±0.1 min, respectively. The linearity of the proposed method was investigated in the range of 5-15 µg/ml and 20-60 µg/ml for clindamycin phosphate and nicotinamide, respectively. Correlation coefficients were 0.998 and 0.999 for clindamycin phosphate and nicotinamide, respectively. The developed method was validated as per ICH guideline, for its accuracy, precision, LOD and LOQ and the results were found to be satisfactory, thus the method is specific, rapid and simple with good sensitivity for estimation of clindamycin phosphate and nicotinamide. These analytical methods are also applicable in ordinary laboratories. It can also be adopted for quality control tests for these drugs in cream formulation....
HPLC is described for determination of the % drug release and estimation of drug in capsule. The method employs a prinstone C8 column (250 x 4.6 mm, 5.0 μ) with an isocratic mixture of Acetonitrile:Water:TEA (600:400:1 v/v/v) pH- 4 adjusted with ortho-phosphoric acid at a flow rate of 1 ml/min and detection at 280 nm. Retention time of Nimesulide and Diclofenac Sodium was 7.6 min and 9.6 min respectively. Method shows linearity in the range of 20 μg/ml - 100 μg/ml for Nimesulide and 10 μg/ml - 50 μg/ml for Diclofenac Sodium with correlation coefficient 0.9993 and 0.9994 for Nimesulide & Diclofenac Sodium respectively. LOD was found to be 0.12 μg/mL and LOQ was found to be 0.37 μg/mL for Diclofenac Sodium and LOD was found to be 1.2 μg/mL and LOQ was found to be 3.6 μg/mL for Nimesulide....
A specific, accurate and simple RP-HPLC method for the simultaneous determination of Paracetamol and Ibuprofen has been developed and validated. The separation was carried out by using a mobile phase consisting of Acetonitrile:Water:Triethylamine (pH 3.5 adjusted by using Ortho phosphoric acid) in ratio of 60:40:0.1 (v/v/v). The column used was Princetons, C8 (250 mm x 4.6 mm i.d., 5 μm) with flow rate of 1 ml/min using UV detection at 220 nm. The retention times of Paracetamol and Ibuprofen were found to be 2.747 min and 10.428 min, respectively. Method shows linearity in the range of 6.5 μg/ml - 32.5 μg/ml for Paracetamol and 8 μg/ml - 40 μg/ml for Ibuprofen with correlation coefficient 0.9997 and 0.9995, respectively. The limit of quantification (LOQ) for Paracetamol and Ibuprofen were found to be 0.6992 μg/ml and 1.5218 μg/ml, respectively....
A simple RP-HPLC method has been developed and validated for simultaneous estimation of cefoperazone sodium and tazobactam sodium in parenteral preparation. The separation was carried out by a mobile phase consisting of phosphate buffer pH 4.0 adjusted with orthophosphoric acid and methanol (70:30). The column used was ODS hypersil C18, (5 μm, 250 mm × 4.6 mm) with flow rate of 1 ml / min using PDA detection at 223 nm. The described method was linear over a concentration range of 24-72 μg/ml and 3-9 μg/ml for the assay of cefoperazone sodium and tazobactam sodium respectively. The retention times of cefoperazone sodium and tazobactam sodium were found to be 3.3 and 5.1 min respectively. Results of analysis were validated statistically and by recovery studies. The limit of quantification (LOQ) for cefoperazone sodium and tazobactam sodium were found to be 5.38 and 0.84 μg/ml respectively. The results of the study showed that this RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of cefoperazone sodium and tazobactam sodium bulk drug and in its pharmaceutical dosage form....
An isocratic reversed phase HPLC method has been developed for the simultaneous determination of hydrocortisone acetate and miconazole nitrate on a HiQ-silC18HS (250 x 4.6 mm) column using a mobile phase consisting of acetonitrile: 0.1 M ammonium acetate (80:20, v/v) at a flow rate of 1 ml/min and the detection was carried out at 225 nm. The retention times of Hydrocortisone Acetate and Miconazole Nitrate were 4.055 (±0.16) min and 13.14 (±0.31) min respectively. The method was validated with respect to specificity, linearity, accuracy, precision, ruggedness and robustness. This method is simple, precise and sensitive and is applicable for simultaneous quantification of hydrocortisone acetate and miconazole nitrate in a cream formulation....
