1. | BINARY RESPONSES OF RETINOPATHY IN T2DM USING GEE MODELING AND GOODNESS OF FIT TESTS |
| V.Rajagopalan1, M.Vijayasankar1* & S.Lakshmi2 |
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ABSTRACT
Retinopathy is a major cause of blindness in DM worldwide. We aimed to study the prevalence of retinopathy in DM by screening and its complications. The risk factors are uncontrolled DM prolonged duration of the disease and lack of regular screening. The above factors are studied using GEE modeling for binary responses from patients of diabetic retinopathy. Two models are fitted and obtained their estimate, standard error and significance of the main effects and interaction. Also two goodness-of-fit tests are proposed for GEE modeling. Keywords: DM (Diabetes Mellitus), DR (Diabetic Retinopathy), GEE (Generalized Estimation Equations), Goodness-of-fit test.
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2. | ANALYTICAL TECHNIQUES FOR THE ESTIMATION OF MIRTAZAPINE IN BULK AND PHARMACEUTICAL DOSAGE FORMS: A REVIEW |
| M. Sumanth*, T. Ramamohan Reddy, A. Ajitha, V. Uma MaheswaraRao |
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ABSTRACTMirtazapine (MRZ) has a piperazinoazepine structure {1,2,3,4,10,14b-hexahydro-2- methylpyrazino [2,1-a]-pyrido[2,3-c][2] benzazepine}. It belongs to the class of noradrenergic and specific serotonergic inhibitor antidepressants (NASSA) .MRZ increases the central noradrenergic and serotonergic activity by blocking α2 adrenergic receptors. MRZ also acts as anantagonist of postsynaptic serotonin type 2 (5-HT2) and type 3 (5-HT3) drug has a different mechanism compared to most ofthe second generation antidepressants, and it is used to treat generalized anxiety , obsessive–compulsive , and post traumaticstress disorders . It has a high affinity for histamine H1 receptors: Literature survey reveals that Mirtazapine is estimatedindividually by Spectrometric ,RP-HPLC, LC/MS/MS ,Force degradation & Stability indicating RP-HPLC,CapallaryEclectrophorosis,HPLC-Fluorescence, LC-UV-LC-MS,Quantification by HPLC-ESI-MS/MS,Determination ofspectrofluoremetric and CZE.Keywords: Mirtazapine,RP-HPLC,LC/MS/MS, Spectrometric, Spectroflurometry, Capillary Electrophorosis. LC-UV-LC-MS,HPLC-ESI-MS/MS,CZE.
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3. | RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF ARTEMETHER AND LUMIFANTRINE IN PURE AND MARKETED FORMULATION |
| D. Chinababu* and M. Sreenivasulu |
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ABSTRACT A simple, rapid, precise and accurate reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of Artemether in combination with Lumefantrine. This method uses a Hypersil ODS C18(4.6×150mm,5μ particle Size) analytical column, a mobile phase of methanol: ammonium acetate buffer pH 3 adjusted with orthophosphoric acid in ratio(65:35 v/v). The instrumental settings are a flow rate of 1.2 ml/min and PDA detector wavelength at 256 nm. The retention times for Artemether and Lumefantrine were 2.8 min and 3.8 min, respectively. The method is validated and shown to be linear. The linearity range for Artemether and Lumefantrine were 10-50μg/ml & 60-300μg/ml respectively. The Percentage recovery for Artemether and Lumefantrine are ranged between 99–102 and 99–102 respectively. The correlation coefficients of Artemether and Lumefantrine were 0.999, and 0.999, respectively. The relative standard deviation for six replicates is always less than 2%. The Statistical analysis proves that the method is suitable for routine analysis of Artemether and Lumefantrine as a bulk drug and in pharmaceutical formulation. Keywords: Artemether, Lumefantrine, RP-HPLC and Validation.
