Current Issue : July-September Volume : 2015 Issue Number : 3 Articles : 31 Articles
A simple, accurate and precise dual wavelength UV spectrophotometric method was developed for simultaneous determination of paracetamol and tramadol in combined pharmaceutical dosage forms. The literature review reveals that there was no dual wavelength method developed for this combination of drugs, hence this method was developed. The wavelengths selected for determination of paracetamol were 255 nm and 282 nm, whereas, the wavelengths selected for determination of tramadol were 230.59 nm and 252.94 nm. Methanol and distilled water were used as the solvents. Regression analysis of Beer’s plots showed good correlation in concentration range of 2-35 μg/ml for paracetamol and 2-30 μg/ml for tramadol. Accuracy of method was found between 98.0-102.0%. The precision (intra-day, inter-day and analyst to analyst) of method was found within limits (% CV<2). LOD was found to be 0.10 μg and 0.63 μg for paracetamol and tramadol respectively and LOQ was found to be 0.30 μg and 1.92 μg for paracetamol and tramadol respectively. The proposed method was successfully applied to determination of these drugs in laboratory-prepared mixtures and commercial tablets....
UV Spectrophotometric absorption correction method was developed for simultaneous estimation of diethylcarbamazine citrate (DEC) and doxycycline hydrochloride (DOXY) in their synthetic mixture. Wavelengths selected for application of method were 348 nm for DOXY and 209 nm for DEC and DOXY. Linearity was observed in concentration range of 6-42 µg/ml for DEC and 2-14 µg/ml for DOXY. Method was validated as per ICH Guidelines and found to be simple, precise and accurate. This method can be used for routine analysis....
Bacopa monnieri is traditional ayurvedic herb that improves intellectual and enhance brain memory which is generally co-cultivated with rice paddy and rice paddy is sprayed with number of organochloro and organophosphate pesticides. A specific, accurate and precise Gas chromatographic method has been developed and validated for detection and quantification of pesticides namely hexachlorobenzene, chlorpyrifos and carbophenothion in Bacopa monnieri. The method development was achieved by using Restek RTX-5 (30 m, 0.25 mm i.d., 0.25 μm) along with electron capture detector using acetone as a solvent with flow rate 5.3 ml/min. The retention time of hexachlorobenzene, chlorpyrifos and carbopenothion were found to be 12.8 min, 17.5 min and 23.5 min respectively. The method was validated as per ICH guidelines. The linearity and range was found to be 0.050 – 0.100 μg/ml for each three pesticides. The co-relation coefficient was found to be 0.9956, 0.9957 and 0.9972 respectively. % RSD of repeatability, intraday and interday precision was found to be less than 2%. % RSD for robustness parameters (flow rate change and Ramp temp change) was found to be less than 2%. The % recovery of hexachlorobenzene, chlorpyrifos and carbopenothion at different levels were found in the range of 86.25% - 91.90%, 88.62% -97.08% and 88.87% - 91.10% respectively. So the developed method was precise, accurate and robust. The developed method was simple, specific, economic and can be used for simultaneous estimation of hexachloro-benzene, chlorpyrifos and carbophenothion in Bacopa monnieri tablet dosage form....
Pharmaceuticals can be classified into inorganic, organic compounds as well as excipients. The need to have a readily adaptable method for the quality control of these compounds has led to the development of a wide range of reactions and procedures. Majority of these pharmaceuticals lack adequate chromophores which can permit analysis at wavelength regions beyond the nonspecific UV‐region of the electromagnetic spectrum. Thus derivatization reactions are carried out to convert these pharmaceuticals to readily determinable compounds whose properties and concentrations can be related to the original compound. The need to have simple methods for the analysis of pharmaceuticals, in spite of the improvement in modern‐day technology, will continue to make these derivatization methodologies relevant in the quality control of these compounds especially in poor‐resource economies. The aim of present work is to find out a simple, specific, colorimetric or visible-spectrophotometric method using analytical and chemical reagents in bulk and pharmaceutical formulations. In present work different reagents, their properties, uses, mechanism of action and applications are enlisted....
