Current Issue : October-December Volume : 2012 Issue Number : 4 Articles : 75 Articles
As a critical part of the system, the quality of pharmaceuticals has been concerning since long time by experts. For that pharmacopoeia is an aspect to be concerned. Here brief information of the IP, BP and USP-NF has been mentioned in that what is the need of pharmacopoeia, missions, vision & its objectives. As well as the details of monograph, preface and date of publication with its revision has been reviewed. It also includes available volume of particular pharmacopoeia and unique characteristics of that pharmacopoeia and difference between them. It also gives details about the formulation body of pharmacopoeia....
The qualitative aspects of infrared spectroscopy are one of the most powerful attributes of this diverse and versatile analytical technique. Over the years, much has been published in terms of the fundamental absorption frequencies which are the key to unlocking the structure–spectral relationships of associated molecular vibrations. Applying this knowledge at the practical routine level tends to be a mixture of art and science. While many purists will argue against this statement, this author believes that it is not possible to teach a person to become proficient as an interpretive spectroscopist by merely presenting the known relationships between structure and the observed spectra. Instead, the practical approach, which has been adopted in this text, is to help the reader appreciate the visual aspects of the spectroscopy and how to interpret these relative to the structure and chemistry of the sample. This is achieved by recognizing characteristic shape and pattern within the spectrum, and by applying the information obtained from published group frequency data, along with other chemical and physical data from the sample. Included in the text is a discussion of the interrelationships that exist between the practical side of acquiring the spectrum, the chemistry and physics of the sample under study, the physical interactions of the sample with its environment, and the impact of the structure on the spectrum. In essence, the interpretation of infrared spectra is much more than simply assigning group frequencies. The spectrum is rich in information, and this article is intended to help the reader to extract the maximum using the knowledge available for the sample and the acquired spectral data. One important factor to bear in mind is that a successful interpretation is based not only on the presence of particular bands within the spectrum, but also the absence of other important bands....
Quality management in the drug industry: philosophy and essential elements, outlines the general concepts of quality assurance as well as the principal components or subsystems of GMP, which are joint responsibilities of top management and of production and quality control management. These include hygiene, validation, personnel, premises, equipment, materials and documentation. “Good practices in production and quality control”, provides guidance on actions to be taken separately by production and by quality control personnel for the implementation of the general principles of quality assurance. This document (Guide) is intended to provide guidance regarding good manufacturing practice (GMP) for the manufacturing of active pharmaceutical ingredients (APIs) under an appropriate system for managing quality. It is also intended to help ensure that APIs meet the requirements for quality and purity that they purport or are represented to possess....
A simple, selective, rapid, precise and economical reverse phase high-pressure liquid chromatographic method has been developed for the simultaneous estimation of S (-) Amlodipine besylate and Nebivolol Hydrochloride for tablet formulations. The chromatographic separation was achieved on Hypercil column (250 × 4.6 mm, 5μ particle size) in isocratic mode with mobile phase consisting of Potassium dihydrogen phosphate buffer : acetonitrile : 0.1% triethylamine (60:40 v/v). The flow rate was 1ml / min and effluent was monitored at 269 nm PDA detection. The retention times of S (-) Amlodipine besylate and Nebivolol Hydrochloride were 7.55 ± 0.05 and 8.75 ± 0.05 minutes respectively. The linearity of the method was studied over the concentration range of 80-120 μg/ml for S (-) Amlodipine besylate and 80-120 μg/ml for Nebivolol Hydrochloride The limit of detection for S (-) Amlodipine besylate and Nebivolol Hydrochloride were found as 0.86μg/ml and 2.13μg/ml and and the limit of quantification for S (-) Amlodipine besylate and Nebivolol Hydrochloride were found as 2.6μg/ml and 6.4μg/ml respectively. The proposed method was applied for the quantitative determination of S (-) Amlodipine besylate and Nebivolol Hydrochloride in commercial combination formulations....
Three simple, accurate and precise spectrophotometric methods have been developed for simultaneous estimation of Rosuvastatin calcium (ROSU) and Aspirin (ASP) from Capsule dosage form. Methanol: Phosphate buffer (80:20), 0.02M, pH 4.0, was used as solvent. First method, Simultaneous equation method, involves the measurement of absorbances at two wavelengths 242 nm (?max of ROSU) and 275 nm (?max of ASP), Second method i.e. Absorption ratio method was carried out at 242 nm (?max of ROSU) and 258 nm (isoabsorptive point of ROSU and ASP). Third method is Area under curve method, area under curve in the range of 237-247 nm (for ROSU) and 270-280 nm (for ASP) were selected for the analysis. The accuracy and precision of the methods were determined and validated. All the methods showed good reproducibility and recovery with % RSD less than 2. The proposed methods were found to be rapid, specific, precise, accurate and can be successfully applied for the routine analysis of ROSU and ASP in bulk and combined dosage form....
A new, simple, precise and accurate method for the estimation of methylcobalamin in bulk and multicomponent pharmaceutical dosage form has been developed. A methanol was chosen as the solvent system. The λmax was found to be 360.0nm. The responses were linear in the range of 2-10μg/ml. The regression equation of the calibration graph and correlation coefficient were found to be y = 0.015x + 0.001 and 0.999 respectively. Validation of the method was done in order to demonstrate accuracy, precision, interday, intraday and assay, of the proposed method. The %RSD values for both intraday and interday precision were less than 2%. The recovery of the drug from the sample was ranged between 98% and 102.0%. multicomponent tablets containing 500mcg of methylcobalamin were analyzed by the proposed method and the results were well within the claimed limits....
Two methods are described for the simultaneous determination of Moxifloxacin HCl (MOX) and Bromfenac Sodium (BROM) in binary mixture. The first method was based on HPTLC separation of the two drugs followed by densitometric measurements of their spots at 260nm. The separation was carried out on Merck HPTLC aluminum sheets of silica gel 60F254 using Methylene chloride: Acetonitrile: Methanol: Ammonia (2.5:2.5:2.0:1.0 v/v/v/v) as mobile phase. The linear regression analysis data was used for the regression line in the range of 108–756ng/spot and 600–4200ng/spot for BROM and MOX, respectively. The second method was based on HPLC separation of the two drugs on the reversed phase ACE column [C18(5μm,150mm×4.6mm,i.d.)] at ambient temperature using a mobile phase consisting of 10mM phosphate buffer pH 7.0 and Acetonitrile (72:28,v/v) and flow rate was 1.0ml/min. Quantitation was achieved with UV detection at 265nm based on peak area with linear calibration curves at concentration ranges 1.8–18μg/ml and 10–100μg/ml for BROM and MOX, respectively. Both methods were validated in terms of precision, robustness, recovery and limits of detection and quantitation.The analysis of variance (ANOVA) and Student’s t-test were applied to correlate the results of BROM and MOX determination in dosage form by means of HPTLC and HPLC method....
Automated analysis is defined as the use of combinations of mechanical and instrumental devices to replace, refine, extend or supplement human effort and facilities in the performance of a given process, in which at least one major operation is controlled without human intervention, by a feedback mechanism. Due to the ongoing demand for speed in industrial chemical analysis, parallel automation processes are beginning to replace serial automation processes, especially in those areas where high numbers of assays or samples are expected. For in situ or on-line situations where sparse strategic sampling is the norm, serial automation will likely play a continued role. Expensive robotic arms, while powerful and flexible do not directly lend themselves to parallel automation systems unless the effort is made to combine them with specialized multichannel hardware. Such hybrid systems are powerful and useful but are extremely complicated to implement and maintain. Hybrid system a combination of both now a day change sinario of analytical field by rapid and multiple analysis of the analytes....
Four different simple, accurate, rapid, economical spectroscopic methods namely Zero order, First derivative, Area Under Curve and Three wavelength spectroscopy have been developed and validated for estimation of Ondansetron in tablet dosage form using methanol as a solvent according to ICH Guidelines Q2R1. Absorbance of each solution was measured at 303.80 nm for zero order spectrophotometry. First derivative spectra are obtained by transformations at Δλ of 4 nm and scaling factor 10 and absorbance measured at 240.20 nm. Peak area is measured between 256.40-278.20 nm for AUC method. For three wavelength spectroscopy, absorbance was recorded at three wavelengths λ1= 255.60 nm, λ2 = 266.60 nm, λ3 = 277.60 nm. Ondansetron show linearity over the range of 4-20 μg/ml for all developed methods. Statistical comparisons by one way ANOVA shows all methods have equal applicability for estimation of Ondansetron in tablet dosage forms....
Present work describes simple, accurate, precise and reproducible RP-HPLC method for estimation of tadalafil from the pharmaceutical formulations using RP-C18. Acetonitrile: water was used as mobile phase at a flow rate of 1.2ml/min in the ratio of 50:50 and the detection wavelength was 284nm the accuracy of the method was found to be 98-101% and RSD was found to be less than 2% indicating high degree of accuracy, precision for the proposed HPLC method....
