Yahya Salma, H. Zakaria, I. Hassan, M. Bouchekara, H. El-Nakat, F. Omar, A. Allouch
The activity of a chiral molecule can vary from one atropisomer to the other. In this study, the separation of racemic-N-(2-methylphenyl), N’-(2-chlorophenyl) thiourea (H 2 L 2 ), a hydrophobic heavy metal trap, has been studied using reversed-phase high-performance liquid chromatography (RP-HPLC) with hydroxypropyl-beta-cyclodextrin (HP-β-CD) as a complexing additive to the racemic mixture and hexane-isopropanol as a mobile phase. The stoichiometry and the overall association constant of the complex have been determined using the continuous variation (Job's plot) method and the Scott's method respectively.
{"title":"Complex of a new racemic thiourea substrate: Spectrophotometric study and separation of atropisomers","authors":"Yahya Salma, H. Zakaria, I. Hassan, M. Bouchekara, H. El-Nakat, F. Omar, A. Allouch","doi":"10.7439/IJPC.V8I1.4681","DOIUrl":"https://doi.org/10.7439/IJPC.V8I1.4681","url":null,"abstract":"The activity of a chiral molecule can vary from one atropisomer to the other. In this study, the separation of racemic-N-(2-methylphenyl), N’-(2-chlorophenyl) thiourea (H 2 L 2 ), a hydrophobic heavy metal trap, has been studied using reversed-phase high-performance liquid chromatography (RP-HPLC) with hydroxypropyl-beta-cyclodextrin (HP-β-CD) as a complexing additive to the racemic mixture and hexane-isopropanol as a mobile phase. The stoichiometry and the overall association constant of the complex have been determined using the continuous variation (Job's plot) method and the Scott's method respectively.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"56 1","pages":"01-06"},"PeriodicalIF":0.0,"publicationDate":"2018-04-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91432357","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}
B. Sivagami, R. Chandrasekar, Pavan Kumar, R. Sireesha, B. ReddyPadmaja
Alzheimer’s disease (AD) is a neurodegenerative disorder characterized by progressive memory defeat and impairment in behavior, language, and visuospatial skills. Current approved drugs for the treatment of Alzheimer disease (AD) include cholinesterase inhibitors (donepezil, galantamine and rivastigmine,) and the NMDA receptor antagonist memantine. These drugs can provide a symptomatic relief but they poorly affect the progression of the disease. There are several risk factors for the development of Alzheimer’s disease which include factors like age, genetic factor family history, Down’s syndrome, head injury and cardiovascular diseases. Cardio vascular risk factors may include blood pressure, cholesterol, diabetes, obesity and smoking. People may experience cognitive mental illness, difficulty in understanding and thinking, forgetting things easily, making things complicated, mental confusion, difficulty in concentrating, inability to create old memories, inability to do simple things, or inability to recognize common things. The main objective of this review is discussion on various analytical methods used, different solvents used as mobile phase and their retention time. This review includes method development and validation of cholinesterase inhibitors like Donepezil, Galantamine, Rivastigmine and Tacrine combination of drugs which include cholinesterase inhibitors like Donepezil and NMDA receptor antagonist Memantine. The review is a collection of data including various analytical methods used, the different columns used, mobile phase used, flow rate, different detectors and detection wavelength and retention time. This review includes discussion on method development and validation of Alzheimer’s drugs and newly developed compounds which have lesser side effects and are proving more efficient for treatment of Alzheimer’s disease.
