Current Issue : October-December Volume : 2014 Issue Number : 4 Articles : 36 Articles
Formulating the 12 principles of Green Analytical Chemistry (GAC), by modification of the Green principles made them more applicable towards Analytical chemistry. These principles hold importance in designing of new methods or instruments. The focus of greening a chemical method is by generating solvent-less techniques or using alternative solvents like ionic liquids. Miniaturization of separation techniques employing FAC instruments would be another approach to reduce solvent consumption and production of analytical wastes. Capillary electrophoresis was rather unknown for its use as an alternative in place of GC, until recently. Owing its wide application and use, greening chromatographic methods like HPLC, GC is the upcoming trend. Various newer techniques complying with the principles of GAC are a safer option over conventional non-green methods for analysis. The article is primarily an overview covering the introduction and development of green methods in analytical chemistry....
A simple, accurate and precise dual wavelength UV spectrophotometric method was developed for simultaneous determination of metformin hydrochloride and gliclazide in combined pharmaceutical dosage forms. The literature review reveals that there is no dual wavelength method was developed for this combination of drugs, hence this method was developed. The wavelengths selected for determination of metformin hydrochloride were 222.35 nm and 228.94 nm, whereas, the wavelengths selected for determination of gliclazide were 229.41 nm and 234.82 nm. Methanol and distilled water were used as the solvents. Regression analysis of Beer’s plots showed good correlation in concentration range of 5-30 μg/ml for metformin hydrochloride and 1-6 μg/ml for gliclazide. 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 0.162 μg and 0.0825 μg for metformin hydrochloride and gliclazide respectively and LOQ was found to be 0.492 μg and 0.25 μg for metformin hydrochloride and gliclazide respectively. The proposed method was successfully applied to determination of these drugs in laboratory-prepared mixtures and commercial tablets....
Donepezil is an oral medication used to treat alzheimer’s disease. Chemically the drug is 2,3-dihydro-5, 6-dimethoxy-2-[(1-(phenyl methyl)-4-piperidinyl) methyl]-1H-inden-1-onehydrochloride. Several methods such as HPLC, LC/MS/MS, HPLC/MS. Donepezil has been tested in other cognitive disorders including lewy body dementia and vascular dementia but it is not currently approved for these indications. Donepezil has been found to improve sleep apnea in Alzheimer’s patients. The studies found that speech of austistic children who were mild to moderately affected appeared to improve from the use of donepezil medication. Memantine HCl (MEM) which is chemically 1‐Amino‐3, 5‐dimethyltricyclo decane hydrochloride is an NMDA (Nmethyl‐D‐aspartate) receptor antagonist 3,4 used to slow or reverse the neuro‐degenerative process of alzheimer’s disease. A number of methods such as UPLC, LC‐MS were reported for the estimation of MEM. Literature survey reveals that visible spectrophotometric methods and stability studies have not been reported for its quantitative determination in combination pharmaceutical formulations. The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamic and pharmacokinetic studies as well as stability study. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed....
Olmesartan medoxomil is a new orally active angiotensin II type 1 receptor antagonist used as an anti-hypertensive agent. It is a prodrug and is rapidly de-esterified during absorption to form olmesartan, the active metabolite. Indapamide is an orally administered diuretic and anti-hypertensive drug. Its molecule contains both a polar sulfamoyl chlorobenzamide moiety and a lipid soluble methyl-indoline moiety. It differs chemically from thiazide in a way that it does not possess the thiazide ring system and contains only one sulfonamide group. Currently most commonly prescribed medicines for hypertension are angiotensin receptor blockers and diuretics. Monotherapy with oral anti-hypertensive agents is not sufficient to achieve target blood pressure levels and henceforth, a combination tablet formulation is beneficial in terms of its convenience and patient compliance. The present drug combination has promising anti-hypertensive effect. The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamic and pharmacokinetic studies as well as stability study. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed. This review covers 50 analytical methods including spectrophotometric methods like spectrophotometry, chromatographic method including HPLC, HPTLC were reported....