The present work describes a validated reverse phase high performance liquid chromatographic method for estimation of Tenoxicam in pharmaceutical dosage form. Chromatography was performed on a Varian C18 column (250 mm x 4.6 mm i.d., 5 µm particle size), column with mobile phase containing methanol and acetate buffer in the ratio (40:60, v/v) and pH of acetate buffer adjusted to 4.6 with glacial acid .The flow rate was 1.2 ml/min and the eluent was monitored at 369 nm. The selected chromatographic conditions were found to effectively separate Tenoxicam (RT- 4.170 min). Linearity for Tenoxicam was found in the range of 4-20μg/ml. The value obtained of LOD was 0.146µg/ml and LOQ was 0.444 µg/ml for Tenoxicam. The proposed method was found to be fast, accurate, precise, reproducible and rugged and can be used for analysis of Tenoxicam in single pharmaceutical formulations....
Lacosamide is a novel antiepileptic drug and is a member of a family of functionalized amino acids, more specifically, analogues of the endogenous amino acid and NMDA-receptor modulator D-serine from BCS Class-I substance (High solubility, High permeability). As per our knowledge, no dissolution method is reported for estimation of lacosamide in tablet dosage form. So, our aim is to develop and validate a simple, accurate, precise, economic dissolution method for estimation of Lacosamide using spectroscopic method. Based on solubility study 500 ml of 0.1 N HCl and distilled water as a dissolution medium was tried for method development using paddle type apparatus with stirring speed of 50 and 75 rpm at a physiological temperature (37±0.5ºC). Sampling was carried out up to 60 min at a different time interval. Optimal conditions to carry out the dissolution were 500 ml of 0.1 N HCl as dissolution medium using paddle at 75 rpm stirring speed with detection by UV spectroscopy at 257.20 nm which was able to give 99.37% drug release. Linearity of developed method was found in the range of 50-150 µg/ml with 0.9998 correlation co-efficient. Limit of detection and Limit of quantification of developed method was 1.5464 and 4.8663 respectively. The Percentage recovery for the developed method was found in the range of 100.33-101.11, 99.53-100.00 and 100.24-100.81 % for Lacasa 50, Lacosam 50 and Lacosam 100 respectively. Analytical method validation was found to be within the acceptance criteria of the guidelines of ICH Q2 R1, FDA and FIP. So, developed method is new advancement for routine quality control analysis for pharmaceutical industry....
A simple, fast, precise, accurate and specific HPTLC method was developed and validated for the simultaneous estimation of Montelukast sodium (MTKT) and Desloratadine (DLOR) from their combined tablet dosage form. Chromatographic separation was achieved on aluminum plates precoated with silica gel G60F254, the solvent system consisted of Methanol: chloroform: ammonia 2.5:7.5:0.1 (v/v/v) as mobile phase. Detection was performed densitometrically at 282 nm. The RF of Montelukast sodium and Desloratadine were 0.64 ± 0.01 and 0.18 ± 0.01 respectively. Linearity was observed in the concentration range of 800-2400 ng/spot for Montelukast sodium and 400-1200 ng/spot for Desloratadine. Percent recoveries obtained for both the drugs were 99.48 ± 0.66% – 101.20 ± 0.35% and 99.15 ± 0.70 – 101.16 ± 0.38%, respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The developed method can be used for the routine analysis of Montelukast sodium and Desloratadine from their combined tablet dosage form....
A simple, precise, accurate, rapid and economical High Performance Thin Layer chromatographic method has been developed and validated for the estimation of Rosuvastatin calcium (ROSU) and Aspirin (ASP) simultaneously in combined capsule dosage forms. The mobile phase used was a mixture of Methanol: Buffer, 0.02M (80:20 v/v, pH 4.0). The detection was carried out at 258 nm. The method was validated in terms of linearity, accuracy, precision, LOD, LOQ, range and robustness. The calibration curve was found to be linear between 8-12 µg/ml for ROSU and 60-90 µg/ml for ASP. The limit of detection and the limit of quantification for ROSU were found to be 0.080µg/ml and 0.244µg/ml respectively, and for ASP, 0.024µg/ml and 0.074µg/ml respectively. The proposed method can be successfully used to determine the drug content of marketed formulation....
A simple, sensitive, rapid, accurate and precise spectrophotometric area under curve method has been developed for the estimation of Cefixime Trihydrate in bulk and pharmaceutical dosage forms. Cefixime Trihydrate shows maximum absorbance at 288 nm. Spectrophotometrically, Cefixime Trihydrate was determined by measuring the AUC at 288 nm with phosphate buffer (pH-6.5) as a solvent. Beer’s law was obeyed in the concentration range of 4-18 μg/ml with coefficient of correlation 0.999. The developed method was applied directly to the analysis of the tablet preparations. R.S.D was found to be 0.00657. The result 100.16-100.54% for recovery studies by derivative method indicate that proposed method is accurate and precise for the determination of Cefixime Trihydrate in tablets. The method was completely validated and proven to be rugged. The excipients did not interfere in the analysis. The results showed that this method can be used for rapid determination of Cefixime Trihydrate in pharmaceutical tablet with precision, accuracy and specificity....
This study describes the development and validation for the simultaneous estimation of Rosuvastatin calcium (RST) and Aspirin (ASP) by the first-order derivative UV spectroscopy method. The quantification was achieved by the first-order derivative spectroscopy method at 255.20 nm 243.40 and nm over the concentration range of 1-12 µg/ml for estimation of Rosuvastatin calcium (r2=0.9999)and 7.5-90 µg/ml Aspirin (r2=0.9997) in a combined tablet formulation. Procedure does not require prior separation of components from the sample. LOD values for RST and ASP are found to be 0.11 μg/ml and 2.225 μg/ml, respectively. LOQ values for RST and ASP are found to be 0.35 μg/ml and 6.744 μg/ml respectively. The results of analysis have been validated statistically and recovery studies carried out in the range 80-120% to confirm the accuracy of the proposed method. The relative standard deviation was found to be <2.0%. The present result shows that the proposed method can be successfully used for simultaneous determination of the drug content in marketed formulations....
Zero order, First order derivative and Dual wavelength Spectrophotometric methods have been developed for simultaneous estimation of two component drug mixture of Ondansetron Hydrochloride and Pantoprazole Sodium in pure and bulk form. All these methods utilize methanol as a solvent. In Zero order spectrophotometry, absorbance of each solution of Ondansetron and Pantoprazole was measured at 303.80 nm and 288.80 nm respectively. In First order derivative spectroscopy method, absorbance of Pantoprazole Sodium was measured at 256.20 nm (Zero Crossing Point of Ondansetron Hydrochloride) and absorbance of Ondansetron Hydrochloride was measured at 289 nm (Zero Crossing Point of Pantoprazole Sodium). The drugs obeyed the Beer’s law in the concentration range of 10-60 µg/ml (r2 = 0.9994) for Pantoprazole Sodium and 1-6 µg/ml (r2 = 0.9998) for Ondansetron Hydrochloride. In Dual wavelength method, the determination of Ondansetron was carried out at the absorbance difference between 282.40 nm and 295.80 nm and of Pantoprazole at the absorbance difference between 296.20 nm and 308.80 nm. The results of analysis have been validated statistically. These methods were found to be simple, rapid and accurate, hence can be used for routine simultaneous estimation of these drugs in formulations. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Tramadol hydrochloride (TRA) and Diclofenac Sodium (DIC) by employing dual wavelength by using methanol as solvent. The two wavelengths for TRA were found to be 264nm and 281.51nm in and for DIC 270nm and 296.36nm in where respective drug gave same absorbance. The linearity was established over the concentration range of 2 - 16 μg/ml in and 5 - 25 μg/ml in for TRA and DIC respectively with correlation coefficient (r2) 0.9916 and 0.9972. The mean % recoveries were found to be in the range of 99.2 % - 99.73 and 99.33 – 99.64 % for TRA and DIC, respectively. The proposed method has been validated as per ICH guidelines and was successfully applied to the estimation of TRA and DIC in their combined Tablet dosage form....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of metoprolol succinate and telmisartan in combined tablet dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra was obtained in methanol and the determinations were made at 219.2nm (ZCP of telmisartan) for metoprolol succinate and 238nm (ZCP of metoprolol succinate) for telmisartan. The linearity was obtained in the concentration range of 4-14μg/ml for metoprolol succinate and 1-6 μg/ml for telmisartan. The mean recovery was 99.6 ± 0.26and 99.43 ± 0.32 for metoprolol succinate and telmisartan, respectively. The method was found to be simple, sensitive, accurate and precise and was applicable for the simultaneous determination of metoprolol succinate and telmisartan in pharmaceutical tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of Rosuvastatin calcium and telmisartan in combined tablet dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra was obtained in methanol and the determinations were made at 248nm (ZCP of telmisartan) for rosuvastatin calcium and 296.7nm (ZCP of rosuvastatin calcium) for telmisartan. The linearity was obtained in the concentration range of 2-18μg/ml for rosuvastatin calcium and 1-6 μg/ml for telmisartan. The mean recovery was 99.85± 0.27and 99.73 ± 0.44 for rosuvastatin calcium and telmisartan, respectively. The method was found to be simple, sensitive, accurate and precise and was applicable for the simultaneous determination of rosuvastatin calcium and telmisartan in pharmaceutical tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
Lafutidine is chemically 2-[(2-furylmethyl) sulfinyl]-N-((2Z)-4-{[4- (piperidin-1- ylmethyl) pyridin-2-yl] oxy}but-2-en-1- yl) acetamide1 is used in the treatment of ulcer. Antisecretory drugs are used in the treatment and prophylaxis of peptic ulcer disease some are also employed in other disorders associated with gastric hyperacidity such as gastro-oesophageal reflux disease and dyspepsia. As Lafutidine is not official in any pharmacopoeia, no official analytical method is there for estimation of this drug. Literature survey reveals few analytical methods like liquid chromatography, stability indicating HPLC, colorimetric and biological assay are reported; there was no mention of a method based on spectrophotometric estimation. The present work describes a validated first order derivative Spectrophotometric method measurement for estimation of Lafutidine. The present work describes a validated first derivative Spectrophotometric method for estimation of Lafutidine in bulk and in tablet formulation. The solvent used was methanol for parent dilution and then sodium hydroxide for further dilution. Absorbance a minimum in first order derivative spectra was found at 284 nm, the drug followed a linear relationship in the range of 10-35μg/ml while the correlation coefficient was found 0.996. The recovery was 99.89% and the coefficient of variance for intraday and interday was found to be less than 5%, LOD and LOQ for this method was found 10 μg/ml and 35 μg/ml respectively. The proposed UV- Visible spectrophotometric method is a simple, specific, rapid, accurate, economic and found suitable for day to day analysis of lafutidine in bulk and its formulation....