{"title":"An analytical review on method development and validation of drugs used for alzheimers disease","authors":"B. Sivagami, R. Chandrasekar, Pavan Kumar, R. Sireesha, B. ReddyPadmaja","doi":"10.7439/ijapa.v7i4.4510","DOIUrl":"https://doi.org/10.7439/ijapa.v7i4.4510","url":null,"abstract":"Alzheimer’s disease (AD) is a neurodegenerative disorder characterized by progressive memory defeat and impairment in behavior, language, and visuospatial skills. Current approved drugs for the treatment of Alzheimer disease (AD) include cholinesterase inhibitors (donepezil, galantamine and rivastigmine,) and the NMDA receptor antagonist memantine. These drugs can provide a symptomatic relief but they poorly affect the progression of the disease. There are several risk factors for the development of Alzheimer’s disease which include factors like age, genetic factor family history, Down’s syndrome, head injury and cardiovascular diseases. Cardio vascular risk factors may include blood pressure, cholesterol, diabetes, obesity and smoking. People may experience cognitive mental illness, difficulty in understanding and thinking, forgetting things easily, making things complicated, mental confusion, difficulty in concentrating, inability to create old memories, inability to do simple things, or inability to recognize common things. The main objective of this review is discussion on various analytical methods used, different solvents used as mobile phase and their retention time. This review includes method development and validation of cholinesterase inhibitors like Donepezil, Galantamine, Rivastigmine and Tacrine combination of drugs which include cholinesterase inhibitors like Donepezil and NMDA receptor antagonist Memantine. The review is a collection of data including various analytical methods used, the different columns used, mobile phase used, flow rate, different detectors and detection wavelength and retention time. This review includes discussion on method development and validation of Alzheimer’s drugs and newly developed compounds which have lesser side effects and are proving more efficient for treatment of Alzheimer’s disease.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"185 1","pages":"32-37"},"PeriodicalIF":0.0,"publicationDate":"2017-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88100072","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}
Bioanalytical method based on a variety of physico-chemical and biological techniques such as chromatography, immunoassay and mass spectrometry, must be validated prior to and during use to give confidence in the results generated. It is the process used to establish that a quantitative analytical method is suitable for biomedical applications. Bioanalytical method validation includes all of the procedures that demonstrate that a particular method used for quantitative measurement of analytes in a given biological matrix, such as blood, plasma, serum, or urine is reliable and reproducible for the intended use. The present manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters is discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery and stability. These validation parameters are described, together with an example of validation methodology applied in the case of chromatographic methods used in bioanalysis, taking in account to the recent Food and Drug Administration (FDA) guidelines and EMA guide
{"title":"Bio-analytical method validation and its importance in pharma research - A review article","authors":"A. Ingle, M. Baheti, S. Wate, K. Bhusari","doi":"10.7439/IJAPA.V7I4.4418","DOIUrl":"https://doi.org/10.7439/IJAPA.V7I4.4418","url":null,"abstract":"Bioanalytical method based on a variety of physico-chemical and biological techniques such as chromatography, immunoassay and mass spectrometry, must be validated prior to and during use to give confidence in the results generated. It is the process used to establish that a quantitative analytical method is suitable for biomedical applications. Bioanalytical method validation includes all of the procedures that demonstrate that a particular method used for quantitative measurement of analytes in a given biological matrix, such as blood, plasma, serum, or urine is reliable and reproducible for the intended use. The present manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters is discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery and stability. These validation parameters are described, together with an example of validation methodology applied in the case of chromatographic methods used in bioanalysis, taking in account to the recent Food and Drug Administration (FDA) guidelines and EMA guide","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"143 1","pages":"28-31"},"PeriodicalIF":0.0,"publicationDate":"2017-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78987285","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. Shahanaz, G. Subiksha, M. Yuha, A. GowriShankarB
Wounds generated from burns are fatal and cause marks that last for a long period of time. The formulation of anti marks cream especially for burns would provide hope for a better way of treating scars. The aim of this study is to prepare an ointment using hair ash and oil along with aloevera followed by the characterization of compounds by using Gas Chromatography and Mass Spectroscopy (GC-MS).The natural compounds used could possibly reduce any side effects on the skin. The GC-MS analysis of the ointment revealed the presence of 30 bioactive compounds. The predominant bioactive compounds were especially fatty acids such as hexadecanoic acid, tetradecanoic acid, dodecanoic acid and octadecanoic acid. The antibacterial, antioxidant, anti-inflammatory, antifungal properties of these bioactive compounds could be effectively used in the treatment of scars.
