Addressing the challenges of tuberculosis drug detection, this study investigates the application of copper(II) oxide modified screen-printed carbon electrodes (CuO/SPCEs) for the electrochemical detection of rifampicin, a critical drug in the treatment of tuberculosis and mycobacterial infections. The CuO/SPCE was fabricated via a constant potential electrodeposition technique and characterized using voltammetry. The bare SPCE surface exhibited a rough, porous structure, whereas the electrodeposition of CuO resulted in a smoother CuO/SPCE surface. The sensor exhibited high sensitivity with a detection limit of 2.89 μM for rifampicin and demonstrated excellent stability with a relative standard deviation of 3.5% over 10 measurements. The reproducibility was confirmed with an RSD of 4.2% across different electrodes. It also showed a linear response to rifampicin concentrations ranging from 10 to 200 μM. The real sample analysis showed a linear relationship between rifampicin concentration and peak current (I = 0.739 + 0.008 c), with a high correlation coefficient (R2 = 0.995). This electrochemical sensor’s simplicity, cost-effectiveness, and rapid response make it a promising tool for point-of-care applications in tuberculosis management.
{"title":"Copper(II) oxide-modified screen-printed carbon electrode for electrochemical detection of tuberculosis and mycobacterial infections treating drugs: rifampicin","authors":"Shengzhou Qiu, Chenxi Wu, Sima Akter, Shaoli Hong, Huihong Liu, Sakil Mahmud","doi":"10.1007/s00706-024-03251-y","DOIUrl":"https://doi.org/10.1007/s00706-024-03251-y","url":null,"abstract":"<p>Addressing the challenges of tuberculosis drug detection, this study investigates the application of copper(II) oxide modified screen-printed carbon electrodes (CuO/SPCEs) for the electrochemical detection of rifampicin, a critical drug in the treatment of tuberculosis and mycobacterial infections. The CuO/SPCE was fabricated via a constant potential electrodeposition technique and characterized using voltammetry. The bare SPCE surface exhibited a rough, porous structure, whereas the electrodeposition of CuO resulted in a smoother CuO/SPCE surface. The sensor exhibited high sensitivity with a detection limit of 2.89 μM for rifampicin and demonstrated excellent stability with a relative standard deviation of 3.5% over 10 measurements. The reproducibility was confirmed with an RSD of 4.2% across different electrodes. It also showed a linear response to rifampicin concentrations ranging from 10 to 200 μM. The real sample analysis showed a linear relationship between rifampicin concentration and peak current (<i>I</i> = 0.739 + 0.008 <i>c</i>), with a high correlation coefficient (<i>R</i><sup>2</sup> = 0.995). This electrochemical sensor’s simplicity, cost-effectiveness, and rapid response make it a promising tool for point-of-care applications in tuberculosis management.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"32 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142186823","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 : 2024-08-24DOI: 10.1007/s00706-024-03250-z
Reem A. K. Al-Harbi
The reaction of 2-(trifluoromethyl)-3,1-benzoxazone with amines was studied. At first, when one mole equivalent of 2-(trifluoromethyl)-3,1-benzoxazone was treated with one mole equivalent of phenylenediamine afforded bis-benzamide derivatives rather than 3-(aminophenyl)quinazolinone derivatives. Many trials to obtain the 3-(aminophenyl)quinazolinones were carried out, and the final result is that it is difficult to obtain the 3-(aminophenyl)quinazolinones in acceptable yield and purity from the reaction of phenylenediamine with 2-(trifluoromethyl)-benzoxazinone. The synthesis of new 6-iodo-3-substituted-2-(trifluoromethyl)quinazolin-4(3H)-one derivatives was studied as follows: when the 6-iodo-2-(trifluoromethyl)-3,1-benzoxazin-4-one was fused with some amines at 140 °C for 10 min, it afforded 5-iodo-N-(methyl and aryl)-2-(trifluoroacetamido)benzamide derivatives. While, when 6-iodo-2-(trifluoromethyl)-3,1-benzoxazinone was condensed with the same amines in acetic acid under reflux conditions, it afforded 6-iodo-3-(methyl and aryl)-2-(trifluoromethyl)quinazolin-4(3H)-one derivatives. Condensation of the 6-iodo-2-(trifluoromethyl)-3,1-benzoxazinone with hydrazine hydrate gave 3-amino-6-iodo-2-(trifluoromethyl)quinazolinone. Condensation of the latter 3-aminoquinazolinone with some aldehydes and isatin afforded the corresponding Schiff's bases. The expected antimicrobial properties of the synthesized compounds were investigated. Most of the compounds showed moderate effects on some bacteria. Most compounds had no effects on fungi. Schiff's base of isatin showed the best results among all the tested compounds. The latter Schiff's base showed potent activity, like ketoconazole toward fungi.