A Simple, Precise, accurate, sensitive and robust method was developed for simultaneous estimation of Levosulpiride (LS) and Rabeprazole sodium (RS) from their combined dosage form using reverse phase High Performance Liquid chromatography (RP-HPLC) equipped with UV-visible detector. The developed method was validated as per ICH Q2A (R1) guidelines. The linearity range for LS and RS was found to be 30-150 µg/ml and 8-40 µg/ml, respectively. The recovery studies were performed at three different levels and the average results were found to be in the range of 99.14-100.64 % for LS and 99.47-100.46% for RS. The developed method was found to be precise when subjected to inter day and intraday precision studies. The robustness of the developed method was established by making deliberate changes in the critical parameters. The method was successfully applied for the estimation of LS and RS from their tablet dosage form. The developed RP-HPLC method can be successfully applied for the quality control and routine analysis of LS and RS from their combined formulations....
A simple, precise, and accurate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of Ofloxacin (OFL) and Cefpodoxime Proxetil (CPD) in their combined tablet dosage form has been developed and validated. Chromatographic separation was carried out on silica gel 60 GF254 HPTLC plates with Ethanol-Ethyl Acetate-Water-Triethylamine (5:3.2:1.8:0.15 v/v/v/v) as mobile phase. Densitometric quantitation was performed at 290 nm. Well-resolved bands were obtained with Rf values 0.24 and 0.61 for Ofloxacin and Cefpodoxime Proxetil respectively. The method was validated for precision, accuracy and specificity. The calibration curve was found to be linear in the concentration range of 200-1000 ng/band for OFL and CPD respectively. Correlation co-efficient is 0.9997 and 0.9990 for OFL and CPD respectively. The method is selective and specific, with potential application in pharmaceutical analysis of these drugs in combined tablet dosage form....
Two Simple, precise and economical methods have been developed and validated for the quantitative estimation of Ritonavir in bulk and pharmaceutical dosage forms. Method A includes analysis of Ritonavir by non aqueous titration using glacial acetic acid and per chloric acid. Method B includes estimation ritonavir by 0.1 N HCl at λ max of 243.5 with linearity range of 10-50 μg/mL. The developed method was validated according to ICH guidelines and was found to be accurate and precise. The proposed method can be successfully applied for the estimation of Ritonavir in bulk and pharmaceutical dosage forms. Results of the analysis were validated statistically and by recovery studies....
A simple high-performance liquid chromatography and ultraviolet spectrophotometric methods were developed and validated for the estimation of alprazolam and melatonion simultaneously in combined pharmaceutical solid dosage form. The wavelength fixed for Q-analysis measurement the two wavelengths fixed are 221.0 nm and 268.0 nm. The linearity obtained for alprazolam in the range of 2-10 μg/ml and 10-50 μg/ml for melatonin by spectrophotometric method with r square value greater than 0.999. The alprazolam and melatonin were analyzed by HPLC using reverse phase C18 column (150 x 4.6 mm i.d., 5 μm particle size), by isocratic mobile phase consisted of acetonitrile and water (80:20 v/v), at a flow rate of 0.8 ml/min in the detection wavelength of 223 nm. The linearity and range of alprazolam are 0.5-2.5 μg/ml and 3-15 μg/ml for melatonin by HPLC method with r square value greater than 0.998. Accuracy of all methods was determined by recovery studies and showed % recovery between 99 to 101%. Intraday and interday precision was checked for all methods and mean %RSD was found to be less than 2 for all the methods. The methods were successfully applied for estimation of alprazolam and malatonin in marketed formulation....
A simple, accurate, rapid, sensitive and precise RP-HPLC method has been developed for estimation of Tapentadol hydrochloride in tablet dosage form using PDA detector. A Reverse phase Develosil ODSUG c18 column (150mm × 4.6 mm I.D., × 5µ particle size) with the Mobile phase consisting of Acetonitrile and Triethyl amine buffer 40:60(v/v) [PH 3±0.02 adjusted with orthophosphoric acid] was used. The Flow rate was 1.00 ml/min and the effluents were monitored at 215nm, and the Injection volume was 10µl. The separation was performed at ambient temperature. Retention time of Tapentadol hydrochloride was found to be 5.3 minutes respectively. The Linearity of the method was found to be 50-150µg/ml. The Correlation co-efficient of Tapentadol hydrochloride was found to be 0.9997. The %Recoveries of Tapentadol hydrochloride were found to be 99.3%. The system suitability parameters such as Theoretical plates and Tailing factor were found to be 2835, 1.563. Hence the proposed method was successfully applied for routine quality control analysis of Tapentadol hydrochloride in tablet dosage form. This method was validated according to ICH guidelines....
A simple, precise, accurate, reproducible RP-HPLC method was developed and validated for the simultaneous estimation of Clonazepam and Propranolol hydrochloride in bulk and in pharmaceutical dosage forms. Chromatographic separation was carried out on a Thermo-hypersil C8 column (250mm×4.6mm i.d,5µm) utilizing a mobile phase consisting of acetonitrile and 0.01M ammonium phosphate buffer (pH adjusted to 3.0 with ortho phosphoric acid) in the ratio of 60:40 v/v at a flow rate of 1ml/min with UV detection at 238nm. The retention times of Clonazepam and Propranolol hydrochloride were 3.362 min. and 2.524 min. respectively. The developed method was validated in terms of accuracy, precision, linearity, specificity, limit of detection and limit of quantification. The linear range was found to be 0.5-3.0µg/ml and 20-120µg/ml for Clonazepam and Propranolol hydrochloride respectively. The proposed method can be used for estimation of these drugs in combined dosage forms....
A simple, rapid, accurate, specific and sensitive reverse phase liquid chromatographic method (RP-HPLC) was developed and validated for the simultaneous estimation of Rabeprazole and Cinitapride in combined dosage form. The method was standardized using a Sunfire C18 column (250mm×4.6mm ID; Particle size 5μm) and the mobile phase consisted of acetonitrile: mixed phosphate buffer at 50:50%v/v. The eluents were monitored at 277nm and at 1ml/min flow rate. The retention time was found to be 3.966min for Rabeprazole and 5.898min for Cinitapride. The developed method was validated in terms of linearity, accuracy, precision, specificity, limit of detection and limit of quantification, in accordance with the ICH guidelines3. Linearity was obtained with correlation coefficient value r2 = 0.999 for Rabeprazole and r2 = 1 for Cinitapride. The proposed method can be used for the estimation of these drugs in combined dosage form....