{"title":"GC-MS analysis of anti-mark ointment formulation for skin burns","authors":"A. Shahanaz, G. Subiksha, M. Yuha, A. GowriShankarB","doi":"10.7439/IJPC.V7I11.4514","DOIUrl":"https://doi.org/10.7439/IJPC.V7I11.4514","url":null,"abstract":"Wounds generated from burns are fatal and cause marks that last for a long period of time. The formulation of anti marks cream especially for burns would provide hope for a better way of treating scars. The aim of this study is to prepare an ointment using hair ash and oil along with aloevera followed by the characterization of compounds by using Gas Chromatography and Mass Spectroscopy (GC-MS).The natural compounds used could possibly reduce any side effects on the skin. The GC-MS analysis of the ointment revealed the presence of 30 bioactive compounds. The predominant bioactive compounds were especially fatty acids such as hexadecanoic acid, tetradecanoic acid, dodecanoic acid and octadecanoic acid. The antibacterial, antioxidant, anti-inflammatory, antifungal properties of these bioactive compounds could be effectively used in the treatment of scars.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"4 1","pages":"155-161"},"PeriodicalIF":0.0,"publicationDate":"2017-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74932021","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}
Tuberculosis is a major disease causing 1.8 million deaths worldwide, every year. It represents the leading cause of mortality resulting from a bacterial infection. This point to an urgent need for new promising drug candidates to combat the drug resistance and control the disease. Recent studies reveal the ability of 1, 3, 4 Oxadiazole derivatives to produce antibacterial, anti-tubercular anticancer and anti-inflammatory activity. In the present research work a series of 4-(1, 3, 4-Oxadiazol-2-yl) pyridine based 1, 3, 4 Oxadiazole derivatives were designed and docked against Mtb enzyme target L, d transpeptidase 2. The selected molecules were synthesized and repeatedly recrystallized to attain the expected purity. All the purified compounds were characterized by various spectral analytical techniques and evaluated for anti- mycobacterial activity against tuberculosis H37RV strain by Microplate Alamar Blue Assay (MABA) method. The experimental results showed that Compounds SA, VS4 and VS5 possesses anti-tubercular activity in the range of 12.5mcg/mL while Compounds VS1 and VS2 showed antitubercular activity with an MIC value of 6.25mcg/mL and compound NA exhibited moderate activity.
结核病是全球每年造成180万人死亡的主要疾病。它是细菌感染导致死亡的主要原因。这表明迫切需要新的有希望的候选药物来对抗耐药性和控制疾病。近年来的研究表明，1,3,4恶二唑衍生物具有抗菌、抗结核、抗肿瘤和抗炎活性。本研究设计了一系列以4-(1,3,4 -恶二唑-2-基)吡啶为基础的1,3,4恶二唑衍生物，并与Mtb酶靶点L, d转肽酶2对接。对选定的分子进行合成并反复重结晶以达到预期的纯度。采用各种光谱分析技术对纯化的化合物进行了结构表征，并采用微孔板Alamar Blue Assay (MABA)法对结核H37RV菌株进行了抑菌活性评价。实验结果表明，化合物SA、VS4和VS5的抗结核活性在12.5mcg/mL范围内，化合物VS1和VS2的抗结核活性MIC值为6.25mcg/mL，化合物NA的抗结核活性中等。
{"title":"Design, synthesis, characterization and biological evaluation of some novel 1, 3, 4 oxadiazole derivatives as anti-tubercular agents targeting L, D transpeptidase 2","authors":"A. Suresh, N. Vidhyashree, S. P. Ramakrishnan","doi":"10.7439/IJPC.V7I10.4443","DOIUrl":"https://doi.org/10.7439/IJPC.V7I10.4443","url":null,"abstract":"Tuberculosis is a major disease causing 1.8 million deaths worldwide, every year. It represents the leading cause of mortality resulting from a bacterial infection. This point to an urgent need for new promising drug candidates to combat the drug resistance and control the disease. Recent studies reveal the ability of 1, 3, 4 Oxadiazole derivatives to produce antibacterial, anti-tubercular anticancer and anti-inflammatory activity. In the present research work a series of 4-(1, 3, 4-Oxadiazol-2-yl) pyridine based 1, 3, 4 Oxadiazole