A simple, accurate, sensitive and rapid second order derivative UV spectroscopic method for simultaneous estimation of both the drug in synthetic mixture. In this method detection was carried out at 292 nm (ZCP of naltrexone hydrochloride) and 240. nm (ZCP of pentazocine hydrochloride). The UV spectroscopic method for naltrexone hydrochloride and pentazocine hydrochloride was found to be linear over the range of 5-9 μg/ml and 500-900 μg/ml respectively for the second derivative method. Correlation coefficient for naltrexone hydrochloride and pentazocine hydrochloride was found to be 0.998 and 0.998 respectively. Accuracy (% recovery) for naltrexone hydrochloride and pentazocine hydrochloride was 98.00% - 99.40% and 98.70% - 99.24% respectively....
A simple, efficient and reproducible RP-HPLC method for the simultaneous estimation of ezetimibe and rosuvastatin in bulk and tablet dosage form has been developed and validated. The separation was carried out on ZORBAX SB C18 column (4.6 mm X 150mm, 3.5 �µm) column using potassium dihydrogen orthophosphate buffer (adjusted to pH2.5 with 0.1% OPA): methanol : acetonitrile in the ratio of 45:40:15 (v/v/v) as eluent. The flow rate was 1.5 ml/min and effluent was detected at 242 nm. The retention time of ezetimibe and rosuvastatin were 5.046 and 3.030 min. respectively. The linear dynamic range was 4-20 ppm for ezetimibe and 4-25 ppm for rosuvastatin respectively. Percentage recoveries for ezetimibe and rosuvastatin were 99.98% and 100.6% respectively. All the analytical validation parameters were determined and found in the limit as per ICH guidelines, which indicates the validity of the method. The developed method was also found to be precise and robust for the simultaneous determination of ezetimibe and rosuvastatin....
Aceclofenac and pregabalin in combination have significant reduction in pain as compared to individual drug in chronic low back pain. Literature reveals that all the reported spectrophotometric methods are either need tedious extraction procedures or do not offer high sensitivity, uses non specific reagent and/or recommend the measurement of absorbance in the near UV region where interference most probably occurs that do not offer suitable linearity range. A novel, accurate, precise and extraction free UV spectrophotometric method has been developed for simultaneous estimation of aceclofenac (ACF) and pregabalin (PGB) in combined dosage form. The method employed was First order derivative method. The method is based on the reaction of pregabalin with 1,2-naphthaquinone-4-sulphonate sodium (NQS), yielding an orange colored product. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. Method involves measurement of ACF at 281.0 nm (ZCP of PGB) and measurement of PGB at 246.0 nm (ZCP of ACF). Rectilinear relationship with good regression coefficient 0.997 and 0.999 were found over the concentration ranges of 5-25 μg/ml and 3.75-18.75 μg/ml for ACF and PGB, respectively with detection limit 0.40 and 0.60 μg/ml and quantitation limit 1.22 and 1.82 μg/ml. The mean percentage recoveries were ranged 98.38 – 99.27 and 98.43 – 100.34 for ACF and PGB, respectively. The developed methods were successfully applied to the analysis of the drug in its commercial tablet....
Atorvastatin is the most efficacious of the currently available HMG-CoA Reductase inhibitors used in anti lipidemic and also used in atherosclerosis, stroke and cardiac risk. The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamics and pharmacokinetic studies as well as stability study. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed. This review covers the most recent many analytical methods including spectrophotometric methods, chromatographic method including HPLC, HPTLC and RP HPLC, liquid chromatography tendam mass spectroscopy were reported....
The main objective of the study was to develop a simple, specific and reliable method for quantification of ivacaftor and its impurities in samples by high performance liquid chromatography. The separation of these compounds was achieved on a C18 column using a gradient mobile phase consisting of phosphoric acid and acetonitrile. The analysis was performed at a flow rate of 1.0 ml/min and detection wavelength of 220 nm. The specificity, linearity, sensitivity, accuracy, precision and robustness were examined as part of method validation. Forced degradation showed that ivacaftor does not undergo degradation under heat, oxidation and photolysis but that it was susceptible to acidic and basic conditions....
