Angel D. Rodriguez-Mackenzie, Lysmarie Santos-Velazquez, Héctor D. Arbelo-Lopez, Troy Wymore, Juan Lopez-Garriga
The chemistry of hydrogen sulfide (H2S) has been directed towards physiologically relevant hemeproteins, including myoglobin, hemoglobin, and other similar proteins. Despite substantial efforts, there remains a need to elucidate the mechanism and identify the species involved in the reaction between oxy-hemeproteins and H2S. Here, we summarize both our experimental data and computational modeling results revealing the mechanisms by which sulfmyoglobin (sulfMb) and sulfhemoglobin (sulfHb) are formed. Our experimental data at pH 7.4 reveal differences in intensity between sulfMb and sulfHb chromophores in the 620 nm charge transfer region. This behavior could be attributed to the incomplete reaction of tetrameric oxy-Hb with H2S, where not all heme groups form sulfheme. The data also show that, for the reaction of oxy-myoglobin (oxy-Mb) and H2S, the 622 nm charge transfer band increases in intensity from a pH of 6.6 to 5.0. This increase is attributed to the presence of the heme pocket distal His64εδ, which is positively charged, resulting in an elevated yield of sulfMb formation compared to the mono-protonated tautomer, His64ε. Computational hybrid QM/MM methods support the conclusion, indicating that oxy-Mb His64εδ (pH 5.0) reacts with H2S in the triplet state, favored by −31.0 kcal/mol over the singlet His64ε (pH 6.6) species. The phenomenon is facilitated by a hydrogen bonding network within the heme pocket, between His64εδ, heme Fe(II)O2, and H2S. The results establish an energetically favored quantitative mechanism to produce sulfMb (−69.1 kcal/mol) from the reactions of oxy-Mb and H2S. Curiously, the mechanism between met-aquo Mb, H2O2, and H2S shows similar reaction pathways and leads to sulfheme formation (−135.3 kcal/mol). The energetic barrier towards intermediate Cpd-0 is the limiting step in sulfheme formation for both systems. Both mechanisms show that the thiyl radical, HS•, is the species attacking the β-β double bond of heme pyrrole B, leading to the sulfheme structure.
{"title":"Mechanistics of pH-Dependent Sulfmyoglobin Formation: Spin Control and His64 Proton Relay","authors":"Angel D. Rodriguez-Mackenzie, Lysmarie Santos-Velazquez, Héctor D. Arbelo-Lopez, Troy Wymore, Juan Lopez-Garriga","doi":"10.1155/2024/4244579","DOIUrl":"https://doi.org/10.1155/2024/4244579","url":null,"abstract":"The chemistry of hydrogen sulfide (H<sub>2</sub>S) has been directed towards physiologically relevant hemeproteins, including myoglobin, hemoglobin, and other similar proteins. Despite substantial efforts, there remains a need to elucidate the mechanism and identify the species involved in the reaction between oxy-hemeproteins and H<sub>2</sub>S. Here, we summarize both our experimental data and computational modeling results revealing the mechanisms by which sulfmyoglobin (sulfMb) and sulfhemoglobin (sulfHb) are formed. Our experimental data at pH 7.4 reveal differences in intensity between sulfMb and sulfHb chromophores in the 620 nm charge transfer region. This behavior could be attributed to the incomplete reaction of tetrameric oxy-Hb with H<sub>2</sub>S, where not all heme groups form sulfheme. The data also show that, for the reaction of oxy-myoglobin (oxy-Mb) and H<sub>2</sub>S, the 622 nm charge transfer band increases in intensity from a pH of 6.6 to 5.0. This increase is attributed to the presence of the heme pocket distal His64<sub><i>εδ</i></sub>, which is positively charged, resulting in an elevated yield of sulfMb formation compared to the mono-protonated tautomer, His64<i>ε</i>. Computational hybrid QM/MM methods support the conclusion, indicating that oxy-Mb His64<sub><i>εδ</i></sub> (pH 5.0) reacts with H<sub>2</sub>S in the triplet state, favored by −31.0 kcal/mol over the singlet His64<i>ε</i> (pH 6.6) species. The phenomenon is facilitated by a hydrogen bonding network within the heme pocket, between His64<sub><i>εδ</i></sub>, heme Fe(II)O<sub>2</sub>, and H<sub>2</sub>S. The results establish an energetically favored quantitative mechanism to produce sulfMb (−69.1 kcal/mol) from the reactions of oxy-Mb and H<sub>2</sub>S. Curiously, the mechanism between met-aquo Mb, H<sub>2</sub>O<sub>2</sub>, and H<sub>2</sub>S shows similar reaction pathways and leads to sulfheme formation (−135.3 kcal/mol). The energetic barrier towards intermediate Cpd-0 is the limiting step in sulfheme formation for both systems. Both mechanisms show that the thiyl radical, HS<sup>•</sup>, is the species attacking the <i>β</i>-<i>β</i> double bond of heme pyrrole B, leading to the sulfheme structure.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"134 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139927517","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Min Ji Kim, Hwi-Ho Lee, Choi Kim, Ja Yeon Lee, Kyung-Sook Chung, Kyung-Tae Lee, Jae Yeol Lee
