A NEW RP-HPLC ASSAY METHOD FOR DETERMINATION AND QUANTITATION OF NITROFURANTOIN API |
Author : Ramchandra Krishna Pawar, Ram Lokhande, Ravi Yadav, Bhanupratap Bind, Shirish Velankar |
Abstract | Full Text |
Abstract :A simple, specific and precise RP-HPLC method was developed and validated for determination of Assay for Nitrofurantoin Active Pharmaceutical ingredient (API). The method validation was performed as per ICH Q2 (R1) and FDA guidelines. The final chromatographic condition comprises of HPLC column i.e. Ascentis Express C18 (dimension 7.5cm x 4.6mm and particle size 2.7µm) and mobile phase containing a mixture of 0.1% Triethylamine pH-3.0 and Acetonitrile in the ratio of 80:20 v/v. The flow rate and column temperature were constantly maintained at 1.0 ml/min and at 30ºC respectively. The detection was performed at wavelength 254 nm using PDA detector. The retention time obtained for Nitrofurantoin peak was about 2.0 minutes. There was no interference due to the mobile phase or diluent was observed at retention time of Nitrofurantoin peak. Also, the data of linear regression analysis shows a linear relationship of Nitrofurantoin over the concentration range of 50-150µg/mL and the correlation coefficient value obtained was 0.9999. The Analytical method validation data shows that the method was Specific, Linear, Precise and Robust for the Assay determination of Nitrofurantoin API. |
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HPLC METHOD DEVELOPMENT FOR TRACE CONTAMINATION OF PLASTIC POLYETHYLENE TEREPHTHALATE (PET) USED FOR VEGETABLES |
Author : Shirish Janardan Velankar, Ram Lokhande, Ravi Yadav, Ramchandra Pawar |
Abstract | Full Text |
Abstract :A simple rugged and user-friendly and cost effective method to quantify low-molecular-weight formaldehyde and acetaldehyde in the food contact plastic, with 2, 4-Dinitrophenyl hydrazine (2, 4-DNPH) is presented using High Pressure Chromatography (HPLC). Use of 2, 4-DNPH ensure that the probable carbonyl compounds in the food contact plastics, can be monitored using the same method. The separation was achieved with Ascentis Express C18 (100 mm x 4.6 mm x 2.7µ) using Water: Acetonitrile (70: 30 v/v) with a flow rate of 2.0 ml /min. The Method was validated for the analytical parameters viz., Specificity, Limit of Detection (LOD), Limit of Quantitation (LOQ), Linearity and Range, Precision – System, Method and Spiked and Accuracy. For Bottle Gourd, the limit of detection and quantitation was found to be 10 and 30 PPM for formaldehyde with respect to (w.r.t.) sample concentration 10 mg/ ml. The limit of detection and quantitation was found to be 20 PPM and 60 PPM for acetaldehyde w.r.t sample concentration 10 mg/ ml. Primary contact plastic: The limit of detection and quantitation was found to be 250 and 750 PPM for formaldehyde w.r.t sample concentration 0.4 mg/ ml. The limit of detection and quantitation was found to be 500 PPM and 1500 PPM for acetaldehyde w.r.t sample concentration 0.4 mg/ ml. |
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DEVELOPMENT AND VALIDATION OF COST EFFECTIVE RP-HPLC ASSAY METHOD FOR DETERMINATION OF METAXALONE |
Author : Avdhoot Rameshwar Malokar, Ram Lokhande, Ravi Yadav |
Abstract | Full Text |
Abstract :Most of the analytical method required, fast and reliable analytical technique as per current requirement of pharmaceutical industry. Hence a simple rugged and cost effective method was developed and validated for Metaxalone. By using this HPLC method, the time for analysis is reduced sensationally as compared to other method published in most of the literatures published. The method was set on Ascentis express C8 column (10cm x 4.0mm, 2.7µ) using 0.1% Triethylamine as a buffer (pH 3.0 with per chloric acid) and acetonitrile as organic modifier. The flow rate was set at 1.0ml\min and analysis time was 4 minutes with gradient elution. The detection was conducted at 210nm. The method was validated as per International Conference of Harmonization (ICH) Guidelines in terms of Specificity linearity and range, precision and robustness. Sample and standard concentration of metaxalone was 0.5mg/ml. linearity of standard was covered from 0.4mg/ml to 0.6mg/ml. |
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ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF ATORVASTATIN AND NIACIN IN BULK AND COMBINED TABLET DOSAGE FORM BY USING UV?VISIBLE SPECTROSCOPY |
Author : Ramreddy Godela, Suresh , Shivakumareddy Rakasi, Vikram S. |
Abstract | Full Text |