The objective was to develop and validate suitable HPTLC method for simultaneous determination of Timolol maleate and Bimatoprost in ophthalmic dosage form. Materials and Methods: Chromatographic separation was carried out on TLC plate pre-coated with silica gel 60F254 using Ethyl acetate: Toluene: Methanol: Formic acid (3.5: 3.0: 1.5: 0.1 v/v/v/v) as mobile phase and scanning the plate at 260 nm. The Rf value for Timolol maleate and Bimatoprost were 0.30 and 0.54 respectively. The method was linear in the concentration of 3417.70-17088.50 ng/band for Timolol maleate and 150-750 ng/band for Bimatoprost with a correlation coefficient of 0.998 and 0.999 for Timolol maleate and Bimatoprost respectively. The percentage recoveries obtained for Timolol and Bimatoprost in the range of 99.31-101.39% and 99.80-101.23% trespectively. The result of analysis have been validated as per the International conference on Harmonisation (ICH) guidelines. The developed methods adequately separated both the drugs. Validation results indicated that the method shows satisfactory linearity, accuracy, precision and found to be specific. So, the proposed methods can be used successfully for routine analysis of Timolol maleate and Bimatoprost in ophthalmic dosage form by HPTLC....
A simple, accurate and rapid reversed phase high performance liquid chromatographic method has been developed and validated for the simultaneous estimation of sildenafil citrate (SIL) and dapoxetine hydrochloride (DPX) in simulated dosage form. The separation was carried out using mobile phase consisting of methanol: 25 mM phosphate buffer (pH, 2.6) (50:50, v/v). The column used was ACE C18, (150 mm x 4.6 mm i.e., 5 µm) with flow rate 1.2 ml/min using PDA detection at 292 nm. The method was linear over a concentration range 30-90 μg/ml for sildenafil citrate (SIL) and 18-54 μg/ml for dapoxetine hydrochloride (DPX) Respectively. The retention time of sildenafil citrateand dapoxetine hydrochloride were found to be 5.2 min and 9.2 min respectively. Results of analysis were validated statistically and by recovery studies. The mean recovery was 99.29±0.54a nd 99.03±0.45for SIL and DPX respectively. The limit of detection (LOD) and the limit of quantification (LOQ) for SIL and DPX were found to be 0.6586 and 1.9956 µg/ml and 0.6169 and 1.8695 µg/ml, respectively. The results of the study showed that the proposed RP-HPLC method was found to be simple, sensitive, precise and accurate and also useful for the routine determination of SIL and DPX in mixture....
A simple, sensitive, rapid and reproducible reversed-phase HPLC methods has been developed and validated for simultaneous determination of cefixime trihydrate and levoflaxacin hemihydrate in pharmaceutical formulation. The HPLC analysis was performed on the C-8, 15 cm, 4.6 mm and 5 micron (waters) column, at ambient temperature using phosphate buffer: acetonitrile (70:30) as mobile phase and pH adjusted to 8.0 with triethyl amine. The flow rate was adjusted to 0.8 ml/min. The detection was carried out at 283 nm. Linearity was found to be in concentration range of 10-50 µg/ml for CEFI and LEVO with coefficient of correlation 0.999 and 0.999 respectively. LOD was found to be 0.00075 and 0.0002 for CEFI and LEVO respectively and LOQ was found to be 0.0022 and 0.059 for CEFI and LEVO respectively. Due to these attributes, the proposed method could be used for routine quality control analysis of these drugs in combined dosage forms. The method was validated as per ICH guidelines....
