Current Issue : April - June Volume : 2012 Issue Number : 2 Articles : 13 Articles
This study describes the development and validation for the simultaneous estimation of desloratadine (DES) and montelukast sodium (MON) by the first-order derivative UV spectroscopy method. The quantification was achieved by the first-order derivative spectroscopy method at 297.20 nm and 339.20 nm over the concentration range of 3-18µg/ml for estimation of desloratadine (r2=0.9993) and 6-36 µg/ml montelukast (r2=0.9999) in a combined tablet formulation. Procedure does not require prior separation of components from the sample. LOD values for DES and MON are found to be 0.08 μg/mL and 0.17 μg/mL, respectively. LOQ values for DES and MON are found to be 0.24 μg/mL and 0.52 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....
A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for simultaneous determination of sitagliptin and simvastatin in bulk drug samples and formulations. The quantitative determination was carried out by using Luna C-18 (250 x 4.6mm, 5μ) column with a mobile phase consisting of a mixture of buffer: acetonitrile: methanol (40:35:25v/v), pH adjusted to 3.5 with orthophosphoric acid and Triethylamine. The mobile phase was filtered through a 0.45μ nylon filter, sonicated for 15 min and delivered at a flow rate of 1.0 ml/min. Analysis was performed at ambient temperature with detection at 254 nm. The calibration curves were linear (r2=0.998) over a concentration range from 50-500µg/ml for sitagliptin and (r2=0.999) over a concentration range from 20 -200 µg/ml for simvastatin. Limit of detection (LOD) and Limit of quantitation (LOQ) were 0.26 μg/ml and 0.77 μg/ml for sitagliptin and 0.06 μg/ml and 0.49 μg/ml for simvastatin respectively. The developed method was fast, accurate, precise and successfully applied to estimate the amount of sitagliptin and simvastatin in bulk sample and tablet dosage forms so it can be used for regular quality control of the drug....
A simple, specific, accurate and stability-indicating high performance liquid chromatographic method was developed\r\nand validated for the determination of Epinastine Hydrochloride in pharmaceutical dosage form. The chromatographic\r\nconditions comprised of a reverse-phase, C18 column (150Ã?â??4.6 mm), 5Ã?µm with a mobile phase consisting of a mixture of\r\naqueous phase (3.8g of sodium pantanesulphonate monohydrate and 4.0g of potassium dihydrogen orthophosphate\r\nwas dissolved in 1L of water and pH of solution was adjusted to 4.5 with o-phosphoric acid) and organic phase\r\n(acetonitrile and methanol was mixed in the ratio of 4:1 v/v) in the ratio of 60:40 v/v at a flow rate of 1.0ml/min.\r\nDetection was carried out at 220nm. The retention time of Epinastine Hydrochloride was found to be 3.5 min. The\r\ncalibration curve was found linear between 2-200Ã?µg/ml. The percentage recoveries of Epinastine Hydrochloride were\r\nfound to be in the range of 99.05-100.50%. The method was validated for accuracy, linearity, precision, detection limit,\r\nquantitation limit and robustness. The drug was subjected to acidic hydrolysis, basic hydrolysis, neutral hydrolysis,\r\noxidation, photochemical and thermal degradation. All the peaks of degraded product were resolved from the active\r\npharmaceutical ingredient with significantly different retention time. As the method could effectively separate the drug\r\nfrom its degradation product, it can be employed as a stability indicating one....
Zero-order and Area Under Curve [AUC] UV-Spectrophotometric methods have been developed and validated for the estimation of Tenofovir disproxil fumarate in bulk and its tablet formulations. The solutions of standard and sample were prepared in water. Tenofovir disproxil fumarate was estimated at 260 nm for the zero order UV-Spectrophotometric method, while area under curve for the zero order spectrum in between 250 nm to 270 nm was measured. Beer’s law was obeyed in the concentration range of 5-30 μg/ml with r2 value 0.999 for zero order. In AUC method, beer’s law was obeyed in the concentration range of 5-30 μg/ml with r2 value 0.999. These methods were tested and validated for various parameters according to ICH guidelines. The proposed methods were successfully applied for the determination of Tenofovir disproxil fumarate in tablet formulations....
