Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2086822
B. Ivanova, M. Spiteller
Abstract The study reports quantification of metronidazole (MTZ) in clinical human urine employing our innovative stochastic dynamic equation D”SD =2.6388.10-17.(–). There are direct analysis without presence of internal standard, using ultra-high accuracy nano-electrospray ionization (ESI) mass spectrometry (MS), quantum chemistry and chemometrics, respectively. The linear calibration D”SD =f(conc.) equations are obtained for concentration range 2.5 to 25000 ng.(mL)-1 of spiked urine samples, examining analyte MS ions at m/z 171.0998, 172.0718, 172.04081, 213.1463, 181.0722 and 151.1114, respectively. There is achieved exact coefficient of linear correlation (|r|=1) between theory and experiment of ion at m/z 172.04081. The major challenge to quantify MTZ in urine sample is that it stabilizes cations [M+H]+ of two tautomers, which equilibrium varies drastically within the standard linear calibration dynamic range. The fragmentation patterns depend on analyte tautomers and it unambiguous assignment in multicomponent samples with complex sample matrix effect (SME) is unable to be made without mediation to an independent physico-chemical law. To solve the problem, herein, is used, again, above equation, which is designed a bridge between quantitative and multidimensional structural analytical chemistry, when is used complementary with Arrhenius’s quantum chemical diffusion parameter (DQC.) There is achieved |r|=0.98 of D”SD=f(DQC’) examining tautomeric molecular and fragment ions of MTZ. GRAPHICAL ABSTRACT
{"title":"Stochastic Dynamic Electrospray Ionization Mass Spectrometric Quantitative Analysis of Metronidazole in Human Urine","authors":"B. Ivanova, M. Spiteller","doi":"10.1080/22297928.2022.2086822","DOIUrl":"https://doi.org/10.1080/22297928.2022.2086822","url":null,"abstract":"Abstract The study reports quantification of metronidazole (MTZ) in clinical human urine employing our innovative stochastic dynamic equation D”SD =2.6388.10-17.(–). There are direct analysis without presence of internal standard, using ultra-high accuracy nano-electrospray ionization (ESI) mass spectrometry (MS), quantum chemistry and chemometrics, respectively. The linear calibration D”SD =f(conc.) equations are obtained for concentration range 2.5 to 25000 ng.(mL)-1 of spiked urine samples, examining analyte MS ions at m/z 171.0998, 172.0718, 172.04081, 213.1463, 181.0722 and 151.1114, respectively. There is achieved exact coefficient of linear correlation (|r|=1) between theory and experiment of ion at m/z 172.04081. The major challenge to quantify MTZ in urine sample is that it stabilizes cations [M+H]+ of two tautomers, which equilibrium varies drastically within the standard linear calibration dynamic range. The fragmentation patterns depend on analyte tautomers and it unambiguous assignment in multicomponent samples with complex sample matrix effect (SME) is unable to be made without mediation to an independent physico-chemical law. To solve the problem, herein, is used, again, above equation, which is designed a bridge between quantitative and multidimensional structural analytical chemistry, when is used complementary with Arrhenius’s quantum chemical diffusion parameter (DQC.) There is achieved |r|=0.98 of D”SD=f(DQC’) examining tautomeric molecular and fragment ions of MTZ. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"43 1","pages":"322 - 348"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83697831","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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2055490
P. Bansod, S. Dharaskar, Shyam M Kodape
