1. | A NEW COLORIMETRIC DEVELOPMENT AND VALIDATION OF VISIBLE METHOD FOR ESTIMATION OF DICLOFENAC IN BULK FORMULATION |
| P.Hrudaya Ranjani, G.Rohit Reddy*, D.Rakesh Goud, VVS.Rajendra Prasad |
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ABSTRACT A simple, sensitive, accurate, precise and economical visible Spectrophotometric method was developed and validated for the estimation of Diclofenac in Bulk form. The method is based on the reaction of Diclofenac with MBTH Reagent [3-Methyl-2-Benzothiazolinone Hydrazone] in the presence of ceric ammonium sulphate giving greenish blue colourchromogen which shows maximum absorbance at 580nm against reagent blank. The Chromogen obeyed Beer’s law in the concentration range of 10-50 μg/ml for Diclofenac. The results of the analysis have been validated statistically and recovery studies. Keywords: Diclofenac, MBTH Reagent [3-Methyl-2-Benzothiazolinone Hydrazone], ceric ammonium sulphate, Visible Spectrophotometric.
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2. | DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS ESTIMATION OF DEXTROMETHORPHAN HYDROBROMIDE AND PHENYLEPHRINE HYDROCHLORIDE |
| Prashanthi M &Venkateshwarlu G* |
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ABSTRACT The combination of Dextromethorphan hydrobromide and phenyl ephrine hydrochloride is used to treat cough, stuffynose and sinus congestion caused by allergies, the common cold or the flu. Five simple, accurate, rapid and precise uv spectrophotometric methods have been developed for simultaneous estimation of Dextromethorphan hydrobromide and phenylephrine hydrochloride in combined formulation, as a syrup.. First method employs solutions of simultaneous equations using, while the second method called Q-ratio or iso-absorptive method based on measurement at iso-absorptive point as well λmax of other drug. The third method viz. Derivative spectrum method, depends on zero crossing points of the derivative spectrum, which enables the construction of calibration for both the drugs in the presence of second one. Dual wavelength, the fourth method developed measures the difference in the absorbance of the mixtures at wavelengths whereas single drug has the same absorbance and viceversa. Mean centered ratio method which depends on construction of calibration by dividing spectra of the one compound with the other is reported as fifth method. All the five methods are tested for accuracy, precision by six replicate experiments and recovery studies using known synthetic mixtures. The calibrations are applied for the analysis of two drugs in the syrup. The methods are validated in terms of ICH guidelines. Keywords: Dextromethorphan hydrobromide, Phenyl ephrine hydrochloride, Simultaneous- equations method, Q-analysis, Derivative spectrophotometry, Mean centered ratio method, dual wavelength, Validation.
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3. | DEVELOPMENT AND VALIDATION OF A CHIRAL LIQUID CHROMATOGRAPHIC METHOD FOR QUANTITATIVE DETERMINATION OF (R)-I-BET762 IN (S)-I-BET762 |
| Narayanan Balaji, Ramesh Mullangi, A. Siva Kumar,* |
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A simple, rapid and robust enantioselective method was developed and validated for the quantitation of I-BET762 enantiomers [(S)-I-BET762 and (R)-I-BET762] with ultra-performance liquid chromatography (UHPLC) as per ICH guidelines. The active [(S)-I-BET762] and inactive [(R)-I-BET762] enantiomers were resolved on a Chiralpak-IA column using 0.1% trifluoro acetic acid in water (v/v) and acetonitrile at a flow rate of 1.2 mL min-1. The resolution between the enantiomers was found to be more than 3.4 in the optimized method. The developed method was extensively validated and proven to be robust. The calibration curve for (R)-I-BET762 showed excellent linearity over the concentration range of 5 to 100 μg mL-1. The limit of detection and the limit on quantitation for (R)-I-BET762 were 2 and 5 μg/mL, respectively. The recovery for the (R)-I-BET762 ranged between 96.1 to 109.2% in the bulk drug sample. The proposed method was found to be suitable and accurate for the quantitative determination of (R)-I-BET762 in the bulk drug. Keywords: I-BET762, Enantiomers, Liquid chromatography, Bulk drug.
