Current Issue : January - March Volume : 2015 Issue Number : 1 Articles : 13 Articles
A simple, accurate and precise dual wavelength UV spectrophotometric method was developed for simultaneous determination of paracetamol and metoclopramide hydrochloride in combined pharmaceutical dosage forms by using standard addition method. The literature review reveals that there was no dual wavelength method was developed for this combination of drugs, hence this method was developed. The wavelengths selected for determination of paracetamol were 266.2 nm (ƛ1) and 276.5 nm (ƛ2), whereas, the wavelengths selected for determination of metoclopramide hydrochloride were 235.4 nm (ƛ3) and 251.7 nm (ƛ4). Methanol and distilled water were used as solvents. Regression analysis of Beer’s plots showed good correlation in concentration range of 5-30 μg/ml for paracetamol and 5-30 μg/ml for metoclopramide hydrochloride. Accuracy of method was found between 98.63-99.50%. The precision (intra-day, inter-day and analyst to analyst) of method was found within limits (% CV<2). LOD was found to be 0.3 μg and 0.116 μg for paracetamol and metocloprmide hydrochloride respectively and LOQ was found to be 0.909 μg and 0.352 μg for paracetamol and metocloprmide hydrochloride respectively. The proposed method was successfully applied to determination of these drugs in laboratory-prepared mixtures and commercial tablets....
A novel, rapid and a stability-indicating reverse phase LC method has been developed and validated for the simultaneous estimation of darunavir and ritonavir in tablet dosage form. The chromatographic separation was achieved on a novel core shell technology C4 stationary phase of particle size 3.6 µ. The method employed a linear gradient elution and the detection wavelength was set at 240 nm. The mobile phases(s) consist of buffer, acetonitrile and tetrahydrofuran delivered at a flow rate of 0.5 ml per minute. Proposed method was extensively validated as per ICH guidelines. Regression analysis shows r value (correlation coefficient) of greater than 0.999 for individual active drug substances. The samples were assayed against a qualified reference standard and the mass balance was found to be close to 98.3%....
In many resource limited countries, availability of cost effective instruments is a major problem. Hence accurate analysis cannot be done. Due to its high cost, HPLC is lacking in such countries. Again the cost of the column, solvents and time required for multiple analysis as well as mobile phase optimization is more. Therefore HPTLC is a good option over HPLC in terms of time as well as overall cost. Metformin HCl and glibenclamide are available in combined dosage form in market. Present study attempted for development and validation of high performance thin layer chromatography (HPTLC) method for simultaneous estimation of metformin HCl and glibenclamide using densitometric detection. Separation was performed using camag HPTLC system on silica gel 60F254 plates. The mobile phase was comprising of toluene: ethanol: formic acid (4.5:4.5:1.0 v/v/v). The detection wavelength was 230 nm. The Rf values of metformin HCl and glibenclamide were found to be 0.24±0.03 and 0.82±0.04, respectively. The method was validated as per ICH guidelines. A F-test indicated that calibration graphs were adequately linear at the evaluated concentration ranges. The pooled % RSD for repeatability of the percentage amount recovered for metformin HCl and glibenclamide were found to be 0.670 and 1.022. The percentage recoveries for the trueness were 99.86%±1.5 for metformin HCl and 99.61%±1.7 for glibenclamide (n = 3). The developed HPTLC method was found to be new, accurate, sensitive, precise and less time consuming as compare to published method. Thus it was successfully used to analyze fixed-dose tablets samples of metformin HCl and glibenclamide....
A novel reversed-phase liquid chromatographic method was developed for the quantitative determination of fingolimod and its related impurities. The chromatographic separation was achieved on a RP18 150 x 4.6 mm, 5 µ column and gradient program with mobile phase A as a pH 3.0 phosphate buffer and acetonitrile as mobile phase B. Fingolimod were monitored at 220 nm. Fingolimod was subjected to the stress conditions of acid, base, oxidative, thermal and photolytic degradation and found to degrade significantly under oxidative stress conditions. The degradation products were well separated from the main peak and its impurities, proving the stability indicating the power of the method. The method was validated according to the ICH guidelines for specificity, linearity, accuracy, precision, limit of detection, limit of quantification, ruggedness and robustness....