A rapid, precise, specific, accurate and robust simple RP-HPLC method for the simultaneous determination of rabeprazole sodium and domperidone has been developed and validated. The separation was carried out by using a mobile phase consisting of modified phosphate buffer pH 7.4 and acetonitrile in the ratio of 65:35% v/v. The column used was thermoscientific hypersil BDS, C18 (250 mm x 4.6 mm i.d., 5 μm) with flow rate of 1.5 ml/min using UV detection at 290 nm. The retention times of rabeprazole sodium and domperidone were found to be 3.8 min and 7.1 min, respectively. Method shows linearity in the range of 10 μg/ml-30 μg/ml for rabeprazole sodium and 5 μg/ml-15 μg/ml for domperidone with correlation coefficient of 0.9999 for both. The limit of detection (LOD) and limit of quantification (LOQ) for rabeprazole sodium and domperidone were found to be 0.08 μg/ml and 0.24 μg/ml and 0.06 μg/ml and 0.18 μg/ml respectively. The % recovery for rabeprazole sodium and domperidone were found within the range of 98.18% - 99.75% and 98.16% - 99.88% respectively. For both rabeprazole sodium and domperidone, the intra-day and inter-day precision, expressed as the relative standard deviation (RSD), of replicates is <2%. The developed RP-HPLC method was innovation, suitable for detecting both Rabeprazole sodium and Domperidone in soft gelatin capsules....
The current method describes the simultaneous equation spectrophotometric method for the estimation of diloxanide furoate and ornidazole from their combined tablet dosage form by using Methanol as a solvent. The two wavelength 259 nm for diloxanide furoate and 312 nm for ornidazole were used for the estimation of diloxanide furoate and ornidazole. The method follows beer’s linearity in the range of 2-10 µg/ml for diloxanide furoate and 2-16 µg/ml for ornidazole. The % recovery was found to be 99.64–100.33 % for diloxanide furoate and 99 - 99.91% for ornidazole. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of diloxanide furoate and ornidazole from their combined Tablet dosage form....
A simple, sensitive, precise and economical UV- spectrophotometric method has been developed for the simultaneous estimation of Naphazoline HCl and Phenylephrine HCl in formulation. Method is first order derivative spectrophotometric method and involved in the estimation of Naphazoline HCl and Phenylephrine HCl in water as solvent using the first-order derivative zero crossing point technique at 245 nm as ZCP of PHE and 283 nm as ZCP of NAPH. Calibration curve was prepared by plotting the derivative absorbance versus concentration. Linearity was obtained in the concentration range of 5-25 mcg/ml for NAPH and 12-60 mcg/ml for PHE. This method was successfully applied to pharmaceutical formulation because no interferences from formulation excipients were found. The suitability of this method for the quantitative determination of both drugs was proved by validation. The proposed method was found to be useful for the routine quality control application in eye drops....
A novel, safe, accurate and sensitive spectrophotometric method was developed using hydrotropes mixture (10 gm niacinamide in 25 ml phenol) as hydrotropic solubilizing agent for the determination of clofazimine. There were more than 70 fold enhancements in the solubility of clofazimine increases in hydrotropes mixture as compared to solubilities in distilled water. Clofazimine shows maximum absorbance at 499 nm. Hydrotropes mixture did not show any absorbance above 300 nm and thus no interferences were seen. Clofazimine obeyed beer’s law in the concentration range of 5-25 μg/ml (r2= 0.9998) in hydrotropes mixture with means recovery 99.76 %. Proposed method is new, simple, economic, safe, rapid, accurate and reproducible. The developed methods were validated according to ICH guideline Q2 (R1) and values of accuracy, precision and other statistical analysis were found to be in good accordance with prescribed values....
The aim of this present work was to develop and validate a simple, rapid, accurate RP-HPLC Stability Indicating Assay Method for the simultaneous estimation of Metformin Hydrochloride (MET) and Gliclazide (GLI) pharmaceutical dosage form. The chromatographic separation was carried out in an isocratic mode using an Kromasil C18 column (250 mm × 4.6 mm, 5 μm particle size) with a mobile phase of mixed phosphate buffer pH 3:acetonitrile(45:55% v/v) of injection volume 20 μL and the eluents were monitored at 230 nm. The retention times of MET and GLI were 2.4 and 9.7 mins respectively. The method was found to be linear over the concentration range of 125-375 μg/mL for MET and 20-60 μg/mL for GLI with a correlation coefficient of 0.999. The proposed RP-HPLC method was validated according to ICH guidelines and was successfully employed for routine quality control analysis in combined dosage forms....
