DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ALISKIREN HEMIFUMARATE AND VALSARTAN IN BULK AND PHARMACEUTICAL DOSAGE FORM

Objective: A new, simple, selective, and reproducible stability indicating reversed - phase high performance liquid chromatography method for thesimultaneous estimation of Aliskiren (ALN) Hemifumarate and Valsartan (VLN) in bulk drug, and tablet dosage form was developed and validated asper ICH guidelines.Methods: The chromatographic separation was performed using a nucleosil C - 18 column and the analytes were detected by a malondialdehyde - 2010photodiode array detector. The mobile phase composed of methanol: potassium dihydrogen ortho phosphate buffer (adjusted to pH 3 withorthophosphoric acid). The flow rate was set at 1 ml/minutes, and the detection was carried out at 225 nm.Results: ALN Hemifumarate and VLN showed a retention time of 3.84 and 5.96 minutes, respectively. The linear dynamic range was found to be5-50 mcg/ml and 5-30 mcg/ml with a co-relation co-efficient of 0.992 and 0.985 for ALN and VLN, respectively, with mean percentage recoveries of99.95% and 99.25%. The results were validated and were found to successfully obey the parameters as per ICH guidelines.Conclusion: Hence, the method can be successfully applied for routine quality control analysis and stability studies for both ALN Hemifumarate andVLN in bulk and tablet dosage form as per regulatory requirements.Keywords: Aliskiren Hemifumarate, Valsartan, Reversed-phase high performance liquid chromatography, Stress degradation study, ICH guidelines

Synthesis of novel chalcone derivatives by conventional and microwave irradiation methods and their pharmacological activities

AbstractChalcones are abundant in edible plants and are considered to be the precursors of flavonoids and isoflavonoids. Chalcones belong to an important class of flavonoids, which may be prepared by Claisen–Schmidt condensation. They possess a wide range of biological activities and industrial applications. The cytotoxicity against tumour cell lines may be the result of disruption of the cell cycle, inhibition of angiogenesis, interference with p53-MDM2 interaction, mitochondrial uncoupling or induction of apoptosis. Chalcones are synthesized by conventional and microwave assisted synthesis methods. By microwave assisted synthesis, a considerable increase in the reaction rate has been observed and that too, with better yields. The compounds have been screened for cytotoxic activity and antioxidant activity

ONE STEP QUANTIFICATION ANALYTICAL METHOD AND CHARACTERIZATION OF VALSARTAN BY LC-MS

Objective: To develop precise LC-MS method for the estimation of valsartan impurities and perform validation as per ICH guidelines.Methods: Valsartan (VLN) and its degradation products were analyzed by reverse phase high-performance liquid chromatography (RP-HPLC) using mobile phase water: acetonitrile: glacial acetic acid: phosphate buffer in the ratio of 500:500:1:0.5 v/v/v/v at 225 nm using column nucleosil C18, 125 ×4.0 mm, 5 µm. VLN sample (VLN SPL) thus obtained an unknown major impurity (UIMP) of 0.5 % at 0.38 retention time ratio (RRt) and purity of VLN was found to be 98.70 % respectively.Results: Estimation of VLN SPL total unknown impurities was found to be 1.3% by RP-HPLC. In similarly by liquid chromatography mass spectroscopy (LC-MS) a typical chromatogram of valsartan (VLN) at Rt 9.03 min and UIMP at Rt 3.3 min were recorded at a total run time of 23 min. Assay of VLN SPL was validated as per international council for harmonization (ICH) guidelines. Average % recovery was found to be 100.04 % for VLN SPL.Conclusion: The proposed work clearly indicates that the method can be easily adapted for the routine one step estimation of VLN active pharmaceutical ingredient (API)

SYNTHESIS AND CYTOTOXIC, ANTI OXIDANT ACTIVITES OF NEW CHALCONE DERIVATIVES

ABSTRACT Chalcones belong to an important class of flavonoids, which may be prepared by Claisen reaction. They possess a wide range of biological activities and industrial applications. Kostanecki was the first to give the term chalcone and who did pioneering work in the synthesis of naturally coloring compounds. Cytotoxicity against tumour cell lines may be the result of disruption of the cell cycle, inhibition of angiogenesis, interference with p53-MDM2 interaction, mitochondrial uncoupling or induction of apoptosis. Structural requirements for cytotoxic activity vary according to the mechanisms of action. Chemoprotection by chalcones may be a consequence of their antioxidant properties, mediated via inhibition or induction of metabolic enzymes, by an anti-invasive effect or a reduction in nitric oxide production. Chalcones are synthesized by conventional and microwave assisted synthesis methods. By microwave assisted synthesis, a considerable increase in the reaction rate has been observed and that too, with better yields. The compounds have been screened for cytotoxic activity and antioxidant activity

Synthesis of 3-(5-phenyl-1, 3, 4-oxadiazol-2-yl)-2<em>H</em>-chromen-2-ones as anticonvulsant agents

737-7453-(5-Phenyl-1,3,4-oxadiazol-2-yl)-2H-chromen-2-one (IVa-IVl) have been synthesized from N-benzylidene2-oxo-2H-chromene-3-carbohydrazide (IIIa-IIIl). The structure of synthesized coumarinyl oxadiazoles have been established by spectral data, elemental analysis and alternative synthetic routes wherever possible. These compounds have been screened for their anticonvulsant activity by using MES and PTZ models. Coumarinyl oxadiazoles have shown potential anticonvlsant activity. Compound IVb shows very good anticonvulsant activity both in MES and PTZ models

<span style="font-size:12.0pt;font-family: "Times New Roman";mso-fareast-font-family:"Times New Roman";mso-ansi-language: EN-GB;mso-fareast-language:EN-US;mso-bidi-language:AR-SA" lang="EN-GB">Synthesis, characterisation and anthelmintic activity of 3-(4-acetyl-5-phenyl-4,5-dihydro-1,3,4-oxadiazol-2-yl)- 2<i style="mso-bidi-font-style: normal">H</i>-chromen-2-one derivatives</span>

422-427<span style="mso-ansi-language: EN-US;mso-bidi-font-weight:bold" lang="EN-US">Convectional synthesis of several coumarin-oxadiazole derivatives from starting compounds 2-hydroxy benzaldehyde and diethylmalonate has been accomplished. Successful synthesis of the derivatives has been confirmed by spectral studies i.e. UV, IR, MS and 1H NMR. All successfully synthesized compounds have been screened for in vitro anthelmintic activity by taking adult Indian earthworms Pheretima posthuma. Among all the derivatives 4-chloro derivatives have shown maximum activity when compared with the standard. </span