A Simple, accurate, rapid, sensitive and precise RP-HPLC method has been developed for estimation of Hydrochlorothiazide and Metoprolol Succinate in tablet dosage form using PDA detector. A Reverse phase Thermo Hypersil ODS c18 column (250mm × 4.6 mm I.D.,× 3µ particle size) with mobile phase consisting of Acetonitrile and Triethylamine buffer 100:900(v/v) [Ph 3±0.02 adjusted with orthophosphoric acid] was used. The flow rate was 1.5ml/min and the effluents were monitored at 238nm, and the injection volume was 10µl. The separation was performed at ambient temperature. Retention time of Hydrochlorothiazide and Metoprolol Succinate was found to be 1.9 and 3.8 minutes respectively. The linearity of the methods was found to be 50-150µg/ml for Hydrochlorothiazide and 50-150µg/ml for Metoprolol Succinate. The correlation co-efficient of Hydrochlorothiazide was found to be 0.9996 and the correlation co-efficient of Metoprolol Succinate was found to be 0.9998. The % Recoveries of Hydrochlorothiazide and Metoprolol Succinate were found to be between 100-102%. The system suitability parameters such as Theoretical plates and Tailing factor were found to be 3250, 1.4 and 4742, 1.1 respectively for Hydrochlorothiazide and Metoprolol Succinate. Hence the proposed method was successfully applied for routine quality control analysis of Hydrochlorothiazide and Metoprolol in combined tablet dosage forms. This method was validated according to ICH guidelines....
A new precise, reproducible and validated RP-HPLC method was developed for the simultaneous estimation of Rosuvastatin calcium and Clopidogrel bisulphate in pharmaceutical dosage form. The chromatographic conditions used for the separation was Zodiac C18 (4.6x250mm, 5μ) mobile phase comprised of Methanol: acetonitrile: water (76:18:06 %v/v). The flow rate was 1.0 ml/min with detection at 241 nm. The retention time of Rosuvastatin calcium and Clopidogrel bisulphate was found to be 4.61 and 9.09 min respectively. The linearity was found to be in the range of 10-50 µg/ml for Rosuvastatin calcium and for Clopidogrel bisulphate 45-450 µg/ml with correlation coefficients of 0.9998 and 0.9994 respectively. The proposed method is accurate with 99.6 – 102.40 % recovery for Rosuvastatin calcium and 98.70-100.10 % recovery for Clopidogerl bisulphate and precise (%RSD of repeatability, intraday and inter day variations were 0.43, 0.98 -1.39, 0.27-0.35 for Rosuvastatin calcium and 0.23, 0.36-0.51, 0.39-0.58 for Clopidogrel bisulphate). The limit of detection (LOD) and limit of quantification (LOQ) for Rosuvastatin Calcium 0.2322, 2.9246 µg/ml and for Clopidogerl Bisulphate 0.7037, 9.044 µg/ml respectively. The method can be used for the estimation of dosage form in routine analysis....
First order derivative spectroscopy method involves the measurement of absorbance of one drug at zero crossing point of the other drug. A new, rapid, precise, accurate and sensitive first derivative spectrophotometric method is proposed for the simultaneous estimation of pantoprazole Sodium and Ondansetron Hydrochloride in combined dosage form. Absorbance of Pantoprazole Sodium was measured at 310 nm (Zero Crossing Point of Ondansetron Hydrochloride) and Absorbance of Ondansetron Hydrochloride was measured at 331 nm (Zero Crossing Point of Pantoprazole Sodium). The drugs obeyed the Beer’s law in the concentration range of 10-50 ug/ml (r2 = 0.9997) for Pantoprazole Sodium and1-5 ug/ml ( r2 = 0.9991) Ondansetron Hydrochloride. In the proposed method,. Accuracy of the method was determined by recovery studies and the average percentage recovery was found to be 99.24 % and 99.37 % for Pantoprazole Sodium and Ondansetron Hydrochloride respectively. The LODs for Pantoprazole Sodium and Ondansetron Hydrochloride were found to be 2.69 μg/ml and 0.29 μg/ml & LOQs were found to be 8.17 μg/ml and 0.89 μg/ml respectively. Statistical analysis proves that the method is selective and sensitive for estimation of Pantoprazole Sodium and Ondansetron Hydrochloride in combined dosage form. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
Two simple, accurate, precise and specific spectrophotometric methods have been developed for simultaneous determination of Tolperisone Hydrochloride (TOL) and Diclofenac Sodium (DFS) in its combined tablet dosage form by using methanol as a solvent. The first method is dual-wavelength method which involves estimation of TOL by absorbance difference at 267.19nm and 297.05nm, and DFS by absorbance difference at 241.26 nm and 266.4 nm. The second method is first order derivative method in which absorption at 282.12 nm (zero cross point of DFS) was used for quantification of TOL and 255.17 nm (zero cross point of TOL) for quantification of DFS. Two methods follow Beer’s linearity in the range of 10-50μg/ml for TOL and DFS both. The mean % recoveries were found to be in the range of 99.63 – 100.67 % and 98.9 – 100.7 % for TOL and DFS respectively for dual-wavelength method and in the range of 98.86 – 100.16% and 99.63 – 100.67% TOL and DFS respectively for first order derivative method. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of TOL and DFS in their combined Tablet dosage form....
A simple, accurate, precise sensitive, repeatable and stability indicating RP-UPLC method was developed for simultaneous determination of metronidazole (MET) and ofloxacin (OFL) in combine dosage form. The method was developed by using reverse phase C18 Purosher star (100 mm × 2.1 mm id, 2µm particle size) as stationary phase with phosphate buffer: acetonitrile (70:30 %v/v) as a mobile phase, pH was adjusted to 2.5 by ortho-phosphoric acid at a flow rate of 0.5 ml/min and and column temperature maintained at 45°C. Quantification of eluted compound was achieved with PDA detector at 317 nm. The combination drug product is exposed to thermal, acid/base hydrolytic and oxidative stress conditions, and the stressed samples were analyzed by proposed method. Metronidazole and ofloxacin followed linearity in the concentration range of 5-35 µg/ml and 2.5-17.5 µg/ml with r2=0.999 (n=6) respectively. Limit of detection (LOD) and limit of quantification (LOQ) values for Metronidazole was 0.162 and 0.492 µg/ml and for ofloxacin was 0.067 and 0.203 µg/ml respectively. Chromatographic peak purity data of MET and OFL indicated no co-eluting peaks with the main peaks of drugs which demonstrated the specificity of assay method for their estimation in presence of degradation products.The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was also successfully applied for estimation of metronidazole and ofloxacin in pharmaceutical formulation....
A stability-indicating HPLC method has been developed and validated for simultaneous estimation chlorzoxazone, diclofenac potassium and paracetamo in bulk drug and pharmaceutical dosage forms. Stress studies were conducted for all three drugs under ICH prescribed stress conditions viz. hydrolysis, oxidation, thermal and neutral stress. An isocratic RP-HPLC method was achieved on younglin HPLC system using Varian C18 (250x4.6 mm i.d, 5 μm particle size) column for separation of drug from its degradation products using mobile phase containing mixture of methanol: phosphate buffer (pH 3.0, adjusted with glacial acetic acid) (70:30, v/v). The flow rate was 0.8ml/min and the eluent was monitored at 280nm. Linearity was found in the range of 5-25μg/ml for diclofenac potassium (DIC), 25-125μg/ml for chlorzoxazone (CHL) and 32.5-182.5μg/ml for paracetamol (PCM). The limit of detection for DIC, CHL & PCM was found to be 0.15μg/ml, 1.82μg/ml and 2.40μg/ml respectively, while limit of quantification was 0.47μg/ml, 5.53μg/ml and 7.29μg/ml respectively. The developed method was found to be fast, accurate, precise, reproducible and suitable for analysis of all three drugs in bulk and pharmaceutical dosage forms....
The present work describes a validated Stability Indicating RP-HPLC method for estimation of Tenoxicam in bulk and pharmaceutical dosage form. Chromatography was performed on a Varian C18 column (250 mm x 4.6 mm i.d., 5 µm particle size), column with mobile phase containing methanol and acetate buffer in the ratio (40:60, v/v) and pH of acetate buffer adjusted to 4.6 with glacial acid .The flow rate was 1.2 ml/min and the eluent was monitored at 369 nm. The selected chromatographic conditions were found to effectively separate Tenoxicam (RT- 4.170 min). Linearity for Tenoxicam was found in the range of 4-20μg/ml. The value obtained of LOD was 0.146µg/ml and LOQ was 0.444 µg/ml for Tenoxicam. The results of stress testing undertaken according to the International Conference on Harmonization (ICH) guidelines reveal that the method is selective and stability-indicating. The proposed method is simple, accurate, and precise and has ability to separate drug from degradation products and excipients found in the dosage forms....