derivatives were designed and docked against Mtb enzyme target L, d transpeptidase 2. The selected molecules were synthesized and repeatedly recrystallized to attain the expected purity. All the purified compounds were characterized by various spectral analytical techniques and evaluated for anti- mycobacterial activity against tuberculosis H37RV strain by Microplate Alamar Blue Assay (MABA) method. The experimental results showed that Compounds SA, VS4 and VS5 possesses anti-tubercular activity in the range of 12.5mcg/mL while Compounds VS1 and VS2 showed antitubercular activity with an MIC value of 6.25mcg/mL and compound NA exhibited moderate activity.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"20 1","pages":"149-154"},"PeriodicalIF":0.0,"publicationDate":"2017-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86939890","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}
Savita R. Shejale, C. Rajput, Shubhangi S. Bansode, M. Kondawar
A new series of substituted PyrazoloPyrimidine & Pyrazolopyridine were designed to meet the structural requirement of antimicrobial ,Analgesic & antifungal drugs which has been known to possess a broad spectrum of biological activities such as analgesic,antimicrobial antifungal etc .(1) The therapeutic importance of these rings prompted us to develop selective molecules. The starting material of 1-{1-phenyl-3-(substituted phenyl)-1H-pyrazol-4-yl}-3-phenyl-1-propen-3-one (Chalcone) (3a-c) prepared from by claisen schmidt reaction from respective 1-phenyl-3-(substituted phenyl)-1H-pyrazoles-4-carboxaldehyde (Vilsmeier-Haack Reaction) ( 2a-c). 1-{1-phenyl-3-(substituted phenyl)-1H-pyrazol-4-yl}-3-phenyl-1-propen-3-one (Chalcone) (3a-c) further treated with thiourea ,3amino-s-triazole,ethylcyanoacetate, cynothioacetamideto produced 1,2,3,4 tetrahydropyrimidine (4 a-c),triazolopyrimidine (5 a,b),cynophenylpyridine(6 a-c) & phenyl pyridine thione derivatives.The structures of newly Synthesised compounds were characterized by spectral data & studied for their antimicrobial & Antifungal activities. Compounds 4a, 4c, 5a, 6c, 7c showed high antimicrobial activity using disc diffusion method with reference to using Amoxicillin as standard drug active active against Bacillus substillus, staphylococcus aureus, Proteus vulgaris.and pseudomonas.Similary compound 4c&7c showed maximum antifungal activity against fungal species candida albicans
{"title":"Synthesis, characterisation, evaluation of antimicrobial & antifungal activity of novel pyrazolopyrimidine & pyrazolopyridine derivatives","authors":"Savita R. Shejale, C. Rajput, Shubhangi S. Bansode, M. Kondawar","doi":"10.7439/IJPC.V7I9.4392","DOIUrl":"https://doi.org/10.7439/IJPC.V7I9.4392","url":null,"abstract":"A new series of substituted PyrazoloPyrimidine & Pyrazolopyridine were designed to meet the structural requirement of antimicrobial ,Analgesic & antifungal drugs which has been known to possess a broad spectrum of biological activities such as analgesic,antimicrobial antifungal etc .(1) The therapeutic importance of these rings prompted us to develop selective molecules. The starting material of 1-{1-phenyl-3-(substituted phenyl)-1H-pyrazol-4-yl}-3-phenyl-1-propen-3-one (Chalcone) (3a-c) prepared from by claisen schmidt reaction from respective 1-phenyl-3-(substituted phenyl)-1H-pyrazoles-4-carboxaldehyde (Vilsmeier-Haack Reaction) ( 2a-c). 