Abstract The available natural energy sources are inadequate to satisfy the demands of an increasing population and control environmental pollution. It is critical to prioritise alternative energy sources like biodiesel. Biodiesel is an eco-sustainable and renewable energy source. But impurities present in biodiesel causes problems in internal combustion engine and emission of hazards gases after burning, it must be separated in accordance with international standards. Conventional techniques are insufficient for separating impurities from biodiesel. Membrane separation technology has been found to be a cost-effective and environmentally friendly technique for biodiesel separation. In this study, 10 KDa polyethersulfone ultrafiltration membranes were used to separate impurities from biodiesel such as free glycerol, diglyceroids, and triglycerides. The response surface was used to analyse the influence of operating variables such as temperature, transmembrane pressure and water addition on impurity separation as well as optimization. The impurities were separated according to international standards and at optimal conditions, 96.45 % free glycerol, 54.37 % diglyceroids and 61.66 % triglycerides were removed at 60°C, 0.3 wt% water addition, and 2.6 bars transmembrane pressure. GRAPHICAL ABSTRACT
{"title":"Application of Response Surface Methodology for Optimization and Separation of Free Glycerol, Diglyceroids and Triglycerides from Biodiesel Using PES Ultrafiltration Membrane","authors":"P. Bansod, S. Dharaskar, Shyam M Kodape","doi":"10.1080/22297928.2022.2055490","DOIUrl":"https://doi.org/10.1080/22297928.2022.2055490","url":null,"abstract":"Abstract The available natural energy sources are inadequate to satisfy the demands of an increasing population and control environmental pollution. It is critical to prioritise alternative energy sources like biodiesel. Biodiesel is an eco-sustainable and renewable energy source. But impurities present in biodiesel causes problems in internal combustion engine and emission of hazards gases after burning, it must be separated in accordance with international standards. Conventional techniques are insufficient for separating impurities from biodiesel. Membrane separation technology has been found to be a cost-effective and environmentally friendly technique for biodiesel separation. In this study, 10 KDa polyethersulfone ultrafiltration membranes were used to separate impurities from biodiesel such as free glycerol, diglyceroids, and triglycerides. The response surface was used to analyse the influence of operating variables such as temperature, transmembrane pressure and water addition on impurity separation as well as optimization. The impurities were separated according to international standards and at optimal conditions, 96.45 % free glycerol, 54.37 % diglyceroids and 61.66 % triglycerides were removed at 60°C, 0.3 wt% water addition, and 2.6 bars transmembrane pressure. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"29 1","pages":"380 - 390"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87522716","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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2073261
Rajiv A. Jadhav, V. Ahirrao, Rushikesh H. Patil, K. More, Anil R. Tile, V. Rane, Pravin S. Sonawane, R. Yeole
Abstract Chiral high performance liquid chromatography method for the separation of (R)-5-(1- Hydroxyethyl)-2-(pyridine-2-yl)-[1, 3, 4]-thiadiazole (R-alcohol) an intermediate of new antibiotic Nafithromycin (NFT) has been developed and validated. NFT is a ketolide class of antibiotic currently under Phase III clinical trials in India to treat community acquired bacterial pneumonia. Chiral separation of the enantiomers with resolution >2 was accomplished on Chiralpak IA column using a mixture of n-hexane and isopropanol (IPA) in the ratio of (90:10; v/v) as an elution solvent, run at a flow rate of 1.2 mL.min-1. The column was maintained at 25°C. The analytes were detected at 254 nm. The developed method was extensively validated as per the international council for harmonisation of technical requirements for pharmaceuticals for human use guideline. Sensitivity of the method was adequate to control the passage of unwanted enantiomer to next step with limit of quantification (LOQ) of the undesired enantiomer (S)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole (S-alcohol) of 0.37 µgmL-1. Mean recovery of the S-alcohol was 98.9±8.7%. During development influence of column oven temperature on the chiral separation was assessed. GRAPHICAL ABSTRACT