The cleaning validation is to verify the effectiveness of the cleaning procedure for removal of product residues, degradation products, preservatives, excipients and cleaning agents so that the analytical monitoring may be reduced to a minimum in the routine phase. As a result of any pharmaceutical unit process, a residual level of the drug substance remains on the equipment and facility even after clean up. Cleaning is a challenging task and the design of the cleaning system depending upon the equipment use (dedicated/multipurpose), manufacture (continuous/batch), cleaning equipment (manual/automated), preparation (commercial product/clinical supplies), product formulation i.e., type of materials being removed from the surface, drugs (low risk/high risk), sterile/non sterile, solids/liquids and solubility (soluble/insoluble) of active ingredients. An acceptable cleaning system should incorporate the following elements. So this paper give the very good information about the cleaning procedure and develop the new method for the cleaning after the production of the tablets and do the validation of that developed analytic cleaning swam method....
Four different simple, accurate, rapid, economical spectroscopic methods namely Zero order, First derivative, Area Under Curve and Three wavelength spectroscopy have been developed and validated for estimation of Pamabrom in tablet dosage form using Distilled Water as a solvent according to ICH Guidelines Q2R1. Absorbance of each solution was measured at 279.60 nm for zero order spectrophotometry. First derivative spectra are obtained by transformations at Δλ of 2 nm and scaling factor 10 and absorbance measured at 268.40 nm. Peak area is measured between 265.00-290.00 nm for AUC method. For three wavelength spectroscopy, absorbance was recorded at three wavelengths λ1= 254.60 nm, λ2 = 279.60 nm, λ3 = 294.00 nm. Pamabrom show linearity over the range of 4-24 μg/ml for all developed methods. Statistical comparisons by one way ANOVA shows all methods have equal applicability for estimation of Pamabrom in tablet dosage forms....
Three methods are described for quantitative estimation of etizolam in bulk and in tablet dosage form by UV spectroscopy, HPTLC and RP-HPLC. In the first method, etizolam was estimated by measuring absorbance at λmax of 249 nm in 0.01 N HCl. In the second method, etizolam was estimated by HPTLC method using precoated plate of silica gel 60F254 and Toluene: Chloroform: Methanol (4.8:4.0:1.2 v/v/v) as mobile phase. The linear regression analysis data was used for the regression line in the range of 400–1600 ng/spot. In the third method, etizolam was estimated by simple and specific RP-HPLC method using the Kromasil column [C18 (5µm, 15 cm×4.6 mm, i.d.)] at ambient temperature using a mobile phase consisting of water: acetonitrile (50:50% v/v) and flow rate was 1.0 ml/min. Quantitation was achieved with UV detection at 241 nm based on peak area with linear calibration curves at concentration ranges 4–32 µg/ml etizolam. The specificity of HPLC method was confirmed by performing forced degradation study under thermal, humidity, acidic, alkaline, oxidative and photolytic conditions. The drug was found to degrade under acidic & oxidative conditions. The developed RP-HPLC method adequately separated the drug from the degradation products proving the specificity of method. The results of RP-HPLC method compared favourably with Japanese pharmacopoeia method. All three methods have been successfully applied to tablet formulation. All three methods were validated in terms of precision, recovery, limit of detection, limit of quantitation and robustness. The analysis of variance (ANOVA) and Student’s t-test were applied to correlate the results of etizolam determination in tablet dosage form by means of UV, HPTLC and RP-HPLC methods....
In acid- base titrations, indicators are used to show a sharp color changes at interval of pH. Natural pigments in plants are highly colored substances and may show color changes with variation of pH. An attempt has been made to investigate the indicator activity of Ipomoea coccinea and Bauhinia Purpurea L ethanolic extract and to replace the synthetic indicators as they have certain disadvantages like chemical hazard. Herbal indicators are evaluated by using strong acid-strong base, strong acid-weak base, weak acid-strong base and weak acid weak base. In all these titrations the extract was found to be very useful and accurate for indicating the neutralization point. Assay of aspirin and citric acid was carried out using flower extract as an indicator. %RSD was found 0.1 and 0.2 respectively for citric acid and aspirin. These indicate that this flower extract can successfully replace phenol red and phenolphthalein....
A simple, sensitive, rapid, accurate and precise derivative spectrophotometric method has been developed for the estimation of Cefixime Trihydrate in bulk and pharmaceutical dosage forms. Cefixime Trihydrate shows maximum absorbance at 288 nm. Spectrophotometrically, Cefixime Trihydrate was determined by measuring the 2D-values at 288 nm with phosphate buffer (pH-6.5) as a solvent. Beer’s law was obeyed in the concentration range of 4-18 μg/ml with coefficient of correlation 0.999. The developed method was applied directly to the analysis of the tablet preparations. R.S.D was found to be 0.0015. The result 100.16-100.54% for recovery studies by derivative method indicate that proposed method is accurate and precise for the determination of Cefixime Trihydrate in tablets. The method was completely validated and proven to be rugged. The excipients did not interfere in the analysis. The results showed that this method can be used for rapid determination of Cefixime Trihydrate in pharmaceutical tablet with precision, accuracy and specificity....
A simple, sensitive, accurate, precise, economic and reproducible UV-Spectrophotometric method for the analysis of Terbinafine HCl in bulk and formulations. The proposed method is validated in accordance with USP and ICH guidelines to check its suitability for the intended analytical application.The method involved estimation of Terbinafine HCl in bulk and formulations using citrate buffer pH 3.0 and Methanol in the 1:1 ratio. Linear response for Terbinafine hydrochloride was observed in the concentration range of 12.50 – 50.00 µg/ml. The correlation coefficient (R2) was found to be 0.9999. This indicates that 99.99% of variation in response is explained by variation in drug concentration. Low values of standard deviation and the % RSD indicates high precision of proposed methods. % Recovery of formulation was done by standard addition method. % Recovery of both the methods i.e., API and formulation lies close to the theoretical value 100 which indicates high accuracy of the proposed methods. From the linearity and accuracy studies, the range of analytical methods for the assay of Terbinafine hydrochloride API and formulation found to be 80% -120% of test concentration. High value of molar absorbtivity and low value of Sandell sensitivity indicates high sensitivity of proposed methods. The proposed UV Spectrophotometric method was found to be new, simple, sensitive, accurate, precise and economic analytical method for the determination of Terbinafine hydrochloride from its bulk drug and pharmaceutical formulations....
A simple, rapid and precise reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of Sildenafil Citrate and Dapoxetine Hydrochloride in tablet dosage form using Kromasil ODS C-18 (5μm), 250 × 4.6 mm reversed-phase column and mobile phase Methanol : Acetonitrile (95:5) with 0.5% Triethylamine in isocratic mode. The flow rate was 1.0 ml/min and individual components were measured at 292 nm. The retention time of Sildenafil Citrate and Dapoxetine Hydrochloride was found to be 3.07 and 4.59 min respectively. The calibration curve was linear over the concentration range of 10-70 µg/ml for Sildenafil Citrate (r2=0.9991) and Dapoxetine Hydrochloride (r2=0.9992). The high percentage of recovery confirms the suitability of the method for the estimation of Sildenafil Citrate and Dapoxetine Hydrochloride in tablet dosage form. The method was validated in terms of accuracy, precision, linearity, limit of detection and limit of quantitation as per ICH guidelines. The procedure was successfully applied for simultaneous determination of both drugs in tablet dosage form....
Indicators used in titration show well marked changes of color in certain intervals of pH. Most of these indicators are organic dyeand are of synthetic origin.In this review importance of Fruits Flavonoids as a Natural Acid Base PH Indicator are described.Today synthetic indicators are the choice of acid-base titrations. But due to environmental pollution, availability and cost, the search for natural compounds as an acid-base indicator was started. The present work highlights the use of the Anthocyanins flavonoids present in the most of fruits used as acid-base titrations. This natural indicator is easy to extract as well as easily available. Titration shows sharp color change at the equivalence point. Therefore, this natural indicator is found to be a very useful, economical, simple and accurate for acid base titration....
It is widely used chromatography procedure among various instrumental techniques our philosophy of HPLC method development is based on several consideration. There exists today a really better practical understanding of chromatographic separation which is varies with sample & experimental condition strategy should based on as many experimental runs as are really required to achieve desire final result. Here by HPLC method development step strategy based on review some basics HPLC separation & more helpful facts that can ensure that method development start out in right direction. All critical steps in method development will be summarized and a sequence of events that required to develop the method efficiently will be proposed. This scheme described in this review will usually work in either situation....
