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.
本文介绍了利用反相高效液相色谱法和强制降解研究产生的降解产物对依托瑞昔布中相关物质的开发和验证。依托昔布经受了酸、碱、氧化、热、光降解等应激条件。除了氧化环境外，在所有这些条件下都是稳定的。采用Inertsil ODS-3V， (4.6x250 mm, 5 μm) C18，在25℃条件下成功分离药物。梯度洗脱，流速1.0 mL/min。流动相为缓冲液:乙腈缓冲液(0.01 M KH2PO4)，比为90:10 (v/v)，紫外检测波长为238 nm。杂质- 05a、杂质-04和依托昔布的Rt值分别为3.09 min、17.01 min和21.45 min，运行时间为45 min。关键词:反相高效液相色谱法，依托昔布，方法验证本研究试图建立依托昔布剂型中相关物质的反相高效液相色谱方法和方法验证。Etoricoxib(图1)的活性成分是arcoxia 1,2, Etoricoxib是选择性COX-2抑制剂，它抑制环氧化酶(COX-2)的第二异构体。由于COX-2在前列腺素的生成中起着至关重要的作用，抑制COX-2可以有效地减轻疼痛。依托昔布适用于类风湿关节炎、银屑病关节炎、骨关节炎、强直性脊柱炎、急性疼痛和痛风的治疗。其化学式为C18H15ClN2O2S，分子量为358.842 g/mol。
{"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}
: 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.
硅酸盐和相关的多孔材料是固体，能够与客体分子、离子和原子相互作用，不仅在其表面，而且在主体内。为了制备具有更好吸附性能的材料，研究了实验室制备的二氧化硅@二氧化硅混合形式的硅酸锡作为吸附长寿命放射性核素152+154 Eu 3+的潜在吸附剂，从含有134 Cs +和60 Co 2+的水溶液中保留。据报道，在pH = 4的恒定条件下，eu3 +的吸附是接触时间、初始离子浓度和温度的函数。在高离子浓度、高温条件下有利于对Eu 3+的吸附，前4 h后未发生明显的吸附。吸附数据与拟二级动力学模式拟合较好，平衡用freundlich型方程进行了肯定验证。此外，为了提高所研究的放射性核素从水介质的分离效率，结果表明，SnSi对放射性核素的吸附具有强烈的温度依赖性。134cs +离子的平衡是放热的，而60co和134cs离子的平衡是吸热的。基于这种矛盾摄取，离子的选择性得到了估计，并实现了Eu 3+与其他竞争离子的分离。热力学参数(∆G◦、∆H◦和∆S◦)表明，134 Cs +的吸附过程是自发的放热过程，而对后面研究的离子则是吸热过程。
{"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}
: 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.
{"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}
: 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.
{"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
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.
{"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
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.
{"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}
: 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.
{"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}
: 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.
{"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}
: 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.
{"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}
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.
{"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}
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