A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of Dexketoprofen trometamol and Thiocolchicoside from tablet dosage form using a Hypersil BDS, C18 column (5�µ, 4.5mm x 250 mm) column and mobile phase composed of 0.05m Potassium Dihydrogen Phosphate:acetonitrile (75:25 v/v) pH 6.0 adjusted with Triethylamine, at flow rate of 1 ml/min. The retention time of Dexketoprofen Trometamol and Thiocolchicoside were found to be 8.732 and 3.256 min respectively. Linearity was established for both drugs in the concentration range of 50-150 �µg/ml. The percentage recoveries of Dexketoprofen Trometamol and Thiocolchicoside were found to be in the range of 98.12%-101.82% and 98.15%-101.8% respectively. Detection was carried out at wavelength 260nm using photodiode array detector. The separation was carried out at 30C temperature. Both the drugs were subjected to acid, alkali, neutral hydrolysis, oxidation, dry heat, and UV degradation. The degradation products of Dexketoprofen trometamol and Thiocolchicoside in uv ligt and alkali were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of Dexketoprofen trometamol and Thiocolchicoside in tablet formulations....
Aim of the present work was to develop a stability indicating high performance liquid chromatographic (HPLC) method for the analysis of alfuzosin HCl and dutasteride. Chromatographic separation achieved isocratically on kromasil C18 column (150 mm x 4.6 mm, 5 μm particle size) utilizing a mobile phase of acetonitrile: phosphate buffer pH 7.0 in the ratio of 65:35 v/v at a flow rate of 1 ml/min and injection volume of 20 µl using UV detection at 242 nm. The retention time of ALFU and DUTA was 2.67, 9.97 min respectively. Both ALFU and DUTA were degraded in acidic, alkali and oxidation condition while only ALFU degraded in photolytic, DUTA in neutral condition. Both the drugs are stable in thermal condition. The method was found linear over concentration range of 20-140 μg/ml of ALFU and 1-7 μg/ml of DUTA with good linearity response of 0.999 and 0.998 respectively. The developed method was validated as per ICH guide line....
A new simple, rapid, accurate, sensitive and precise spectrophotometric method in colorimetric region has been developed for determination of ezetimibe in bulk and pharmaceutical dosage form by MBTH reagent. The principle involved in this method is iron catalyzed coupling reaction of MBTH with the drug in the presence of Fecl3 to form green colored compound which exhibited maximum absorbance at 621 nm in methanol. Beer's law was found to be obeyed in the concentration range 20-100 µg/ml. Regression equation was found to be 0.009x and coefficient of correlation was 0.9922. The developed method was validated respect to stability, linearity, precision, accuracy. The proposed method is useful for the routine estimation of ezetimibe in bulk and pharmaceutical dosage form....
Two chemometric methods, Classical least square and Inverse least square were applied for simultaneous estimation of gatifloxacin and ketorolac tromethamine in their ophthalmic dosage form. A considerable spectral overlap (90.3%) was observed in the range of 281 nm-329 nm. Beer’s law was obeyed for both drugs in the concentration ranges of 6-18 µg/ml for both gatifloxacin and ketorolac tromethamine. 25 mixtures were prepared and analysed at 25 wavelength points between 281-329 nm with the interval of 2 nm (Δλ = 2 nm). A validation set design of the concentration data corresponding to the gatifloxacin and ketorolac tromethamine mixtures was organized statistically to maximize the information content from the spectra and to minimize the error of multivariate calibrations. Good percentage recoveries and proper statistical data obtained proved the suitability and efficiency of the proposed procedures for routine analysis. The numerical calculations were performed with the MATLAB® R2010a software and Microsoft excel....
An accurate, precise and relatively simple High Performance Thin Layer Chromatographic Method was developed for the simultaneous estimation of Brimonidine Tartarte (BRT) and Timolol Maleate (TM) in pure form as well as in pharmaceutical formulation. Chromatographic Separation was carried out on TLC aluminium sheet pre-coated with silica gel G 60 F254 using Hexane: Iso-propyl alcohol : ammonia (5:2:0.5 v/v/v) as mobile phase. Detection was carried out densitometrically at 281 nm. The Rf value of BRT and TM was found to be 0.36 and 0.65 respectively. The method was validated for linearity, accuracy, precision, LOD and LOQ. The linearity range of Brimonidine Tartrate was to be between 200-600 ng/spot and that of Timolol Maleate was found to be 500-1500 ng/spot with regression coefficient values of 0.996 and 0.995 for Brimonidine Tartrate and Timolol Maleate respectively. The accuracy of the method was assessed by performing recovery studies at 80%, 100% and 120%. The % recovery for Brimonidine Tartrate was found to be 100.37-101.3% and that of Timolol Maleate was found to be 99.93-100.44%. The LOD and LOQ values for Brimonidine Tartrate were found to be 21.16 and 64.11 ng/spot respectively and Timolol Maleate were found to be 101.2 and 306.63 ng/spot respectively. Precision of the method was assessed by performing repeatability, intra-day and inter-day precision studies. Thus, the developed method was found to be accurate, precise and relatively simple for the simultaneous estimation of Brimonidine Tartrate and Timolol Maleate in pure form as well as in marketed formulation....
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