Two Simple, precise, accurate and economical UV methods have been developed and validated for the quantitative estimation of cefdinir in bulk and pharmaceutical dosage form. Cefdinir has the absorbance maxima at 286 nm in methanol: distilled water (20:80). In the Method A, first order derivative spectra, cefdinir showed absorbance maxima at 273 nm and method B involved solving simultaneous equations based on measurement of area under curve at wavelength range 284-288 nm. The linearity for cefdinir was in the range of 5-50 μg/ml. The developed methods were validated according to ICH guidelines and were found to be accurate, economic and precise. The proposed methods can be successfully applied for the estimation of Cefdinir in bulk and pharmaceutical dosage forms....
A simple, efficient and reproducible stability indicating RP-HPLC method for the simultaneous determination of esomeprazole and domperidone in pharmaceutical dosage form has been developed and validated. The separation was carried out on hypersil BDS column C18 (250 mm X 4.6 mm X 5µm) column using acetonitrile: potassium dihydrogen orthophosphate buffer (adjusted to pH 4.8 with 0.1% OPA): methanol in the ratio of 40:40:20 (v/v/v) as eluent. The flow rate was 1.0 ml/min and effluent was detected at 285 nm. The retention time of esomeprazole and domperidone were 2.959 and 3.465 min. respectively. The linear dynamic range was 20-120 ppm for esomeprazole and 15-90 ppm for domperidone, respectively. Percentage recoveries for esomeprazole and domperidone were 99.84% and 99.91% respectively. All the analytical validation parameters were determined and found in the limit as per ICH guidelines, which indicates the validity of the method. The developed stability indicating method was also found to be precise and robust for the simultaneous determination of esomeprazole and domperidone in capsule dosage forms....
The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric method for estimation of guaifenesin. This method was based on area under curve of UV spectrum between 268 to 278 nm and validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 10-70 µg/ml. The value of correlation coefficient was 0.999. 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 (96.42 % to 96.88 %) showed accuracy of the method. LOD and LOQ were calculated as 1.69 µg/ml and 5.13 µg/ml, respectively. The developed method can be used for routine estimation of guaifenesin in bulk and tablet dosage forms....
The aim of present was to develop an accurate, precise, reproducible and economical UV spectrophotometric area under curve method for estimation of propranolol hydrochloride. This area under curve of UV spectrum between 279 to 299 nm was validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 5-30 μg/ml. The value of correlation coefficient was 0.999. 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 (99.33% to 99.99%) showed accuracy of the method. LOD and LOQ were calculated as 0.2310 μg/ml and 0.7001 μg/ml, respectively. The developed method can be used for routine estimation of propranolol hydrochloride in bulk and tablet dosage forms....
A simple, accurate, precise and sensitive UV spectrophotometric method was developed for the determination of fexofenadine HCl in bulk and suspension dosage form. The solvent used is methanol and the wavelength corresponding to maximum absorbance of the drug was found at 220 nm. Beer’s law was observed in the concentration range of 5 – 20 μg/ml with correlation coefficient 0.993. The linear regression equation obtained by least square regression method were y=0.051x + 0.002, where y is the absorbance and x is the concentration of the pure drug solution. The method was validated for several parameters like accuracy, precision as per ICH guidelines Q2 (R1). The values of relative standard deviation and % recovery were found to be satisfactory, indicating that the proposed method is precise and accurate and hence can be used for the routine analysis of fexofenadine hydrochloride in bulk and suspension dosage form....
A simple, sensitive, reproducible, and cost-effective UV-spectrophotometric method has been developed and validated for the estimation of terbinafine hydrochloride in semisolid dosage forms. The method was based on detection of terbinafine hydrochloride at 221 nm using phosphate buffer solution pH 5.8 as the solvent system since this allows detection of the drug at the pH of skin (5-6). The developed method was validated with respect to linearity, accuracy (recovery), precision (inter-day and intra-day variations) and sensitivity (LOD and LOQ). Linearity was observed in the concentration range of 1-5 μg/ml with correlation coefficient of 0.9938. Results of the analysis were validated statistically and by recovery study. The per cent recovery of terbinafine hydrochloride ranged from 98.47–102.03%. The developed method was found to be precise with % RSD value of 0.903%. The study concluded that the UV-spectrophotometric method could be used for the quantification of terbinafine hydrochloride in pure form as well as in pharmaceutical formulations....