{"title":"Enantiomeric Separation of (R)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole, an Intermediate of Nafithromycin on Immobilized Amylose Based Stationary Phase","authors":"Rajiv A. Jadhav, V. Ahirrao, Rushikesh H. Patil, K. More, Anil R. Tile, V. Rane, Pravin S. Sonawane, R. Yeole","doi":"10.1080/22297928.2022.2073261","DOIUrl":"https://doi.org/10.1080/22297928.2022.2073261","url":null,"abstract":"Abstract Chiral high performance liquid chromatography method for the separation of (R)-5-(1- Hydroxyethyl)-2-(pyridine-2-yl)-[1, 3, 4]-thiadiazole (R-alcohol) an intermediate of new antibiotic Nafithromycin (NFT) has been developed and validated. NFT is a ketolide class of antibiotic currently under Phase III clinical trials in India to treat community acquired bacterial pneumonia. Chiral separation of the enantiomers with resolution >2 was accomplished on Chiralpak IA column using a mixture of n-hexane and isopropanol (IPA) in the ratio of (90:10; v/v) as an elution solvent, run at a flow rate of 1.2 mL.min-1. The column was maintained at 25°C. The analytes were detected at 254 nm. The developed method was extensively validated as per the international council for harmonisation of technical requirements for pharmaceuticals for human use guideline. Sensitivity of the method was adequate to control the passage of unwanted enantiomer to next step with limit of quantification (LOQ) of the undesired enantiomer (S)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole (S-alcohol) of 0.37 µgmL-1. Mean recovery of the S-alcohol was 98.9±8.7%. During development influence of column oven temperature on the chiral separation was assessed. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"95 1","pages":"409 - 418"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83922032","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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2063069
S. Sanap, Amol Chhatrapati Bisen, Abhijit Deb Choudhury, S. Verma, Mukesh Kumar, R. Bhatta
Abstract A simple reverse-phase UHPLC (RP-UHPLC) analytical method was developed and validated according to International Council on Harmonization (ICH) guidelines for simultaneous estimation of ofloxacin (OFX) and fluconazole (FCZ) using a Response surface aided central composite design (CCD, Design-Expert®, Version 11.1.2.0). The method was validated for linearity, selectivity, sensitivity, accuracy, precision, limits of detection and quantification, solution stability and robustness. OFX and FCZ separation were achieved using Agilent 1290 Infinity II UHPLC system encompassed with Waters Atlantis® T3 (150 × 4.6 mm2 i.d., 3 µm particle size) column, water containing 0.1% v/v formic acid and methanol as isocratic mobile phase. OFX and FCZ eluted at 4.1 and 10.5 min with no interference of the excipients used in formulation at λmax 260 nm. The developed method was envisaged to determine total drug content, in vitro drug release study and ex-vivo corneal permeation study of conventional as well as novel drug delivery formulations. The proposed method is simple, cost-effective, dependable and reproducible and could be used for the regular analysis of OFX and FCZ in bulk and quality controls in the research and pharmaceutical industries. GRAPHICAL ABSTRACT
{"title":"A Qbd Driven Approach for Development and Validation of an RP-UHPLC Method for Simultaneous Estimation of Ofloxacin and Fluconazole: An Application to Pharmaceutical Analysis","authors":"S. Sanap, Amol Chhatrapati Bisen, Abhijit Deb Choudhury, S. Verma, Mukesh Kumar, R. Bhatta","doi":"10.1080/22297928.2022.2063069","DOIUrl":"https://doi.org/10.1080/22297928.2022.2063069","url":null,"abstract":"Abstract A simple reverse-phase UHPLC (RP-UHPLC) analytical method was developed and validated according to International Council on Harmonization (ICH) guidelines for simultaneous estimation of ofloxacin (OFX) and fluconazole (FCZ) using a Response surface aided central composite design (CCD, Design-Expert®, Version 11.1.2.0). The method was validated for linearity, selectivity, sensitivity, accuracy, precision, limits of detection and quantification, solution stability and robustness. OFX and FCZ separation were achieved using Agilent 1290 Infinity II UHPLC system encompassed with Waters Atlantis® T3 (150 × 4.6 mm2 i.d., 3 µm particle size) column, water containing 0.1% v/v formic acid and methanol as isocratic mobile phase. OFX and FCZ eluted at 4.1 and 10.5 min with no interference of the excipients used in formulation at λmax 260 nm. The developed method was envisaged to determine total drug content, in vitro drug release study and ex-vivo corneal permeation study of conventional as well as novel drug delivery formulations. The proposed method is simple, cost-effective, dependable and reproducible and could be used for the regular analysis of OFX and FCZ in bulk and quality controls in the research and pharmaceutical industries. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"42 1","pages":"310 - 321"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86886954","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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2073262
Azmat Ali Khan, Fatima Khitab, J. Shah, M. R. Jan
Abstract Dyestuffs are very persistent in nature and are present in large number in wastewater of different industries. The wastewater of different industries contains many pollutants which are hazardous for human health and environment. In the present study, sonophotocatalytic degradation of Acid red 17 (AR-17) dye in aqueous solution was investigated using silver impregnated zinc oxide (Ag/ZnO). Silver impregnated zinc oxide (Ag/ZnO) catalyst was prepared by wet impregnation method and characterized by SEM, EDX, XRD and band gap. Removal of dye was carried out at 40 kHz frequency ultrasound waves under visible light (Tungsten lamp) of 100 W. The effect of various operating conditions and reagents like H2O2 concentration, pH of the solution, amount of catalyst and concentration of AR-17 dye were investigated. At the own pH of dye using 7 mmole H2O2 concentration 92.9 % degradation of acid red 17 was observed. The degradation increased with increase in irradiation and sonication time of 30 minutes and with 0.25 g /100 mL Ag/ZnO highest degradation 92.94 % was found. The TOC analysis was also carried out sonophotocatalytically and 80 % removal of total organic compounds was observed. The degradation of AR-17 followed pseudo-second-order kinetics with high value of correlation coefficient. GRAPHICAL ABSTRACT
摘要染料具有很强的持久性，大量存在于工业废水中。不同行业的废水中含有许多对人体健康和环境有害的污染物。采用银浸渍氧化锌(Ag/ZnO)对酸性红17 (AR-17)染料在水溶液中的声光催化降解进行了研究。采用湿浸渍法制备了银浸渍氧化锌(Ag/ZnO)催化剂，并用SEM、EDX、XRD和带隙对其进行了表征。在100 W可见光(钨丝灯)下，以40 kHz频率的超声波去除染料。考察了H2O2浓度、溶液pH、催化剂用量、AR-17染料浓度等操作条件和试剂的影响。在染料自身pH条件下，H2O2浓度为7摩尔，对酸性红17的降解率为92.9%。随着辐照时间和超声时间的增加，降解率逐渐提高，在0.25 g/ 100 mL Ag/ZnO条件下，降解率最高达92.94%。对TOC进行了声光催化分析，观察到总有机化合物去除率达80%。AR-17的降解遵循伪二级动力学，相关系数较高。图形抽象
{"title":"Highly Impressive Sonophotocatalytic Degradation of Acid Red 17 using visible light induced Ag Impregnated ZnO Photocatalyst","authors":"Azmat Ali Khan, Fatima Khitab, J. Shah, M. R. Jan","doi":"10.1080/22297928.2022.2073262","DOIUrl":"https://doi.org/10.1080/22297928.2022.2073262","url":null,"abstract":"Abstract Dyestuffs are very persistent in nature and are present in large number in wastewater of different industries. The wastewater of different industries contains many pollutants which are hazardous for human health and environment. In the present study, sonophotocatalytic degradation of Acid red 17 (AR-17) dye in aqueous solution was investigated using silver impregnated zinc oxide (Ag/ZnO). Silver impregnated zinc oxide (Ag/ZnO) catalyst was prepared by wet impregnation method and characterized by SEM, EDX, XRD and band gap. Removal of dye was carried out at 40 kHz frequency ultrasound waves under visible light (Tungsten lamp) of 100 W. The effect of various operating conditions and reagents like H2O2 concentration, pH of the solution, amount of catalyst and concentration of AR-17 dye were investigated. At the own pH of dye using 7 mmole H2O2 concentration 92.9 % degradation of acid red 17 was observed. The degradation increased with increase in irradiation and sonication time of 30 minutes and with 0.25 g /100 mL Ag/ZnO highest degradation 92.94 % was found. The TOC analysis was also carried out sonophotocatalytically and 80 % removal of total organic compounds was observed. The degradation of AR-17 followed pseudo-second-order kinetics with high value of correlation coefficient. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"47 1","pages":"358 - 370"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76524889","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}