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4. | STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF LAMIVUDINE AND RALTIGRAVIR IN PHARMACEUTICAL DOSAGE FORM |
| M. Susmitha, V. Vasu Naik, P. Nagaraju*, G. Indira Priyadarshini and V. Mounika |
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A simple stability indicating high performance liquid chromatographic method has been developed for the simultaneous determination of Lamivudine in combination with Raltigravir using reverse phase Inertsil ODS C18 column (150 × 4.6 mm, 5μm) with UV detection at 254 nm. The mobile phase consisting of Methanol and 0.1% ortho phosphoric acid in a ratio of (70:30, v/v) and at a flow rate of 1.0 mL/min. The method was linear over the concentration range for Lamivudine 15-75 μg/mL and for Raltigravir 30-150 μg/mL. The recoveries of active pharmaceutical ingredient (API)Lamivudine and Raltigravir were found to be in the range of 99.82-100.82% and 100.71-102.43% respectively. The method was validated and was successfully employed for the routine quantitative analysis of pharmaceutical formulations containing Lamivudine and Raltigravir in combined tablet dosage form. Keywords: Lamivudine, Raltigravir, HPLC, Validation.
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5. | SCREENING OF ANTI-DIABETIC ACTIVITY OF METHANOLIC EXTRACT OF GRACILARIA DURA (AG.) J.AG. (RED SEAWEED) IN HARE ISLAND, THOOTHUKUDI, TAMIL NADU, INDIA |
| John Peter Paul J* and Iniya Udhaya C |
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ABSTRACT The present research was aimed to study the anti-diabetic activity of Gracilaria dura (Ag.) J.Ag., an important red seaweed collected from Hare Island, Thoothukudi, Tamil Nadu, India. The methanolic extract of Gracilaria dura (Ag.)J.Ag. was given via intraperitoneal injection at a dose of 200 and 400mg/kg mice on alloxan induced hyperglycemic Wistar albino mice. The fasting blood glucose level, body weight and the glucose level after the treatment of diabetic mice were measured. The animals treated with 200mg/kg methanolic extract were shown the best result of decrease in blood glucose level at a regular interval when the time increased up to 7h as compared to the dose of 400mg/kg methanolic extract treated animals. The result of the present study expressed that the anti-diabetic activity of the methanol extract was dose dependent. Keywords: Seaweed, Anti-diabetic, Gracilaria dura, Methanolic extract, Wistar albino rats.
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6. | NOVEL VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR THE DETERMINATION OF BAMIFYLLINE HYDROCHLORIDE IN BULK AND PHARMACEUTICAL FORMULATION |
| G.Indirapritadashini*, Y.Sirisha, Konda Ravi Kumar |
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A simple, accurate and precise Stability indicating RP-HPLC method for the estimation of Bamifylline hydrochloride in pure and pharmaceutical dosage form has been reported. Chromatography was performed with Shimadzu HPLC equipment comprising Enable C18 (25 × 2.6 × 5μ) column with photodiode array detector. A Rheodyne injector fitted with a 10μL loop was also used and data was recorded and evaluated using LC-20 solutions software. The mobile phase consists of 50% Methanol and 50% phosphate buffer solution and at a flow rate of 1 milliliter/minute. The Bamifylline hydrochloride was eluted at approximately 3.314 minutes. The wavelength was found to be 272nm. A linear response was observed in the concentration ranges of 20-120μg/ml with a regression coefficient of 0.999. Forced degradation studies were performed on pure sample of Bamifylline hydrochloride using acid (0.1 Normal (N) hydrochloric acid), base (0.1 N sodium hydroxide), peroxide (30% H2O2) and thermal (105°C) conditions. The developed method was validated with respect to specificity, precision (% RSD about 0.4%), linearity (linearity of range about 20-120 μg/mL), robustness, LOD and LOQ values were found to be 0.362 μg/ml and 1.096 μg/mL respectively. Keywords: High performance liquid chromatography, Naloxegol.
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7. | SIMULTANEOUS UV SPECTROPHOTOMETRIC METHOD FOR THE ESTIMATION OF AZITHROMYCIN AND CEFEXIME IN COMBINED DOSAGE FORM |
| Dodla Sony, Kandra Roja, G Devipriya, K Durga Devi, T Sandhya, G Swarnalatha and D Jothieswari* |
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A UV SPECTROSCOPY method was developed and validated for quantitative determination of Azithromycin and Cefexime in pure and tablet dosage forms. Simple, accurate and reproducible spectrophotometric methods have been developed for the simultaneous estimation of Azithromycin and Cefexime in pharmaceutical tablet dosage forms. The method involved the determination using the Simultaneous equation method, the sampling wavelengths selected are 275 nm and 240 nm over the concentration ranges of 2.5-12.5μg/ml and 2-10 μg/ml for Azithromycin and Cefexime respectively. The results of the analysis were validated statistically and recovery studies were carried out as per ICH guidelines. Keywords: Azithromycin, Cefexime, UV Spectrophotometer, Methanol.
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