Diltiazem is a calcium channel blocker type antihypertensive drug. Diltiazem is a class of calcium channel blockers, used in the treatment of hypertension, angina pectoris and some types of arrhythmia. It is also an effective preventive medication for migraine. The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamic and pharmacokinetic studies as well as stability study. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed. This review covers the most recent many analytical methods including spectrophotometric methods, chromatographic method including HPLC and RP HPLC, liquid chromatography tendam mass spectroscopy, colorimetry and potentiometry were reported....
Pharmaceuticals impurities are the unwanted chemicals that are either generated during the formulation of the dosage form or are present during the initial synthesis. Thus the control of pharmaceutical impurities is currently a very critical issue to the pharmaceutical industry. The International Conference on Harmonization has formulated a workable guideline to control the impurities of the pharmaceuticals. Impurity profiling helps in the detection, identification and quantification of various types of impurities as well as residual solvents present in bulk drugs as well as in pharmaceutical formulation is done with the help of impurity profiling. Identification of the presence of impurities below 0.1% level is not considered to be important as per the ICH guidelines on impurities in new drug product unless the potential impurities are expected to be unusually potent or toxic. However in all cases, impurities should be qualified as it is the best way to characterize quality and stability of bulk drugs and pharmaceutical formulations. It is imperative to review problems related to impurities present in the drug substances and drug products with their solutions due to rapid development of the analytical methodology. 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....
Two precise, simple, accurate, reproducible, rapid and economical UV spectrophotometric methods have been developed for simultaneous estimation of norfloxacin and loperamide in capsule dosage form by using 0.1M methanolic HCl as a solvent. Method I is based on simultaneous equation method, known as vierodt’s method. Norfloxacin and loperamide show absorbance maxima at 277 nm and 259 nm respectively. Method II is based on principle of Q-analysis, known as absorbance ratio method in which absorbance of both drugs was measured at 268 nm (Isobestic point) and 277 nm (λmax of norfloxacin). Norfloxacin and loperamide obeys Beer’s law in the concentration range of 5 to 30 µg/ml and 10 to 60 µg/ml respectively. Both methods are validated according to ICH guidelines and can be applied for routine analysis of these drugs in capsule dosage form....
A high performance liquid chromatography method is used for the determination of dabigatran and its impurities in the presence of its degradation products using a reverse phase chromatography tech by C8 column at 30°C temperature with a mobile phase consisting of phosphate buffer and acetonitrile with gradient program. The flow rate was 0.8 ml/min. Quantification was achieved with UV detection at 220 nm based on maximum absorbance. The method was validated for specificity, linearity, accuracy, precision, sensitivity and robustness. The method was found to be suitable for the quality control of dabigatran in bulk drug and dosage form....
Nifedipine is a calcium channel blocker type antihypertensive drug. Nifedipine is a class of calcium channel blockers, used in the treatment of hypertension, angina pectoris and some types of arrhythmia. It is also an effective preventive medication for migraine. The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamic and pharmacokinetic studies as well as stability study. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed. This review covers the most recent many analytical methods including spectrophotometric methods, chromatographic method including HPLC and RP HPLC, liquid chromatography tendam mass spectroscopy, colorimetry and potentiometry were reported....
The polymorphism of drugs has been the subject of intense interest in the pharmaceutical industry. Polymorphism presents a challenge to pharmaceutical scientists who wish to produce drugs of consistent quality. The potential impact of changing crystal forms during late-stage drug development, in terms of cost and product delay, justifies systematic and early characterization of polymorphs. The techniques considered – crystallography, spectroscopy, microscopy and thermal techniques – examine different aspects of structure, dynamics and energetics of a compound in the solid state. DSC is a thermal method of analysis that is widely used to study thermal transitions. HSM is an analytical technique which combines the properties of microscopy and thermal analysis to enable the solid state characterization of materials. The XRPD technique captures the three dimensional diffraction patterns in a two-dimensional plot. NMR spectroscopy indicates the presence of configurational or conformational multiplicity present in the solid state. All these techniques have enabled comprehensive and advanced understanding of polymorphic forms which are recorded more quickly and accurately....