Endogenous prostaglandin E2 (PGE2) plays an important role in maintaining the homeostasis conditions. However, the overexpression of PGE2 in response to various inflammatory stimulations is an important target of anti-inflammatory drugs. Both inducible COX-2 (cyclooxygenase-2) and mPGES-1 (microsomal prostaglandin E2 synthase-1) enzymes are responsible for the inflammatory overexpressed PGE2 production. Among them, mPGES-1 is regarded as a more promising ideal target for anti-inflammatory drugs without the gastrointestinal and cardiovascular side effects. As our continuous research for the discovery of novel mPGES-1 inhibitors, we have characterized MPO-0144 as a selective mPGES-1 inhibitor with a selectivity index of >270 over COX-1 and >25 over COX-2, respectively. Herein, we evaluated the anti-inflammatory effect of MPO-0144 in an adjuvant-induced arthritis rat model. MPO-0144 attenuated the inflammatory responses without severe gastrointestinal side effects and organ toxicities. These overall data suggest a possibility that MPO-0144 downregulates PGE2 production by potent mPGES-1 and weak COX-2 inhibitory activities, thus attenuating the paw swelling in AIA (adjuvant-induced arthritis) rat models. MPO-0144 also exhibited favorable ADMET profiles. However, MPO-0144 did not show any inhibitory effects on human mPGES-1 enzyme at a high concentration. Therefore, MPO-0144 represents a valuable pharmacological tool for the study of regulation of inducible mPGES-1 in an inflammatory arthritis rat model.
{"title":"Selective mPGES-1 Inhibitor Ameliorated Adjuvant-Induced Arthritis in the Rat Model","authors":"Min Ji Kim, Hwi-Ho Lee, Choi Kim, Ja Yeon Lee, Kyung-Sook Chung, Kyung-Tae Lee, Jae Yeol Lee","doi":"10.1155/2024/5531519","DOIUrl":"https://doi.org/10.1155/2024/5531519","url":null,"abstract":"Endogenous prostaglandin E<sub>2</sub> (PGE<sub>2</sub>) plays an important role in maintaining the homeostasis conditions. However, the overexpression of PGE<sub>2</sub> in response to various inflammatory stimulations is an important target of anti-inflammatory drugs. Both inducible COX-2 (cyclooxygenase-2) and mPGES-1 (microsomal prostaglandin E<sub>2</sub> synthase-1) enzymes are responsible for the inflammatory overexpressed PGE<sub>2</sub> production. Among them, mPGES-1 is regarded as a more promising ideal target for anti-inflammatory drugs without the gastrointestinal and cardiovascular side effects. As our continuous research for the discovery of novel mPGES-1 inhibitors, we have characterized MPO-0144 as a selective mPGES-1 inhibitor with a selectivity index of >270 over COX-1 and >25 over COX-2, respectively. Herein, we evaluated the anti-inflammatory effect of MPO-0144 in an adjuvant-induced arthritis rat model. MPO-0144 attenuated the inflammatory responses without severe gastrointestinal side effects and organ toxicities. These overall data suggest a possibility that MPO-0144 downregulates PGE<sub>2</sub> production by potent mPGES-1 and weak COX-2 inhibitory activities, thus attenuating the paw swelling in AIA (adjuvant-induced arthritis) rat models. MPO-0144 also exhibited favorable ADMET profiles. However, MPO-0144 did not show any inhibitory effects on human mPGES-1 enzyme at a high concentration. Therefore, MPO-0144 represents a valuable pharmacological tool for the study of regulation of inducible mPGES-1 in an inflammatory arthritis rat model.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"30 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139768183","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abraham Dilnesa Gashaw, Kibrom Gebreheiwot Bedane, Taye B. Demissie, Japheth O. Ombito, Estifanos Ele Yaya, Mekonnen Abebayehu Desta
Myricasalicifolia A Rich (Myricaceae) is a tree growing in Central and East Africa. Traditionally, the plant is used to treat malaria, respiratory disorders, inflammations, and infections. A new compound, 3β-O-trans-caffeoylisomyricadiol (7), was isolated from MeOH : CHCl3 (2 : 1) extract of the stem bark of Myrica salicifolia along with seven known compounds, namely, myricanone (1), myricanol (2), myricanol-11-O-β-D-xylopyranoside (3), taraxerone (4), taraxerol (5), myricadiol (6), and methyl-β-D-glucopyranoside (8). This is the first report of the isolation of taraxerene-type triterpenes from this plant. The structures were determined by a comprehensive analysis of 1D/2D NMR spectroscopy, HR-MS, and by comparison with literature data. The compounds showed a