{"title":"Synthesis and antimicrobial activity of 6-iodo-2-(trifluoromethyl)-4(3H)-quinazolinone derivatives","authors":"Reem A. K. Al-Harbi","doi":"10.1007/s00706-024-03250-z","DOIUrl":"https://doi.org/10.1007/s00706-024-03250-z","url":null,"abstract":"<p>The reaction of 2-(trifluoromethyl)-3,1-benzoxazone with amines was studied. At first, when one mole equivalent of 2-(trifluoromethyl)-3,1-benzoxazone was treated with one mole equivalent of phenylenediamine afforded bis-benzamide derivatives rather than 3-(aminophenyl)quinazolinone derivatives. Many trials to obtain the 3-(aminophenyl)quinazolinones were carried out, and the final result is that it is difficult to obtain the 3-(aminophenyl)quinazolinones in acceptable yield and purity from the reaction of phenylenediamine with 2-(trifluoromethyl)-benzoxazinone. The synthesis of new 6-iodo-3-substituted-2-(trifluoromethyl)quinazolin-4(3<i>H</i>)-one derivatives was studied as follows: when the 6-iodo-2-(trifluoromethyl)-3,1-benzoxazin-4-one was fused with some amines at 140 °C for 10 min, it afforded 5-iodo-<i>N</i>-(methyl and aryl)-2-(trifluoroacetamido)benzamide derivatives. While, when 6-iodo-2-(trifluoromethyl)-3,1-benzoxazinone was condensed with the same amines in acetic acid under reflux conditions, it afforded 6-iodo-3-(methyl and aryl)-2-(trifluoromethyl)quinazolin-4(3<i>H</i>)-one derivatives. Condensation of the 6-iodo-2-(trifluoromethyl)-3,1-benzoxazinone with hydrazine hydrate gave 3-amino-6-iodo-2-(trifluoromethyl)quinazolinone. Condensation of the latter 3-aminoquinazolinone with some aldehydes and isatin afforded the corresponding Schiff's bases. The expected antimicrobial properties of the synthesized compounds were investigated. Most of the compounds showed moderate effects on some bacteria. Most compounds had no effects on fungi. Schiff's base of isatin showed the best results among all the tested compounds. The latter Schiff's base showed potent activity, like ketoconazole toward fungi.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"58 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142186824","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 : 2024-08-13DOI: 10.1007/s00706-024-03246-9
Radek Chalupa, Karel Nesměrák
Although artificial intelligence (AI) has been used in chemistry, more or less covertly, for many decades (databases for data management, programs for designing synthesis, toxicological expert systems, etc.), the massive emergence of user-friendly artificial intelligence presents an interesting opportunity and challenge for chemists to improve the communication power of chemistry and its position in society. Although repeatedly questioned by many critics per se value-neutral generative AI stands a good chance of becoming an important tool for presenting chemical information throughout all strata of society. Additionally, it can support the spread of science-based opinions on chemistry to the public and help popularize science in general as well. AI allows virtually every scientist to become a major player in science communication. This could lead to a containment of chemophobia. However, the use of AI as a communication tool requires continuous education, personal development and training of those who use it, in this case chemists and scientists in general. They will play a crucial role as arbiters of the appropriateness, adequacy and factual accuracy of the content generated by generative AI. The democratization of communication made possible by generative AI entails the need to adapt the dialogue to the communication preferences, demography and education of the interlocutors. Thus, generative AI empowers both those who enter the prompts and those who receive the subsequent results. Most scientists do not realize it, but generative AI puts the public, not scientists, at the center of communication. It is important to recognize this and use generative AI to target communication, education, and overall community development. The clash of narratives that may be a natural consequence of the growing number of generative AI users and the increasing amount of content being created may, perhaps unexpectedly for many, lead to the opposite result – a new Enlightenment. Either way, chemists would do well to be there; for their ability to understand the laws of matter, the beginning and end of things; for the dual nature of chemistry as an art and a science.