The present investigation aims at to evaluate the insilico analysis of the ethanolic extract of Passiflora incarnata.L (EEPI). Ethanol extract of Passiflora incarnata.L was subjected to preliminary phytochemical screening and the pharmacological effect of EEPI was assessed by employing in-vivo methods. Compounds present in the ethanol extract of the plant were identified using GC-MS and attempts were made to understand the mechanism of action using in silico methods.Present study revealed that Passiflora incarnata.L(EEPI) possessed significant parmacological activity.....
Intellectual Property refers to creation of mind i.e. inventions, industrial designs for article, literary & artistic work, symbols etc. used in commerce. Intellectual property is divided into two categories: industrial property, which includes inventions (patents), trademarks, industrial designs, and geographic indications of source: and Copyright, which includes literary and artistic works such as novels, poems, plays, films and musical works etc. According to the TRIPS Agreement, the intellectual property has been classified into-Patents, Industrial Designs, Trade Marks, Copyright, Geographical Indications, Layout Designs of Integrated Circuits, and Protection of Undisclosed Information/Trade Secrets. Different IP Rights vary in the protection they provide....
A simple, specific, accurate, and precise reverse phase high performance liquid chromatographic method was developed and validated for the estimation of Itraconazole in capsule dosage form. A dionex C-18, 5 µm column having 250 x 4.6 mm internal diameter in isocratic mode with mobile phase containing Potassium dihydrogen phosphate buffer solution and Methanol in the ratio of 60:40 v/v was used. The flow rate was 1.5 ml/min and effluents were monitored at 306 nm. The retention time of Itraconazole was found to be 5.2 min. The method was validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantification and robustness. Limit of detection and limit of quantification was found to be 0.0018594 mg/ml and 0.006197 mg/ml respectively and recovery of Itraconazole from capsule formation was found to be 99 to 100%. The system suitability parameters such as theoretical plates and tailing factor were found to be 8609 and 1.13. The proposed method was successfully applied to the quantitative determination of Itraconazole in capsule formulation....
Material Safety Data Sheet (MSDS) is a document that contains information on the potential health effects on exposure to chemicals, or other potentially dangerous substances, and on safe working procedures when handling chemical products. A Material Safety Data Sheet (MSDS), Safety Data Sheet (SDS), or Product Safety Data Sheet (PSDS) is an important component of product stewardship and workplace safety. SDS information may include instructions for the safe use and potential hazards associated with a particular material or product. These data sheets can be found anywhere where chemicals are being used. It is intended to provide workers and emergency personnel with procedures for handling or working with that substance in a safe manner and includes information such as physical data (melting point, boiling point, flash point, etc.), toxicity, health effects, first aid, reactivity, storage, disposal, protective equipment, and spill-handling procedures. MSDS formats can vary from source to source within a country depending on national requirements....
A simple and sensitive HPTLC method has been developed for determination of Metoprolol succinate and Telmisartan in its pharmaceutical dosage forms. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. Toluene: Ethyl acetate: Methanol: Glacial acetic acid (6:2:2:0.1v/v/v/v) as a mobile phase at ahe room temperature. The Rf value of metoprolol succinate is 0.25 and of Telmisartan is 0.64 were found. The linearity for both the drugs was in the range of 1000-5000 ng/ml and 800-4000 ng/ml. The % recoveries of metoprolol succinate and telmisartan were found to be in the range of 99.17-99.72 and 99.07-99.45, respectively. The proposed method was validated and successfully applied to the estimation of metoprolol succinate and telmisartan in combined dosage form....
This paper describes developed and validated thin layer liquid chromatography (TLC) method for the simultaneous estimation of Rosuvastatin calcium and Telmisartan in a combined dosage form. Rosuvastatin calcium and Telmisartan were determined by High Performance Thin Layer chromatography method (HPTLC) in tablet dosage form. The method was carried out in TLC Precoated silica gel on aluminum plate 60 F 254, (10 cm ×10 cm, prewashed by methanol and activated at 60° C for 5 min prior to chromatography). The solvent system wasToluene: Methanol: Glacial acetic acid in the proportion of 8.5:1.5:0.1, (v/v/v/v) with Rf Value for rosuvastatin calcium and telmisartan was 0.29 and 0.37 respectively. The linearity regression analysis for calibration showed 0.996 and 0.998 for rosuvastatin calcium and telmisartan with respect to peak area and height in the concentration range of 4- 20ng/band and 16-80ng/band respectively. The method developed can be used for routine analysis of drugs content in tablet dosage form. The method was validated as per ICH (International Conference on Harmonisation) Guidelines, proving its utility in estimation of Rosuvastatin calcium and Telmisartan in combined dosage form....
The present work describes a simple, precise and accurate HPLC method for estimation of montelukast. The separation was achieved by using C18 column with acetonitrile: water 90:10 v/v as a mobile phase at a flow rate of 1.5 ml/min. Detection was carried out at 285 nm. The retention time of montelukast was found to be 6.7 min. The proposed method was ascertained by evaluating validation parameters like linearity (1-100 µg/ml) with R2=0.999. The proposed method is successfully applied for the determination of drugs in commercial tablet preparation. The results of the analysis have been validated statistically and by recovery studies....
A reliable and sensitive isocratic stability indicating RP-UPLC method has been developed and validated for Quantitative analysis and Content Uniformity study of Terazosin Hydrochloride Dihydrate in tablets. An isocratic method for analysis of Terazosin Hydrochloride Dihydrate was archived on Acquity UPLC BEH C18 (100*2.1) mm particle size 1.7 µ columns within shorter runtime of 6 min with a flow rate of 0.250 ml/min and using a photodiode array detector to monitor the eluent at 246 nm. The mobile phase consisted of Buffer-Acetonitrile (80:20 v/v), (Buffer: 20 mM ortho phosphoric acid in 1L water). The drug was subjected to oxidation, hydrolysis, photolysis and thermal degradation. Response was a liner function of drug concentration in the range of 20-80 µg/ml (r2= 0.9999). Accuracy (recovery) was between 98.21 to 101.60%. Degradation products resulting from the stress studies did not interfere with the detection of Terazosin Hydrochloride Dihydrate and the assay is stability-indicating....
A new, simple, accurate and precise validated RP-HPLC method for estimation of Embelin has been developed and validated. Analysis was carried out on LC-2010 CHT Shimadzu system with ACE C18 column (5µ, 150mm) using Methanol: water (85:15) as mobile phase with flow rate of 1.2 ml/min. The detection was carried out using UV detector set at 288 nm. For this method, Beer’s law is obeyed in the concentration range of 50.0 to 250.0 ppm of embelin. The method was validated with respect to linearity, precision and accuracy as per the International Conference on Harmonization (ICH Q2-R1) guidelines....
The present study describes a simple, accurate, precise and cost effective UV-Spectrophotometric method for the estimation of Ritonavir, an anti-HIV drug, in bulk and pharmaceutical dosage form. The drug was first dissolved in isopropyl alcohol and final volume wasmadeup with distilled water. The λmax or the absorption maxima of the drug was found to be 245nm. A linear response was observed in the range of 10- 60μg/ml with a regression coefficient of 0.999. The method was then validated for different parameters as per the ICH (International Conference for Harmonization) guidelines. This method can be used for the determination of Ritonavir in quality control of formulation without interference of the excipients....
Capillary electromigration methods are powerful analytical tool which help to provide useful information on chemical properties of complex systems. The different electromigration methods apply to monitor release of drugs and polymers are reviewed in this paper. There are several principles of different capillary electromigration methods used to monitor the degradation or solubilization of the polymeric matrices from drug delivery systems with help of in vitro and in vivo assays....
A comprehensive review is given on what quality assurance means, the various methods used for quality assurance in different aspects of clinical trials and the impact of this quality assurance on outcome and every day practice. Recently there is a need of reliable data from clinical drug trials, the role and presence of quality assurance within a research site becomes more important. The use of a “Total quality management program” can be used to train and educate new clinical research coordinators and study physicians. Quality control and quality assurance are parts of quality management. Quality assurance is focused on providing confidence that quality requirements are fulfilled....
Citicoline sodium is chemically Cytidine 5‘-{trihydrogendiphosphate} p‘-[2-{trimethylammonio} ethyl] ester inner salt. Citicoline sodium is primarily used in pharmacotherapy of brain insufficiency and other related neurological disorders viz., as stroke, brain trauma and Parkinsonism’s disease. Citicoline is not official in any pharmacopoeia. Few analytical methods like simple UV Spectrophotometric method, Second order Spectrophotometric methods, liquid chromatography, stability indicating HPLC, colorimetric and biological assay have been established for the estimation of Citicoline in bulk and tablet dosage form, there was no mention of a method based on AUC measurement of spectrum in Spectrophotometric estimation. The proposed UV- Visible Spectrophotometric method is based on AUC measurement of first order derivative spectra is a simple, specific, rapid, accurate and economic for quantitative estimation of Citicoline sodium. The solvent used was double distilled water. Absorption minima in first order derivative spectra was found 288nm (method-I) and area under curve was measured from 272-304nm (method-II), the drug followed a linear relationship in the range of 10-20 μg/ml while the correlation coefficient was at 0.995 & 0.998 respectively. The recovery was 99.49% ±0.50 and the coefficient of variance for intraday and interday was found to be less than 5%, LOD and LOQ for this method was found 2 μg/ml and 10 μg/ml respectively. This method is found suitable for day to day analysis of Citicoline sodium in bulk and its formulation....