wide range of DPPH scavenging activities from very weak (IC50 value = 282.61 μM) to very strong (IC50 = 13.48 μM). Antibacterial activities of the compounds were evaluated using the disk diffusion agar method, where some of the compounds showed modest antibacterial activities against S. pyogenes and S. aureus at 250 μg/mL. Compounds 2, 3, and 7 were assessed for their in silico molecular docking analysis. The lowest binding affinity for compound 7 was found to be −7.26 to −10.35 kcal/mol against PqsA protein of P. aeruginosa, pyruvate kinase (PK) enzyme of S. aureus, LuxS protein of S. pyogenes, and DNA gyrase B of E. coli, which showed better binding affinity compared to the standard drug ampicillin (−7.36 to −8.03 kcal/mol) and ciprofloxacin (−6.19 to −6.83 kcal/mol). In silico ADMET predictions revealed that compounds 3 and 8 met all the requirements for pharmacokinetic properties.
{"title":"Antibacterial and Antioxidant Activities of Triterpenoids and Cyclic 1,7-Diarylheptanoids from the Stem Bark of Myrica salicifolia: A Combined Experimental and Computational Study","authors":"Abraham Dilnesa Gashaw, Kibrom Gebreheiwot Bedane, Taye B. Demissie, Japheth O. Ombito, Estifanos Ele Yaya, Mekonnen Abebayehu Desta","doi":"10.1155/2024/2013446","DOIUrl":"https://doi.org/10.1155/2024/2013446","url":null,"abstract":"<i>Myrica</i><i>salicifolia</i> A Rich (Myricaceae) is a tree growing in Central and East Africa. Traditionally, the plant is used to treat malaria, respiratory disorders, inflammations, and infections. A new compound, 3<i>β</i>-O-trans-caffeoylisomyricadiol (7), was isolated from MeOH : CHCl<sub>3</sub> (2 : 1) extract of the stem bark of <i>Myrica salicifolia</i> along with seven known compounds, namely, myricanone (<b>1</b>), myricanol (<b>2</b>), myricanol-11-<i>O</i>-<i>β</i>-D-xylopyranoside (<b>3</b>), taraxerone (<b>4</b>), taraxerol (<b>5</b>), myricadiol (<b>6</b>), and methyl-<i>β</i>-D-glucopyranoside (<b>8</b>). This is the first report of the isolation of taraxerene-type triterpenes from this plant. The structures were determined by a comprehensive analysis of 1D/2D NMR spectroscopy, HR-MS, and by comparison with literature data. The compounds showed a wide range of DPPH scavenging activities from very weak (IC<sub>50</sub> value = 282.61 <i>μ</i>M) to very strong (IC<sub>50</sub> = 13.48 <i>μ</i>M). Antibacterial activities of the compounds were evaluated using the disk diffusion agar method, where some of the compounds showed modest antibacterial activities against <i>S. pyogenes</i> and <i>S. aureus</i> at 250 <i>μ</i>g/mL. Compounds <b>2</b>, <b>3</b>, and <b>7</b> were assessed for their <i>in silico</i> molecular docking analysis. The lowest binding affinity for compound <b>7</b> was found to be −7.26 to −10.35 kcal/mol against PqsA protein of <i>P. aeruginosa</i>, pyruvate kinase (PK) enzyme of <i>S</i>. <i>aureus</i>, LuxS protein of <i>S. pyogenes</i>, and DNA gyrase B of <i>E.</i> coli, which showed better binding affinity compared to the standard drug ampicillin (−7.36 to −8.03 kcal/mol) and ciprofloxacin (−6.19 to −6.83 kcal/mol). <i>In silico</i> ADMET predictions revealed that compounds <b>3</b> and <b>8</b> met all the requirements for pharmacokinetic properties.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"5 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139768184","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wayne C. Liao, Collin S. Liao, Yu-Chen Lin, Ching-Yi Lien
Gold nanoparticles have been used as drug carriers and imaging reagents. The plant extract-capped gold nanoparticles provide better properties than chemically synthesized gold nanoparticles. In this study, Zingiber zerumbet extract-mediated green production of gold nanoparticles (Z. zerumbet@Au NPs) was established. Based on the UV-visible spectroscopy and transmission electron microscope (TEM) results, most Z. zerumbet@Au NPs were spherical. When more Z. zerumbet extracts were added, more spherical nanoparticles were formed. The hydrodynamic size changed slightly along with time, and the average size was approximately 170 nm. Capping of Z. zerumbet extract on the surface of gold nanoparticles was confirmed by Fourier transform infrared spectroscopy (FTIR). In general, phenolic compounds or flavonoid compounds were considered to be the reducing agent. However, zerumbone was identified as the reducing agent in this study. The resulting oxidized products were characterized by high-performance liquid chromatography-mass spectrometry (HPLC-MS). As a result, the solvent was proven to be involved in nanoparticle synthesis. Overall, Z zerumbet@Au NPs showed great potential to be used in cosmetic- or biomedicine-related fields.