The present work describes Q-absorbance spectrophotometric method for simultaneous estimation of tapentadol and thiocolchicoside in tablet dosage form. It employs development of Q-absorption ratio method using two wavelengths 272 nm of tapentadol and 265 nm an Iso-bestic point of both the drug. The method obeys beer’s law in the employed concentration range of 5-35 μg/ml for thiocolchicoside and 50-250 μg/ml for tapentadol at their respective wavelengths. Results of analysis were validated statistically and by recovery studies....
The aim of present work was to develop an accurate, precise, reproducible and economical UV spectrophotometric method for estimation of Agomelatine. This method was based on Area Under Curve of UV spectrum between 225 to 235 nm and validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 0.5-3�µg/ml. The value of correlation coefficient was 0.999. 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 (99.66 % to 99.95 %) showed accuracy of the method. LOD and LOQ were calculated as 0.581�µg/ml and 1.935�µg/ml, respectively. The developed method can be used for routine estimation of Agomelatine in bulk and tablet dosage forms....
A simple, sensitive, rapid and reproducible reversed-phase HPLC method has been developed and validated for estimation of salbutamol sulphate and beclomethasone dipropionate in metered dose inhaler formulation. The assay involved an isocratic elution of these two components on water spherisorb, CN, ( 250 mm × 4.6 mm, 10.0 µm) column using a mobile phase composition of buffer: acetonitrile: (60:40). The flow rate was 1.2 ml/min; column oven temperature 25°C and the analytes monitored at 265 nm. Separation was completed within 10 min. Calibration curves were linear with coefficient correlation (R2) 0.999 over a concentration range of 1.0-14.95 μg/ml for salbutamol sulphate and 0.51-7.58 μg/ml for beclomethasone dipropionate respectively. All the validation parameters were within the acceptance range according to ICH norms. The Method has been successfully applied for analysis of drugs in pharmaceutical formulation. Results of analysis were validated statistically and by recovery studies....
A simple, rapid and accurate reversed-phase HPLC method was developed and validated for the simultaneous determination of lamivudine (LMV) and zidovudine (ZDV) in tablet dosage form and applied for stress degradation studies. The proposed RP-HPLC method utilizes qualisilgold C18, 5 µm, 250 mm×4.6 mm i.d. column, mobile phase consisting of methanol and water in the proportion of 30:70 (v/v) at a flow rate of 1 ml/min and UV detection at 266 nm using photodiode array detector. The linearity of the proposed method was investigated in the range of 2-24 µg/ml (r = 0.999) for LMV and 3-48 µg/ml (r = 0.999) for ZDV. The limit of detection was 0.01 µg/ml and 0.1 µg/ml for LMV and ZDV. The limits of quantification were 0.05 µg/ml and 0.3 µg/ml for LMV and ZDV, respectively. LMV, ZDV and their combination were exposed to hydrolytic, oxidative, thermal and photolytic stress conditions as recommended by ICH guidelines. Degradation products produced as a result of stress studies did not interfere with the detection of LMV and ZDV and can be applied to the analysis of samples obtained during stability studies....
Now-a-days there is increase in the prevalence of co-existent type 2 diabetes mellitus and hypertension due to sedentary lifestyle and changing food habits. Number fixed dose combinations are available in the market, for treatment of co-existent type 2 diabetes mellitus and hypertension. Large group of population is being treated successfully with the combination of metformin HCl, telmisartan and atorvastatin calcium. There is need to establish a simultaneous detection method for these pharmacological agents. So a multi-component UV spectroscopic method for the simultaneous determination of anti diabetic and anti hypertensive drugs like metformin HCl, telmisartan and atorvastatin calcium has been developed and validated. method for Estimation of drugs was done at four wavelengths 225 nm, 255 nm, 285 nm and 315 nm. Method was validated by accuracy and precision studies....