Alkyl tosylates or alkyl p-toluene sulfonates are very well known class of genotoxic impurities. As a genotoxic impurity, specified limits for these impurities are very low; hence sensitive analytical techniques are required for analyzing these impurities. Gas chromatographic method with mass spectrometer as detector was developed and validated for evaluating methyl tosylate, Isopropyl tosylate and butyl tosylate in clopidogrel bisulphate API. DB-5MS capillary column of 60 m length, 0.25 mm I.D and film thickness 0.25 m was selected. Ionization technique used was EI and the single Quadruple mass analyzer was used. By performing method validation it was verified that the method is sensitive, precise, accurate and linear. The maximum recommended daily dose of clopidogrel bisulphate is 300 mg. Hence, based on daily dose, evaluation as well as further specification limit is 5 µg/g. Limit of detection is 0.39 µg/g (0.02 µg/ml), 0.57 µg/g (0.03 µg/ml) and 0.16 µg/g (0.01 µg/ml) for methyl tosylate, isopropyl tosylate and butyl tosylate respectively. Similarly, Limit of quantification for methyl tosylate, isopropyl tosylate and butyl tosylate is 1.18 µg/g (0.06 µg/ml), 1.72 µg/g (0.09 µg/ml) and 0.5 µg/g (0.03 µg/ml) respectively. Linearity of all the three impurities is verified from LOQ to 150% of the evaluation level. Accuracy and precision of the method are evaluated. Analysis of commercial batches of Clopidogrel bisulphate is performed for these impurities and is concluded that the method is suitable to be extended for routine analysis....
Felbinac is a topical medicine, belonging to the family of medicines known as nonsteroidal anti-inflammatory drugs (NSAIDs). It is from the arylpropionic acid class; chemically the drug is 4-biphenyl acetic acid. It is used to treat muscle inflammation and arthritis. It is an active metabolite of fenbufen. Use as Analgesic, Antipyretic and anti-inflammatory agent. This review covers the most recent many analytical methods including chromatographic methods like Bioanalytical HPLC, HPLC, LC-MS/MS, fluorometric determination were reported....
Current research work describes rapid high performance thin layer chromatographic determination of artemether and lumefantrine form its combined pharmaceutical formulation. The mentioned drugs were spotted on silica gel F254 TLC plates under pure nitrogen stream by linomat TLC spotter. Separation was carried out by using chloroform, methanol, ethyl acetate and triethylamine as mobile phase in ratio of 4:2.5:3.5:0.1 v/v/v/v. Developed TLC plates were scanned by CAMAG TLC scanner and detection was carried out at 235 nm. Rf value of separated drugs was found to be 0.48 and 0.78 for artemether and nlumefantrine respectively. The developed method was validated as per ICH guidelines by studying various validation parameters like accuracy, precision, robustness, LOD, LOQ and solvent stability. The developed and validated method was successfully applied for determination of artemether and lumefantrine from its combined pharmaceutical formulation....
Escitalopram oxalate is antidepressant of the serotonin reuptake inhibitor (SSRI) class. It is used in for the treatment for the adults with major depressive disorder and generalized anxiety disorder. In the manufacturing process of Escitalopram, 3-Dimethylaminopropyl chloride hydrochloride (3-DMAPC) is one of the process raw materials. Also methane sulfonyl chloride is one of the reagent as well as Isopropyl alcohol is used as a solvent in the process. It is a well known reaction, that methane sulfonyl chloride reacts with alcohols to form respective alkyl methane sulfonate, hence monitoring of Isopropyl methane sulfonate (IPMS) was required in Escitalopram drug substance. The study was proposed for the analysis of 3-Dimethylaminopropyl chloride and Isopropyl methanesulfonate in Escitalopram oxalate drug substance. Method development and validation was conducted with Gas chromatography using Mass spectrometer as detector. Validation of the method was conducted based on International Conference on Harmonization (ICH) guidelines. The LOD and LOQ values were found to be 3 µg/g and 9 µg/g (i.e. 0.15 µg/mL and 0.45 µg/mL) respectively for 3-Dimethylaminopropyl chloride. The LOD and LOQ values were found to be 3 µg/g and 8 µg/g (i.e. 0.15 µg/mL and 0.40 µg/mL) respectively for Isopropyl methanesulfonate. Accuracy results for both the impurities were well within the acceptance criteria of 90 to 100%. Correlation coefficient values for linearity parameter were 0.9992 and 0.9991 for 3-DMAPC and IPMS respectively. Three batches of Escitalopram oxalate were analyzed for the analysis of 3-Dimethylaminopropyl chloride and Isopropyl methanesulfonate. The content for the both the compounds was not detected in all the three batches....