Lafutidine 2-[(2-furylmethyl) sulfinyl]-N-((2Z)-4-{[4- (piperidin-1- ylmethyl) pyridin-2-yl] oxy} but-2-en-1- yl) acetamide are used in the treatment of anti ulcer. Antisecretory drugs are used in the treatment and prophylaxis of peptic ulcer disease some are also employed in other disorders associated with gastric hyperacidity such as gastro-oesophageal reflux disease and dyspepsia. Few analytical methods like liquid chromatography, stability indicating HPLC and biological assay are reported, there was no mention of a method based on spectrophotometric estimation. The proposed UV- Visible spectrophotometric method is a simple, specific, rapid, accurate and economic for quantitative estimation of lafutidine. The solvent used was methanol for parent dilution and then sodium hydroxide for further dilution. Aabsorption minima in first order derivative spectra was found 284 nm and area under curve was measured from 275-295nm, the drug followed a linear relationship in the range of 10-35μg/ml while the correlation coefficient was at 0.999. The recovery was 99.89% (+0.50) and the coefficient of variance for intraday and inter day was found to be less than 5%, LOD and LOQ for this method was found 10 μg/ml and 35 μg/ml respectively. This method is found suitable for day to day analysis of lafutidine in bulk and its formulation....
Methylcobalamin (MCB or MeB12) is a cobalamin used in the treatment of peripheral neuropathy, diabetic neuropathy, and as a preliminary treatment for amyotrophic lateral sclerosis. It is a form of vitamin B12 and differs from cyanocobalamin in that the cyanide is replaced by a methyl group. Methylcobalamin features an octahedral cobalt (III) centre. Methylcobalamin can be obtained as bright red crystals. Literature survey reveals that HPLC & simple UV spectrophotometric methods have been established for the estimation of MCB in bulk and tablet dosage form. The aim of present study was to establish a method for estimation of MCB in tablet dosage form by using first order derivative spectroscopy (method A) & area under curve methods (method B & C). Absorption minima in first order derivative spectra was found to be 384 nm (method-A) and area under curve was measured from 260-275 nm for zero order spectra (method-B) and 310-360 nm for first order spectra (method-C), the drug followed a linear relationship in the range of 10-40 μg/ml while the correlation coefficient was at 1.000, 0.999 and 0.999 respectively. The recovery was 99.52% ±0.56 (method-A) and the coefficient of variance for intraday and interday was found to be less than 2%, LOD and LOQ for this method was found 01 μg/ml and 05 μg/ml (method-B) respectively. This method is found suitable for day to day analysis of MCB in tablet dosage form....
A simple, precise, specific, accurate and validated RP-HPLC method has been developed to determine Aspirin (ASP) and Rosuvastatin calcium (RSV) in capsule dosage form. Chromatographic separation achieved on ACE, C18 column (150 mm x 4.6mm i.d, 5µ), and Acetonitrile : 25mM phosphate buffer (pH 3.0) in the ratio of 40:60 (v/v) as the mobile phase, at a flow rate of 1 ml/min and injection volume 10µl. Detection was carried out at 260 nm. The retention times for ASP and RSV was found to be 3.3±0.16 and 7.8±0.27 min respectively. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the ICH guidelines. The method was linear in the concentration range of 15-120 μg/ml for ASP and 2-16 μg/ml for RSV with correlation coefficient of 0.999 and 0.999 respectively. The recoveries obtained for ASP and RSV were 99.27-101.85% and 98.86-102% respectively. The developed method was found to be accurate, precise, specific and sensitive for simultaneous estimation of ASP and RSV....
A new, simple and sensitive spectrometric method in ultraviolet region has been developed for determination of desonide in bulk and pharmaceutical formulations. Desonide exhibit absorption maxima at 247nm with apparent molar Absorptivity 4.2000×104L/mol.cm in methanol .beer’s law was found to be obeyed in concentration range of 2-22 ug/mL The method is accurate, simple, precise, reproducible, requiring no prior separation and economical procedures for Estimation of desonide in topical cream formulation. In this method, there is no interference from any common pharmaceutical additives and diluents. Results of the analysis were validated statistically and recovery studies....
The reversed phase HPLC method has been developed for the simultaneous estimation of Etodolac & Thiocolchicoside in bulk and tablet dosage form. The proposed HPLC method utilizes Hypersil C18column (250mm × 4.6mm i.d., 5μm) and a mobile phase comprising of phosphate buffer (pH 6.8): acetonitrile in ratio of 70:30v/v with flow rate of 1ml/min. The retention time of THIO and ETO was found to be 3 min and 12min respectively. Quantitation was achieved with UV detection at 260nm.The method has been validated for Etodolac and Thiocolchicoside in terms of accuracy, precision, linearity, solution stability and robustness. The developed validated stability-indicating HPLC method was found to be simple, specific, accurate and reproducible for the determination of instability of these drugs in bulk and commercial products....
In the present study, two different chemometric methods – partial least squares (PLS) and principal component regression (PCR) for simultaneous determination of montelukast sodium and fexofenadine hydrochloride in pharmaceuticals are described. These two approaches were successfully applied to resolve the overlapped data and quantify the two components in the studied mixture using the calibrations constructed with the absorption data matrix corresponding to the concentration data matrix with measurements in the range of 240-400 nm (Δλ = 1 nm) of the zero order spectra. The calibration range was found to be 5-25 µg mL-1 for montelukast sodium and 60-300 µg mL-1 for fexofenadine hydrochloride, respectively. The PLS and PCR methods neither require any separation step, nor any prior graphical treatment of the overlapping spectra of the two drugs in a mixture. The calibration of the chemometric models were evaluated by internal validation (prediction of components in its own designed training set of calibration) and by external validation over synthetic and pharmaceutical preparations. Both studied methods can be considered acceptable for the pharmaceutical quality assurance of montelukast sodium and fexofenadine hydrochloride in combined dosage forms....
In the present study attempt was made to develop a simple, precise and economical spectrophotometric methods have been developed for the simultaneous estimation of atenolol and nifedipine in bulk and combined tablet dosage form. Both the drugs obey the Beer’s law in the concentration ranges employed10-16μg/ml for atenolol and 2-12μg/ml for nifedipine at λmax of 274nm and 238 nm. The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization. All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of atenolol and Nifedipine in bulk and combined tablet dosage forms. Recovery studies for atenolol and nifedipine are 99.58 and 99.50 in case of 120% recovery studies confirming the accuracy of the proposed method. The utility of the developed method has been successfully applied for the analysis of commercially available tablet dosage forms....
Olmesartan medoxomil and hydrochlorothiazide are available in tablet dosage form in the ratio 20: 12.5. Two simple, accurate, precise and economic method, simultaneous equation method and multicomponent method, have been described for the simultaneous estimation of olmesartan medoxomil and hydrochlorothiazide in tablet dosage form. Absorption maxima of olmesartan medoxomil and hydrochlorothiazide in distilled water were found to be 256.0 nm and 271.5 nm, respectively. Beer’s law was obeyed in the concentration range of 5-40 µg/ml for olmesartan medoxomil as well as for hydrochlorothiazide. The methods allow rapid analysis of binary pharmaceutical formulation with accuracy. Results of two methods were validated statistically and by recovery studies, and were found to be satisfactory....
Simple and cost effective spectrophotometric methods were developed for the determination of almotriptan. Colorometric methods were developed with the reagents MBTH , tropaeolin ooo , Brucine , Alizarin red.S , 2,4 bi pyrimidine, 1,10 Phenanthroline FC, K3FECN6 ,PNA ,and woolfat blue .All the proposed methods obeyed Beer’s Law was . The experimental parameters were optimized and validated. The statistical analysis of results revealed high accuracy and good precision. The proposed methods were successfully applied for the determination of almotriptan active pharmaceutical ingredient (API) in bulk drug....