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4. | DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF NICOTINAMIDE AND CLINDAMYCINE IN BULK AND PHARMACEUTICAL FORMULATIONS |
| Anil Kumar S.M.*, A. Satishkumar Shetty, N. D. Satyanarayan |
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ABSTRACT The objective of the current study was to develop a simple, accurate, precise and rapid RP-HPLC method and subsequently validate as per ICH guidelines for the determination of Nicotinamide (NIC) and Clindamycine (CLI) using mobile phase [A mixture of 0.02M disodium hydrogen phosphate buffer and acetonitrile (pH-2.9), in the ratio of 71:29 v/v was considered to be the optimal composition] as the solvent. The proposed method involves the measurement of retention time at selected analytical wavelength. 195.0 nm was selected as the analytical wavelength. The retention time of NIC and CLI was found to be 1.864 and 3.642 respectively. The linearity of the proposed method was investigated in the range of 2-10 μg/ml (r = 0.9999) for NIC and 10-50 μg/ml (r = 0.999) for CLI respectively. The method was statistically validated for its linearity, accuracy and precision. Both inter-day and intra-day variation was found to be showing less % RSD (Relative Standard Deviation) value indicating high grade of precision of the method. Keywords: RP-HPLC method, Nicotinamide, Clindamycine, Validation.
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5. | DEVELOPMENT AND VALIDATION OF ASSAY METHOD FOR MELOXICAM TABLETS BY RP-HPLC |
| D. China babu, M .Sreenivasulu, M . Naga priyanka |
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ABSTRACT A simple, rapid, and accurate reversed phase high-performance liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the determination of meloxicam .The separation was carried out using a mobile phase consisting of phosphate buffer and acetonitrile in the ratio of 60: 40. The pH of the mobile phase was adjusted to 7.0 with triethylamine. The column used was X Terra C18 (150 × 4.6 mm, 5 μm) with flow rate of 0.8 mL/min using UV detection at 344nm. The total run time was 6 min and the retention time of meloxicam was 2.4 min. The described method was linear for the assay of meloxicam over a concentration range of 10 μg/mL respectively. Results of the analysis have been validated statistically and by recovery studies. The Limit of quantification and Limit of detection were found to be 0.135 μg/mL and 0.05μg/mL respectively. The results of the studies showed that the proposed RP-HPLC method is simple, rapid, precise, and accurate, which is useful for the routine determination of meloxicam bulk drug and its pharmaceutical dosage form. Keywords: Meloxicam, HPLC.
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6. | RP-HPLC METHOD DEVELOPMENT & VALIDATION FOR SIMULTANEOUS ESTIMATION OF TRITHIOPARAMETHOXYPHENYL PROPANE (ANETHOLE TRITHIONE) AND CHLORPHENIRAMINE MALEATE IN TABLET DOSAGE FORM |
| Dave Parth A*, Patel Ajay I, Vyas Amit J, Patel Ashok B, Chauhan Vipula B |
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ABSTRACT A Simple, precise and rapid RP-HPLC method was developed and validated for simultaneous Estimation of Trithiparamethoxyphenyl propene (Anetholetrithione) and Chlorpheniramine Maleate in tablet dosage form. Separation was achieved on Phenomenex Luna C18 (250mm × 4.6 mm, 5 μm) using an isocratic mobile phase Consisting of Acetonitrile and Mixture of 0.1% Ortho phosphoric acid & 0.1% triethylamine in water, (80:20,v/v). The analysis was performed at a flow rate of 1.0 ml / min. Detection was done by UV absorbance at 232 nm and the runtime was 8.0 minutes within which the compounds were separated. The retention time for Chlorpheniramine maleate and Anetholetrithione were found to be 2.42 min and 5.51 min respectively. The method was linear in the range of 20-100 μg/ml (r2 = 0.9976) and 5-25 μg/ml (r2 = 0.9988) for Anetholetrithione and Chlorpheniramine maleate respectively. The method was validated as per ICH guideline with respect to system suitability, Specificity, Linearity, accuracy, precision and robustness. Accuracy was assessed by the standard addition method. The recoveries were obtained in range of 99.56 -101.46% and 99.22-101.87% for CPM and ATT respectively. The repeatability was determined and %RSD for CPM and ATT were found to be 0.66% and 0.41% respectively. The intraday precision was determined and %RSD for CPM and ATT were found to 0.28-0.39% and 0.17-0.49 % respectively. The interday precision was determined and %RSD for CPM and ATT were found to be 0.34-0.73% and 0.54-0.75% respectively. The LOD and LOQ value for CPM was found to be 0.14 and 0.13μg/ml. Keywords: Anetholetrithione, Chlorpheniramine maleate, Hepasulfol-AA® tablets, RP-HPLC.