{"title":"Characterization of Gold Nanoparticles Synthesized with Zingiber zerumbet Extracts","authors":"Wayne C. Liao, Collin S. Liao, Yu-Chen Lin, Ching-Yi Lien","doi":"10.1155/2024/1358495","DOIUrl":"https://doi.org/10.1155/2024/1358495","url":null,"abstract":"Gold nanoparticles have been used as drug carriers and imaging reagents. The plant extract-capped gold nanoparticles provide better properties than chemically synthesized gold nanoparticles. In this study, <i>Zingiber zerumbet </i>extract-mediated green production of gold nanoparticles (Z. <i>zerumbet</i>@Au NPs) was established. Based on the UV-visible spectroscopy and transmission electron microscope (TEM) results, most <i>Z. zerumbet</i>@Au NPs were spherical. When more <i>Z. zerumbet</i> extracts were added, more spherical nanoparticles were formed. The hydrodynamic size changed slightly along with time, and the average size was approximately 170 nm. Capping of <i>Z. zerumbet</i> extract on the surface of gold nanoparticles was confirmed by Fourier transform infrared spectroscopy (FTIR). In general, phenolic compounds or flavonoid compounds were considered to be the reducing agent. However, zerumbone was identified as the reducing agent in this study. The resulting oxidized products were characterized by high-performance liquid chromatography-mass spectrometry (HPLC-MS). As a result, the solvent was proven to be involved in nanoparticle synthesis. Overall, Z zerumbet@Au NPs showed great potential to be used in cosmetic- or biomedicine-related fields.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"37 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139768182","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Anoud Saud Alshammari, Ghada Mohamed Aleid, Alamri Rahmah Dhahawi Ahmad, Asma D. Alomari, Shehu Sa’ad Abdullahi, Rania Edrees Adam Mohammad
Microbial fuel cell (MFC) is a new and interesting technology that can be used to treat wastewater without using electricity. The current research focuses on electron generation, which is one of the technique’s major challenges. According to the latest literature, the study was planned to successfully remove the metals from artificial wastewater at high concentrations and generate electricity. On average, after 18 days of operation, it offered 610 mV with 1000 ῼ constant external resistance. The internal resistance was found to be 520 ῼ. The achieved power density was 3.164 mW/m2 at an external resistance of 1000 ῼ. The achieved removal efficiencies of Pb2+, Cd2+, Cr3+, and Ni2+ were 83.67%, 84.10%, 84.55%, and 95.99%, respectively. The operation lasted for 25 days. The cyclic voltameter studies show that there is a gradual oxidation rate of organic substances, while on day 25, the removal efficiency reached its maximum. The specific capacitance was found to be high between days 15 and 20, i.e., 0.0000540 F/g. It also indicated that biofilm was stable around day 18. Furthermore, the biological characterization also demonstrated that MFC operation was very smooth throughout the process, even at high concentrations (100 mg/L) of metal ions. Finally, there is the MFC method, as well as some new challenges and future recommendations.