Abstract :A simple, precise, rapid and sensitive UV spectrophotometric method was developed and validated for estimation of Niacin (NCN) and Atorvastatin (ATR) in pure and tablet dosage form using methanol: water (10:90 v/v) mixture as solvent by simultaneous equation method. The absorption maxima were found to be 257nm and 242 nm for Niacin and Atorvastatin calcium respectively. Beer’s law range was in the concentration range of 10-60 µg/ml for Niacin and 5-30 µg/ml for Atorvastatin calcium with correlation coefficient within the range of 0.997 – 0.998 for both the drugs. Recovery studies were performed to assess the accuracy of the methods, the results were found to be between 99.8% to100.1% for Atorvastatin and 98.75% to 100.6% for Niacin. LOD and LOQ were found to be 0.366 µg/ml and 1.1 µg/ml for Atorvastatin and 1.65 µg/ml and 5.0µg/ml for Niacin. Robustness was done by slightly changing the solvent composition and ?max. The above method has been validated according to ICH guidelines. Hence the above methods can be used for routine analysis of Niacin and Atorvastatin in pharmaceutical industries. |
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EVALUATION OF IN VITRO ANTICANCER POTENTIALS OF PVP STABILIZED SILVER, COPPER AND NICKEL NANOPARTICLES |
Author : S. Kanchana and J. Santhanalakshmi |
Abstract | Full Text |
Abstract :Despite formidable global efforts, cancer continues to be the leading cause of human death. Prevailing anticancer drugs, although effective in controlling neoplastic growth, the eventual toxicity on normal cells and other health complications caused by them are inevitable. The metal nanoparticles by virtue of their specificity and selective toxicity are promising to be safe anticancer drugs. In this study, Polyvinyl Pyrrolidone (PVP) capped three transition metal nanoparticles namely copper (PVP-CuNP), nickel (PVP-NiNP) and silver (PVP-AgNP) were synthesized by bottom up wet chemical method. Using MTT assay the cytotoxic and anticancer potentials of these nanoparticles were tested against normal (Vero) and human lung cancer (A549) cells in vitro. The cytotoxicity and anticancer efficacy of these nanoparticles were determined in terms of IC50 value and longevity of inhibitory effect on relative growth rate (RGR). Continuous culturing of cells in the presence of IC50 doses of these nanoparticles was carried out to determine the longevity of their anticancer activity. The toxic doses (µg/mL) of PVP-CuNP, PVP-NiNP and PVP-AgNP on Vero (normal) cell lines respectively were 11.80, 6.70 and 6.35, while were 1.75, 1.90 and 1.40 on A549 cells. The longevity of anticancer efficacy in terms of displaying qualified grade of activity of these nanoparticles were 3, 5 and 3 days respectively. Overall, the silver nanoparticles (PVP-AgNP) demonstrated better efficacy and moderate cytotoxicity with longer anticancer activity at minimal doses. |
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ISOLATION AND IDENTIFICATION OF NEW C-FLAVANOL GLYCOSIDES FROM ALLIUM CEPA |
Author : Paramita Das, Padmavathi P Prabhu, Jitender Reddy |
Abstract | Full Text |
Abstract :In this study, penta hydroxy flavonoid quercetin-4-glycoside was isolated from the ethanolic extract of Allium cepa which was then eluted in the solvents chloroform and methanol. The crude ethanolic extract was collected and subjected to column chromatography and sub fractionated with solvent chloroform and methanol. Isolate was further processed and selected sub fraction was subjected to fresh column chromatography. Washing was continued till TLC shows a single spot observed under UV at 254 nm and 366nm after spraying ANS reagent. Quercetin-4-glycoside was established on the chemical and spectral analysis and HPLC-PDA was developed for the standardization and estimation of compound. The results of analysis of the compound suggested that the compound may be used as a marker for standardization, and the developed isolation method is cost effective compared to all other existing methods reported in literature. |
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MICROWAVE ASSISTED SYNTHESIS OF PYRIDO [2,3,4-KL] ACRIDINES UNIT OF SOME MARINE ALKALOIDS |
Author : Preeti S. Zade and M.M.V. Ramana |
Abstract | Full Text |
Abstract :Microwave irradiation is well known for its ability to reduce reaction times dramatically, to increase product yields, and to enhance product purities by reducing unwanted side reactions compared with conventional heating. Many marine alkaloids are known which have a common structural feature of tetracyclic pyrido [2,3,4-kl] acridine system. Most of these molecules exhibit very interesting biological properties like antitumor, cytotoxic and antiviral activities. This is due to their interesting biological activities and challenging structures. We report a simple and convenient synthesis of pyrido [2, 3, 4-kl] acridine utilizing microwave irradiated intramolecular nitrene insertion reaction as key step for generating the tetracyclic framework of marine alkaloids. |
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SCHIFF BASE METAL COMPLEXES OF BIOINORGANIC AND MEDICINAL RELEVANCE: A REVIEW |
Author : Archana Singh, Suman Malik and Amar Sohail Mirza |
Abstract | Full Text |
