{"title":"Analytical Method Development and Validation of Related Substances in Etoricoxib (API) by Using RP-HPLC","authors":"K. Susmetha, K. Nataraj, A. S. Rao","doi":"10.7598/cst2019.1563","DOIUrl":"https://doi.org/10.7598/cst2019.1563","url":null,"abstract":"This article describes the development and validation of related substances in Etoricoxib by using RP-HPLC and degradation products generated from the forced degradation studies. Etoricoxib was subjected to stress conditions such as acid, alkaline, oxidative, thermal and photo degradation. It was found to be stable in all these conditions except in oxidation environment. Successful separation of drugs was achieved on Inertsil ODS-3V, (4.6x250 mm, 5 μm) C18 at 25 oC. Gradient elution at a flow rate of 1.0 mL/min. The mobile phase consisted of mixture of Buffer: Acetonitrile Buffer (0.01 M KH2PO4) in the ratio of 90:10 (v/v) respectively and UV detection wavelength was 238 nm. The Rt value of Impurity-05A, Impurity-04 and Etoricoxib was found to be 3.09 min, 17.01 min and 21.45 min respectively with a run time of 45 min. Keyword: RP-HPLC, Etoricoxib, Method validation Introduction In this present study an attempt was made to develop RP-HPLC method and method validation of related substances in Etoricoxib in dosage form. The Etoricoxib (Figure 1) active ingredient is arcoxia 1,2 , etoricoxib is selective COX-2 inhibitor it inhibits the second isoform of cyclooxygenases enzyme (COX-2). Since COX-2 is crucial 3 in the production of prostaglandins, inhibition of COX-2 effectively decreases pain. Etoricoxib is indicated for the treatment of rheumatoid arthritis, Psoriatic arthritis, Osteoarthritis, ankylosing spondylitis, acute pain and gout. Its chemical formula is C18H15ClN2O2S and molecular weight 4 is 358.842 g/mol.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"21 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74084448","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"152/154Eu(III) Ions Sorption on Stannic Silicate Granules: A Radiotracer Study","authors":"I. Ali","doi":"10.7598/cst2019.1565","DOIUrl":"https://doi.org/10.7598/cst2019.1565","url":null,"abstract":": Silicates and related porous materials are solids able to interact with guest molecules, ions and atoms not only at their surfaces but also within the bulk. With the objective of producing materials showing better sorption properties, a laboratory prepared stannic silicate in mixed SnO 2 @SiO 2 form was investigated as potential sorbent for retention of long lived radionuclides 152+154 Eu 3+ from aqueous solution containing 134 Cs + and 60 Co 2+ . Sorption of Eu 3+ has been reported as a function of contact time, initial ion concentration and temperatureat a constant pH equal to 4. The uptake of Eu 3+ was found to be favored at high ion concentration, high temperature and no significant sorption took place after the first 4 h. A pseudo second order kinetic pattern fitted the sorption data well, while equilibrium was positively verified with Freundlich-type equation. Further, in attempt to enhance the separation efficiency of the studied radionuclides from aqueous medium, results showed that the sorption on SnSi was found strongly temperature–dependent. Ions equilibrium was found exothermic in case of 134 Cs + however it endothermic in case of both 60 Co and 134 Cs ions. Based on this contradict uptake, selectivity of ions has been estimated and separation of Eu 3+ from other competing ions was achieved.The thermodynamic parameters ( ∆ G ◦ , ∆ H ◦ and ∆ S ◦ ) showed that the adsorption process is spontaneous and exothermic in case of 134 Cs + but it endothermic in case of the later studied ions.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89639690","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Experimental and Theoretical Investigation of 3D-Metal Complexes Derived from N-(1H-Benzimidazol-2-yl)-2-mercaptoacetamide Derivative","authors":"G. Anuradha, S. Sreekanth, B. Manogna","doi":"10.7598/cst2019.1571","DOIUrl":"https://doi.org/10.7598/cst2019.1571","url":null,"abstract":": New trinuclear metal complexes of Co(II), Ni(II), Cu(II) and Zn(II) with N -(1 H -benzimidazol-2-yl)-2-mercaptoacetamide (BMA) were synthesized from chloride salts of relative metals in butanol medium. Synthesized metal complexes were characterized by elemental analysis, conductance measurements, IR, UV-Vis, ESR, TGA & DTA and magnetic susceptibility measurements. IR spectral data suggest that the ligand behaves as monobasic tridentate (NOS) with donor sites of azomethine nitrogen (ring), oxygen atom of carbonyl group and thio group. Physico-chemical data suggest tetrahedral geometry for Co(II), Ni(II) and Zn(II) complexes. Square planar intended for Cu(II) complex and all these complexes exhibits non-elecrolytic nature. The complexes were evaluated for their antimicrobial activity by in-vitro antimicrobial screening against bacteria Staphylococcus aureus, Bacillus subtilis , Escherichia coli and Klebsiella Pneumonia . The results indicate that antimicrobial activity increased during metallation. A detailed analysis is done theoretically using DFT method with B3LYP/6-311G/LanL2DZ functional for ligand and complexes. Docking studies of ligand and metal complexes carried out using OPLS 2005 force field in Schrodinger suite.