{"title":"Chemophobia and AI: artificial intelligence as a possible solution in the forthcoming clash of narratives","authors":"Radek Chalupa, Karel Nesměrák","doi":"10.1007/s00706-024-03246-9","DOIUrl":"https://doi.org/10.1007/s00706-024-03246-9","url":null,"abstract":"<p>Although artificial intelligence (AI) has been used in chemistry, more or less covertly, for many decades (databases for data management, programs for designing synthesis, toxicological expert systems, etc.), the massive emergence of user-friendly artificial intelligence presents an interesting opportunity and challenge for chemists to improve the communication power of chemistry and its position in society. Although repeatedly questioned by many critics per se value-neutral generative AI stands a good chance of becoming an important tool for presenting chemical information throughout all strata of society. Additionally, it can support the spread of science-based opinions on chemistry to the public and help popularize science in general as well. AI allows virtually every scientist to become a major player in science communication. This could lead to a containment of chemophobia. However, the use of AI as a communication tool requires continuous education, personal development and training of those who use it, in this case chemists and scientists in general. They will play a crucial role as arbiters of the appropriateness, adequacy and factual accuracy of the content generated by generative AI. The democratization of communication made possible by generative AI entails the need to adapt the dialogue to the communication preferences, demography and education of the interlocutors. Thus, generative AI empowers both those who enter the prompts and those who receive the subsequent results. Most scientists do not realize it, but generative AI puts the public, not scientists, at the center of communication. It is important to recognize this and use generative AI to target communication, education, and overall community development. The clash of narratives that may be a natural consequence of the growing number of generative AI users and the increasing amount of content being created may, perhaps unexpectedly for many, lead to the opposite result – a new Enlightenment. Either way, chemists would do well to be there; for their ability to understand the laws of matter, the beginning and end of things; for the dual nature of chemistry as an art and a science.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"13 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142186827","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 : 2024-08-11DOI: 10.1007/s00706-024-03247-8
Matthias G. Käfer, Jan Pecak, Berthold Stöger, Karl Kirchner
The synthesis and characterization of two Co(II) complexes stabilized by NCN pincer ligands are described. The paramagnetic Co(II) complex [Co(κ3NCN-NCNCH2-iPr)Br] is obtained via a transmetalation protocol from CoBr2 and NC(C–Br)NCH2-iPr in THF. Surprisingly, the dinuclear complex [Co2(κ3NCN-μ2-NCNCH2-iPr)(μ-Cl)(Cl)2] was synthesized following the same synthetic protocol but using an ultrasonicated CoCl2 suspension instead of CoBr2 in the same solvent. Both complexes are paramagnetic species exhibiting solution magnetic moments of 1.9(1) and 5.8(3) μB, respectively. This corresponds to low-spin and high-spin d7 configurations featuring one and three unpaired electrons at the metal centers. X-ray structures of both complexes are presented.
{"title":"The striking influence of solubility on the nuclearity of cobalt NCN pincer complexes","authors":"Matthias G. Käfer, Jan Pecak, Berthold Stöger, Karl Kirchner","doi":"10.1007/s00706-024-03247-8","DOIUrl":"https://doi.org/10.1007/s00706-024-03247-8","url":null,"abstract":"<p>The synthesis and characterization of two Co(II) complexes stabilized by NCN pincer ligands are described. The paramagnetic Co(II) complex [Co(κ<sup>3</sup><i>NCN-</i>NCN<sup>CH2</sup>-<i>i</i>Pr)Br] is obtained via a transmetalation protocol from CoBr<sub>2</sub> and NC(C–Br)N<sup>CH2</sup>-<i>i</i>Pr in THF. Surprisingly, the dinuclear complex [Co<sub>2</sub>(κ<sup>3</sup><i>NCN</i>-μ<sub>2</sub>-NCN<sup>CH2</sup>-<i>i</i>Pr)(μ-Cl)(Cl)<sub>2</sub>] was synthesized following the same synthetic protocol but using an ultrasonicated CoCl<sub>2</sub> suspension instead of CoBr<sub>2</sub> in the same solvent. Both complexes are paramagnetic species exhibiting solution magnetic moments of 1.9(1) and 5.8(3) μ<sub>B</sub>, respectively. This corresponds to low-spin and high-spin d<sup>7</sup> configurations featuring one and three unpaired electrons at the metal centers. X-ray structures of both complexes are presented.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"3 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932464","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 : 2024-08-07DOI: 10.1007/s00706-024-03241-0
Alexandra Hadbavníková, Stanislav Musil, Jakub Hraníček, Eliška Nováková
Chemical vapor generation (CVG) of Zn was carried out in a multimode sample introduction system (MSIS) and coupled to inductively coupled plasma mass spectrometry (ICP-MS) for detection. CVG conditions were studied and 0.4% (m/v) 8-hydroxyquinoline as the reaction modifier in 0.08 mol dm–3 H2SO4 and 3.0% NaBH4 in 0.1 mol dm–3 NaOH were found optimal, providing the limits of detection and quantification of 2.8 ng cm–3 and 9.3 ng cm–3, respectively. The overall CVG efficiency of 5.3 ± 0.1% was determined from comparison with solution nebulization-ICP-MS, while 5.7 ± 0.1% was determined using 65Zn radiotracer and radiometry. The developed methodology was verified by determination of Zn in the standard reference material of fresh water (NIST 1643f). Interference study conducted with 13 hydride-forming and transition elements did not prove ability of any of the tested element to further increase the CVG efficiency, but at the same time, none of them exhibited serious interference except Ag.