1-{1-phenyl-3-(substituted phenyl)-1H-pyrazol-4-yl}-3-phenyl-1-propen-3-one (Chalcone) (3a-c) further treated with thiourea ,3amino-s-triazole,ethylcyanoacetate, cynothioacetamideto produced 1,2,3,4 tetrahydropyrimidine (4 a-c),triazolopyrimidine (5 a,b),cynophenylpyridine(6 a-c) & phenyl pyridine thione derivatives.The structures of newly Synthesised compounds were characterized by spectral data & studied for their antimicrobial & Antifungal activities. Compounds 4a, 4c, 5a, 6c, 7c showed high antimicrobial activity using disc diffusion method with reference to using Amoxicillin as standard drug active active against Bacillus substillus, staphylococcus aureus, Proteus vulgaris.and pseudomonas.Similary compound 4c&7c showed maximum antifungal activity against fungal species candida albicans","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"28 1","pages":"144-148"},"PeriodicalIF":0.0,"publicationDate":"2017-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85434046","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}
Vijayalakshmi Marella, Aisha J Syed, M. Lakshmiprasanna, B. N. Nalluri
The objective of the present study was to develop a simple, specific and accurate reverse phase high performance liquid chromatographic method for the determination of Canagliflozin in bulk and pharmaceutical dosage forms. The method is optimized on an inertsil ODS-3(250.6mm, 5) column with a mobile phase combination of 0.02% Formic acid: Acetonitrile (40:60) at a flow rate 1.2ml/min and the eluents were monitored at 230nm. Under these LC conditions Canagliflozin peak was eluted at 4.4 min. The developed method was validated as per ICH guidelines. The calibration curve was linear over a concentration range of 10-50g/ml (R 2 =0.999) and the mean percentage assay was found to be 98.2. The statistical data proved that proposed method is accurate, precise and reproducible. The method which is LC-MS compatible can be adopted in the routine analysis of Canagliflozin in bulk and pharmaceutical dosage forms.
{"title":"A novel validated RP-HPLC method for the estimation of canagliflozin in bulk and pharmaceutical dosage forms","authors":"Vijayalakshmi Marella, Aisha J Syed, M. Lakshmiprasanna, B. N. Nalluri","doi":"10.7439/IJAPA.V7I3.4350","DOIUrl":"https://doi.org/10.7439/IJAPA.V7I3.4350","url":null,"abstract":"The objective of the present study was to develop a simple, specific and accurate reverse phase high performance liquid chromatographic method for the determination of Canagliflozin in bulk and pharmaceutical dosage forms. The method is optimized on an inertsil ODS-3(250.6mm, 5) column with a mobile phase combination of 0.02% Formic acid: Acetonitrile (40:60) at a flow rate 1.2ml/min and the eluents were monitored at 230nm. Under these LC conditions Canagliflozin peak was eluted at 4.4 min. The developed method was validated as per ICH guidelines. The calibration curve was linear over a concentration range of 10-50g/ml (R 2 =0.999) and the mean percentage assay was found to be 98.2. The statistical data proved that proposed method is accurate, precise and reproducible. The method which is LC-MS compatible can be adopted in the routine analysis of Canagliflozin in bulk and pharmaceutical dosage forms.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"1 1","pages":"24-27"},"PeriodicalIF":0.0,"publicationDate":"2017-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89918346","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 spectrophotometric method was developed for the simultaneous determination of pseudoephedrine HCl (PSE) and triprolidine HCl (TRI) in bulk and dosage forms. The method involved the determination of pseudoephedrine in the presence of triprolidine using two wavelengths (257 nm & 290 nm). Beers law was obeyed in the concentration (152-760 ?g/ml) and (6.4-32 ?g/ml) with good linearity (0.9996 and 0.9996) for pseudoephedrine and triprolidine respectively. The accuracy and the precision of the developed method were very good (RSD ? 2%). The validity of the proposed method was confirmed through the statistical comparison of the obtained data with those of the official USP method.