A simple liquid chromatographic method has been developed for the determination of Pyridine-4-aldehyde in donepezil hydrochloride drug substance. The method was validated as per ICH guideline in terms of LOD, LOQ, Method precision, accuracy and specificity. The LOD and LOQ values were found to be 7 ppm (7 µg/ml) and 21 ppm (21 µg/ml) respectively....
The present work deals with development and validation of oneprecise and accurate spectrophotometric method for the estimation of Levosulpiride and Pantoprazole Sodiumin bulk and Capsuledosage form. A Q-Absorbance maxima method where absorbance maxima of the drug was recorded at 236nm for Levosulpiride and 288 nm for Pantoprazole sodiumby using Co-solvent method (methanol as a starting solvent and further water as a solvent).Linearity was observed in the concentration range 5-35µg/ml for both the drugs (r2 = 0.999 for both the drugs). The results of analysis were validated statistically, which confirmed the accuracy and reproducibility of the methods. The method were found to be simple, precise and accurate and can be employed for routine quality control analysis of Levosulpiride and Pantoprazole Sodium in bulk and capsule dosage form....
The present work deals with development and validation of two precise and accurate spectrophotometric methods for the estimation of Levamisole HCl in bulk and tablet dosage form. Method A is the absorbance maxima method where an absorbance maximum of the drug was recorded at 213 nm. Method B is area under the curve in which wavelength range 208-218 nm was selected for estimation of Levamisole HCl by using Co-solvent method (methanol as a starting solvent and further water as a solvent). Linearity was observed in the concentration range 2-14 µg/ml for both the methods (r2 = 0.999 for method A and r2 = 0.9991 for method B). The results of analysis were validated statistically, which confirmed the accuracy and reproducibility of the methods. Both the methods were found to be simple, precise and accurate and can be employed for routine quality control analysis of Levamisole HCl in bulk as well as in its solid dosage form....
A simple, accurate, precise, rapid and bathochromically shifted UV spectrophotometric method has been developed using phosphate buffer (pH-12.2) and methanol (for solubility purpose) to determine the nateglinide in bulk and tablet dosage formulations. At bathochromically shifted λmax from 209 nm to 214.7 nm, it was proved linear in the range of 10 – 60 mg/ml and exhibited good correlation coefficient (r2 = 0.9995) and excellent mean recovery (98.58 – 100.02%). The limit of detection (LOD) and limit of quantitation (LOQ) were found to be 1.12 μg/ml and 3.41 μg/ml respectively. The method was validated statistically and satisfactory values of percent relative standard deviation for system and method precision indicated that the method was precise....
Two simple, accurate and precise UV Spectroscopic methods were developed for the simultaneous estimation of escitalopram oxalate (ESO) and bupropion hydrochloride (BUP) in their synthetic mixture. For First order derivative spectrophotometric method 251 nm was selected for the estimation of escitalopram oxalate (ZCP for bupropion hydrochloride) and 237 nm was selected for the estimation of bupropion hydrochloride (ZCP for escitalopram oxalate). For dual wavelength method 235.6 nm and 240 nm were selected for the determination of bupropion hydrochloride, similarly 245 nm and 257.6 nm were selected for the determination of escitalopram oxalate. The linearity range was found to be 10-30 µg/ml for both ESO and BUP in first order derivative method and 5-25 µg/ml for both ESO and BUP in dual wavelength method. For first order derivative method correlation coefficient were found to be 0.9993 and 0.9994 for ESO and BUP respectively and the assay value was found to be 100.53% and 99.73% respectively, similarly for dual wavelength method correlation coefficient were found to be 0.9991 and 0.9994 for ESO and BUP respectively and the assay vale was found to be 99.1% and 99.4% respectively. The methods were validated as per the ICH guidelines. The proposed validated methods were successfully used for the quantitative analysis of synthetic mixture....