{"title":"Enhancing the efficiency of chemical vapor generation of zinc in a multimode sample introduction system","authors":"Alexandra Hadbavníková, Stanislav Musil, Jakub Hraníček, Eliška Nováková","doi":"10.1007/s00706-024-03241-0","DOIUrl":"https://doi.org/10.1007/s00706-024-03241-0","url":null,"abstract":"<p>Chemical vapor generation (CVG) of Zn was carried out in a multimode sample introduction system (MSIS) and coupled to inductively coupled plasma mass spectrometry (ICP-MS) for detection. CVG conditions were studied and 0.4% (<i>m</i>/<i>v</i>) 8-hydroxyquinoline as the reaction modifier in 0.08 mol dm<sup>–3</sup> H<sub>2</sub>SO<sub>4</sub> and 3.0% NaBH<sub>4</sub> in 0.1 mol dm<sup>–3</sup> NaOH were found optimal, providing the limits of detection and quantification of 2.8 ng cm<sup>–3</sup> and 9.3 ng cm<sup>–3</sup>, respectively. The overall CVG efficiency of 5.3 ± 0.1% was determined from comparison with solution nebulization-ICP-MS, while 5.7 ± 0.1% was determined using <sup>65</sup>Zn radiotracer and radiometry. The developed methodology was verified by determination of Zn in the standard reference material of fresh water (NIST 1643f). Interference study conducted with 13 hydride-forming and transition elements did not prove ability of any of the tested element to further increase the CVG efficiency, but at the same time, none of them exhibited serious interference except Ag.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"85 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932466","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 : 2024-08-06DOI: 10.1007/s00706-024-03242-z
Martin Baroch, Juraj Dian
This review discusses the electrochemical behavior of chlorophylls and bacteriochlorophylls as individual molecules, as well as their complexes, like reaction centers and photosystems I and II. The first part is devoted to describing chlorophylls and bacteriochlorophylls structures, and oxidation and reduction processes on various electrode materials in various solvents. The dependence of number, positions, and reversibility of the observed redox peaks on the solvent composition and aggregation is also discussed. The following part is aimed at reaction centers and photosystems naturally occurring in living organisms. Attention is paid to proper electrode modification, orientation of the studied systems on the electrode surface and reproducibility of the observed phenomena. The differences in electrochemical behavior at metallic and graphitic electrodes are discussed. In the last part, possible future opportunities are pronounced, like modern electrode materials, in situ studies and extension of the redox studies to the reaction centers and photosystems from other organisms.
Graphical abstract
这篇综述讨论了叶绿素和细菌叶绿素作为单个分子以及它们的复合物（如反应中心和光系统 I 和 II）的电化学行为。第一部分专门描述叶绿素和细菌叶绿素的结构，以及在各种溶剂中不同电极材料上的氧化和还原过程。还讨论了观察到的氧化还原峰的数量、位置和可逆性与溶剂成分和聚集的关系。下一部分针对生物体内自然存在的反应中心和光系统。注意电极的适当修饰、所研究系统在电极表面的定向以及观察到的现象的再现性。还讨论了金属电极和石墨电极电化学行为的差异。最后一部分指出了未来可能出现的机遇，如现代电极材料、原位研究以及将氧化还原研究扩展到其他生物的反应中心和光系统。
{"title":"Electrochemical behavior of chlorophylls, bacteriochlorophylls, and related macrostructures—a review","authors":"Martin Baroch, Juraj Dian","doi":"10.1007/s00706-024-03242-z","DOIUrl":"https://doi.org/10.1007/s00706-024-03242-z","url":null,"abstract":"<p>This review discusses the electrochemical behavior of chlorophylls and bacteriochlorophylls as individual molecules, as well as their complexes, like reaction centers and photosystems I and II. The first part is devoted to describing chlorophylls and bacteriochlorophylls structures, and oxidation and reduction processes on various electrode materials in various solvents. The dependence of number, positions, and reversibility of the observed redox peaks on the solvent composition and aggregation is also discussed. The following part is aimed at reaction centers and photosystems naturally occurring in living organisms. Attention is paid to proper electrode modification, orientation of the studied systems on the electrode surface and reproducibility of the observed phenomena. The differences in electrochemical behavior at metallic and graphitic electrodes are discussed. In the last part, possible future opportunities are pronounced, like modern electrode materials, in situ studies and extension of the redox studies to the reaction centers and photosystems from other organisms.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"9 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932469","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 : 2024-08-06DOI: 10.1007/s00706-024-03243-y
Alicja Chromiec, Renata Wietecha-Posłuszny