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"5 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86929502","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Facile Protocol for Synthesis of Some Novel 2-phenethyl-1H-benzimidazole Derivatives and Screening of In-Vitro Anti-inflammatory and Antimicrobial Activities","authors":"R. Shastri, S. Jadhav","doi":"10.7598/cst2019.1566","DOIUrl":"https://doi.org/10.7598/cst2019.1566","url":null,"abstract":": A convenient and efficient method for the preparation of some novel 2-phenethyl-1 H benzimidazole derivatives (4a-h) has been achieved by the condensation of phenyl propionic acids (2a-h) with o -phenylenediamine (3) in POCl 3 . The advantages of this method is excellent yields, short reaction time, no side reaction and operational simplicity and ease product isolation The structure of all the synthesized compounds were characterized by FT-IR, 1 H NMR and MS data. Furthermore, compounds (4a-h) were screened for their antibacterial activity against gram negative ( E. coli ) and gram positive ( B.subtilis ) bacteria, antifungal activity against Aspergillusniger and Penicillium chrysogenum and anti-inflammatory activities. Some of the compounds exhibited promising antibacterial, antifungal and anti-inflammatory activities.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"9 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86496302","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. H. Hamed, S. K. Ibrahim, S. Dhahir, Amal H. Mhemeed
{"title":"Indirect Spectrophotometric Determination of Amoxicillin by Oxidative with Cerium ammonium Nitrate Using Arsenazo III as a Reagent","authors":"A. H. Hamed, S. K. Ibrahim, S. Dhahir, Amal H. Mhemeed","doi":"10.7598/cst2019.1602","DOIUrl":"https://doi.org/10.7598/cst2019.1602","url":null,"abstract":"A simple, accurate and sensitive spectrophotometric way used for preparation. The suggested method depends on using arsenazo III as reagent. The current method was depending on oxidative coupling reaction of amoxicillin by cerium ammonium nitrate with arsenazo III in the presence of sulfuric acid as acidic media. Then reaction Ce(III) with arsenazo III to form pink water-soluble dye product that has a maximum absorption at max 500 nm. Beers law is obeyed in the concentration of (1-10 μgmL). The molar absorptivity is 3x10 L.mol.cm, a sandal sensitivity of 0.012 μgcm. Limit of detection (LOD) and limit of quantitation are 0.00874 μgmL, (LOQ) 0.0291 μgmL respectively. The analytical recovery of the new method was good (100.72%). The method successfully applied for the determination of Amoxicillin in pharmaceutical preparations.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"9 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90212925","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Manjunatha, N. Banu, Mohamed Ziaulla, F. Rehman, Puttaraje Gowda
{"title":"Synthesis and Crystal Structure Studies of Bis- [1-(p-methoxybenzyl)-2-(p-methoxyphenyl)-1H-benzimidazole]tetrabromidocadmate(II)","authors":"M. Manjunatha, N. Banu, Mohamed Ziaulla, F. Rehman, Puttaraje Gowda","doi":"10.7598/cst2019.1580","DOIUrl":"https://doi.org/10.7598/cst2019.1580","url":null,"abstract":"The complex Cd(L)2Br4, contains a dibromocadmate(II) coordinated to two benzimidazole moiety. In the crystal structure the molecules are further interconnected with weak intermolecular CH⋅⋅⋅O hydrogen bonds generating a three-dimensional network. Further the supramolecular assembly is stabilized by Intermolecular C-H⋅⋅⋅π and π⋅⋅⋅π interactions provide additional stability to the structure. Additionally the metal ion Cd(II) exhibits a distorted tetrahedral coordination of the bromine atoms.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"25 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75575770","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Synthesis and Electrochemical Performance of Tungsten Carbide","authors":"I. Joshi, K. Khati, A. Bisht, S. Mehtab, M. Zaidi","doi":"10.7598/cst2019.1550","DOIUrl":"https://doi.org/10.7598/cst2019.1550","url":null,"abstract":": Tungsten carbide (WC) was synthesized via modified polymer precursor method. The formation of WC was ascertained through Fourier-transform infrared spectra (FT-IR), x-ray diffraction (XRD), thermogravimetry analysis (TGA) and differential thermo analysis (DTA). The WC electrode was synthesized over 316 stainless steel to evaluate electrochemical performance through cyclic voltammetry (CV). The CV curves of WC electrode were found in the potential span of -0.6 to 0.0V in KOH (1.0 M). The WC electrode shows specific capacitance (Cs) of 110 F/g at 0.001 V/s and good cyclic stability over 500 cycles.