Pub Date : 2023-07-04DOI: 10.1080/22297928.2023.2256339
S. Vhatkar, Kumar Abhisek, Helen Treasa Mathew, Ramesh Oraon
Abstract Hydrotropes are a class of compounds that improve aqueous solubility of certain organic compounds. The aqueous solubility arising from interfacial incompatibility has been a critical industrial concern, limiting various applications. Among many such hydrotropes, the purpose of this work is to study the effect of n-octyl tetra ammonium bromide (TOAB) over the organic-inorganic incompatibility of an indole water system experimentally through conductometry and stalagmometry, for the first time. The study focussed on conductometry to determine minimum hydrotrope concentration (MHC) through specific conductivity at different temperatures. The MHC is essential in ensuring the spontaneous self-assembly of organic molecules (such as indole) in water systems. In addition to this, MHC was also determined using stalagmometry at room temperature to analyse the hydrotropic effect of TOAB. Consequently, the Hydrotropy-assisted cooperative solubilization of indole in water was investigated by specific conductivity (7.64 µs/cm), surface tension (40.29 mN/m) and Gibb’s free energy at the minimum hydrotrope concentration (MHC∼ 0.95 mM) at room temperature. In conclusion, the experimental observation over the MHC is in good agreement with thermodynamic studies, suggesting the promising nature of TOAB in improving the aqueous solubility of Indole in water. GRAPHICAL ABSTRACT
{"title":"A promising hydrotropic effect of Tetra n-octyl ammonium bromide (TOAB) for thermodynamic investigation of surface tension, conductivity of indole in water","authors":"S. Vhatkar, Kumar Abhisek, Helen Treasa Mathew, Ramesh Oraon","doi":"10.1080/22297928.2023.2256339","DOIUrl":"https://doi.org/10.1080/22297928.2023.2256339","url":null,"abstract":"Abstract Hydrotropes are a class of compounds that improve aqueous solubility of certain organic compounds. The aqueous solubility arising from interfacial incompatibility has been a critical industrial concern, limiting various applications. Among many such hydrotropes, the purpose of this work is to study the effect of n-octyl tetra ammonium bromide (TOAB) over the organic-inorganic incompatibility of an indole water system experimentally through conductometry and stalagmometry, for the first time. The study focussed on conductometry to determine minimum hydrotrope concentration (MHC) through specific conductivity at different temperatures. The MHC is essential in ensuring the spontaneous self-assembly of organic molecules (such as indole) in water systems. In addition to this, MHC was also determined using stalagmometry at room temperature to analyse the hydrotropic effect of TOAB. Consequently, the Hydrotropy-assisted cooperative solubilization of indole in water was investigated by specific conductivity (7.64 µs/cm), surface tension (40.29 mN/m) and Gibb’s free energy at the minimum hydrotrope concentration (MHC∼ 0.95 mM) at room temperature. In conclusion, the experimental observation over the MHC is in good agreement with thermodynamic studies, suggesting the promising nature of TOAB in improving the aqueous solubility of Indole in water. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"8 1","pages":"451 - 460"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139362890","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 : 2023-07-04DOI: 10.1080/22297928.2023.2256337
Alêssa Gomes Siqueira, Bruno Elias dos Santos Costa, Lincoln Lucílio Romualdo, Vanessa Nunes Alves
Abstract A new solid phase extraction procedure, known as in situ surfactant-based solid phase extraction, has been proposed to detect the presence of CrIII in infusions of medicinal plants. In this work, a small amount of cetyltrimethylammonium bromide was injected into a sample containing CrIII, which was complexed by 1-(2-pyridylazo)-2-naphthol. After shaking, a small volume of NaClO Was added to the solution as an ion-pairing agent. After preconcentration, the settled phase was dissolved in a specific volume of HCl and then analyzed by Flame Atomic Absorption Spectrometry. A Doehlert matrix was used to optimize the CrIII complex formation conditions, such as the chelating agent concentration (0.18 mmol L-1) and pH of 9.5 in the reaction medium. A 23 factorial design was used to screen the variables that influence the extraction of the complex. The concentration of ionic-pairing agent (0.26 mol L-1) and the vortex mixer agitation time (7.51 minutes) were significant and optimized using response surface methodology. The limit of detection, limit of quantification, and preconcentration factor were 1.66 μg L-1, 5.5 μg L-1 and 12, respectively. The linear range was 5.5-5000 μg L-1. The method proved accuracy by the comparison with certified reference material APS-1071 (p>0.05), and the optimized conditions were successfully applied for the determination of CrIII in samples of medicinal plant infusions. GRAPHICAL ABSTRACT