A simple, rapid and specific reversed-phase HPLC method has been developed for analysis of withaferin-A in a polyherbal formulation containing Withania somnifera extracts. HPLC analysis was performed on a C18 column using a 60:40 (v/v) mixture of acetonitrile and water as isocratic mobile phase at a flow rate of 1 ml/min. UV detection was at 230 nm. The method was validated for accuracy, precision, linearity, specificity and sensitivity in accordance with international conference on harmonization guidelines. Validation revealed that method was specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r2> 0.9993) were obtained for calibration plots in the ranges tested. Limit of detection was 0.05 and limit of quantification was 0.16 μg. Intra and inter-day RSD of retention times and peak areas were less than 2%. Recovery was between 98.15 and 100.69% obtained for withaferin-A. The established HPLC method was appropriate and withaferin-A was well resolved. The method was successfully used for quantitative analysis of withaferin-A in a polyherbal formulation....
A simple, rapid and precise reverse phase liquid chromatographic (RP-HPLC) method was developed and subsequently validated for simultaneous estimation of glipizide and simvastatin in bulk drug and in a synthetic mixture. The analysis was carried out using standard BDS C18 (BDS 100 x 4.6 mm, 5 μm, Make: Thermo electronics), prepacked column. The separation was carried out using a mobile phase containing 0.1% ortho phosphoric acid buffer and acetonitrile (20:80 v/v), was pumped at a flow rate of 1 ml/min with PDA detection at 234 nm. Both the drugs were well resolved on the stationary phase and the retention times were around 2.357 minute for glipizide and 6.140 minute for simvastatin. The method was validated and shown to be linear for glipizide and simvastatin. The correlation coefficients for glipizide and simvastatin are 0.9997 and 0.9999 respectively....
New stability indicating RP-HPLC method was developed and validated for the estimation of cinacalcet hydrochloride in tablet dosage form. The separation was achieved on C18, (250 mm x 4.6 mm x 5 µm) column using a mobile phase composition of 0.2% triethyl amine in water (pH-6.5 with OPA) and methanol (20:80% V/V). Eluents were detected at 225 nm at 1 ml/min flow rate. Stress studies were performed with milder conditions followed by stronger conditions so as to get sufficient degradation around 20%. A total of five degradation products were detected and separated from analyte. The linearity of the proposed method was investigated in the range of 40 - 160 µg/ml for cinacalcet. The limit of detection and limit of quantification was found to be 0.89 µg/ml and 2.69 µg/ml respectively. Precision % RSD was found to be less than 2% and the recovery was between 99-101%....
A simple, rapid and precise reverse phase liquid chromatographic (RP-HPLC) method was developed and subsequently validated for simultaneous estimation of moxifloxacin and metronidazole in bulk drug and in a synthetic mixture. The analysis was carried out using Hypersil ODS C18 (250 mm x 4.6 mm, 5m Make: thermo scientific) pre packed column. The separation was carried out using a mobile phase containing a buffer and acetonitrile taken in the ratio (45:55 v/v), was pumped at a flow rate of 0.8 ml/min with UV-detection at 314 nm. Both the drugs were well resolved on the stationary phase and the retention times were around 2.174 minutes for moxifloxacin and 3.467 minutes for metronidazole. The method was validated and shown to be linear for moxifloxacin and metronidazole. The correlation coefficients for moxifloxacin and metronidazole are 0.9997 and 0.9992 respectively....
Two simple, sensitive and accurate spectrophotometric methods for the determination of tizanidine hydrochloride have been developed. The methods are based on reaction of tizanidine hydrochloride with folin-ciocalteu reagent under basic condition and dissociation which reduces the folin-ciocalteu reagent giving a blue coloured solution (Method A), while tizanidine hydrochloride in presence of acidic medium reacts with excess amount of ceric ammonium sulfate and the unreacted ceric ammonium sulfate reacts with crystal violet to produce greenish blue colour. The final solutions were made to produce 100 µg/ml with distilled water for both method A and method B. The λmax was found to be at 723 nm and 448 nm and the linearity was found in concentration range of 10-50 μg/ml and 10-60 μg/ml respectively for method A and method B. The correlation coefficient was found to be 0.9979 and 0.9991 respectively for method A and method B. The methods were validated as per USP and ICH guidelines....
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