A weak electrochemiluminescence (ECL) of isoniazid in NaOH solution was observed at a platinum wire anode. When cetyltrimethylammonium bromide (CTAB) was present, the weak ECL was enhanced. The stronger ECL mechanism of isoniazid in NaOHââ?¬â??CTAB solution could be described as follows: isoniazid was electrochemically oxidized via one-electron and one-proton transfer to isoniazid hydrazyl radical. Then the formed radical was further chemically oxidized by dissolved oxygen to the excited state isonicotinate that subsequently emitted light. Based on the stronger ECL phenomenon of isoniazid, a flow injection ECL method for the determination of isoniazid was proposed. The ECL intensity was linear with isoniazid concentration in the range of 4.0 Ã?â?? 10-7 to 1.0 Ã?â?? 10-5 mol l-1 and the limit of detection (s/n = 3) was 1.9 Ã?â?? 10-7 mol l-1. The proposed method was simple and convenient operation, and has been applied to the determination of isoniazid in pharmaceutical preparations and human urine....
This review summarizes the current state of green analytical chemistry with special emphasis on environment friendly sample preparation techniques. Green analytical chemistry is a part of the sustainable development concept. Miniaturization of analytical devices and shortening the time elapsing between performing analysis and obtaining reliable analytical results are important aspects of green analytical chemistry. Some of the principles of green chemistry such as prevention of waste generation and design energy efficiency to minimize the potential of chemical accidents. Some naturally green or possibly green analytical techniques are also discussed. Presently, spectroscopic methods dominate the area of green analytical chemistry. This makes an analytical laboratory comparable with the fine chemicals or pharmaceutical industries. Solvent less extraction techniques, the application of alternative solvents and assisted extractions are considered to be the main approaches complying with green analytical chemistry principles. The purpose of this report is to arouse more attention to green analytical chemistry to serve the sustainable development of the modern society....
In the present study, the barks of Bridelia retusa Spreng, family: Euphorbiaceae were selected for phytochemical evaluation. Alcoholic extract was used for TLC and HPTLC study. Column chromatography was carried out for separation of phytoconstituent from alcoholic extract. In TLC study, alcoholic extract showed the presence of two coloured (pinkish) spots in toluene: methanol: formic acid (9: 1:0.5). After confirmation of the presence of sterol by TLC, the extract was subjected to isolation of sterol by column chromatography. The column chromatography was developed by using graded solvent mixtures of toluene and methanol. HPTLC study was carried out for alcoholic extract as well as for confirmation of isolated compound....
A sensitive, simple and selective spectrofluorimetric method was developed for the determination of Pregabalin in pharmaceutical formulation and in biological fluids. The method is based on the reaction between the drug and 1-dimethylaminonaphthalene- 5-sulphonyl chloride in the presence of mixture (acetone: 0.5 M sodium carbonate, 3:1) at pH 9.8 to yield a highly fluorescent derivative that is measured at 440 nm after excitation at 332 nm. Different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence concentration plot was rectilinear over the range of 0.04 – 0.24 µg/ml with a lower detection limit (LOD) of 0.01 µg/ml and the limit of quantitation (LOQ) of 0.04 µg/ml. The proposed method was successfully applied to the analysis of commercial tablets. Furthermore, the method was applied for the determination of Pregabalin in spiked human plasma, the mean % recovery (n = 5) is 97.82 ± 0.373. A proposal of the reaction pathway was also presented....
In this study a new HPLC-DAD method for simultaneous determination of coumarin, o-coumaric acid, dihydrocoumarin and syringaldehyde in guaco extracts and pharmaceutical preparations without sample pretreatment has been developed. The chromatographic separation was carried out on a XBridge C18 (150 x 4.6mm, 5�µm) column maintained at room temperature. The mobile phase consisted of water/methanol/acetonitrile/formic acid (65:30:5:1, v/v/v/v) eluted at a flow rate of 1.0 mL min-1 in an isocratic system. The validation procedures showed excellent selectivity and linearity over a range of 1.0 to 200 �µg mL-1 for all compounds (r > 0.999). The range of recovery was 97.9 to 101.8% with a RSD < 5% for intra-day and inter-day precision. The robustness study indicated that flow rate was the only critical factor. Sample analyses demonstrated a lack of standardization in the amounts of the main guaco metabolites among the evaluated samples. The new method is presented as an alternative for the quality control of guaco extracts and pharmaceutical preparations....