{"title":"Use of in-situ surfactant-based solid phase extraction for determination of low concentrations of CrIII in infusions of medicinal plants","authors":"Alêssa Gomes Siqueira, Bruno Elias dos Santos Costa, Lincoln Lucílio Romualdo, Vanessa Nunes Alves","doi":"10.1080/22297928.2023.2256337","DOIUrl":"https://doi.org/10.1080/22297928.2023.2256337","url":null,"abstract":"Abstract A new solid phase extraction procedure, known as in situ surfactant-based solid phase extraction, has been proposed to detect the presence of CrIII in infusions of medicinal plants. In this work, a small amount of cetyltrimethylammonium bromide was injected into a sample containing CrIII, which was complexed by 1-(2-pyridylazo)-2-naphthol. After shaking, a small volume of NaClO Was added to the solution as an ion-pairing agent. After preconcentration, the settled phase was dissolved in a specific volume of HCl and then analyzed by Flame Atomic Absorption Spectrometry. A Doehlert matrix was used to optimize the CrIII complex formation conditions, such as the chelating agent concentration (0.18 mmol L-1) and pH of 9.5 in the reaction medium. A 23 factorial design was used to screen the variables that influence the extraction of the complex. The concentration of ionic-pairing agent (0.26 mol L-1) and the vortex mixer agitation time (7.51 minutes) were significant and optimized using response surface methodology. The limit of detection, limit of quantification, and preconcentration factor were 1.66 μg L-1, 5.5 μg L-1 and 12, respectively. The linear range was 5.5-5000 μg L-1. The method proved accuracy by the comparison with certified reference material APS-1071 (p>0.05), and the optimized conditions were successfully applied for the determination of CrIII in samples of medicinal plant infusions. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"23 1","pages":"355 - 368"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139363351","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 : 2023-07-04DOI: 10.1080/22297928.2023.2258132
P.N. Baraskar, R.A. Samant, V. L. Gurav
Abstract In this work, Cellulose was extracted from rice husk and chemically modified to produce Nano-Cellulose. It was characterized by FTIR, XRD, SEM/EDS, TEM, BET surface area analyzer, Particle size analyzer and tested for the removal of metal ions i.e. Zn(II), Cd(II), As(III), Pb(II) and Sn(II) from aqueous solution. The removal method was validated by differential pulse voltammetry (DPV). An adsorption experiment was performed to investigate the effects of initial pH, adsorbent dose, contact time and initial concentration of heavy metal ions on the adsorption capacity of nanocellulose. The experimental results revealed that the removal of metal ions on the nanocellulose was a pH-dependent process with the maximum adsorption capacity at the initial solution pH of 5–6. An adsorbent dose of 8mg/mL was sufficient for effective adsorption. In addition, the kinetics and equilibrium data are well described by pseudo-second-order kinetics and the Freundlich adsorption isotherm model at 50 min contact time and 50 mg/L initial concentration. Moreover, the desorption and re-adsorption performance was also studied, and the results revealed that the Nano-cellulose still showed good adsorption performance up to eight cycles of regeneration. GRAPHICAL ABSTRACT