A rapid and sensitive high performance liquid chromatography method for determination of paracetamol, Diclofenac sodium and Caffeine has been developed. The chromatography system used a reversed phase Hypersil 250 x 4.6 mm ODS (5 µm) column with UV- Vis detection at 230 nm. Mobile phase consisted of Phosphate Buffer pH 2.5: Acetonitrile (30: 70) (Adjust pH 2.5 with o-phosphoric acid) at a flow rate of 0.5 ml/min .The calibration curve was linear in the concentration range of 2-40 μg/ml for paracetamol, 2-32 μg/ml for Caffeine and 4-20 μg/ml for diclofenac sodium.The retention times of Paracetamol, Caffeine and Diclofenac Sodium were found to be 5.10, 5.81 and 10.38 min respectively. The results of the study showed that the proposed HPLC method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability, which is useful for the routine determination of Paracetamol, Diclofenac Sodium and Caffeine, in bulk drug and in its pharmaceutical dosage form....
Present work describes a precise, accurate and reproducible stability indicating Reverse phase High Performance Liquid Chromatographic (RP-HPLC) method for simultaneous estimation of Escitalopram Oxalate and Clonazepam on Kromasil 100 C18, 5µ (150×4.6 mm) column using Methanol: 0.025 M KH2PO4 Buffer (45:55 v/v) pH 3.0 adjusted with o-phosphoric acid as mobile phase at a flow rate of 1.0 ml/min and the detection wavelength was 254 nm. The retention time for ESC and CLO was found to be 6.8 and 12.7 min, respectively. The method was validated for linearity, precision, accuracy, robustness, solution stability and specificity. The method was linear in the concentration range of 20-140µg/ml for ESC and 2-14 µg/ml for CLO with a correlation coefficient of 0.999 and 0.999 for respective drugs. The % RSD for intra-day precision was found to be in the range of 0.28-0.54 and 0.34 -0.58; while inter-day precision was found to be in the range of 0.36-0.97 and 0.46-0.75 for ESC and CLO, respectively. The percent recovery was found in the range of 99.23-101.96 % and 99.42-101.96 % for ESC and CLO, respectively. The specificity of HPLC method was confirmed by performing forced degradation study of ESC and CLO under thermal, humidity, acidic, alkaline, neutral, oxidative and photolytic conditions. Escitalopram degraded significantly in basic condition, while clonazepam degraded significantly under acidic, alkaline, oxidative, thermal & humidity conditions and marginally in thermal condition. The developed RP-HPLC method adequately separated the drug from the degradation products proving the specificity of method and can be used for stability analysis....
A simple, sensitive, reproducible stability indicating UV Spectrophotometric method has been developed for the estimation of Glimepiride in bulk and its various marketed brands of tablets (B1, B2, B3, B4, and B5). Methanol was used as a solvent and 228 nm was selected as maximum wavelength for absorption. Beer’s law was obeyed in the concentration range of 2.5-15 g/ml with correlation coefficient r = 0.9993.The bulk drug and marketed tablet brands (B1, B2, B3, B4 and B5) of glimepiride were subjected to various stress conditions like acid hydrolysis, base hydrolysis, oxidation, photolysis and thermal degradation. Results of the analysis were validated as per ICH guidelines. This method can be used for the routine and quality control analysis of glimepiride in bulk and various pharmaceutical formulations....
A simple, precise, accurate, and stability indicating UV-method has been developed and validated for estimation of Metoprolol succinate (METO). UV, HPLC, HPTLC, and many more methods were reported by taking single drug and also by combining with other drugs. However, stress degradation by Uv spectroscopy method was not reported. In both methods, METO has the absorbance maxima at 223 nm. Method A involves method development and validation and Method B involves stress degradation study. In these methods, methanol was used as a solvent. Linearity was observed in the concentration range of 6–24 μg/ml. Validation experiments were performed to demonstrate system suitability, specificity, precision, linearity, accuracy, robustness, LOD, and LOQ as per International Conference on Harmonization guidelines(ICH). Furthermore stability studies of METO were carried out under acidic, alkali, neutral, oxidation, photolytic, and thermal degradation as per stability indicating assay methods. The results of analysis have been validated, and recovery studies were carried out using a standard addition method by adding specific drug amount (50%, 100%, and 150%) and show recovery studies in the range 98.00–100.53%. The proposed method can be successfully applied for method development, validation, and stability study of METO....
The antimicrobial effectiveness test demonstrates that the effectiveness of the preservative system in a product. A product is inoculated with a controlled quantity of specific microorganism then compares the level of microorganisms found on a control sample vs. test sample over a period of 28 day. Antimicrobial preservatives are the substances added to the non sterile dosage form to protect them from microbial growth or from micro organism that are introduced in advertently during or subsequent manufacturing process. All antimicrobial substances are toxic in nature when given to the patient for maximum protection. So, concentration of preservative should be below the toxic level to the human beings. It’s necessary to check the concentration of preservatives in a dosage form through various methods to maintain the quality products....
Ultra Performance Convergence Chromatography (UPC2) is a new category of separations science in chromatography that makes the complex analysis routine. It combines the potential of SFC technique with available UPLC technique. Use of compressed carbon dioxide CO2 (green solvent) and co-solvent as a mobile phase makes the technique inexpensive and non toxic and it avoids use of toxic, expensive and volatile organic solvents. Along with sub-2 μm particle column chemistries, system gives the ability to precisely vary mobile phase strength, pressure, and temperature. With the ability to fine-tune the resolving power and selectivity of the system, one can exercise better control over the retention of analytes like natural products, traditional medicines, drugs, food additives or contaminants, pesticides, surfactants, polymer additives, or biofuels-all compounds that are often difficult to separate by any other means. It is also best complement to MS with low solvent load, high resolution, narrow peaks and fast separation. Waters Corporation has been awarded the prestigious 2012 Pittcon Editors’ Gold Award for the Waters ACQUITY UPC2 System as the best new product at the 2012 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy....
Two Simple, fast, accurate, precise, robust, rugged and economical UV- Spectrophotometric methods have been developed for simultaneous estimation of Montelukast Sodium (MTKT) and Desloratadine (DLOR) in combined tablet dosage form. Methanol was used as solvent. In method-I (Multicomponant mode of analysis) two wavelengths wasselected on basis ofλmax, for MTKT 283nm and DLOR244nm. MTKT and DLOR at their respective λmax show linearity in the concentration range of 18-26μg/ml and 9-13μg/ml respectively. In Method-II (First order derivative spectroscopy) absorbance was measured at 280.8nm (zero crossing point of MTKT) and 241.4nm (zero crossing point of DLOR), at these zero crossing points both drugs shows linearity in the concentration range of 8-40μg/ml and 4-20μg/ml for MTKT and DLOR respectively.The mean % recoveries were 99.99% and 100.80% in method-I and 100.42% and 100.12% in method-II for MTKT and DLOR respectively.Precision was good with acceptable limits of detection (LOD) and quantitation (LOQ) for both compounds. Percent label claim of the compounds were100.25% and 99.96% in method-I and 100.29% and 99.11% in method-II for MTKT and DLOR respectively. The optimized methods showed good reproducibility with percent relative standard deviation less then 2.0%....
Moxifloxacin hydrochloride (MOXI) and Dexamethasone sodium phosphate (DEXA) are used in combined dosage form for the treatment of steroid-responsive inflammatory ocular conditions. Literature describes, no method has been reported for the simultaneous estimation of MOXI and DEXA in combined dosage form by UV spectrophotometry. For the simultaneous estimation of MOXI and DEXA by two UV spectrophotometry methods have been developed. The, (1) First order derivative method, and (2) Second order derivative method has been developed. For the linearity for MOXI and DEXA are lies between 30-60 µg/mL and 6-12 µg/mL respectively with co-relation co-efficient > 0.990. The solvent is used is Distilled Water. For the first order derivative method the wavelength selected are 241.30 nm for MOXI and 261.90 nm for DEXA, for the second order derivative method the wavelength selected are 266 nm for MOXI and 241 nm for DEXA. All the developed methods are validated according to ICH guidelines. The proposed methods for estimation of MOXI and DEXA were found to be simple, precise, accurate, economical and statistically validated and are applicable for the simultaneous determination of MOXI and DEXA in ophthalmic dosage form....
Pharmaceuticals impurities are the unwanted chemicals that remain or are generated during the formulation of medicines. Impurity profiling helps in detection, identification and quantification of various types of impurities as well as residual solvents in bulk drugs and in pharmaceutical formulations. It is a best way to characterize quality and stability of bulk drugs and pharmaceutical formulations. Due to rapid development of the analytical methodology it is imperative to review problems related to impurities present in the drug substances and drug products. Identification of impurities is done by variety of Chromatographic and Spectroscopic techniques, either alone or in combination with other techniques. There are different methods for detecting and characterizing impurities with TLC, HPLC, HPTLC, AAS etc. Conventional Liquid Chromatography, particularly, HPLC has been exploited widely in field of impurity profiling; the wide range of detectors, and stationary phases along with its sensitivity and cost effective separation. Thus enlightening the need of impurity profiling of drug substances in pharmaceutical research this review focuses on various analytical methods for identification as well as quantification of impurities present in the pharmaceuticals....
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