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7. | AN OVERVIEW ON HIGH PERFORMANCE CAPILLARY ELECTROPHORESIS |
| Sudheer Kumar N*, Shilpa KT, Ajitha A, Uma Maheshwara Rao V |
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High performance Capillary electrophoresis (HPCE) is a separation technique in which the analytes are separated onthe basis of differences in their charge-to-size ratios. This makes HPCE especially suitable for the analysis of molecules withabroad range of sizes, charge and hydrophobicity, as proteins and peptides. Another attractive feature of HPCE is its ability tohandle minute sample amounts, with nano-litre injection volumes, which makes it ideal for applications when the samplevolumes are limited, as often is the case in analysis of body fluids, single cells and other small volume analysis of biofluids.Electrophoresisisperformed innarrow-bore (25- to 75-J.m id), fused silica capillaries. High voltages (10 to 30 kV) and highelectricfields (100 to 500 V/cm) are applied across the capillary. In addition, the small injection volume has often beenconsidered as a drawback of the HPCE technique in analysis of complex biological samples, as well as the nature of itsinjection has represented a reproducibility problem in quantitative chemical analysis.
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8. | METHOD DEVELOPMENT AND VALIDATION OF SIMULTANEOUS ESTIMATION OF EZETIMIBE AND GLIMEPIRIDE BY RP-HPLC |
| Sudheer Kumar N*, Shilpa K, Ajitha A , Uma Maheswara Rao V |
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A sensitive, selective and precise high performance liquid chromatographic method has been developed and validatedfor the simultaneous determination of Ezetimibe and Glimepiride in tablet dosage form. The method employed like C18column, Symmetry C18 (4.6 x 250mm, 5ïm, Make: Waters) as the stationary phase while Phosphate buffer (pH 3.6),Acetonitrile in proportion 45:55 v/v respectively. was used as mobile phase. The Retention time of Ezetimibe and Glimepiridewere observed to be 2.273 and 3.630 minutes, respectively. The flow rate was found to be 1ml/min and effluents weremonitored at 228 nm. The linear regression analysis data for the calibration plots showed a good linear relationship for bothEzetimibe and Glimepiride and over a concentration range of 10-50 μg/ml. with correlation co-efficient of 0.9989 for Ezetimibeand and 0.9999 for Glimepiride. The LOQ was found to be 4.52 and 3.67μg/ml respectively for Ezetimibe and Glimepiride.The method was validated as per ICH guideline and it was found to be accurate, precise and robust. Marketed formulation wasanalyzed successfully.
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9. | DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF TIANEPTINE IN API AND TABLET DOSAGE FORM |
| A. Prateep Reddy*, K. Shilpa, A. Ajitha, V. Uma Maheswara Rao |
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A rapid and precise Reverse Phase High Performance Liquid Chromatographic method has been developed for thevalidated of Tianeptine, in its pure form as well as in tablet dosage form. Chromatography was carried out on a Zorbax C18 (4.6x 250mm, 5μm) column using a mixture of Water and Methanol (85:15% v/v) as the mobile phase at a flow rate of 1.0ml/min,the detection was carried out at 218nm. The retention time of the Tianeptine was 5.430±0.02min respectively. The methodproduce linear responses in the concentration range of 10-50 μg/ml of Tianeptine. The method precision for the determinationof assay was below 2.0%RSD. The method is useful in the quality control of bulk and pharmaceutical formulations.
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10. | ANALGESIC AND ANTI-INFLAMMATORY ACTIVITIES OF BARK AND LEAF EXTRACTS OF KUNSTLERIA KERALENSIS |
| Kumar MD1*, Sathishkumar Shetty A1, Satyanarayan ND2, Vijay kumar ML3,Vasudeva Nayak P |
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The hexane, chloroform and methanolic extracts of bark and leaf of the plant “Kunstleria keralensis” belonging to thefamily Fabaceae were screened for analgesic and anti-inflammatory activity. The analgesic activity was evaluated by tail flickand hot plate method. The anti-inflammatory activity was evaluated by Carrageenan induced paw edema method. The hexaneextract (HB) and methanol extract (MB) of bark showed significant analgesic and anti- inflammatory activity at prefixed time.The chloroform extract (CB) of bark and hexane extract (HL) of leaf showed moderate analgesic and anti- inflammatoryactivity at prefixed time. The chloroform extract (CL) of leaf and methanol extract (ML) showed in signifiacant analgesic andanti-inflammatory activity.
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