{"title":"Oil Palm Biomass Sap-Rotten Rice as a Source to Remove Metal Ions and Generate Electricity as By-Products through Microbial Fuel Cell Technology","authors":"Anoud Saud Alshammari, Ghada Mohamed Aleid, Alamri Rahmah Dhahawi Ahmad, Asma D. Alomari, Shehu Sa’ad Abdullahi, Rania Edrees Adam Mohammad","doi":"10.1155/2024/5570011","DOIUrl":"https://doi.org/10.1155/2024/5570011","url":null,"abstract":"Microbial fuel cell (MFC) is a new and interesting technology that can be used to treat wastewater without using electricity. The current research focuses on electron generation, which is one of the technique’s major challenges. According to the latest literature, the study was planned to successfully remove the metals from artificial wastewater at high concentrations and generate electricity. On average, after 18 days of operation, it offered 610 mV with 1000 ῼ constant external resistance. The internal resistance was found to be 520 ῼ. The achieved power density was 3.164 mW/m<sup>2</sup> at an external resistance of 1000 ῼ. The achieved removal efficiencies of Pb<sup>2+</sup>, Cd<sup>2+</sup>, Cr<sup>3+</sup>, and Ni<sup>2+</sup> were 83.67%, 84.10%, 84.55%, and 95.99%, respectively. The operation lasted for 25 days. The cyclic voltameter studies show that there is a gradual oxidation rate of organic substances, while on day 25, the removal efficiency reached its maximum. The specific capacitance was found to be high between days 15 and 20, i.e., 0.0000540 F/g. It also indicated that biofilm was stable around day 18. Furthermore, the biological characterization also demonstrated that MFC operation was very smooth throughout the process, even at high concentrations (100 mg/L) of metal ions. Finally, there is the MFC method, as well as some new challenges and future recommendations.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"19 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139768181","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
N, N-disubstituted glycosylated ureas have been synthesized in good-to-excellent yields by 1,4-conjugate addition of amines to glycosylated olefinic esters followed by reaction of resulting glycosyl β-amino esters with diisocyanates. The developed sugar-based molecules were well characterized by extensive standard spectroscopic analysis including NMR (1H, 13C, and DEPT), IR, MS, and elemental analysis and were screened for their biological activity against Mycobacterium tuberculosis (M. Tb.), where some of them displayed potent antitubercular activity. The molecules have been designed keeping in view the well-known inhibitors of the enzymes involved in the biosynthesis of mycobacterial cell wall polymers and may be further explored as lead molecules for the successful development of a potential antitubercular drug candidate.
{"title":"Synthesis and Antitubercular Evaluation of Diverse Glycosylated Ureas from D-Glucose","authors":"Neetu Tripathi, Vinod K. Tiwari","doi":"10.1155/2024/8709672","DOIUrl":"https://doi.org/10.1155/2024/8709672","url":null,"abstract":"<i>N</i>, <i>N</i>-disubstituted glycosylated ureas have been synthesized in good-to-excellent yields by 1,4-conjugate addition of amines to glycosylated olefinic esters followed by reaction of resulting glycosyl <i>β</i>-amino esters with diisocyanates. The developed sugar-based molecules were well characterized by extensive standard spectroscopic analysis including NMR (<sup>1</sup>H, <sup>13</sup>C, and DEPT), IR, MS, and elemental analysis and were screened for their biological activity against <i>Mycobacterium tuberculosis</i> (<i>M. Tb.</i>), where some of them displayed potent antitubercular activity. The molecules have been designed keeping in view the well-known inhibitors of the enzymes involved in the biosynthesis of mycobacterial cell wall polymers and may be further explored as lead molecules for the successful development of a potential antitubercular drug candidate.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"22 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139668752","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ni’meh Al-Shami, Hani Naseef, Ramzi Moqadi, Feras Kanaze
A simple, fast, and accurate high-performance liquid chromatographic (HPLC) method is developed, optimized, and validated for a fixed-dose combination of apixaban (APX) and clopidogrel (CLOP) tablets according to ICH guidelines. Chromatographic separation of the drugs was performed on a BDS Hypersil C18 (4.6 150 mm, 5 μm), with acetonitrile (ACN) and trifluoroacetic acid (TFA) in the ratio 48 : 52 (v/v) as a mobile phase, at a flow rate of 0.9 ml/min., injection volume of 5 μL, and column temperature 45°C. The proposed method was linear over the level 25–200% for a concentration of APX 5 μg/ml and CLOP 75 μg/ml (R2 > 0.999). The detection limit for APX and CLOP was found to be 0.3465 and 3.8496 μg/ml, whereas the quantification limit was 1.0499 and 11.6656 μg/ml, respectively. The recovery was more than 99% using the standard addition method. The developed method was found to be specific, accurate, precise, and robust against changes in column temperature (±5°C) and mobile phase composition (±5% ACN); hence, it can be used for the determination of APX and CLOP in the fixed-dose combination tablets.