A simple and economical first order derivative spectrophotometric method and dual wavelength method were developed for simultaneous estimation of ketorolac tromethamine (KET) and phenylephrine (PHE) in its synthetic mixture. The wavelengths selected for first order spectrophotometric method were 331 nm for KET (zero crossing point for PHE) and 231 nm for PHE (zero crossing point for KET). For the Dual wavelength method 315 and 341.8 nm for KET and 266.2 and 278.2 nm for PHE wavelengths were selected. The linearity range was found to be 6-14 µg/ml for KET and 24-56 µg/ml for PHE for first order derivative and dual wavelength method. The co-relation coefficient was found to be 0.9991 and 0.9994 and the assay value was found to be 98.9% and 99.7% for first order spectroscopic method. For dual wavelength method the co-relation coefficient was found to be 0.9993 and 0.9995 and the assay value was found to be 98.5 % and 99.72% respectively for KET and PHE. All the methods were found to be simple, accurate and reproducible. The methods were validated as per ICH Guidelines....
The present manuscript describes new, simple, accurate and precise high performance thin layer chromatography method for the simultaneous determination of mebeverine hydrochloride and chlordiazepoxide in combined pharmaceutical dosage form. Chromatographic separation of the drugs was performed on aluminium plates pre coated with silica gel 60 F254 as the stationary phase and the solvent system consisted of Diethyl ether: Methanol: Ethyl acetate: Triethylamine (7:2:1:0.1, v/v/v/v). Densitometric evaluation of the separated zones was performed at 273 nm. The two drugs were satisfactorily resolved with Rf values 0.35 and 0.63 for mebeverine hydrochloride and chlordiazepoxide, respectively. The linear regression data for the calibration plots showed good relationship with r2 = 0.9990 from 1350-8100 ng/spot for mebeverine hydrochloride and r2 = 0.9995 from 50-300 ng/spot for chlordiazepoxide. The methods were validated for precision, accuracy and recovery. The percentage recovery for mebeverine hydrochloride was found to be 99.10 –100.76% and 99.90 – 100.72% for chlordiazepoxide. The limits of detection and quantification were 148.20 and 5.78 ng/spot per spot for mebeverine hydrochloride and 449.11 and 17.52 ng/spot per spot for chlordiazepoxide, respectively....
The aim of present work was to develop a simple and sensitive, HPTLC method for the quantitative estimation of Tinidazole in its single component tablet formulations 300 mg). Tinidazole was chromatographed on silica Gel 60 F254 TLC plate using Chloroform: Methanol: Ammonia (9:1:0.1 v/v) as mobile phase. Tinidazole in methanol was scanned by Camag TLC scanner 4 with UV visible detector over wavelength range 200 to 400 nm. Tinidazole showed Rf value 0.53 and scanned at 310 nm using camag TLC scanner. The method was validated in terms of linearity (3-9 μg/ml), Precision (intra-day variation 1.26, inter-day variation 1.4), accuracy (83.57 to 91.80%) and specificity. The limit of detection and limit of quantification for tinidazole were found to be 0.15 µg/ml and 0.47 µg/ml, respectively. It can be concluded from the results that the proposed method was accurate, precise and consistent the determination of tinidazole in tablet dosage form. This method was validated as per ICH guideline Q2 (R1). Results suggest that this method can be used for routine estimation of tinidazole in bulk and pharmaceutical dosage forms....
In the present study a simple precise, rapid and reproducible reverse phase HPLC method has been developed and validated and the degradation behaviour of acyclovir under different stress conditions were performed. The chromatographic separation was achieved by using reverse phase stainless steel column of 4.6Ã?â??250 mm hypersil C18 HPLC column with 5 Ã?µm (particles packing) and mobile phase consists of a mixture of acetonitrile and 0.05M ammonium acetate in the ratio of 2:98 v/v. Flow rate of 1.5 ml per minute and injection volume 20 ?l was maintained. Elute was analyzed by a UV detector set at 251 nm. The retention time was found to be 7.55 min. The method is validated with respect to linearity, precision and robustness. The correlation coefficient was found to be 0.998 with relative standard deviation less than 2%. Acyclovir was found to degrade in all studied conditions but the extent of degradation was different. The method was completely validated showing satisfactory data for all method validated parameters tested. The developed method can be used for the stability indicating samples....