Agomelatine is a new melatonergic antidepressant with a unique pharmacological action. A UV spectroscopy and stability-indicating RP-HPLC method was developed and validated for the determination of agomelatine in active pharmaceutical ingredient and tablet dosage form. In UV spectroscopic method methanol was used as solvent and λmax was found at 230 nm. Beer’s law was observed in the concentration range of 0.5-3 μg/ml (R2 = 0.997). LOD and LOQ were 0.04798 and 0.145395 μg/ml respectively. The method was validated for several parameters like accuracy, precision. The values of % RSD and % recovery were found to be satisfactory. RP-HPLC method was developed using thermo BDS hypersil C18 column (250 × 4.6 mm, 5μm) in isocratic mode. The mobile phase consisted of acetonitrile: 15 mM phosphate buffer pH 5 (40:60 v/v) with a flow rate of 1.0 ml/min (UV detection- 230nm). The retention time was found to be 6.9 min. Linearity was observed over the concentration range of 5-30 μg/ml (R2 = 0.996). The method is accurate and recovery was found to be in the range of 99.89-100.19%. The limit of detection of agomelatine was found to be 0.1218 μg/ml and limit of quantitation was found to be 0.3691 μg/ml. Agomelatine was subjected to stress conditions including acidic, alkaline, neutral, oxidation and thermal degradation. Agomelatine is more sensitive to acidic, basic and oxidative degradation. These methods were validated according to ICH guidelines....
The objective was to develop a simple, economical, accurate and precise stability indicating RP-HPLC for simultaneous estimation of levofloxacin and ambroxol in combined tablet dosage form. Stability indicating RP-HPLC method was developed and validated for simultaneous estimation of levofloxacin and ambroxol using ACE C18 column (5 µ,150 × 4.6mm) and methanol: buffer KH2PO4 (pH 5 ) in a volume 35:65 v/v as mobile phase with 221 nm. Stability indicating RP-HPLC method was developed and validated. The method successfully separated levofloxacin and ambroxol from its degradation product formed under stressed conditions. Levofloxacin and ambroxol degraded significantly under acidic, alkaline and oxidative conditions. The method was found to be linear in range at 20-100 μg/ml of LVF and 3-15 μg/ml of AMB and the % recovery was found in the range of 98.43 - 98.72% and 99.18 - 99.99% and % assay was found to be 99.46 and 100.54 for LVF and AMB, respectively. The proposed SIAM method was found to be simple, accurate, economical, robust and reproducible....
A fixed dose combination of levofloxacin hemihydrate (quinolone antibiotic) and cefpodoxime proxetil (cephalosporin) was used in ratio of 1:1.25 as tablet for the treatment of resistant lower respiratory tract and other infections. A simple, precise and accurate stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for determination of levofloxacin hemihydrate (LVF) and cefpodoxime proxetil (CPD) in tablet dosage form. Isocratic RP-HPLC separation was achieved on an ACE C18 column (150 × 4.6 mm id, 5 µm particle size) using the mobile phase consists a mixture of 0.5% (v/v) triethylamine in 25 mM Sodium dihydrogen ortho-phosphate dihydrate buffer (pH 6.0)–methanol (52:48 v/v) at a flow rate of 1.0 ml/min. The retention time of levofloxacin hemihydrate and isomers of cefpodoxime proxetil were 4.7 min and 9.6, 11.6 min, respectively. The detection was performed at 273 nm. The method was validated for linearity, precision, accuracy, robustness, solution stability and specificity. The method was linear in the concentration range of 6.25–37.5 µg/ml for levofloxacin hemihydrate and 5–30 µg/ml for cefpodoxime proxetil, with a correlation coefficient of 0.9999 and 0.9999 for the respective drugs. The accuracy (recovery) was found to be in the range of 98.56-100.16% and 99.1–100.81% for levofloxacin hemihydrate and cefpodoxime proxetil, respectively. Levofloxacin hemihydrate was only degraded under oxidative conditions while cefpodoxime proxetil was degraded in all conditions. The drugs could be effect effectively separated from different degradation products and hence the method can be used for stability analysis....