A simple, fast, and precise reverse phase, High Performance Liquid Chromatography (HPLC) method was developed for the separation and quantification of Lamivudine, Zidovudine and Nevirapine in bulk drug and pharmaceutical dosage form. The quantification was carried out using C18 (250 × 4.6mm, 5μm) column and mobile phase comprising of methanol and phosphate buffer (pH 3) in proportion of 45:55 (v/v). Flow rate was maintained at rate of 0.8 ml/min and the effluent was monitored at 280 nm. The retention time of Lamivudine Zidovudine and Nevirapine were 3.12, 5.01 and 7.08 min respectively. Method was validated in terms of linearity, precision, accuracy, specificity, limit of detection and limit of quantitation. Linearity was 5.0-100.47 μg/ml for lamivudine, 10.0-170.0 μg/ml for zidovudine and 5.0-60.0 μg/ml for nevirapine respectively. Percentage recoveries of the drugs from the tablet formulation were found to be 99.7.%, 99.6% and 99.3% for Lamivudine, Zidovudine and Nevirapine respectively. Hence, proposed method was found to be suitable for simultaneous determination of Lamivudine Zidovudine and Nevirapine in pharmaceutical dosage form and bulk drug when compared to the reported method in terms of sensitivity, precision and accuracy....
Development and validation of UV Spectrophotometric method for simultaneous estimation of clotrimazole and beclomethasone dipropionate in their combined dosage form. First method is based on Q‐absorption Ratio method using two wavelengths, 260.6 nm (λmax of CT) and 250.8 nm (Isoabsorptive point). The second method is the dual wavelength method, where 237 nm and 241 nm were selected as λ1 and λ2 for the determination of Clotrimazole and 259 nm and 264 nm were selected similarly for the determination of Beclomethasone. The last method involves the use of First order derivative technique. Here 239 nm, the zero crossing point of Beclomethasone, was selected for the determination of Clotrimazole and 260.8 nm, the zero crossing point of Clotrimazole, was selected for the determination of Beclomethasone. Clotrimazole showed linearity in the range of 100‐450μg/mL and Beclomethasone showed linearity in the range of 6-34μg/mL in all the methods. All methods were validated statistically and recovery studies were carried out. All methods were found to be accurate, precise and reproducible. These methods were applied to the assay of the drugs in marketed formulation, which were found in therange of 98.0% to 100.0% of the labeled value for both Clotrimazole and Beclomethasone. Three new, simple, accurate and precise UV spectrophotometric methods have been developed and validated for the simultaneous determination of Clotrimazole (CT) and Beclomethasone dipropionate (BD) in their combined dosage forms....
An accurate, precise and ecofriendly spectrophotometric method is presented for the determination of Cefixime based on the formation of a yellow colour product with ninhydrin in the presence of bicarbonate with an absorption maximum at 438 nm. The reaction proceeds quantitatively at 97 ± 1°C in 15 min. The calibration curve is linear over the range of 45-65 μg/ml and is described by the regression equation A = (-) 0.858 + 0.021 C with a regression coefficient (r) of 0.9987 (n = 5). The calculated molar absorptivity and Sandell sensitivity values are 4.1536 x 10 3 L/mol/cm and 0.0072 μg/cm2, respectively. The limits of detection (LOD) and quantification (LOQ) calculated as per ICH guidelines are 1.13 and 3.40 μg/ml, respectively. The within-day accuracy expressed as relative error was better than 2.5% with precision (RSD) ranging from 1.02 to 1.93%. The between-day accuracy ranged from 1.5-3.0% with a precision less than 4%. Accuracy was also checked by placebo blank and synthetic mixture analyses besides a recovery study via standard addition procedure....
The present study was aimed to develop an analytical method of estimation of atenolol tablets using three different mixed co-solvents having varying composition of urea, PEG 400, hydroxy propyl β-cyclodextrin and PEG 6000. Beer’s law was obeyed in the concentration range of 4-24μg/ml. The solubility of atenolol in distilled water was found to be 9.34mg/ml, where as in mixed co-solvents it was 14.43 mg/ml in UPCD, 15.35 mg/ml in UPGP and 13.32 mg/ml in UPPE. The enhancement in solubility was observed to greater extent. The analysis of tablets indicated good correlation between estimated and label claim. The results of recovery study revealed that any small change in the drug concentration in the solution could be accurately determined by the proposed method. The low values of LOD and LOQ of acyclovir in the solvent mixture indicated good sensitivity of proposed method. As urea, PEG 400, PEF 6000 and HP-βCD were cheaper than most of the organic solvents, these can be used as a substitute for organic solvents. The study proved that mixed co-solvency phenomenon is an effective technique in enhancement of aqueous solubility of poorly water soluble drugs. The proposed method is new, simple, accurate, non-toxic and precise method that can be successfully employed for estimation of drugs in routine analysis of atenolol tablets....
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