{"title":"Spectrophotometric Method for the Simultaneous Determination of Pseudoephedrine and Triprolidine in Bulk and Tablet Forms","authors":"Imad Osman Abu Reid, Tasneem Awad Widaa","doi":"10.7439/IJAPA.V7I3.4160","DOIUrl":"https://doi.org/10.7439/IJAPA.V7I3.4160","url":null,"abstract":"A spectrophotometric method was developed for the simultaneous determination of pseudoephedrine HCl (PSE) and triprolidine HCl (TRI) in bulk and dosage forms. The method involved the determination of pseudoephedrine in the presence of triprolidine using two wavelengths (257 nm & 290 nm). Beers law was obeyed in the concentration (152-760 ?g/ml) and (6.4-32 ?g/ml) with good linearity (0.9996 and 0.9996) for pseudoephedrine and triprolidine respectively. The accuracy and the precision of the developed method were very good (RSD ? 2%). The validity of the proposed method was confirmed through the statistical comparison of the obtained data with those of the official USP method.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"46 1","pages":"21-23"},"PeriodicalIF":0.0,"publicationDate":"2017-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83947141","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}
The process of producing a series of chemical combinations of 2-methoxy-6-phenyl-5H-pyrrolo[3,4-b]pyrazine-5,7(6H)-dione descendant [103-110] and 7-hydroxy-3-methoxy-6-phenyl-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine-5-one descendant [111-119], magnetized significant regard in prospective of curative requisition. The fusion was conved by conducting 2-hydroxyfuro [3,4-b]pyrazine-5,7-dione with equimolar Bromomethane in dry toluene at 0-5C to get combination 2-methoxyfuro[3,4- b ]pyrazine-5,7-dione which further at reflux condense with aniline derivatives to 2-methoxy-6-phenyl-5H-pyrrolo[3,4-b]pyrazine-5,7(6H)-dione derivatives with Potassium borohydride granules in methanol at 0-20C converted to 7-hydroxy-3-methoxy-6-phenyl-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine-5-one descendant. The distinctive nature of all the incorporated combinations have been described by manipulating basic inspection (elemental analysis), IR, 1 H NMR, 13 C NMR spectroscopical.
{"title":"synthesis and characterization of 2-methoxy-6-phenyl-5h-pyrrolo[3,4-b]pyrazine-5,7(6h)-dione and 7-hydroxy-3-methoxy-6-phenyl-6,7-dihydro-5h-pyrrolo[3,4-b]pyrazine-5-one and some derivatives","authors":"K. Saraswat, Shashi Pandey","doi":"10.7439/IJPC.V7I8.4267","DOIUrl":"https://doi.org/10.7439/IJPC.V7I8.4267","url":null,"abstract":"The process of producing a series of chemical combinations of 2-methoxy-6-phenyl-5H-pyrrolo[3,4-b]pyrazine-5,7(6H)-dione descendant [103-110] and 7-hydroxy-3-methoxy-6-phenyl-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine-5-one descendant [111-119], magnetized significant regard in prospective of curative requisition. The fusion was conved by conducting 2-hydroxyfuro [3,4-b]pyrazine-5,7-dione with equimolar Bromomethane in dry toluene at 0-5C to get combination 2-methoxyfuro[3,4- b ]pyrazine-5,7-dione which further at reflux condense with aniline derivatives to 2-methoxy-6-phenyl-5H-pyrrolo[3,4-b]pyrazine-5,7(6H)-dione derivatives with Potassium borohydride granules in methanol at 0-20C converted to 7-hydroxy-3-methoxy-6-phenyl-6,7-dihydro-5H-pyrrolo[3,4-b]pyrazine-5-one descendant. The distinctive nature of all the incorporated combinations have been described by manipulating basic inspection (elemental analysis), IR, 1 H NMR, 13 C NMR spectroscopical.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"29 1","pages":"121-130"},"PeriodicalIF":0.0,"publicationDate":"2017-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80498606","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}