{"title":"Removal of heavy metal ions using nano-cellulose prepared from rice husk: validation by differential pulse voltammetry","authors":"P.N. Baraskar, R.A. Samant, V. L. Gurav","doi":"10.1080/22297928.2023.2258132","DOIUrl":"https://doi.org/10.1080/22297928.2023.2258132","url":null,"abstract":"Abstract In this work, Cellulose was extracted from rice husk and chemically modified to produce Nano-Cellulose. It was characterized by FTIR, XRD, SEM/EDS, TEM, BET surface area analyzer, Particle size analyzer and tested for the removal of metal ions i.e. Zn(II), Cd(II), As(III), Pb(II) and Sn(II) from aqueous solution. The removal method was validated by differential pulse voltammetry (DPV). An adsorption experiment was performed to investigate the effects of initial pH, adsorbent dose, contact time and initial concentration of heavy metal ions on the adsorption capacity of nanocellulose. The experimental results revealed that the removal of metal ions on the nanocellulose was a pH-dependent process with the maximum adsorption capacity at the initial solution pH of 5–6. An adsorbent dose of 8mg/mL was sufficient for effective adsorption. In addition, the kinetics and equilibrium data are well described by pseudo-second-order kinetics and the Freundlich adsorption isotherm model at 50 min contact time and 50 mg/L initial concentration. Moreover, the desorption and re-adsorption performance was also studied, and the results revealed that the Nano-cellulose still showed good adsorption performance up to eight cycles of regeneration. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"380 1","pages":"432 - 450"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139363035","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 : 2023-07-04DOI: 10.1080/22297928.2023.2266726
V. P. Gaonkar, Vinodh Kumar Mannur, Kirankumar Hullatti
Abstract Gymnemic acids are the group of phytocompounds from Gymnema sylvestre known to possess hypoglycemic activity. Quantitative estimation of Gymnemic acid in terms of Gymnemagenin is essential for the standardization of G. sylvestre. In the present work, methodology combining reversed-phase HPLC with an Analytical Quality by-design approach was utilized for quantitative analysis of Gymnemagenin in G. sylvestre leaves. The quality assessment was performed by evaluating various pharmacognostic parameters as per WHO guidelines. Initially, the Analytical Target Profile and Critical Quality Attributes were identified. The method was optimized using 22 full factorial designs with a concentration of orthophosphoric acid in the aqueous phase (X1) and mobile phase ratio (X2) selected as an independent variable and, tailing factor (R1) and theoretical plates (R2) chosen as dependent variables. The optimized chromatographic conditions were identified with mobile phase, Methanol and Water (0.1% OPA) in the ratio of 85:15 v/v with flow rate of 0.8 mL/min and detection wavelength of 210 nm. Further, the amount of Gymnemagenin in crude G. sylvestre leaves and its extract was found to be 5.108% and 6.23% w/w respectively. The quality evaluation parameters were found to be within the given standard limit. Finally, it can be concluded that the combination of the HPLC method with the AQbD approach resulted in a more precise and accurate method for quantification of total Gymnemic acids in terms of Gymnemagenin. The developed method involves advantages such as efficient separation, well-defined peaks, and reduced analytical time and can be successfully applied for the analysis of Gymnemagenin in different Gymnema species and their herbal products. GRAPHICAL ABSTRACT
{"title":"Quality assessment and analytical quality by design-driven RP-HPLC method development for estimation of Gymnemagenin in Gymnema sylvestre","authors":"V. P. Gaonkar, Vinodh Kumar Mannur, Kirankumar Hullatti","doi":"10.1080/22297928.2023.2266726","DOIUrl":"https://doi.org/10.1080/22297928.2023.2266726","url":null,"abstract":"Abstract Gymnemic acids are the group of phytocompounds from Gymnema sylvestre known to possess hypoglycemic activity. Quantitative estimation of Gymnemic acid in terms of Gymnemagenin is essential for the standardization of G. sylvestre. In the present work, methodology combining reversed-phase HPLC with an Analytical Quality by-design approach was utilized for quantitative analysis of Gymnemagenin in G. sylvestre leaves. The quality assessment was performed by evaluating various pharmacognostic parameters as per WHO guidelines. Initially, the Analytical Target Profile and Critical Quality Attributes were identified. The method was optimized using 22 full factorial designs with a concentration of orthophosphoric acid in the aqueous phase (X1) and mobile phase ratio (X2) selected as an independent variable and, tailing factor (R1) and theoretical plates (R2) chosen as dependent variables. The optimized chromatographic conditions were identified with mobile phase, Methanol and Water (0.1% OPA) in the ratio of 85:15 v/v with flow rate of 0.8 mL/min and detection wavelength of 210 nm. Further, the amount of Gymnemagenin in crude G. sylvestre leaves and its extract was found to be 5.108% and 6.23% w/w respectively. The quality evaluation parameters were found to be within the given standard limit. Finally, it can be concluded that the combination of the HPLC method with the AQbD approach resulted in a more precise and accurate method for quantification of total Gymnemic acids in terms of Gymnemagenin. The developed method involves advantages such as efficient separation, well-defined peaks, and reduced analytical time and can be successfully applied for the analysis of Gymnemagenin in different Gymnema species and their herbal products. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"132 1","pages":"475 - 486"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139363116","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 : 2023-07-04DOI: 10.1080/22297928.2023.2263449
Muhammad Hidhir Khawory, Azimah Amanah, N. Salin, Mohd Ferdaues Mohd Subki, Nurul Nadieya Mohd Nasim, M. I. Noordin, H. Wahab
Abstract The aim of this study is to assess how gamma irradiation affects the chemical profiles of medicinal plants. Two different forms; methanol leaf extracts and dried leaves, of the three medicinal plants were investigated. Utilising FTIR, HPLC, and LCMS techniques, the qualitative measurement of gallic acid (GA) in three different medicinal plants for both plant extract and dried plant before and after the gamma radiation treatment was carried out. In the meantime, HPLC has been used to do a quantitative analysis of GA in these plants in order to show the percentage concentration of phenolic acid. For these medicinal herbs, the FTIR study revealed that both plant extract and dried plant had comparable functional groups both before and after gamma radiation therapy. The chromatogram of the HPLC profile for these medicinal plants was similar in chemical constituents before and after gamma irradiation, but the samples that were treated with gamma irradiation had a slight increase in intensity (between 0.0002-0.0009 Au). Additionally, gamma irradiation at levels of 6-12 kGy and 9-13 kGy caused the mass peak of GA to deteriorate in mass spectrometry analysis. Furthermore, the percentage concentration of GA increased significantly as the gamma radiation dose increased for both forms. GRAPHICAL ABSTRACT
摘要 本研究旨在评估伽马辐照如何影响药用植物的化学成分。研究了三种药用植物的两种不同形式：甲醇叶提取物和干叶。利用傅立叶变换红外光谱（FTIR）、高效液相色谱（HPLC）和液相色谱分析（LCMS）技术，对伽马辐射处理前后三种不同药用植物的提取物和干燥植物中的没食子酸（GA）进行了定性测量。同时，使用 HPLC 对这些植物中的没食子酸进行定量分析，以显示酚酸的百分比浓度。对于这些药材，傅立叶变换红外光谱研究显示，在伽马射线治疗前后，植物提取物和干燥植物都具有相似的功能基团。这些药用植物在伽马射线照射前后的高效液相色谱图中的化学成分相似，但经过伽马射线照射处理的样品的化学成分强度略有增加（0.0002-0.0009 Au 之间）。此外，6-12 kGy 和 9-13 kGy 的伽马辐照会导致质谱分析中 GA 的质量峰恶化。此外，随着伽马辐照剂量的增加，两种形式的 GA 的百分比浓度都显著增加。图表摘要
{"title":"Evaluation of gamma irradiation on medicinal plants for both qualitative and quantitative analysis of phenolic acid","authors":"Muhammad Hidhir Khawory, Azimah Amanah, N. Salin, Mohd Ferdaues Mohd Subki, Nurul Nadieya Mohd Nasim, M. I. Noordin, H. Wahab","doi":"10.1080/22297928.2023.2263449","DOIUrl":"https://doi.org/10.1080/22297928.2023.2263449","url":null,"abstract":"Abstract The aim of this study is to assess how gamma irradiation affects the chemical profiles of medicinal plants. Two different forms; methanol leaf extracts and dried leaves, of the three medicinal plants were investigated. Utilising FTIR, HPLC, and LCMS techniques, the qualitative measurement of gallic acid (GA) in three different medicinal plants for both plant extract and dried plant before and after the gamma radiation treatment was carried out. In the meantime, HPLC has been used to do a quantitative analysis of GA in these plants in order to show the percentage concentration of phenolic acid. For these medicinal herbs, the FTIR study revealed that both plant extract and dried plant had comparable functional groups both before and after gamma radiation therapy. The chromatogram of the HPLC profile for these medicinal plants was similar in chemical constituents before and after gamma irradiation, but the samples that were treated with gamma irradiation had a slight increase in intensity (between 0.0002-0.0009 Au). Additionally, gamma irradiation at levels of 6-12 kGy and 9-13 kGy caused the mass peak of GA to deteriorate in mass spectrometry analysis. Furthermore, the percentage concentration of GA increased significantly as the gamma radiation dose increased for both forms. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"1 1","pages":"369 - 393"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139363250","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 : 2023-07-04DOI: 10.1080/22297928.2023.2256333
Akshita Jain, Sarita Beniwal, Naveen Sharma, N. Fahmi
Abstract This paper includes the synthesis of a Schiff base ligand and its palladium(II) complexes by conventional and green microwave-assisted techniques. They were characterized by conductivity measurements, mass spectrometry, FTIR, electronic spectroscopy, 1H NMR, and X-ray powder diffraction techniques. Based on analytical and spectral data, a square planar geometry was proposed for the metal complexes. The ligand(LH) and its metal complex[Pd(L) ] were screened for antimicrobial activity against pathogenic bacterial(Escherichia coli, Staphylococcus aureus) and fungal(Aspergillus niger, Penicillium chrysogenum) strains. Ciprofloxacin and Ketoconazole were used as standard drugs for antibacterial and antifungal activities respectively. The compounds showed moderate activity. The starting material(PdCl ), ligand(LH), and the metal complex [Pd(L) ] were screened for in vitro cytotoxic activity by MTT assay against cancerous cell lines (HeLa, MCF-7). Cisplatin was used as the standard drug. The metal complex, [Pd(L) ] was also screened for cytotoxic activity against normal cell line(HEK 293) to determine the selectivity index. The values of S.I(3.70-4.58) indicated that the complex [Pd(L) ] was more sensitive towards cancerous cell lines than normal cell line and may be studied further to assess its potential as cytotoxic agent. GRAPHICAL ABSTRACT
{"title":"Green synthesis, structural elucidation, antimicrobial, and cytotoxic activities of a Schiff base and its Pd(II) complexes","authors":"Akshita Jain, Sarita Beniwal, Naveen Sharma, N. Fahmi","doi":"10.1080/22297928.2023.2256333","DOIUrl":"https://doi.org/10.1080/22297928.2023.2256333","url":null,"abstract":"Abstract This paper includes the synthesis of a Schiff base ligand and its palladium(II) complexes by conventional and green microwave-assisted techniques. They were characterized by conductivity measurements, mass spectrometry, FTIR, electronic spectroscopy, 1H NMR, and X-ray powder diffraction techniques. Based on analytical and spectral data, a square planar geometry was proposed for the metal complexes. The ligand(LH) and its metal complex[Pd(L) ] were screened for antimicrobial activity against pathogenic bacterial(Escherichia coli, Staphylococcus aureus) and fungal(Aspergillus niger, Penicillium chrysogenum) strains. Ciprofloxacin and Ketoconazole were used as standard drugs for antibacterial and antifungal activities respectively. The compounds showed moderate activity. The starting material(PdCl ), ligand(LH), and the metal complex [Pd(L) ] were screened for in vitro cytotoxic activity by MTT assay against cancerous cell lines (HeLa, MCF-7). Cisplatin was used as the standard drug. The metal complex, [Pd(L) ] was also screened for cytotoxic activity against normal cell line(HEK 293) to determine the selectivity index. The values of S.I(3.70-4.58) indicated that the complex [Pd(L) ] was more sensitive towards cancerous cell lines than normal cell line and may be studied further to assess its potential as cytotoxic agent. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"16 1","pages":"416 - 431"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139362915","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}
Abstract Efonidipine hydrochloride ethanolate (EFE), a dihydropyridine calcium channel blocker, is used for the treatment of hypertension. To find the EFE in pre-clinical samples (rat plasma), an HPLC method was devised for the current experiment. The biological samples were prepared using the methanolic extraction procedure to eliminate solvent effects. Using a C18 column, a pH-adjusted mobile phase of methanol and water (90:10, v/v) at a flow rate of 1 mL/min, and UV detection at 252 nm were utilized for chromatographic separation. The retention time of EFE was found to be 5.2 min. The developed bioanalytical method was validated with different validation parameters. The validation parameter results are within the acceptable range of the International Council for Harmonization guidelines. The method was successfully employed to evaluate the pharmacokinetic properties in Wistar albino rats following a single oral administration of 10 mg/kg of EFE. Therefore, the simple method would make it possible to detect EFE quickly and affordably from biological material. GRAPHICAL ABSTRACT
{"title":"Bioanalytical method development and Validation for determination of efonidipine hydrochloride ethanolate in rat plasma by high-performance liquid chromatography: applications for pharmacokinetic study","authors":"Swati Bharati, Vinod Gaikwad, Bothiraja Chellampillai","doi":"10.1080/22297928.2023.2263012","DOIUrl":"https://doi.org/10.1080/22297928.2023.2263012","url":null,"abstract":"Abstract Efonidipine hydrochloride ethanolate (EFE), a dihydropyridine calcium channel blocker, is used for the treatment of hypertension. To find the EFE in pre-clinical samples (rat plasma), an HPLC method was devised for the current experiment. The biological samples were prepared using the methanolic extraction procedure to eliminate solvent effects. Using a C18 column, a pH-adjusted mobile phase of methanol and water (90:10, v/v) at a flow rate of 1 mL/min, and UV detection at 252 nm were utilized for chromatographic separation. The retention time of EFE was found to be 5.2 min. The developed bioanalytical method was validated with different validation parameters. The validation parameter results are within the acceptable range of the International Council for Harmonization guidelines. The method was successfully employed to evaluate the pharmacokinetic properties in Wistar albino rats following a single oral administration of 10 mg/kg of EFE. Therefore, the simple method would make it possible to detect EFE quickly and affordably from biological material. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"2015 1","pages":"394 - 402"},"PeriodicalIF":0.0,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139363067","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 : 2023-05-04DOI: 10.1080/22297928.2023.2243267
Kesari Singh, R. Yadava, R. Yadav
Abstract Here we are reporting a new bioactive flavanone glycoside. The compound having molecular formula C21H22O11, melting point 123-125°C, and ESI-MS m/z 451 was isolated from the methanolic extract of Tradescantia Spathacea Sw. Its characterization and structure elucidation was done with the help of various chemical degradation, color reactions, and spectral data like UV-Visible, FT-IR, electrospray ionization mass spectrometry technique, nuclear magnetic resonance spectroscopy, etc. It was recognized as 5,7,3’4’-tetrahydroxy flavanone 3’-O-D-mannopyranoside. This study was also designed to examine the efficacy of an isolated compound against various bacteria which are responsible for food spoilage and pathogens in humans. The organic flavanone glycoside of methanolic extract exhibited a promising antibacterial activity towards Escherichia coli (gram negative) MTCC 724, Bacillus subtilis MTCC 441, Staphylococcus aureus MTCC 737, Pseudomonas aerugenosa MTCC 424, and Salmonella typhimurium MTCC 3224. A new flavanone glycoside possesses potent anti-bacterial activity so it can be utilized as a potent source of antibacterial agents for food and pharmaceutical interest. GRAPHICAL ABSTRACT
摘要本文报道了一种新的生物活性黄酮苷。化合物的分子式为C21H22O11，熔点为123 ~ 125℃，ESI-MS为m/z 451。通过各种化学降解、显色反应以及紫外可见光谱、傅里叶红外光谱、电喷雾质谱技术、核磁共振波谱等光谱数据对其进行了表征和结构解析。鉴定为5,7,3 ' 4 ' -四羟基黄酮3 ' - o - d -甘露吡喃苷。这项研究还旨在检验一种分离化合物对导致食物变质和人体病原体的各种细菌的功效。甲醇提取物的有机黄酮苷对大肠杆菌(革兰氏阴性)MTCC 724、枯草芽孢杆菌MTCC 441、金黄色葡萄球菌MTCC 737、铜绿假单胞菌MTCC 424和鼠伤寒沙门氏菌MTCC 3224具有良好的抑菌活性。一种新型的黄酮苷具有较强的抗菌活性，可作为食品和医药领域的一种有效的抗菌剂。图形抽象
{"title":"Antibacterial activity of new flavanone glycoside isolated from Tradescantia spathacea Sw.","authors":"Kesari Singh, R. Yadava, R. Yadav","doi":"10.1080/22297928.2023.2243267","DOIUrl":"https://doi.org/10.1080/22297928.2023.2243267","url":null,"abstract":"Abstract Here we are reporting a new bioactive flavanone glycoside. The compound having molecular formula C21H22O11, melting point 123-125°C, and ESI-MS m/z 451 was isolated from the methanolic extract of Tradescantia Spathacea Sw. Its characterization and structure elucidation was done with the help of various chemical degradation, color reactions, and spectral data like UV-Visible, FT-IR, electrospray ionization mass spectrometry technique, nuclear magnetic resonance spectroscopy, etc. It was recognized as 5,7,3’4’-tetrahydroxy flavanone 3’-O-D-mannopyranoside. This study was also designed to examine the efficacy of an isolated compound against various bacteria which are responsible for food spoilage and pathogens in humans. The organic flavanone glycoside of methanolic extract exhibited a promising antibacterial activity towards Escherichia coli (gram negative) MTCC 724, Bacillus subtilis MTCC 441, Staphylococcus aureus MTCC 737, Pseudomonas aerugenosa MTCC 424, and Salmonella typhimurium MTCC 3224. A new flavanone glycoside possesses potent anti-bacterial activity so it can be utilized as a potent source of antibacterial agents for food and pharmaceutical interest. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"17 1","pages":"289 - 296"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83227373","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 : 2023-05-04DOI: 10.1080/22297928.2023.2242857
Pallavi Chiprikar, V. Mastiholimath
Abstract A robust as well as precise technique aimed at determining the concentration of Cariprazine in bulk drugs along with formulations using RP-HPLC has been developed. The robustness study was optimized using Box Behnken statistical design. Separation was achieved using an Agilent 1260 Infinity II HPLC with an Agilent Zorbax Bonus RP column, as well as the mobile phase contained of methanol and 0.1% trifluoroacetic acid buffer (52.5:47.5) at a flow rate of 1 ml/min. The wavelength was set at 248 nm, and the method had an overall running period of 8 minutes, with the Cariprazine peak retention time at 3.83 min. The method exhibited linearity and accuracy for concentrations ranging from 80 to 120 μg/ml, with an R2 of 0.999 and accuracy RSD of 0.2%, 0.13%, and 0.05% for 80%, 100%, and 120%, respectively. Stress stability testing under basic conditions revealed 53.32% degradation. The technique’s limit of detection (LOD) and limit of quantification (LOQ) were very low, at 44.80 ng/ml and 135.60 ng/ml, correspondingly. These findings suggest that this method may be helpful during regular quality control evaluation of Cariprazine Hydrochloride in a variety of pharmaceutical formulations. GRAPHICAL ABSTRACT
{"title":"Development of RP-HPLC based analytical method for determination of cariprazine hydrochloride in bulk drug and pharmaceutical dosage form using box-behnken statistical design","authors":"Pallavi Chiprikar, V. Mastiholimath","doi":"10.1080/22297928.2023.2242857","DOIUrl":"https://doi.org/10.1080/22297928.2023.2242857","url":null,"abstract":"Abstract A robust as well as precise technique aimed at determining the concentration of Cariprazine in bulk drugs along with formulations using RP-HPLC has been developed. The robustness study was optimized using Box Behnken statistical design. Separation was achieved using an Agilent 1260 Infinity II HPLC with an Agilent Zorbax Bonus RP column, as well as the mobile phase contained of methanol and 0.1% trifluoroacetic acid buffer (52.5:47.5) at a flow rate of 1 ml/min. The wavelength was set at 248 nm, and the method had an overall running period of 8 minutes, with the Cariprazine peak retention time at 3.83 min. The method exhibited linearity and accuracy for concentrations ranging from 80 to 120 μg/ml, with an R2 of 0.999 and accuracy RSD of 0.2%, 0.13%, and 0.05% for 80%, 100%, and 120%, respectively. Stress stability testing under basic conditions revealed 53.32% degradation. The technique’s limit of detection (LOD) and limit of quantification (LOQ) were very low, at 44.80 ng/ml and 135.60 ng/ml, correspondingly. These findings suggest that this method may be helpful during regular quality control evaluation of Cariprazine Hydrochloride in a variety of pharmaceutical formulations. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"59 1","pages":"297 - 312"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84291453","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 : 2023-05-04DOI: 10.1080/22297928.2023.2242866
Binal Patel, Hitesh J Vekaria
Abstract The development and validation of an easy and rapid stability-indicating RP-HPLC technique for Tenofovir alafenamide and its impurities. In this newly developed method, chromatographic separation of Tenofovir alafenamide and its impurities was achieved on an Inertsil ODS-3V C18 (250 mm x 4.6 mm, 5 μ) column. The impurities were extracted by a mixture of Mobile Phase A: buffer solution: Acetonitrile: Purified water (20:02:78) and Mobile Phase B: Solvent Mixture and Purified water (75:25), The injection volume was 20 μL, the column temperature was 40°C, the flow rate was 1 mL/min, and the detection was carried out at 262 nm. The retention time of Tenofovir alafenamide, PMPA, PMPA anhydrate, Phenyl PMPA and PMPA isopropyl alaninate were 56.24, 5.69, 8.71, 25.89 and 37.13 respectively. The Correlation Coefficient within the acceptance criteria is not less than 0.999. The evaluated concentrations for Tenofovir alafenamide and its impurities were in the range of 0.5–7.5 ppm. The average recovery value was in the range of 90.2–113.9%. Tenofovir alafenamide’s LOD and LOQ were determined to be 0.1 μg/mL and 0.5 μg/mL respectively. Tenofovir alafenamide solution degradation behaviour was assessed using solution stability studies. A new, accurate, and precise method has been developed, evaluated, and elevated for the detection of impurities in Tenofovir alafenamide tablet dosage form. The results obtained from the validation study established that this method is specific, reliable, precise and effective. As a result, the proposed strategy can serve as an alternate method to determine related substances in routine analysis of tablet dosage form. GRAPHICAL ABSTRACT
建立了一种简便、快速的反相高效液相色谱法测定替诺福韦阿拉那胺及其杂质的方法。在Inertsil ODS-3V C18 (250 mm × 4.6 mm, 5 μ)柱上实现了替诺福韦alafenamide及其杂质的色谱分离。采用流动相a:缓冲溶液:乙腈:纯净水(20:02:78)和流动相B:溶剂混合物与纯净水(75:25)的混合萃取，进样量为20 μL，柱温为40℃，流速为1 mL/min，检测波长为262 nm。替诺福韦alafenamide、PMPA、PMPA无水、苯基PMPA和PMPA异丙酸酯的保留时间分别为56.24、5.69、8.71、25.89和37.13。验收标准内的相关系数不小于0.999。替诺福韦阿拉那胺及其杂质的评价浓度在0.5-7.5 ppm范围内。平均回收率为90.2 ~ 113.9%。替诺福韦阿拉那胺的定量限和定量限分别为0.1 μg/mL和0.5 μg/mL。使用溶液稳定性研究评估替诺福韦阿拉那胺溶液的降解行为。开发、评价和提高了一种新的、准确的、精确的替诺福韦阿拉那胺片剂型中杂质检测方法。验证研究结果表明，该方法具有特异性、可靠性、精密度和有效性。因此，该策略可作为片剂剂型常规分析中相关物质测定的替代方法。图形抽象
{"title":"Forced degradation studies and development of RP-HPLC method for related substances of Tenofovir alafenamide in tablet dosage form","authors":"Binal Patel, Hitesh J Vekaria","doi":"10.1080/22297928.2023.2242866","DOIUrl":"https://doi.org/10.1080/22297928.2023.2242866","url":null,"abstract":"Abstract The development and validation of an easy and rapid stability-indicating RP-HPLC technique for Tenofovir alafenamide and its impurities. In this newly developed method, chromatographic separation of Tenofovir alafenamide and its impurities was achieved on an Inertsil ODS-3V C18 (250 mm x 4.6 mm, 5 μ) column. The impurities were extracted by a mixture of Mobile Phase A: buffer solution: Acetonitrile: Purified water (20:02:78) and Mobile Phase B: Solvent Mixture and Purified water (75:25), The injection volume was 20 μL, the column temperature was 40°C, the flow rate was 1 mL/min, and the detection was carried out at 262 nm. The retention time of Tenofovir alafenamide, PMPA, PMPA anhydrate, Phenyl PMPA and PMPA isopropyl alaninate were 56.24, 5.69, 8.71, 25.89 and 37.13 respectively. The Correlation Coefficient within the acceptance criteria is not less than 0.999. The evaluated concentrations for Tenofovir alafenamide and its impurities were in the range of 0.5–7.5 ppm. The average recovery value was in the range of 90.2–113.9%. Tenofovir alafenamide’s LOD and LOQ were determined to be 0.1 μg/mL and 0.5 μg/mL respectively. Tenofovir alafenamide solution degradation behaviour was assessed using solution stability studies. A new, accurate, and precise method has been developed, evaluated, and elevated for the detection of impurities in Tenofovir alafenamide tablet dosage form. The results obtained from the validation study established that this method is specific, reliable, precise and effective. As a result, the proposed strategy can serve as an alternate method to determine related substances in routine analysis of tablet dosage form. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"7 1","pages":"321 - 336"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76158176","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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