{"title":"HPLC Method Development and Validation for the Determination of Apixaban and Clopidogrel in Novel Fixed-Dose Combination Tablets","authors":"Ni’meh Al-Shami, Hani Naseef, Ramzi Moqadi, Feras Kanaze","doi":"10.1155/2024/2675736","DOIUrl":"https://doi.org/10.1155/2024/2675736","url":null,"abstract":"A simple, fast, and accurate high-performance liquid chromatographic (HPLC) method is developed, optimized, and validated for a fixed-dose combination of apixaban (APX) and clopidogrel (CLOP) tablets according to ICH guidelines. Chromatographic separation of the drugs was performed on a BDS Hypersil C<sub>18</sub> (4.6 <svg height=\"6.01072pt\" style=\"vertical-align:-0.04980993pt\" version=\"1.1\" viewbox=\"-0.0498162 -5.96091 7.75925 6.01072\" width=\"7.75925pt\" xmlns=\"http://www.w3.org/2000/svg\" xmlns:xlink=\"http://www.w3.org/1999/xlink\"><g transform=\"matrix(.013,0,0,-0.013,0,0)\"></path></g></svg> 150 mm, 5 <i>μ</i>m), with acetonitrile (ACN) and trifluoroacetic acid (TFA) in the ratio 48 : 52 (v/v) as a mobile phase, at a flow rate of 0.9 ml/min., injection volume of 5 <i>μ</i>L, and column temperature 45°C. The proposed method was linear over the level 25–200% for a concentration of APX 5 <i>μ</i>g/ml and CLOP 75 <i>μ</i>g/ml (<i>R</i><sup>2</sup> > 0.999). The detection limit for APX and CLOP was found to be 0.3465 and 3.8496 <i>μ</i>g/ml, whereas the quantification limit was 1.0499 and 11.6656 <i>μ</i>g/ml, respectively. The recovery was more than 99% using the standard addition method. The developed method was found to be specific, accurate, precise, and robust against changes in column temperature (±5°C) and mobile phase composition (±5% ACN); hence, it can be used for the determination of APX and CLOP in the fixed-dose combination tablets.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"54 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139561780","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yang Xu, Xianwen Yue, Jihong Chi, Huailei Yang, Ying Wang, Yongsheng Wang, Peng Yu, Huiwei Bao
Oviductus Ranae (OR) is one of the “treasures of Changbai Mountain” in China. It is used clinically for the treatment of infirmity after illness, fatigued spirit, cough, hemoptysis, and so forth. In this study, a simple and sensitive high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed for the simultaneous determination of five main effective components (1-methyl hydantoin, estradiol, cholesterol, 7-keto-cholesterol, and 4-cholesten-3-one) in OR and its different processed products. The results indicated that these five components showed good linear relationships within their own concentration ranges along with coefficients of determination ≥0.9996. Average recoveries ranged from 97.67% to 100.06%, with RSDs of 1.45%–1.99%. The proposed method was found to be simple, accurate, and stable, which provided an effective analytical method for quality control and evaluation of OR and its different processed products.