Krishna Katta, T. S. Rao, J. Mosesbabu, D. V. Rao, V. Malati, K. Sasikala
The objective of the research work is to synthesize potential genotoxic impurity 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate and to develop suitable UPLC method to quantify the above genotoxicimpurity in Escitalopram Oxalate at 15 ppm level. The above genotoxic impurity was synthesized by regio selective tosyaltion of Diol compound, under controlled temperature conditions at 0-5C with TsCl/pyridine/chloroform and characterized. A new UPLC method was developed by using UPLC BEH Shield RP18 100 x 2.1 mm, 1.7 column. The mobile phase used is the mixture of 0.05% ortho phosphoric acid and acetonitrile in the ratio of 8:2 (v/v) as solvent-A and 3:7 (v/v) as solvent-B at a flow rate of 0.4 mL/minute. Detector wavelength monitored at 228nm and column temperature was maintained at 27C. The UPLC method was validated as per International conference on harmonization guidelines. This method is proven as highly sensitive with a detection limit of 5ppm and quantification limit of 15 ppm. Regression analysis showed that the correlation coefficient value of 0.99999. The accuracy of the method was established based on the recovery obtained for 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate. The present research work provided the route of synthesis as well as an advanced analytical methodology to quantify the above critical Genotoxic impurity known as 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate in Escitalopram oxalate.
{"title":"Synthesis and Quantitation of Genotoxic impurity 5-cyano-2-((4-fluorophenyl) (hydroxy) benzyl 4-methyl benzene sulfonate in Escitalopram Oxalate by RP-UPLC","authors":"Krishna Katta, T. S. Rao, J. Mosesbabu, D. V. Rao, V. Malati, K. Sasikala","doi":"10.7439/IJPC.V7I8.4292","DOIUrl":"https://doi.org/10.7439/IJPC.V7I8.4292","url":null,"abstract":"The objective of the research work is to synthesize potential genotoxic impurity 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate and to develop suitable UPLC method to quantify the above genotoxicimpurity in Escitalopram Oxalate at 15 ppm level. The above genotoxic impurity was synthesized by regio selective tosyaltion of Diol compound, under controlled temperature conditions at 0-5C with TsCl/pyridine/chloroform and characterized. A new UPLC method was developed by using UPLC BEH Shield RP18 100 x 2.1 mm, 1.7 column. The mobile phase used is the mixture of 0.05% ortho phosphoric acid and acetonitrile in the ratio of 8:2 (v/v) as solvent-A and 3:7 (v/v) as solvent-B at a flow rate of 0.4 mL/minute. Detector wavelength monitored at 228nm and column temperature was maintained at 27C. The UPLC method was validated as per International conference on harmonization guidelines. This method is proven as highly sensitive with a detection limit of 5ppm and quantification limit of 15 ppm. Regression analysis showed that the correlation coefficient value of 0.99999. The accuracy of the method was established based on the recovery obtained for 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate. The present research work provided the route of synthesis as well as an advanced analytical methodology to quantify the above critical Genotoxic impurity known as 5-cyano-2-((4-fluorophenyl) (hydroxyl) benzyl 4-methyl benzene sulfonate in Escitalopram oxalate.","PeriodicalId":14317,"journal":{"name":"International Journal of Pharmaceutical Chemistry","volume":"16 1","pages":"131-138"},"PeriodicalIF":0.0,"publicationDate":"2017-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78233311","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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