Abstract :Schiff bases are versatile ligands and play important role in medicinal and bioinorganic fields because of their wide spectrum of biological activities. Schiff bases are multipurpose ligands which are amalgamated from the condensation of carbonyl compounds with an amino compound. Schiff bases and their metal complexes are also used for industrial purposes and their metal complexes have been screened for their in vitro biological activities against bacteria, fungi and yeast. These complexes also show significant growth inhibitory activity against the bacteria like Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Klebsilla Pneumonia, etc. than the free ligands. Most of them show biological activities such as antibacterial, antifungal antioxidant, biocidal, antiviral as well as antitumor activity. It has been observed that the antimicrobial activities of these metal complexes are higher than that of the free ligand. |
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DEVELOPMENT AND VALIDATION OF UV-VISIBLE SPECTROPHOTOMETRIC METHOD OF ESTIMATION OF TERBUTALIN SULPHATE IN BULK DRUG USING NINHYDRIN |
Author : Gajanan A Vaishnav, Sushama Vaishnav-Hota, Shital Godse, Angadi S.S. and Patil S. J.3 |
Abstract | Full Text |
Abstract :An accurate, precise and simple spectrophotometric method for the determination of Terbutalin sulphate based on the formation of a yellow color product with Ninhydrin in the presence of sodium bicarbonate with an ?max at 346 nm. The Reaction heating temperature was 80°C for 30 min. The calibration curve was linear over the range of 10-60 µg/ml and the regression equation obtained was y=0.0263x+0.2 with a regression coefficient (r) of 0.98 (n=10). The limit of Detection (LOD) and limit of Quantification (LOQ) calculated as per ICH guidelines were 18.15µg/ml and 55µg/ml, respectively |
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NEW ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR IMATINIB MESYLATE BY RP-HPLC METHOD |
Author : K. Sunand, Vasudha Bakshi, Sai Preethi, Mahesh Reddy, K. Pavan Kumar, Yuvatha |
Abstract | Full Text |
Abstract :A simple, accurate, precise, and, economical RP- HPLC method has been developed for the rapid estimation of Imatinib Mesylate. The separation was achieved on C18 column, X terr 18.5 µm, using Phosphate buffer (55%): Acetonitrile (45%) as mobile phase, with a injecting volume of 5 µl at a flow rate of 0.9 ml/min. Detection was carried out at 256 nm and drug eluted with a retention time of 3.648 min. The method had been validated according to ICH guide lines for accuracy, precision, linearity, robustness, ruggedness, LOD and LOQ. The method was found to be accurate, and precise, robust, rugged and sensitive. The proposed method was convenient for quantitative routine analysis and quality control of Imatinib Mesylate in tablets. The results of compound were good agreement with the label claims |
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STRAW AS A UNIQUE DELIVERY SYSTEM FOR HERBAL MEDICINES |
Author : Rujvi R Mehendre, Rahul Yadav, Dinesh Dantkale,Urmila Joshi |
Abstract | Full Text |
Abstract :Herbal medicines to be taken with water or milk can be easily delivered using straw delivery format. Curcumin was formulated into flavoured granules, which were then incorporated into straw. The straw design prevents the granules from falling out during sipping through milk or water. Curcumin was coated on sugar beads using pan coating process. The content was estimated, and granules equivalent to 15 mg curcumin was filled into the straws. The straws were evaluated in 6 volunteers for taste and feel. The overall feedback from the volunteers regarding easy of sipping, flavor, and feel was good. |
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DEVELOPMENT OF UV SPECTROPHOTOMETRIC AND HPTLC TECHNIQUE FOR ESTIMATION OF LOXAPINE IN FORMULATION |
Author : Chitra Bhojan, Manjula Devi Ananda Vally Sukumaran Nair and Thengungal Kochupappy Ravi |
Abstract | Full Text |
Abstract :UV spectrophotometric and chromatographic methods which are simple, accurate and precise have been developed and validated for the determination of Loxapine in its pharmaceutical formulation. The UV spectroscopic analysis was performed using water as solvent and detection was done at 297 nm. The HPTLC method was performed using Pre-coated silica gel G60 F254 plate using the mobile phase chloroform and methanol in the ratio of 9.5:0.5 v/v/v followed by analysis at 297 nm. Linearity was found over the concentration range of 10- 80 µg/ml for UV method and 2 – 12 ng/spot for HPTLC method with correlation coefficient 0.9991 and 0.9933 respectively. Repeatability, Intraday and Interday studies shows % RSD less than 2, which indicates the precision of the developed method. The developed methods are more sensitive and cost effective. As no methods were developed for Loxapine by UV and HPTLC techniques they can be routinely used for the determination Loxapine in formulations. |
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