乌药是中国 "长白山瑰宝 "之一。临床用于治疗病后体虚、神疲乏力、咳嗽、咯血等症。本研究建立了一种简便灵敏的高效液相色谱-二极管阵列检测器（HPLC-DAD）方法，用于同时测定 OR 及其不同加工品中的五种主要有效成分（1-甲基海因、雌二醇、胆固醇、7-酮基胆固醇和 4-胆甾烯-3-酮）。结果表明，这五种成分在各自的浓度范围内呈良好的线性关系，测定系数≥0.9996。平均回收率为 97.67% 至 100.06%，RSD 为 1.45% 至 1.99%。该方法简便、准确、稳定，为 OR 及其不同加工产品的质量控制和评价提供了一种有效的分析方法。
{"title":"Analysis of the Influence of Different Processing Methods on the Main Effective Components in Oviductus Ranae by High-Performance Liquid Chromatography with Diode Array Detector","authors":"Yang Xu, Xianwen Yue, Jihong Chi, Huailei Yang, Ying Wang, Yongsheng Wang, Peng Yu, Huiwei Bao","doi":"10.1155/2024/3524367","DOIUrl":"https://doi.org/10.1155/2024/3524367","url":null,"abstract":"<i>Oviductus Ranae</i> (OR) is one of the “treasures of Changbai Mountain” in China. It is used clinically for the treatment of infirmity after illness, fatigued spirit, cough, hemoptysis, and so forth. In this study, a simple and sensitive high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed for the simultaneous determination of five main effective components (1-methyl hydantoin, estradiol, cholesterol, 7-keto-cholesterol, and 4-cholesten-3-one) in OR and its different processed products. The results indicated that these five components showed good linear relationships within their own concentration ranges along with coefficients of determination ≥0.9996. Average recoveries ranged from 97.67% to 100.06%, with RSDs of 1.45%–1.99%. The proposed method was found to be simple, accurate, and stable, which provided an effective analytical method for quality control and evaluation of OR and its different processed products.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"33 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139561629","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Uzma Jehangir, Shoaib Khan, Rafaqat Hussain, Yousaf Khan, Farhan Ali, Asma Sardar, Samina Aslam, Mozhgan Afshari
It is well recognized that heterocyclic compounds have exceptional biomedical applications, which has led scientists to become increasingly interested in their use in this field in the recent past. It is the aim of this study, using a multistep method based on thiazolidinone derivative synthesis, to synthesize thiazolidinone derivatives derived from pyrazine molecules (1–12). As a result of analyzing 1H-NMR, 13C-NMR, and HREI-MS data, the structures of these derivatives were determined. The minimum inhibitory concentration (MIC) of these drugs was also determined alongside the donepezil (IC50 = 10.10 ± 0.10 µM) to determine their potential as anti-Alzheimer agents. Among the screened derivatives, 1 (IC50 = 4.10 ± 0.20 µM), 2 (IC50 = 2.20 ± 0.20 µM), 4 (IC50 = 2.30 ± 0.20 µM), 5 (IC50 = 5.80 ± 0.30 µM), 6 (IC50 = 6.30 ± 0.20 µM), 8 (IC50 = 5.20 ± 0.10 µM), 9 (IC50 = 5.20 ± 0.40 µM), 10 (IC50 = 8.30 ± 0.40 µM), and 11 (IC50 = 8.10 ± 0.70 µM) showed potent activity. In addition, the synthesized moieties were screened against E. coli to determine whether there were any antimicrobial properties. It was found that most of the compounds were more potent inhibitors of bacterial growth in comparison to streptomycin, the reference drug. There have been several molecular docking experiments conducted to gain a deeper understanding of how these compounds interact with the active sites of enzymes to gain a greater understanding of their functional mechanisms.
{"title":"Development of Thiazolidinone-Based Pyrazine Derivatives: Synthesis, Molecular Docking Simulation, and Bioevaluation for Anti-Alzheimer and Antibacterial Activities","authors":"Uzma Jehangir, Shoaib Khan, Rafaqat Hussain, Yousaf Khan, Farhan Ali, Asma Sardar, Samina Aslam, Mozhgan Afshari","doi":"10.1155/2024/8426930","DOIUrl":"https://doi.org/10.1155/2024/8426930","url":null,"abstract":"It is well recognized that heterocyclic compounds have exceptional biomedical applications, which has led scientists to become increasingly interested in their use in this field in the recent past. It is the aim of this study, using a multistep method based on thiazolidinone derivative synthesis, to synthesize thiazolidinone derivatives derived from pyrazine molecules (<b>1</b>–<b>12</b>). As a result of analyzing 1H-NMR, 13C-NMR, and HREI-MS data, the structures of these derivatives were determined. The minimum inhibitory concentration (MIC) of these drugs was also determined alongside the donepezil (IC<sub>50</sub> = 10.10 ± 0.10 <i>µ</i>M) to determine their potential as anti-Alzheimer agents. Among the screened derivatives, <b>1</b> (IC<sub>50</sub> = 4.10 ± 0.20 <i>µ</i>M), <b>2</b> (IC<sub>50</sub> = 2.20 ± 0.20 <i>µ</i>M)<b>, 4</b> (IC<sub>50</sub> = 2.30 ± 0.20 <i>µ</i>M), <b>5</b> (IC<sub>50</sub> = 5.80 ± 0.30 <i>µ</i>M), <b>6</b> (IC<sub>50</sub> = 6.30 ± 0.20 <i>µ</i>M), <b>8</b> (IC<sub>50</sub> = 5.20 ± 0.10 <i>µ</i>M), <b>9</b> (IC<sub>50</sub> = 5.20 ± 0.40 <i>µ</i>M), <b>10</b> (IC<sub>50</sub> = 8.30 ± 0.40 <i>µ</i>M), and <b>11</b> (IC<sub>50</sub> = 8.10 ± 0.70 <i>µ</i>M) showed potent activity. In addition, the synthesized moieties were screened against <i>E. coli</i> to determine whether there were any antimicrobial properties. It was found that most of the compounds were more potent inhibitors of bacterial growth in comparison to streptomycin, the reference drug. There have been several molecular docking experiments conducted to gain a deeper understanding of how these compounds interact with the active sites of enzymes to gain a greater understanding of their functional mechanisms.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"10 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139516606","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chunyan Yu, Meiling Pu, Qiuyang Chen, Shitao Yu, Lu Li
As a biological macromolecule, silk fibroin (SF) has great application potential in anticoagulant. However, its complex molecular structure leads to its poor solubility, which limits the application of SF. In this study, a novel SF film with strong anticoagulant properties was fabricated through the synergistic effect of LiBr deep eutectic solvents (DESs) and UV-light irradiation. Under the optimum conditions, the plasma recalcification time of SF film was 182 s, the hemolysis rate was 3.93%, and the dynamic coagulation time remained at a high level up to 60 min. The synergistic effect of UV-light and DES can promote the enhancement of hydrophilicity and the decrease of surface roughness of SF films, and thus the anticoagulant properties of the films were enhanced. The structure change, wettability, and roughness of SF films were characterized by XRD, FTIR, contact angle, and AFM. In the meantime, the wavelength of the UV-light and the irradiation time have an effect on the anticoagulant properties of the SF films. Furthermore, the improvement of the anticoagulant properties of SF films exhibits good universality for different LiBr DESs. The study provides a new direction for the preparation of strong anticoagulation SF films, as well as its application in life sciences.
作为一种生物大分子，蚕丝纤维素（SF）在抗凝剂方面具有巨大的应用潜力。然而，其复杂的分子结构导致其溶解性较差，从而限制了 SF 的应用。本研究通过硼酸锂深共晶溶剂（DESs）和紫外光照射的协同作用，制备了一种具有强抗凝血性能的新型 SF 薄膜。在最佳条件下，SF 薄膜的等离子体再钙化时间为 182 秒，溶血率为 3.93%，动态凝固时间保持在较高水平，最长可达 60 分钟。紫外光和 DES 的协同作用可促进 SF 薄膜亲水性的增强和表面粗糙度的降低，从而增强薄膜的抗凝特性。通过 XRD、傅立叶变换红外光谱、接触角和原子力显微镜对 SF 薄膜的结构变化、润湿性和粗糙度进行了表征。同时，紫外光的波长和照射时间对 SF 薄膜的抗凝特性也有影响。此外，对于不同的硼酸锂 DESs，SF 膜抗凝性能的改善表现出良好的普遍性。该研究为强抗凝 SF 膜的制备及其在生命科学领域的应用提供了新的方向。
{"title":"Fabrication of Silk Fibroin Film with Strong Anticoagulant Property from the Synergy of Deep Eutectic Solvents and UV-Light Irradiation","authors":"Chunyan Yu, Meiling Pu, Qiuyang Chen, Shitao Yu, Lu Li","doi":"10.1155/2024/5580782","DOIUrl":"https://doi.org/10.1155/2024/5580782","url":null,"abstract":"As a biological macromolecule, silk fibroin (SF) has great application potential in anticoagulant. However, its complex molecular structure leads to its poor solubility, which limits the application of SF. In this study, a novel SF film with strong anticoagulant properties was fabricated through the synergistic effect of LiBr deep eutectic solvents (DESs) and UV-light irradiation. Under the optimum conditions, the plasma recalcification time of SF film was 182 s, the hemolysis rate was 3.93%, and the dynamic coagulation time remained at a high level up to 60 min. The synergistic effect of UV-light and DES can promote the enhancement of hydrophilicity and the decrease of surface roughness of SF films, and thus the anticoagulant properties of the films were enhanced. The structure change, wettability, and roughness of SF films were characterized by XRD, FTIR, contact angle, and AFM. In the meantime, the wavelength of the UV-light and the irradiation time have an effect on the anticoagulant properties of the SF films. Furthermore, the improvement of the anticoagulant properties of SF films exhibits good universality for different LiBr DESs. The study provides a new direction for the preparation of strong anticoagulation SF films, as well as its application in life sciences.","PeriodicalId":15348,"journal":{"name":"Journal of Chemistry","volume":"32 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139516594","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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