The present work describes development and validation of a stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination of trace level impurities of metoprolol succinate (MET) and hydrochlorothiazide (HCTZ) in their tablets. The stressed degradation study including acid, base, H2O2, thermal and photolytic conditions were performed on MET and HCTZ tablets as per ICH guidelines to prove the stability-indicating capability of the developed method. Degradation was observed in acidic, alkaline, oxidative, thermal condition while no degradation in UV radiation conditions. Chromatographic separation was achieved on Hypersil BDS C18 150*4.6mm column using methanol:water:acetronitrile (60:20:20 v/v/v) using mobile phase. Flow rate was 1.0 ml/min and detection wavelength was carried out at 226 nm. All the known and degradation impurities were separated within 7 minutes. The LOD of MET and HCTZ were found to be 0.34 and 0.10 respectively. The LOQ of MET and HCTZ were found to be 1.03 and 0.31 respectively....
The present work describes development and validation of a simple, sensitive, precise, robust and stability-indicating high-performance liquid chromatographic method of analysis of flunarizine dihydrochloride, as a bulk drug. The separation was achieved by using a mobile phase of acetonitrile: monobasic ammonium phosphate buffer 0.1M pH 3.1 (55:45, v/v) and thermoscientific BDS-Hypersil column (250 mm X 4.6 mm, 5 μm) at flow rate of 1.0 ml/min. The detection was done at 253 nm. The retention time of flunarizine dihydrochloride was 6.48±0.5 min. This method has been successively applied to pharmaceutical dosage form. No chromatographic interference from the tablet excipient was found. Flunarizine dihydrochloride was subjected to stress conditions of hydrolysis, oxidation and thermal degradation. The degraded products were well resolved from the pure drug with significantly different retention time values. Linearity was found to be in the range of 25–100 μg/ml with significantly high value of correlation coefficient. The method was validated for precision, robustness and recovery. The limit of detection and quantization were 1.35 μg/ml and 4.11 μg/ml. The acid degraded product of flunarizine dihydrochloride was subjected to LCMS analysis. From the mass spectral data of degraded product, possible degradation pathway was outlined....
The CRO as well as Pharmaceutical manufacturers must validate their cleaning procedure to ensure compliance with GMP guidelines. Minimizing equipment downtime has the potential to influence the efficacy and economics of pharmaceutical production. The main purpose of cleaning validation is to prove the effectiveness and consistency of cleaning in a given pharmaceutical production equipment to prevent cross contamination and adulteration of drug products with other active ingredients like unintended compounds or microbiological contamination, leads to prevent several serious problems and also useful in related studies like packaging component cleaning validation. So it is necessary to validate the cleaning procedures to ensure safety, efficacy, quality of the subsequent batches of drug product and regulatory requirements in Active Pharmaceutical Ingredients (API) product manufacture. The benefits due to cleaning validation are compliance with federal regulations, identification and correction of potential problems, previously unsuspected which could compromise the safety and efficacy of drug products. In this article cleaning, validation and importance are discussed in brief....
A simple, precise, accurate and economical spectrophotometric method has been developed for estimation of guaifenesin. The standard and sample solutions were prepared by using methanol as a solvent. Quantitative determination of the drug was performed at 273 nm. The linearity was established over the concentration range of 10-70 μg/ml. The correlation coefficient was found to be 0.998. Precision studies showed that % relative standard deviation was within range of acceptable limits (<2). The mean percentage recovery was found to be 99.22%. The proposed method has been validated as per ICH Q2 (R1) guidelines....
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