Simple, specific, accurate, precise and reproducible RP-HPLC method has been developed and validated for the simultaneous estimation of five drugs in their combined semi-solid dosage form. In RP-HPLC, analysis was carried out using Acetonitrile and 0.1M Ammonium Acetate buffer adjusted to pH 4.0 with Glacial Acetic Acid (10:90 v/v) as mobile phase and hypersil ODS-BP C18 column (250 mm x 4.6 mm, 5.0 ? particle size) as stationary phase with detection wavelength of 239 nm. Linearity was obtained in the concentration range of 30-90 ?g/ml, 11.25-33.75 ?g/ml, 3-9 ?g/ml, 15-45 ?g/ml and 0.75-2.25 ?g/ml for Ornidazole (ORN), Ofloxacin (OFL), Methyl Paraben (MP), Terbinafine hydrochloride (TRH) and Clobetasol Propionate (CLP) respectively. The average retention time for ORN, OFL, MP, TRH and CLP was 3.43 minutes, 4.51 minutes, 7.23 minutes, 8.02 minutes and 15.37 minutes respectively. The % recovery was in the range of 101.821 ââ?¬â??101.995% for ORN, 100.438 ââ?¬â??101.934% for OFL, 100.551 ââ?¬â??101.027% for MP, 100.281 ââ?¬â??100.889% for TRH and 100.659 ââ?¬â?? 101.622% for CLP. Limit of quantification for ORN, OFL, MP, TRH and CLP was found to be 4.453 Ã?µg/ml, 1.011 Ã?µg/ml, 0.248 Ã?µg/ml, 1.128 Ã?µg/ml and 0.107 Ã?µg/ml respectively. Method was statistically validated for accuracy, precision, specificity, LOQ, robustness and ruggedness according to ICH guidelines and can be used for analysis of combined dosage form....
Stability indicating RP-HPLC method has been developed for the simultaneous estimation of Cilnidipine (CIL) and Olmesartan Medoxomil (OLM) in bulk and its pharmaceutical dosage form. In RP-HPLC method, chromatographic separation was achieved using C18 column (250 mm x 4.6 mm, 5 μm) and 10 mM dipotassium hydrogen phosphate : acetonitrile (60:40 v/v, pH 6.4) as mobile phase at flow rate of 1.0 ml/min with detection wavelength of 254 nm. The linearity of CIL and OLM were found in the range of 80-120 μg/ml and 320-480 μg/ml. Retention times in RP-HPLC method were found to be 4.6 min and 3.2 min for CIL and OLM respectively. The % recoveries were found to be 99.33±0.97 for CIL and 99.67±0.21 for OLM. The proposed method was validated as per ICH guidelines and successfully applied for the determination of drugs in pharmaceutical formulation....
Easy, sensitive, cost effective and consistent uv-spectrophotometric method has been developed for simultaneous estimation of quercetin and curcumin in topical gel formulation and validated. Quercetin and curcumin shows absorption maxima at 371 nm and 424 nm respectively. The developed method has followed linearity in the range of 2-7 μg/ml for quercetin and 1-6 μg/ml for curcumin. The value of correlation coefficient was 0.9993 and 0.999 respectively. Satisfactory values of percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. Results of the recovery studies (100 to 105%) showed accuracy of the method. LOD and LOQ were calculated as 0.0357 μg/ml and 0.1086 μg/ml for quercetin and 0.1133 μg/ml and 0.3434 μg/ml for curcumin respectively. The developed method can be used for routine estimation of quercetin and curcumin in pharmaceutical topical gel....
The present work deals with development and validation of two rapid, precise and accurate spectrophotometric methods for the estimation of midodrine HCl in bulk and tablet dosage form. Method A is the absorbance maxima method where absorbance maxima of the drug was recorded at 289 nm. Method B is area under the curve in which wavelength range 285-295 nm was selected for estimation of midodrine HCl. Linearity was observed in the concentration range 10-90 µg/ml for both the methods (r2=0.9994 for method A and method B). The results of analysis were validated statistically, which confirmed the accuracy and reproducibility of the methods. Both the methods were found to be simple, precise and accurate and can be employed for routine quality control analysis of midodrine HCl in bulk as well as in its solid dosage form....
Simple, fast and reliable spectrophotometric methods were developed for determination of Loratidine in bulk and pharmaceutical dosage forms. The solutions of standard and the sample were prepared in Methanol. The quantitative determination of the drug was carried out using the second order Derivative Area under Curve method values measured at 244-256nm. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of Loratidine using 2-10 μg/ml (r²=0.9952) for second order Derivative Area under Curve spectrophotometric method. All the proposed methods have been extensively validated as per ICH guidelines. There was no significant difference between the performance of the proposed methods regarding the mean values and standard deviations. The developed methods were successfully applied to estimate the amount of Loratidine in pharmaceutical formulations....
Simple, fast and reliable spectrophotometric methods were developed for determination of Prednisolone in bulk and pharmaceutical dosage forms. The solutions of standard and the sample were prepared in Methanol. The quantitative determination of the drug was carried out using the second order Derivative Area under Curve method values measured at 241-251 nm. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of Prednisolone using 2-10 μg/ml (r² = 0.9980) for second order Derivative Area under Curve spectrophotometric method. All the proposed methods have been extensively validated as per ICH guidelines. There was no significant difference between the performance of the proposed methods regarding the mean values and standard deviations. The developed methods were successfully applied to estimate the amount of Prednisolone in pharmaceutical formulations....
The present paper describes the potential and frequent problems occurring during estimation of commonly used artimisinine derivatives and other potential antimalarial agents used in treatment of falciparum from biological samples, pharmaceutical formulation and bulk as the effectiveness of the treatment depends upon the stability of samples. The focus is also on associated problems of stability of such agents during estimation period so one can utilize the knowledge for betterment in maintaining controls and measures during analysis....
An accurate and precise RP-HPLC method was developed for the simultaneous estimation of metoprolol succinate and telmisartan in tablets. The chromatographic analysis was performed on 4.6´250 mm BDS hypersil C18 HPLC column with 5 mm (particles) packing with mobile phase consisting of acetonitrile and potassium di-hydrogen orthophosphate buffer (pH-3.01) in the ratio 50:50v/v, at a flow rate of 1.0 ml/min and eluents monitored at 225 nm. The retention time for metoprolol succinate was found to be 2.250 and for telmisartan it was found to be 6.397 minutes. The proposed method was simple, accurate and precise and could be successfully employed in routine quality control for the simultaneous estimation of telmisartan and metoprolol succinate in tablet formulation....
A simple reverse phase high performance liquid chromatographic (RP-HPLC) method was developed for the simultaneous estimation of atropine sulphate, chloramphenicol and dexamethasone sodium phosphate in eye drops formulation. The determination was carried Hiber® 250-4.6 mm, Lichrosher® 100, RP-18 (5 µm, 250 mm L × 4.6 mm Ø) column using a mobile phase of acetonitrile and phosphate buffer (pH 3, 0 min 10:90% v/v and 10 min 60:40% v/v, gradient). The flow rate was 1.2 ml/min with detection at 227 nm. The retention time for atropine sulphate was 9.34, for chloramphenicol 10.62 min and for dexamethasone sodium phosphate 13.50 min. The linearity range was 120-200 µg/ml, 60-100 µg/ml and 12-20 µg/ml for atropine sulphate, chloramphenicol and dexamethasone sodium phosphate respectively. The percentage recoveries obtained for atropine sulphate, chloramphenicol and dexamethasone sodium phosphate ranges from 99.62% - 100.62%, 99.23% - 98.70% and 98.62% - 100.73% respectively....
A simple, rapid, accurate, precise and economic RP-HPLC method was developed for the estimation of pharmaceutical dosage forms using c18 column (250×4.6 mm i.d; 5µm) with mobile phase comprising of methanol and phosphate buffer in ratio of 30:70 (% v/v) triethylamine as ion pair reagent. The flow rate 1.2 ml/min and the detection was carried out at 221 nm with variable wavelength detector. The retention time (t r) of calcium dobesilate and docusate sodium was found to be 1.93 and 2.20 min, respectively. The method has permitted linear response in concentration range of 5-25 µm/ml for and limit of detection and limit of quantification of calcium dobesilate and docusate sodium was found to be 4.60 and 1.29, respectively. The percentage recovery was found to be 99.66 to101.0 and % RSD of system precision and method precision of calcium dobesilate and docusate sodium was found to be 1.038, 1.29 and 1.03, 1.70 respectively. The method was validated as per ICH guidelines for various parameters such as accuracy, precision, linearity, robustness....
A simple method is developed and validated for the simultaneous determination of imipenem (IMI) and Cilastatin (CIL) by RP-HPLC. Chromatographic separation of the drugs, achieved on Syncronis C-18 (250×4.6mm, 5µ) column at 245 nm using mobile phase, comprising a mixture of Methanol:Buffer (0.5% w/ v Potassium dihydrogen orthophosphate, pH adjusted to 6 with 1N NaOH) in the ratio of 50:50 v/v, at a flow rate of 1 ml/min. Cilastatin and Imipenem were eluted at the retention times of 2.51 min. and 4.10 min. respectively. Calibration curves were linear over the range of 10 µg – 1000 μg/ml and r2 values were 0.999 for both drugs. The % assay of imipenem and cilastatin were found to be 99.8% and 100.6% respectively. The performance of the method was validated according to ICH guidelines. The proposed method was successfully applied for the determination of Imipenem and cilastatin in injection formulation....
The present research work describes two simple, sensitive and economically new methods for simultaneous determination of atorvastatin calcium and fenofibrate. The first method was based on UV spectrophotometric determination of two drugs using simultaneous equation method. It involves, the bulk and marketed formulations were estimated using methanol:water (50:50 v/v) as a solvent and maximum absorbance were determined at 243 nm for atorvastatin calcium and 292 nm for fenofibrate. Both the drugs were linear in the concentration range of 5-25 µg/ml and 3-15 µg/ml for atorvastatin calcium and fenofibrate respectively. The correlation coefficients also calculated from the calibration curve for both the drugs respectively were 0.999 and 0.9993 and the method was precise with % RSD of less than 2. The percent recovery was found to be 98.48-99.9 for atorvastatin calcium and 98.7-99.45 for fenofibrate. The second method was based on HPLC separation of two drugs in reverse phase mode using C18 column (Agilent ODS UG 5 Column 250 mm × 4.5 mm). Optimum results were obtained at 273 nm using acetonitrile : methanol : water (50:40:10) v/v as a mobile phase. The chromatograms confirm the presence of atorvastatin calcium and fenofibrate without any interference at 1.5 and 5.11 min, respectively. Linearity obtained in the concentration range of 10-50 µg/ml for both the drugs. The proposed methods were successfully applied for the simultaneous determination of drugs in a pharmaceutical formulation. The developed methods were validated according to ICH guidelines....
Simple, accurate and economic method of HPTLC has been described for the simultaneous estimation of abacavir sulfate and lamivudine from tablet dosage form. Abacavir sulfate shows absorption maximum at 284.0 nm and lamivudine shows absorption maximum at 270.0 nm in distilled water. Beers law was obeyed in the concentration range of 100-700 ng/spot for both abacavir sulfate and lamivudine in tablet dosage form. The coefficient correlations were found to be 0.997 for LAM and 0.9979 for ABAC respectively in tablet dosage form. Analytical methods employed for quantitative determination of drugs are the key determinants in generating reproducible and reliable data that in turn are used in the evaluation and interpretation of bioavailability, bioequivalence and pharmacokinetics. Absolute recovery of abacavir sulfate ranged from 99.70% while lamivudine recoveries found to be 100.23%....
A simple, sensitive, precise and accurate new UV-visible spectrophotometric method has been developed for estimation of ibuprofen and carisoprodol in synthetic mixture. The method was based on employing absorption ratio method for analysis of both drugs. The proposed method employs the derivatization of carisoprodol by reagent 1,2-Naphthoquinone-4-sulfonic acid sodium salt in the presence of borate buffer at optimize condition. Linearity range was observed in the concentration range of 40-90 ?g/ml for carisoprodol and 80-180 ?g/ml for Ibuprofen. The method involved simultaneous analysis based on the measurement of absorbance at two wavelengths, i.e., iso-absorptive point of both drugs (260.60 nm) and ?max of ibuprofen (265.0 nm). The method was validated statistically and recovery study was performed to confirm the accuracy of the method....
Eugenol shows various biological activities such as antioxidant, anti-inflammatory, antibacterial, antifungal and antiviral. The present study describes the degradation behaviour of eugenol under different stress conditions (hydrolysis, oxidation, photolysis and thermal decomposition) in order to establish a validated stability-indicating high-performance liquid chromatography method. The method which was developed have the acetonitrile and phosphate buffer (85:15) as a mobile phase and the detection was carried out at 280 nm, at flow rate of 1.2 ml/min. The retention time of eugenol was 7 minutes. Validation of the method was also performed in which linearity, precision, limit of detection, limit of quantitation and robustness was performed....
This paper discussed the requirement of GMP that manufacturer identifies what validation work is needed to prove control of the critical aspects of their particular operations. The legal requirement for all regulatory guidelines is that any system or process can only be regarded as validated if it is in full compliances with GMPs. It is important to remember that c-GMP are simply the best manufacturing practices industries can follow to produce product safely and efficiently while ensuring the highest possible quality. Furthermore elaboration of relationship between validation and GMP a major challenge in the pharmaceutical industry is to know where to apply GMP controls because if they are applied inappropriately, GMP tends to lock in practices and create barriers to effective changes. Validation is never to be restricted because they provide guidance in establishing and maintaining best possible manufacturing operations. Validation is a substantive discipline, requires by law; failure to comply is prosecutable as a criminal act in some countries....
Two chemometric methods, Classical least square and Inverse least square were applied for simultaneous estimation of aspirin and dipyridamole in their marketed pharmaceutical formulation. A considerable spectral overlap (87.1%) was observed in the range of 210 nm-360 nm. Beer’s law was obeyed for both drugs in the concentration ranges of 1-17 µg/ml and 3-23 µg/ml for both aspirin and dipyridamole, respectively. 25 mixtures were prepared and analyzed at 25 wavelength points between 210 nm-360 nm with the interval of 2 nm (Δλ = 2 nm). A validation set design of the concentration data corresponding to the aspirin and dipyridamole 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....
Cardiovascular diseases are one of the leading causes of death whereas hypertension remains a significant cause of cardiovascular morbidity and mortality. Failure of effective treatment forms a tremendous scope for the formulator to develop the new anti-hypertensive entity, dosage form or fixed dose combinations such as a newly approved combination of angiotensin receptor blocker and thiazide diuretic. With increase in development of fixed dose combinations there should be simultaneous increase in development of validated method for detection. In the present work RP-HPLC dissolution method was developed for simultaneous detection of azilsartan medoxomil potassium and chlorthalidone from the formulated tablet. The method was carried out using Zorbax XDB column (C8, 150 X 4.6 mm, 5 µ). The mobile phase was Buffer (pH 7.8): acetonitrile (650:350) and 2 ml of triethylamine with flow rate 1.0 ml/min at 240 nm detector wavelength. The retention time for azilsartan medoxomil potassium was found to be 2.6 min. and for chlorthalidone it was found to be 8.7 minutes. The developed method was found to be stable, simple and robust....
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