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"11 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74292244","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Effect of Synthesis Parameters on Photoactivity of CdS Nanoparticles","authors":"M. J. Pawar, Archana Ingle, Rahul K. Tayawade","doi":"10.7598/cst2019.1549","DOIUrl":"https://doi.org/10.7598/cst2019.1549","url":null,"abstract":": In the present work, CdS nanoparticles were synthesized by four different routes using ammonium sulphide ((NH 4 ) 2 S) as source of (Sulphide) S 2- ions. CdS nanoparticles were grown by simple chemical precipitation reactions in aqueous medium at room temperature. The effect of stabilizers on the stability and size of CdS nanoparticles was studied. The effect of different reaction parameters on the size of nanoparticles, absorbance and respective band gaps and crystalline structure were studied. The microstructure and morphology of the synthesized CdS nanoparticles have been characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. XRD pattern reveals that as-synthesized CdS nanoparticles exhibit both hexagonal and cubic phases. The size of the particles calculated by Debye Scherrer formula according to the XRD spectra has been found to be about 3-30 nm. The optical properties of the sample have been studied by UV-Visible and photoluminescence spectroscopy. The existence of blue shift in UV-Visible spectroscopy reveals the quantum confinement effect of CdS nanoparticles. Finally, the synthesized CdS nanoparticles were exploited for the degradation of acid blue-29 (AB-29), under UV light. The photocatalytic efficiency of the synthesized nanoparticles, using different reaction routes were compared and optimized.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"72 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83559995","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Spectrophotometric Determination and Cloud Point Extraction of Cefixime Drugs in Pure form and Pharmaceutical Preparation","authors":"S. Dhahir, J. Noor","doi":"10.7598/cst2019.1600","DOIUrl":"https://doi.org/10.7598/cst2019.1600","url":null,"abstract":": A simple, rapid, accurate, sensitive and eco friendly method has been developed for the quantitative determination of cefixime(CFX) in pure form and pharmaceutical preparations by using a combination of cloud point extraction with UV-Visible absorption spectrophotometric method. Analytical applications of complexation with metal ions by reacting cefixime (CFX) with copper(II) and iron(III) to form chelate complexes under limited experimental conditions. The method based to dissolved CFX in 0.1 M NaOH, 10% (v/v) triton x-114 and mixed with (1000 µ gmL -1 ) copper(II) or (1000 µ gmL -1 ) iron(III). The formation of CFX-Cu(II) complex at pH 13 and wavelength 827 while the complex of CFX-Fe(III) was formatted at pH 11 and wavelength at 439 nm. The complexes of CFX-Cu(II) and CFX-Fe(III) obey Beer’s Law in the range 10-130 and 10-160 µ g/mL respectively. LOD and LOQ values for these complexes were 1.6906 µ g/mL and 5.6355 µ g/mL and LOQ values were 1.58655 µ g/mL and 5.2887 µ g/mL respectively. Method was validated and successfully applied to drug formulations like syrup infusion marketed in Amman and cefixime capsules marketed in Iraq. The results of analysis have been validated statistically by recovery studies and were found satisfactory.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89280067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Design, Synthesis and Biological Evaluation of Some Novel Chalcone-Sulfonamide Hybrids","authors":"Mahammadali M. Khanusiya","doi":"10.7598/cst2019.1538","DOIUrl":"https://doi.org/10.7598/cst2019.1538","url":null,"abstract":"A series of novel chalcone tethered sulphonamide hybrids 3a-5f were fabricated by condensing appropriate sulphonamide scaffold with methoxy and/or hydroxy substituted chalcones as a multi-target drug for therapeutic treatment. Chalcones were prepared by Claisen-Schmidt condensation of a substituted aldehyde with para aminoacetophenone. The synthesized chalconesulphonamide hybrids were screened by means of their antibacterial activity by NCCLS method. Among all these compounds, 5e and 5c were observed to displaying more potent growth inhibitory activity against bacterial strain and hybrid 5a shows more obvious antifungal activity. FT-IR, NMR and HR-LCMS spectral study assert the structures of synthesized sulphonamide chalcone hybrids.","PeriodicalId":10087,"journal":{"name":"Chemical science transactions","volume":"141 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87873461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}