This study introduces a miniaturised solid-phase extraction (µ-SPE) method coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous quantification of 23 compounds, including psychoactive drugs, narcotics and their metabolites, in urine samples. The µ-SPE method, using standard laboratory equipment such as a centrifuge, was developed and validated, offering a practical and economical alternative to more traditional SPE methods. The key extraction parameters: elution solvent composition, sample and elution volumes, and sorbent mass were optimized to enhance performance. The method demonstrated high sensitivity, with detection limits between 0.06 and 0.41 ng cm−3 and quantification limits from 0.19 to 1.24 ng cm−3. The precision was confirmed with an intra-day precision ranging from 0.2% to 7.5% and an inter-day precision from 1.2% to 13.4%. Recovery rates ranged from 84.2% to 109.4%, with minimal matrix effects observed for most analytes (|ME|< 10%). The relative error remained below 5%, indicating good accuracy. The method was also evaluated in terms of greenness, practical, and analytical aspects using the WAC model. Based on the validation results, it was concluded that the developed method could be a good confirmatory method for results obtained by immunochemical tests and could also be used in both clinical analyses and forensic toxicology.
{"title":"Micro-solid phase extraction with in-lab-packed columns for cost-efficient drug extraction from urine samples","authors":"Alicja Chromiec, Renata Wietecha-Posłuszny","doi":"10.1007/s00706-024-03243-y","DOIUrl":"https://doi.org/10.1007/s00706-024-03243-y","url":null,"abstract":"<p>This study introduces a miniaturised solid-phase extraction (µ-SPE) method coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous quantification of 23 compounds, including psychoactive drugs, narcotics and their metabolites, in urine samples. The µ-SPE method, using standard laboratory equipment such as a centrifuge, was developed and validated, offering a practical and economical alternative to more traditional SPE methods. The key extraction parameters: elution solvent composition, sample and elution volumes, and sorbent mass were optimized to enhance performance. The method demonstrated high sensitivity, with detection limits between 0.06 and 0.41 ng cm<sup>−3</sup> and quantification limits from 0.19 to 1.24 ng cm<sup>−3</sup>. The precision was confirmed with an intra-day precision ranging from 0.2% to 7.5% and an inter-day precision from 1.2% to 13.4%. Recovery rates ranged from 84.2% to 109.4%, with minimal matrix effects observed for most analytes (|ME|< 10%). The relative error remained below 5%, indicating good accuracy. The method was also evaluated in terms of greenness, practical, and analytical aspects using the WAC model. Based on the validation results, it was concluded that the developed method could be a good confirmatory method for results obtained by immunochemical tests and could also be used in both clinical analyses and forensic toxicology.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"193 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932473","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 : 2024-08-06DOI: 10.1007/s00706-024-03248-7
D. Sumanth, J. G. Manjunatha
In the present study, electrochemical sensing electrode based on uniform poly(arginine)-modified carbon nanotube paste electrode (PAMCNTPE) is introduced for concurrent determination of caffeic acid and paracetamol. Scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS) were used to characterize the surface of the sensor. In addition, cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to investigate the performance of PAMCNTPE. The redox optimum current of caffeic acid was increased dramatically at the PAMCNTPE surface alongside bare carbon nanotube paste electrode (BCNTPE) and their overpotentials decreased. SEM images shows the morphological differences between bare and modified electrode which shows the evidence of modification. The effects of pH, polymerization cycle, and potential were investigated on the electrochemical redox response of caffeic acid based on response surface methodology. In addition, scan rate technique showed the process is adsorption controlled. Under the optimized conditions, linear response was obtained over the range of 10–200 μM, and also, detection limits were found to be 0.13 μM by DPV method on the surface of PAMCNTPE. The PAMCNTPE showed good stability, reproducibility, and repeatability as well as high recovery. The practical application of the PAMCNTPE was demonstrated by measuring the concentration of caffeic acid in apple juice as real sample. The proposed technique is simple, rapid, and cost-effective, serving as an important analytical tool for quality control in the pharmaceutical industry.
{"title":"Detection of caffeic acid using a nanotube paste-based electrochemical sensor","authors":"D. Sumanth, J. G. