Pub Date : 2022-09-03DOI: 10.1080/22297928.2022.2132876
S.K. Madhavi Harika, M. Sudhakar, V. V. Basava Rao
Abstract The purpose of the study is to develop floating in situ gelling oral delivery system of carvedilol. Before formulating into in situ gels, carvedilol was first made into solid dispersions to enhance its solubility. The solvent evaporation method was employed for making solid dispersions. Drug content, solubility, dissolution, SEM, DSC, and XRD studies were done for solid dispersions. In situ gel formulations were prepared using the optimized solid dispersion formulation. Sodium alginate and HPMC K100M were used as gelling agent and viscosity enhancing agent respectively. In vitro characterizations like gelling capacity, floating time, drug content, viscosity, and % cumulative drug release studies were done. In vivo pharmacokinetic parameters like Cmax, Tmax, half-life, AUC, AUMC, and MRT were studied. FTIR studies ruled out any drug-excipient interactions. The drug release pattern showed a burst effect in the first 30 minutes then followed by a steady release for 12 hours. Stability data indicated that the formulation remained stable with no significant changes in drug content, viscosity, and percent cumulative drug release upon storage. In vivo pharmacokinetic study results were found to be satisfactory. A stable, sustained release, liquid oral floating in-situ gelling systems of carvedilol were successfully formulated and evaluated. GRAPHICAL ABSTRACT
{"title":"Formulation and Characterization of Carvedilol In situ Gels for Oral Delivery-In vitro and In vivo Pharmacokinetic Studies","authors":"S.K. Madhavi Harika, M. Sudhakar, V. V. Basava Rao","doi":"10.1080/22297928.2022.2132876","DOIUrl":"https://doi.org/10.1080/22297928.2022.2132876","url":null,"abstract":"Abstract The purpose of the study is to develop floating in situ gelling oral delivery system of carvedilol. Before formulating into in situ gels, carvedilol was first made into solid dispersions to enhance its solubility. The solvent evaporation method was employed for making solid dispersions. Drug content, solubility, dissolution, SEM, DSC, and XRD studies were done for solid dispersions. In situ gel formulations were prepared using the optimized solid dispersion formulation. Sodium alginate and HPMC K100M were used as gelling agent and viscosity enhancing agent respectively. In vitro characterizations like gelling capacity, floating time, drug content, viscosity, and % cumulative drug release studies were done. In vivo pharmacokinetic parameters like Cmax, Tmax, half-life, AUC, AUMC, and MRT were studied. FTIR studies ruled out any drug-excipient interactions. The drug release pattern showed a burst effect in the first 30 minutes then followed by a steady release for 12 hours. Stability data indicated that the formulation remained stable with no significant changes in drug content, viscosity, and percent cumulative drug release upon storage. In vivo pharmacokinetic study results were found to be satisfactory. A stable, sustained release, liquid oral floating in-situ gelling systems of carvedilol were successfully formulated and evaluated. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"72 1","pages":"599 - 614"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84099756","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 : 2022-09-03DOI: 10.1080/22297928.2022.2132875
Arvind Parashar, R. Jain, K. S. Thakur, R. Jain
Abstract The adsorption of the ranitidine on 3D porous NiFe2O4 nanoparticles was studied under different experimental conditions. Adsorbent used in this study, was characterized by SEM, XRD, EDX and BET. The prepared highly pure 3D porous NiFe2O4 nanoparticles displayed a high specific surface area of 65.179 m2/g with a total pore volume of 8.495 nm. The effect of ranitidine concentration, mass of 3D porous NiFe2O4 nanoparticles as adsorbent, contact time (5-30 min.), temperature (30–50 0C), and pH (2-10) on adsorption process were investigated. The adsorption of ranitidine reached equilibrium within 15 min, indicating that 3D porous NiFe2O4 is a promising adsorbent for removing pharmaceuticals from aqueous media. Equilibrium isotherms for the adsorption viz, Freundlich, Langmuir and DR equation were applied and determined characteristic parameters for each adsorption isotherm. Thermodynamic analysis of the adsorption data showed negative ΔG0 and positive ΔH0 suggesting that the adsorption was a spontaneous and endothermic process, associated with mainly physical adsorption.
{"title":"Equilibrium, Kinetic and Thermodynamic Studies of Adsorption Behaviour of 3D Porous NiFe Nanoparticles for The Removal of Antacid Drug Ranitidine from Waste Water","authors":"Arvind Parashar, R. Jain, K. S. Thakur, R. Jain","doi":"10.1080/22297928.2022.2132875","DOIUrl":"https://doi.org/10.1080/22297928.2022.2132875","url":null,"abstract":"Abstract The adsorption of the ranitidine on 3D porous NiFe2O4 nanoparticles was studied under different experimental conditions. Adsorbent used in this study, was characterized by SEM, XRD, EDX and BET. The prepared highly pure 3D porous NiFe2O4 nanoparticles displayed a high specific surface area of 65.179 m2/g with a total pore volume of 8.495 nm. The effect of ranitidine concentration, mass of 3D porous NiFe2O4 nanoparticles as adsorbent, contact time (5-30 min.), temperature (30–50 0C), and pH (2-10) on adsorption process were investigated. The adsorption of ranitidine reached equilibrium within 15 min, indicating that 3D porous NiFe2O4 is a promising adsorbent for removing pharmaceuticals from aqueous media. Equilibrium isotherms for the adsorption viz, Freundlich, Langmuir and DR equation were applied and determined characteristic parameters for each adsorption isotherm. Thermodynamic analysis of the adsorption data showed negative ΔG0 and positive ΔH0 suggesting that the adsorption was a spontaneous and endothermic process, associated with mainly physical adsorption.","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"32 1","pages":"615 - 628"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90983236","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 : 2022-09-03DOI: 10.1080/22297928.2022.2132877
A. A. Nagargoje, Satish V Akolkar, M. Shaikh, H. Akolkar, D. Raut, Parshuram M. Pisal, V. Khedkar, B. Shingate
Abstract In the present investigation, we report the synthesis, anti-inflammatory activity and molecular docking of monocarbonyl analogues of curcumin. The anti-inflammatory activity of the synthesized compounds was gauzed using the protein denaturation assay using Diclofenac sodium as reference standard. Among the tested compounds, 3d, 3e, 3f, 3j, 3k, 3l and 3m displayed excellent anti-inflammatory activity by exhibiting good range of percentage inhibition as compared to the standard DFS. In silico binding affinity study against Cyclooxygenase (COX-2) enzyme could provide valuable insight into their plausible mechanism of action. Also, in silico ADME prediction of synthesized monocarbonyl curcumin analogues showed excellent pharmacokinetic parameters by not violating Lipinski’s rule of five. GRAPHICAL ABSTRACT
{"title":"Investigation of the Anti-inflammatory potential of Mono-carbonyl Analogues of Curcumin","authors":"A. A. Nagargoje, Satish V Akolkar, M. Shaikh, H. Akolkar, D. Raut, Parshuram M. Pisal, V. Khedkar, B. Shingate","doi":"10.1080/22297928.2022.2132877","DOIUrl":"https://doi.org/10.1080/22297928.2022.2132877","url":null,"abstract":"Abstract In the present investigation, we report the synthesis, anti-inflammatory activity and molecular docking of monocarbonyl analogues of curcumin. The anti-inflammatory activity of the synthesized compounds was gauzed using the protein denaturation assay using Diclofenac sodium as reference standard. Among the tested compounds, 3d, 3e, 3f, 3j, 3k, 3l and 3m displayed excellent anti-inflammatory activity by exhibiting good range of percentage inhibition as compared to the standard DFS. In silico binding affinity study against Cyclooxygenase (COX-2) enzyme could provide valuable insight into their plausible mechanism of action. Also, in silico ADME prediction of synthesized monocarbonyl curcumin analogues showed excellent pharmacokinetic parameters by not violating Lipinski’s rule of five. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"33 1","pages":"586 - 598"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79444452","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 : 2022-09-03DOI: 10.1080/22297928.2022.2142844
B. Ivanova, M. Spiteller
Abstract The study provides new function tested on labetalol in large infusion volumes (Vinf = 80-115 µL) via electrospray ionization mass spectrometry, tandem MS2–MS7 operation modes and collision energy: 0, 0.1, 10, 20, 25, 26, 30 and 35 eV, respectively. It is derived from the stochastic dynamic mass spectrometric equation D”SD = 2.6388.10-17.(-2), which exactly quantifies analyte concentration in solution. Also, it determines 3D conformations and electronic structures. The description of mass spectrometric intensity data as random variables and the shown relation, there are written two new linear functions among D”SD parameters, average total intensity values of fragmentation peaks, infusion volume, and collision energy. They introduce covariance of datasets of variables per short span of scan time of ions in any experimental conditions “l” and “m”. They are: D”SD;m,l = D”SD,l + D”SD,m + 5.2776.10-17.{–.}≈+ and +≈|rl,m|.sd(yEr±)1.sd(yEr±)m. Those relations yields to new formula D”SD,l+ D”SD,m = |rl,m|.sd(yEr±)l.sd(yEr±)m, providing exact function of mass spectrometric variable intensity of any peaks of analyte ion in any two sets of experimental conditions of measurements and diffusion parameters according to the first formula. Correlation between theory and experiment of fragmentation processes of labetalol shows |r|=1–0.99999. Chemometrics is used. GRAPHICAL ABSTRACT
摘要采用电喷雾电离质谱法，采用MS2-MS7串联工作模式，碰撞能量分别为0、0.1、10、20、25、26、30和35 eV，对大输液量(Vinf = 80-115µL)的拉贝他洛尔进行了新的功能检测。它由随机动态质谱方程D”SD = 2.6388.10-17.(-2)推导而来，能准确地定量测定溶液中被分析物的浓度。此外，它还决定了三维构象和电子结构。将质谱强度数据描述为随机变量，并根据所示关系，写出了D”SD参数、破碎峰平均总强度值、注入体积和碰撞能量之间的两个新的线性函数。它们在任何实验条件“l”和“m”中引入了每短时间内离子扫描时间的变量数据集的协方差。SD: D”;m, l = D“SD, l + D“SD, m + 5.2776.10-17。{-。}≈+和+≈|rl,m|.sd(yEr±)1.sd(yEr±)m。这些关系得到了新的公式D " SD,l+ D " SD,m = 1 / rl,m = 1 / rl . SD (yEr±)l. SD (yEr±)m，给出了在任意两组测量实验条件和扩散参数下，分析物离子任意峰的质谱变强度的精确函数。拉贝他洛尔破碎过程的理论与实验的相关性表明:|r|= 1-0.99999。使用化学计量学。图形抽象
{"title":"Exact Quantifying of Mass Spectrometric Variable Intensity of Analyte Peaks with Respect to Experimental Conditions of Measurements – A Stochastic Dynamic Approach","authors":"B. Ivanova, M. Spiteller","doi":"10.1080/22297928.2022.2142844","DOIUrl":"https://doi.org/10.1080/22297928.2022.2142844","url":null,"abstract":"Abstract The study provides new function tested on labetalol in large infusion volumes (Vinf = 80-115 µL) via electrospray ionization mass spectrometry, tandem MS2–MS7 operation modes and collision energy: 0, 0.1, 10, 20, 25, 26, 30 and 35 eV, respectively. It is derived from the stochastic dynamic mass spectrometric equation D”SD = 2.6388.10-17.(-2), which exactly quantifies analyte concentration in solution. Also, it determines 3D conformations and electronic structures. The description of mass spectrometric intensity data as random variables and the shown relation, there are written two new linear functions among D”SD parameters, average total intensity values of fragmentation peaks, infusion volume, and collision energy. They introduce covariance of datasets of variables per short span of scan time of ions in any experimental conditions “l” and “m”. They are: D”SD;m,l = D”SD,l + D”SD,m + 5.2776.10-17.{–.}≈+ and +≈|rl,m|.sd(yEr±)1.sd(yEr±)m. Those relations yields to new formula D”SD,l+ D”SD,m = |rl,m|.sd(yEr±)l.sd(yEr±)m, providing exact function of mass spectrometric variable intensity of any peaks of analyte ion in any two sets of experimental conditions of measurements and diffusion parameters according to the first formula. Correlation between theory and experiment of fragmentation processes of labetalol shows |r|=1–0.99999. Chemometrics is used. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"16 1","pages":"542 - 561"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79668084","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 : 2022-09-03DOI: 10.1080/22297928.2022.2132878
Y. Satyawana, N. Sharma, R. Singh,, N. Fahmi
Abstract Eight metal complexes with Schiff base ligands, HL1 [2-{1-(2-fluorophenyl)ethyledene}] hydrazinecarboxamide and HL2 [2-{1-(2-fluorophenyl)ethyledene}] hydrazinecarboxathioamide were synthesized with Co(II) and Ni(II). These were characterized by analytical as well as various spectroscopic techniques like FT-IR, 1H NMR, electronic absorption spectra. The spectral results revealed the formation of octahedral complexes. To determine the concentration of cobalt in Schiff base metal complex flame atomic absorption spectroscopy (FAAS) was done. The accuracy of results was verified by inductively coupled plasma mass spectroscopy (ICP-MS). In vitro cytotoxic activity of the ligands HL1, HL2 and their Schiff base metal complexes was examined, in which A549 (human lung cancer cell line) and L929 (mouse normal fibroblast cell line) were used in the screening test. Among all the synthesized Schiff base ligands and metal complexes, Ni(II) thiosemicarbazone based complex i.e. (Ni (L2)2.2H2O) exhibited a significant cytotoxic effect towards A549 cell line with a mean IC50 value of 36.43 μΜ. Plant growth regulatory activity of the ligands (HL1, HL2) and their metal complexes have also been performed on chick pea plant. The PGR activity of the ligands and their complexes were compared and it was found that the thiosemicarbazone based metal complexes possess higher PGR activity. GRAPHICAL ABSTRACT
{"title":"Synthesis, Structural Elucidation, Cytotoxic activity and Plant Growth Studies of Some Novel Schiff Base Cobalt(II) and Nickel(II) Complexes of Sulfur/Oxygen and Nitrogen Donor Agents","authors":"Y. Satyawana, N. Sharma, R. Singh,, N. Fahmi","doi":"10.1080/22297928.2022.2132878","DOIUrl":"https://doi.org/10.1080/22297928.2022.2132878","url":null,"abstract":"Abstract Eight metal complexes with Schiff base ligands, HL1 [2-{1-(2-fluorophenyl)ethyledene}] hydrazinecarboxamide and HL2 [2-{1-(2-fluorophenyl)ethyledene}] hydrazinecarboxathioamide were synthesized with Co(II) and Ni(II). These were characterized by analytical as well as various spectroscopic techniques like FT-IR, 1H NMR, electronic absorption spectra. The spectral results revealed the formation of octahedral complexes. To determine the concentration of cobalt in Schiff base metal complex flame atomic absorption spectroscopy (FAAS) was done. The accuracy of results was verified by inductively coupled plasma mass spectroscopy (ICP-MS). In vitro cytotoxic activity of the ligands HL1, HL2 and their Schiff base metal complexes was examined, in which A549 (human lung cancer cell line) and L929 (mouse normal fibroblast cell line) were used in the screening test. Among all the synthesized Schiff base ligands and metal complexes, Ni(II) thiosemicarbazone based complex i.e. (Ni (L2)2.2H2O) exhibited a significant cytotoxic effect towards A549 cell line with a mean IC50 value of 36.43 μΜ. Plant growth regulatory activity of the ligands (HL1, HL2) and their metal complexes have also been performed on chick pea plant. The PGR activity of the ligands and their complexes were compared and it was found that the thiosemicarbazone based metal complexes possess higher PGR activity. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"1 1","pages":"562 - 575"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91393885","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 : 2022-09-03DOI: 10.1080/22297928.2022.2148558
N. Desai, K. Shah, B. Dave, V. Khedkar
Abstract This study analysed the interactions between the chemical structures and antimicrobial activities of various functional groups containing organic compounds. The spectral methods confirmed the structure of these compounds after efficient synthesis was carried out. Two Gram-positive and two Gram-negative bacteria were tested for in vitro antibacterial activity of the synthesised compounds. For antifungal activity, three fungal strains were tested. Compound 5n showed a potent inhibitory effects against E. coli and P. aeruginosa with MIC values of 12.5 µg/ml and 6.25 µg/ml, respectively (Glide Docking score: -9.190). S. aureus and S. pyogenus were both positively affected by compound 5i with MIC values of 12.5 µg/ml and 25 µg/ml, respectively (Glide Docking score: -9.111). Based on the results, compounds 5a and 5f have excellent activity against C. albicans with MIC values of 200 µg/ml. Molecular docking study against microbial peptide deformylase could provide insight into the binding affinity and orientation of the active site. A very significant correlation was obtained between the in silico binding affinity data with an average Glide docking score of -8.412 and Glide binding energy: -43.074 kcal/mol. Compound 5n produced a relatively higher binding affinity (Glide dock score: -9.190 and Glide binding energy: -51.226 kcal/mol) which was also translated in its higher antimicrobial activity. GRAPHICAL ABSTRACT
摘要本研究分析了含有机化合物不同官能团的化学结构与抗菌活性之间的相互作用。在高效合成后，用光谱方法证实了这些化合物的结构。对两种革兰氏阳性菌和两种革兰氏阴性菌进行了体外抗菌活性测试。对3株真菌进行了抗真菌活性测试。化合物5n对大肠杆菌和铜绿假单胞菌具有较强的抑制作用，MIC值分别为12.5µg/ml和6.25µg/ml (Glide Docking评分:-9.190)。化合物5i对金黄色葡萄球菌和脓链球菌均有正向影响，MIC值分别为12.5µg/ml和25µg/ml(滑翔对接评分:-9.111)。结果表明，化合物5a和5f对白色念珠菌具有良好的抑制活性，MIC值为200µg/ml。通过对微生物肽脱甲酰基酶的分子对接研究，可以深入了解活性位点的结合亲和力和取向。滑翔对接分数为-8.412的硅结合亲和度数据与滑翔结合能为-43.074 kcal/mol具有极显著的相关性。化合物5n具有较高的结合亲和力(Glide dock score: -9.190, Glide结合能:-51.226 kcal/mol)，并具有较高的抗菌活性。图形抽象
{"title":"Design, Synthesis, Antimicrobial Activity and Molecular docking Studies of Pyridine Based Thiazolidine-4-one and Its 5-Arylidene Derivatives","authors":"N. Desai, K. Shah, B. Dave, V. Khedkar","doi":"10.1080/22297928.2022.2148558","DOIUrl":"https://doi.org/10.1080/22297928.2022.2148558","url":null,"abstract":"Abstract This study analysed the interactions between the chemical structures and antimicrobial activities of various functional groups containing organic compounds. The spectral methods confirmed the structure of these compounds after efficient synthesis was carried out. Two Gram-positive and two Gram-negative bacteria were tested for in vitro antibacterial activity of the synthesised compounds. For antifungal activity, three fungal strains were tested. Compound 5n showed a potent inhibitory effects against E. coli and P. aeruginosa with MIC values of 12.5 µg/ml and 6.25 µg/ml, respectively (Glide Docking score: -9.190). S. aureus and S. pyogenus were both positively affected by compound 5i with MIC values of 12.5 µg/ml and 25 µg/ml, respectively (Glide Docking score: -9.111). Based on the results, compounds 5a and 5f have excellent activity against C. albicans with MIC values of 200 µg/ml. Molecular docking study against microbial peptide deformylase could provide insight into the binding affinity and orientation of the active site. A very significant correlation was obtained between the in silico binding affinity data with an average Glide docking score of -8.412 and Glide binding energy: -43.074 kcal/mol. Compound 5n produced a relatively higher binding affinity (Glide dock score: -9.190 and Glide binding energy: -51.226 kcal/mol) which was also translated in its higher antimicrobial activity. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"143 1","pages":"639 - 654"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74531256","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 : 2022-09-03DOI: 10.1080/22297928.2022.2131467
Urvi Chotaliya, Hiteksha J. Dobariya, Disha L. Barad, A. Vyas, Dhruvanshi Gol
Abstract RP-HPLC stability indicating specific, precise, accurate, cost-effective and isocratic method was developed and validated for quantitative analysis of Atorvastatin calcium and Teneligliptin hydrobromide hydrate in synthetic mixture with presence of its degradants. Separation was achieved by using Gemini, C18, using mobile phase composition [Methanol: 20 mM Ammonium acetate (70:30 v/v)] using a flow rate of 1.0 ml/min, injection volume 10µl with UV detection at 245 nm. Atorvastatin calcium and Teneligliptin hydrobromide hydrate were eluted with retention time 7.47min and 4.74min respectively. This method was validated as per ICH guideline Q2(R1). The calibration plots were over the concentration range of 10-100 μg/ml and 5-50 μg/ml for Atorvastatin calcium and Teneligliptin hydrobromide hydrate with correlation coefficient 1 and 0.9999 respectively. Percentage recovery was obtained between 98.00-100.51 % and 98.90-100.7 % for Atorvastatin calcium and Teneligliptin hydrobromide hydrate respectively. In case of Precision, Repeatability and Robustness RSD should be found less than 2. LOD were found to be 1.22 μg/ml and 0.54 μg/ml and LOQ were found to be 3.70 μg/ml and 1.64 μg/ml for Atorvastatin calcium and Teneligliptin hydrobromide hydrate respectively. The results showed that the developed method is appropriate for the routine analysis of Atorvastatin calcium and Teneligliptin hydrobromide hydrate in a synthetic mixture in presence of its degradants. GRAPHICAL ABSTRACT
{"title":"Stability Indicating RP-HPLC-DAD Method For Simultaneous Estimation of Atorvastatin Calcium and Teneligliptin Hydrobromide Hydrate in Synthetic Mixture","authors":"Urvi Chotaliya, Hiteksha J. Dobariya, Disha L. Barad, A. Vyas, Dhruvanshi Gol","doi":"10.1080/22297928.2022.2131467","DOIUrl":"https://doi.org/10.1080/22297928.2022.2131467","url":null,"abstract":"Abstract RP-HPLC stability indicating specific, precise, accurate, cost-effective and isocratic method was developed and validated for quantitative analysis of Atorvastatin calcium and Teneligliptin hydrobromide hydrate in synthetic mixture with presence of its degradants. Separation was achieved by using Gemini, C18, using mobile phase composition [Methanol: 20 mM Ammonium acetate (70:30 v/v)] using a flow rate of 1.0 ml/min, injection volume 10µl with UV detection at 245 nm. Atorvastatin calcium and Teneligliptin hydrobromide hydrate were eluted with retention time 7.47min and 4.74min respectively. This method was validated as per ICH guideline Q2(R1). The calibration plots were over the concentration range of 10-100 μg/ml and 5-50 μg/ml for Atorvastatin calcium and Teneligliptin hydrobromide hydrate with correlation coefficient 1 and 0.9999 respectively. Percentage recovery was obtained between 98.00-100.51 % and 98.90-100.7 % for Atorvastatin calcium and Teneligliptin hydrobromide hydrate respectively. In case of Precision, Repeatability and Robustness RSD should be found less than 2. LOD were found to be 1.22 μg/ml and 0.54 μg/ml and LOQ were found to be 3.70 μg/ml and 1.64 μg/ml for Atorvastatin calcium and Teneligliptin hydrobromide hydrate respectively. The results showed that the developed method is appropriate for the routine analysis of Atorvastatin calcium and Teneligliptin hydrobromide hydrate in a synthetic mixture in presence of its degradants. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"39 1","pages":"629 - 638"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80184251","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 : 2022-09-03DOI: 10.1080/22297928.2022.2140072
Mukesh N. Kher, S. Dholakia, Grisha G. Shah, D. Sureja, Vaibhav Bhatt, D. Sheth
Abstract Vitamins are pivotal ingredients in dietary supplements and nutraceutical products. Since many vitamins are unstable and rapidly degraded, it’s crucial to keep track of their loss throughout processing and storage. Monitoring hydrophilic vitamins may be more crucial than monitoring those lipophilic vitamins because the body does not maintain them as well. There seems to be a need for an all-encompassing method to estimate hydrophilic vitamins. In this study, we have developed a high-performance thin layer chromatography method for estimation of four water-soluble vitamins simultaneously using HPTLC silica-gel 60GF254 plates and ethyl acetate: methanol: hydrochloric acid (0.1N) (8.5:1:0.5 v/v/v) as a mobile phase, which was successfully validated as per the ICH guideline. All the validation parameters were within the acceptable range established by the ICH guideline. The method is precise, reproducible, easy, reliable, and applicable for the estimation of water-soluble vitamins in marketed products. To best of our knowledge, it is simpler, less time-consuming, and more economical than other approaches that have been published for the same purposes GRAPHICAL ABSTRACT
{"title":"High-Performance Thin Layer Chromatography Method for Simultaneous Estimation of Water-Soluble Vitamins: Analytical Method Development, Validation and Applications","authors":"Mukesh N. Kher, S. Dholakia, Grisha G. Shah, D. Sureja, Vaibhav Bhatt, D. Sheth","doi":"10.1080/22297928.2022.2140072","DOIUrl":"https://doi.org/10.1080/22297928.2022.2140072","url":null,"abstract":"Abstract Vitamins are pivotal ingredients in dietary supplements and nutraceutical products. Since many vitamins are unstable and rapidly degraded, it’s crucial to keep track of their loss throughout processing and storage. Monitoring hydrophilic vitamins may be more crucial than monitoring those lipophilic vitamins because the body does not maintain them as well. There seems to be a need for an all-encompassing method to estimate hydrophilic vitamins. In this study, we have developed a high-performance thin layer chromatography method for estimation of four water-soluble vitamins simultaneously using HPTLC silica-gel 60GF254 plates and ethyl acetate: methanol: hydrochloric acid (0.1N) (8.5:1:0.5 v/v/v) as a mobile phase, which was successfully validated as per the ICH guideline. All the validation parameters were within the acceptable range established by the ICH guideline. The method is precise, reproducible, easy, reliable, and applicable for the estimation of water-soluble vitamins in marketed products. To best of our knowledge, it is simpler, less time-consuming, and more economical than other approaches that have been published for the same purposes GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"45 1","pages":"576 - 585"},"PeriodicalIF":0.0,"publicationDate":"2022-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89728140","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 : 2022-07-04DOI: 10.1080/22297928.2022.2121662
S. Neha, A. Mishra, Laxmi Rani, Suraj P. Verma, P. K. Sahoo
Abstract The emotional control monoamines neurotransmitter catecholamine group of chemicals is dopamine. It has been described and recognized that a lack of dopamine containing neurons contributes to neurological issues, such as Parkinsonism. Due to the incapability of dopamine HCl to cross the blood brain barrier, the advanced novel drug delivery of dopamine HCl is performed in the form of nano structure lipid carrier system (NLC-DOPA) to bypass the blood brain barrier using intranasal route of administration with improved compliance bioavailability and less side effect. The NLC-DOPA was prepared by the high pressure homogenizer ultra-probe sonicator and characterized by the particle size analyzer, zeta potential, transmission electron microscopy (TEM) and X-Ray diffraction (XRD). The determination of dopamine hydrochloride in formulation was evaluated by drug entrapment efficiency further it is validated by analytical method development using high performance liquid chromatography (HPLC) with C18 ODS column and 0.05 M KH2PO4 buffer pH 2.5 and Methanol (90:10) along with retention time 4.872 min at 280 nm wavelength. The method was validated for dopamine HCl in formulation with linearity, precision and recovery analysis. The study was shown that method was easy, rapid, accurate, specific and precise for quality analysis of dopamine HCl in NLC-DOPA formulation. The validated method of HPLC was further used for the biological application in term of the pharmacokinetic study to find out the concentration of drug in blood as well as brain. The pharmacokinetic parameters were calculated with help of the software PK solver 2.0 to determine the maximum concentration (Cmax), Maximum time (Tmax), Elimination half life (t1/2), Area under the curve (AUC0-t), volume of distribution (Vz/F_obs) and Clearance (Cl/F_obs) of all groups of animals (n=3). The study showed that the NLC-DOPA was producing a sustained and controlled release in appropriate amount of drug through intranasal bypass delivery into brain. GRAPHICAL ABSTRACT
控制情绪的单胺类神经递质儿茶酚胺类化学物质是多巴胺。人们已经描述并认识到，缺乏含有多巴胺的神经元会导致神经系统问题，如帕金森病。由于多巴胺HCl不能穿过血脑屏障，先进的新型给药多巴胺HCl以纳米结构脂质载体系统(NLC-DOPA)的形式通过鼻内给药途径绕过血脑屏障，具有更高的顺应性、生物利用度和更小的副作用。采用高压均质机超探针超声制备了NLC-DOPA，并用粒度分析仪、zeta电位、透射电子显微镜(TEM)和x射线衍射仪(XRD)对其进行了表征。采用高效液相色谱法(HPLC)，色谱柱为C18 ODS，缓冲液为0.05 M KH2PO4, pH为2.5，甲醇(90:10)，保留时间为4.872 min，波长为280 nm。该方法对盐酸多巴胺的线性、精密度和回收率进行了验证。结果表明，该方法简便、快速、准确、特异、精密度高，可用于NLC-DOPA制剂中多巴胺盐酸的质量分析。将验证后的高效液相色谱法进一步应用于生物药代动力学研究，了解药物在血药浓度和脑药浓度。利用PK求解器2.0软件计算药代动力学参数，确定各组动物(n=3)的最大浓度(Cmax)、最大时间(Tmax)、消除半衰期(t1/2)、曲线下面积(AUC0-t)、分布体积(Vz/F_obs)和清除率(Cl/F_obs)。研究表明，NLC-DOPA在适当剂量的情况下，通过鼻内旁路给药进入大脑，产生持续的、可控的释放。图形抽象
{"title":"Characterization and HPLC Method Validation for Determination of Dopamine Hydrochloride in Prepared Nano Particles and Pharmacokinetic Application","authors":"S. Neha, A. Mishra, Laxmi Rani, Suraj P. Verma, P. K. Sahoo","doi":"10.1080/22297928.2022.2121662","DOIUrl":"https://doi.org/10.1080/22297928.2022.2121662","url":null,"abstract":"Abstract The emotional control monoamines neurotransmitter catecholamine group of chemicals is dopamine. It has been described and recognized that a lack of dopamine containing neurons contributes to neurological issues, such as Parkinsonism. Due to the incapability of dopamine HCl to cross the blood brain barrier, the advanced novel drug delivery of dopamine HCl is performed in the form of nano structure lipid carrier system (NLC-DOPA) to bypass the blood brain barrier using intranasal route of administration with improved compliance bioavailability and less side effect. The NLC-DOPA was prepared by the high pressure homogenizer ultra-probe sonicator and characterized by the particle size analyzer, zeta potential, transmission electron microscopy (TEM) and X-Ray diffraction (XRD). The determination of dopamine hydrochloride in formulation was evaluated by drug entrapment efficiency further it is validated by analytical method development using high performance liquid chromatography (HPLC) with C18 ODS column and 0.05 M KH2PO4 buffer pH 2.5 and Methanol (90:10) along with retention time 4.872 min at 280 nm wavelength. The method was validated for dopamine HCl in formulation with linearity, precision and recovery analysis. The study was shown that method was easy, rapid, accurate, specific and precise for quality analysis of dopamine HCl in NLC-DOPA formulation. The validated method of HPLC was further used for the biological application in term of the pharmacokinetic study to find out the concentration of drug in blood as well as brain. The pharmacokinetic parameters were calculated with help of the software PK solver 2.0 to determine the maximum concentration (Cmax), Maximum time (Tmax), Elimination half life (t1/2), Area under the curve (AUC0-t), volume of distribution (Vz/F_obs) and Clearance (Cl/F_obs) of all groups of animals (n=3). The study showed that the NLC-DOPA was producing a sustained and controlled release in appropriate amount of drug through intranasal bypass delivery into brain. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"41 1","pages":"528 - 541"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75315037","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 : 2022-07-04DOI: 10.1080/22297928.2022.2100276
Victor O. Omondi, Geoffrey O. Bosire, J. Onyari, M. N. Getahun
Abstract In the rapidly increasing field of metabolomic research, fast and accurate trapping of volatile odor compounds from biological samples is critical. Here a comparative evaluation of HS-SPME and PoraPak-Q adsorbent odor trapping methods followed by GC-MS analysis were used to determine volatile compounds in cattle rumen. Compared to the PoraPak-Q adsorbent, the HS-SPME method was more effective in trapping diverse metabolites including low molecular weight and highly volatile compounds such as carbon dioxide, acetic and butyric acid. Additionally, using the HS-SPME method, shorter trapping times were achieved (30 minutes) whilst the PoraPak-Q adsorbent required longer time extending beyond 1 hour for effective volatile trapping. In the context of metabolomics analysis from biological samples, the two different methods vary in determination of chemo-diversities, qualitatively and abundance of shared odor, and time required to trap odors, which are critical in such studies. GRAPHICAL ABSTRACT
{"title":"A Comparative Investigation of Volatile Organic Compounds of Cattle Rumen Metabolites using HS-SPME and PoraPak-Q Odor Trapping Methods","authors":"Victor O. Omondi, Geoffrey O. Bosire, J. Onyari, M. N. Getahun","doi":"10.1080/22297928.2022.2100276","DOIUrl":"https://doi.org/10.1080/22297928.2022.2100276","url":null,"abstract":"Abstract In the rapidly increasing field of metabolomic research, fast and accurate trapping of volatile odor compounds from biological samples is critical. Here a comparative evaluation of HS-SPME and PoraPak-Q adsorbent odor trapping methods followed by GC-MS analysis were used to determine volatile compounds in cattle rumen. Compared to the PoraPak-Q adsorbent, the HS-SPME method was more effective in trapping diverse metabolites including low molecular weight and highly volatile compounds such as carbon dioxide, acetic and butyric acid. Additionally, using the HS-SPME method, shorter trapping times were achieved (30 minutes) whilst the PoraPak-Q adsorbent required longer time extending beyond 1 hour for effective volatile trapping. In the context of metabolomics analysis from biological samples, the two different methods vary in determination of chemo-diversities, qualitatively and abundance of shared odor, and time required to trap odors, which are critical in such studies. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"21 1","pages":"451 - 459"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73679372","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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