Pub Date : 2022-04-27DOI: 10.1080/22297928.2022.2036233
Kiranba F. Jadeja, H. Joshi
Abstract In this current research framework, an efficient greener synthesis has been developed for new pyridine derivatives using one-pot four-component reaction. We have synthesized a new series of 1,4-dihydropyridine derivatives in excellent yield via telescopic multicomponent reaction among the aldehyde, malononitrile, anilines and diethyl acetylenedicarboxylate in the presence of piperidine at mild reaction condition without further purification. All the synthesized compounds were characterized by 1H NMR, 13C NMR, FT-IR and mass spectrometry analysis. GRAPHICAL ABSTRACT
{"title":"Rapid, Greener and One-pot Four Component Synthesis of 1, 4-Dihydropyridine Derivatives","authors":"Kiranba F. Jadeja, H. Joshi","doi":"10.1080/22297928.2022.2036233","DOIUrl":"https://doi.org/10.1080/22297928.2022.2036233","url":null,"abstract":"Abstract In this current research framework, an efficient greener synthesis has been developed for new pyridine derivatives using one-pot four-component reaction. We have synthesized a new series of 1,4-dihydropyridine derivatives in excellent yield via telescopic multicomponent reaction among the aldehyde, malononitrile, anilines and diethyl acetylenedicarboxylate in the presence of piperidine at mild reaction condition without further purification. All the synthesized compounds were characterized by 1H NMR, 13C NMR, FT-IR and mass spectrometry analysis. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"492 1","pages":"371 - 379"},"PeriodicalIF":0.0,"publicationDate":"2022-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77797927","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}
Pub Date : 2022-03-04DOI: 10.1080/22297928.2022.2049869
A. Dalvi, P. S. Remya Devi, K. K. Swain
Abstract An in-house radiochemical procedure for the separation of 231Pa from siliceous cake - a waste stream of monazite processing plant, followed by its determination using gamma ray spectrometry, has been developed in our laboratory. Evaluation of reliability of analytical results of the radiochemical procedure is important for validating the fitness of purpose of an analytical method. The present paper describes the statistical evaluation of the analytical results obtained, by estimating the overall uncertainty in the measurement process. The bottom-up approach, also called as ISO approach (ISO/IEC guide 98-3:2008), was adopted to evaluate the overall uncertainty in which the individual sources were identified, evaluated and propagated. The major contribution to the combined uncertainty in measurement of 231Pa was from efficiency calibration. Besides this, counting statistics in the sample and chemical yield of the process incorporated significant contribution to combined uncertainty. The precision of the results obtained was found to be acceptable, as ascertained by the Horwitz Ratio, for the performance of a single laboratory. GRAPHICAL ABSTRACT
{"title":"Method Validation and Measurement Uncertainty Evaluation of the Radiochemical Procedure for the Determination of 231Pa in Siliceous Cake by Gamma Spectrometry","authors":"A. Dalvi, P. S. Remya Devi, K. K. Swain","doi":"10.1080/22297928.2022.2049869","DOIUrl":"https://doi.org/10.1080/22297928.2022.2049869","url":null,"abstract":"Abstract An in-house radiochemical procedure for the separation of 231Pa from siliceous cake - a waste stream of monazite processing plant, followed by its determination using gamma ray spectrometry, has been developed in our laboratory. Evaluation of reliability of analytical results of the radiochemical procedure is important for validating the fitness of purpose of an analytical method. The present paper describes the statistical evaluation of the analytical results obtained, by estimating the overall uncertainty in the measurement process. The bottom-up approach, also called as ISO approach (ISO/IEC guide 98-3:2008), was adopted to evaluate the overall uncertainty in which the individual sources were identified, evaluated and propagated. The major contribution to the combined uncertainty in measurement of 231Pa was from efficiency calibration. Besides this, counting statistics in the sample and chemical yield of the process incorporated significant contribution to combined uncertainty. The precision of the results obtained was found to be acceptable, as ascertained by the Horwitz Ratio, for the performance of a single laboratory. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"45 1","pages":"174 - 184"},"PeriodicalIF":0.0,"publicationDate":"2022-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76470982","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}
Pub Date : 2022-03-04DOI: 10.1080/22297928.2021.1983873
Priti K. Parmar, Navneet P. Mori, V. Khedkar, Gaurav Sanghavi, R. Khunt
Abstract Thiazole is a well-established scaffold due to its wide range of therapeutic activities. Moreover, the chromane nucleus is also associated with various biological activities such as antibacterial, anticancer, anti-inflammatory, and anti-HIV. We have reported herein thiazole derivatives clubbed with chromane nucleus intending to enhance the action as hybrid molecules. All the synthesized molecules have been confirmed based on spectroscopic techniques such as PMR, CMR, FT-IR & further supported by mass spectrometry. To check the potency of newly synthesized molecules, they have been evaluated against different strains of bacteria. Furthermore, to gain an insight into their plausible mechanism of action and thermodynamic interaction governing the binding of these molecules to their biological target, a molecular docking study was performed against bacterial DNA gyrase. The results of in silico binding affinity were found to be in harmony with the experimental activity. A complete design, synthesis, biological screening, and molecular docking experiment was planned and executed to lead with compounds exhibiting potential antibacterial activity. GRAPHICAL ABSTRACT
{"title":"Synthesis, Characterization & Molecular Docking Study of Hydrazinylthiazole Derivatives as Antibacterial Agents","authors":"Priti K. Parmar, Navneet P. Mori, V. Khedkar, Gaurav Sanghavi, R. Khunt","doi":"10.1080/22297928.2021.1983873","DOIUrl":"https://doi.org/10.1080/22297928.2021.1983873","url":null,"abstract":"Abstract Thiazole is a well-established scaffold due to its wide range of therapeutic activities. Moreover, the chromane nucleus is also associated with various biological activities such as antibacterial, anticancer, anti-inflammatory, and anti-HIV. We have reported herein thiazole derivatives clubbed with chromane nucleus intending to enhance the action as hybrid molecules. All the synthesized molecules have been confirmed based on spectroscopic techniques such as PMR, CMR, FT-IR & further supported by mass spectrometry. To check the potency of newly synthesized molecules, they have been evaluated against different strains of bacteria. Furthermore, to gain an insight into their plausible mechanism of action and thermodynamic interaction governing the binding of these molecules to their biological target, a molecular docking study was performed against bacterial DNA gyrase. The results of in silico binding affinity were found to be in harmony with the experimental activity. A complete design, synthesis, biological screening, and molecular docking experiment was planned and executed to lead with compounds exhibiting potential antibacterial activity. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"3 1","pages":"244 - 254"},"PeriodicalIF":0.0,"publicationDate":"2022-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78508478","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}
Pub Date : 2022-03-04DOI: 10.1080/22297928.2022.2034528
R. Seetharaman, K. Lakshmi
Abstract The present study represents four simple UV spectrophotometric methods that are accurate, precise, and ecofriendly for estimating flupirtine maleate and thiocolchicoside in pharmaceutical formulation. The four methods are the second order derivative of zero order spectra, the first derivative of ratio spectra, the extended ratio subtraction technique, and the absorption factor method. The proposed methods have linear calibration curves in the range of 14-26 to 2.80-5.2 µg mL-1 for flupirtine maleate and thiocolchicoside, correspondingly. The proposed methods are evaluated toward synthetic mixtures of the drugs as mentioned earlier and then extended to commercial pharmaceutical formulations of the analytes of interest. The findings of the assay for determining the cited drugs in pharmaceutical tablets were statistically analysed with those of the published HPLC method, implying that no discernible difference exists between the suggested and published procedures. The analytical Eco scale, Agree metrics, and Green analytical procedure index was used to assess the method's greenness scores. The methods have been validated according to ICH criteria and confirmed to be within acceptable limits. GRAPHICAL ABSTRACT
{"title":"Ecofriendly Spectrophotometric Methods for the Simultaneous Determination of Flupirtine Maleate and Thiocolchicoside: Evaluation of Greenness Profile","authors":"R. Seetharaman, K. Lakshmi","doi":"10.1080/22297928.2022.2034528","DOIUrl":"https://doi.org/10.1080/22297928.2022.2034528","url":null,"abstract":"Abstract The present study represents four simple UV spectrophotometric methods that are accurate, precise, and ecofriendly for estimating flupirtine maleate and thiocolchicoside in pharmaceutical formulation. The four methods are the second order derivative of zero order spectra, the first derivative of ratio spectra, the extended ratio subtraction technique, and the absorption factor method. The proposed methods have linear calibration curves in the range of 14-26 to 2.80-5.2 µg mL-1 for flupirtine maleate and thiocolchicoside, correspondingly. The proposed methods are evaluated toward synthetic mixtures of the drugs as mentioned earlier and then extended to commercial pharmaceutical formulations of the analytes of interest. The findings of the assay for determining the cited drugs in pharmaceutical tablets were statistically analysed with those of the published HPLC method, implying that no discernible difference exists between the suggested and published procedures. The analytical Eco scale, Agree metrics, and Green analytical procedure index was used to assess the method's greenness scores. The methods have been validated according to ICH criteria and confirmed to be within acceptable limits. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"67 1","pages":"283 - 291"},"PeriodicalIF":0.0,"publicationDate":"2022-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85786875","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}
Pub Date : 2022-03-04DOI: 10.1080/22297928.2022.2049868
S. Sonawane, Abhijit S. Deore, Kirti Jadhav, Prachi A. Khapare, Umesh D. Laddha, M. Patil, S. Chhajed
Abstract Drug degradation may change the pharmacological action and results in altered therapeutic and toxicological profile of drug. Identification of degradation product is good opportunity in the drug discovery, as non-toxic impurities can be considered for the new pharmacological potentials. Additionally, development of computer based in-silico model and methods further assist in prediction of pharmacokinetic, dynamic as well as biological activities which make drug discovery process more unfailing. In present work, Febuxotat (FEB) was subjected to forced degradation experiments and the formed degradation products were separated and resolved using optimized HPLC method. Further the study was extended to enrich its alkali degradation product and was ascertained using 1H NMR spectroscopy and mass spectrometry. The ADME/Toxicological properties of alkali degradation product were determined by using Admet SAR 2.0. The method was validated as per ICH guidelines Q2 (R1). In forced degradation experiments, substantial degradation of FEB was observed under acid, alkali, wet heat, dry heat and oxidative conditions, however, FEB was found stable to photolytic conditions. The drug and its formed degradation products separated and resolved from each other on Waters SunFire C8 (250 × 4.6 mm, 5 µm) column using blend of methanol: 20 mM potassium phosphate buffer (pH 3.0) (80: 20 % v/v). From the 1H NMR spectroscopy and mass spectrometry the enriched alkali degradation product was confirmed as 2-[3-carboxy-4-(2-methylpropoxy) phenyl]-4-methyl-1,3-thiazole-5-carboxylic acid (diacid FEB). Febuxostat and diacid Febuxostat was found non-toxic for carcinogenicity (binary), eye corrosion, eye irritation and Ames mutagenesis during ADME/Tox studies. However, both were found hepatotoxic. A simple, accurate, precise, and robust stability indicating HPLC method was developed and validated for the estimation of FEB in bulk and tablet dosage form. Based on ADME/Tox both were found to hepatotoxic. Henceforth, based on our evidences, one should use FEB with precaution in patient suffering from liver disease. GRAPHICAL ABSTRACT
摘要药物降解可以改变药物的药理作用，从而改变药物的治疗和毒理学特征。降解产物的鉴定是药物发现的好机会，因为无毒杂质可以被认为是新的药理潜力。此外，基于计算机的计算机模型和方法的发展进一步有助于预测药物的药代动力学、动力学和生物活性，使药物发现过程更加顺利。本研究对非布索他(FEB)进行强制降解实验，并采用优化的高效液相色谱法对所形成的降解产物进行分离和分解。进一步对其碱降解产物进行了富集研究，并用1H NMR谱和质谱对其进行了确证。采用Admet SAR 2.0对碱降解产物的ADME/毒理学特性进行了测定。该方法按照ICH指南Q2 (R1)进行验证。在强制降解实验中，FEB在酸、碱、湿热、干热和氧化条件下都有明显的降解，但在光解条件下FEB是稳定的。药物及其形成的降解产物在Waters SunFire C8 (250 × 4.6 mm, 5µm)柱上使用甲醇:20 mm磷酸钾缓冲液(pH 3.0) (80: 20% v/v)进行分离和分离。经1H NMR和质谱分析证实，富集的碱降解产物为2-[3-羧基-4-(2-甲基丙氧基)苯基]-4-甲基-1,3-噻唑-5-羧酸(二酸FEB)。在ADME/Tox研究中发现，非布司他在致癌性(二元)、眼睛腐蚀、眼睛刺激和Ames诱变方面无毒。然而，两者都被发现有肝毒性。建立了简便、准确、精密度高、稳定性好的高效液相色谱法测定原料药和片剂中FEB的含量。根据ADME/Tox，两者都被发现有肝毒性。因此，根据我们的证据，患有肝脏疾病的患者应谨慎使用FEB。图形抽象
{"title":"Bridging Pharmaceutical Analysis with Computational Chemistry to Ascertain the Pharmacokinetic and Toxicological Profiling of Febuxostat and its Diacid Impurity","authors":"S. Sonawane, Abhijit S. Deore, Kirti Jadhav, Prachi A. Khapare, Umesh D. Laddha, M. Patil, S. Chhajed","doi":"10.1080/22297928.2022.2049868","DOIUrl":"https://doi.org/10.1080/22297928.2022.2049868","url":null,"abstract":"Abstract Drug degradation may change the pharmacological action and results in altered therapeutic and toxicological profile of drug. Identification of degradation product is good opportunity in the drug discovery, as non-toxic impurities can be considered for the new pharmacological potentials. Additionally, development of computer based in-silico model and methods further assist in prediction of pharmacokinetic, dynamic as well as biological activities which make drug discovery process more unfailing. In present work, Febuxotat (FEB) was subjected to forced degradation experiments and the formed degradation products were separated and resolved using optimized HPLC method. Further the study was extended to enrich its alkali degradation product and was ascertained using 1H NMR spectroscopy and mass spectrometry. The ADME/Toxicological properties of alkali degradation product were determined by using Admet SAR 2.0. The method was validated as per ICH guidelines Q2 (R1). In forced degradation experiments, substantial degradation of FEB was observed under acid, alkali, wet heat, dry heat and oxidative conditions, however, FEB was found stable to photolytic conditions. The drug and its formed degradation products separated and resolved from each other on Waters SunFire C8 (250 × 4.6 mm, 5 µm) column using blend of methanol: 20 mM potassium phosphate buffer (pH 3.0) (80: 20 % v/v). From the 1H NMR spectroscopy and mass spectrometry the enriched alkali degradation product was confirmed as 2-[3-carboxy-4-(2-methylpropoxy) phenyl]-4-methyl-1,3-thiazole-5-carboxylic acid (diacid FEB). Febuxostat and diacid Febuxostat was found non-toxic for carcinogenicity (binary), eye corrosion, eye irritation and Ames mutagenesis during ADME/Tox studies. However, both were found hepatotoxic. A simple, accurate, precise, and robust stability indicating HPLC method was developed and validated for the estimation of FEB in bulk and tablet dosage form. Based on ADME/Tox both were found to hepatotoxic. Henceforth, based on our evidences, one should use FEB with precaution in patient suffering from liver disease. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"50 1","pages":"221 - 232"},"PeriodicalIF":0.0,"publicationDate":"2022-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88908260","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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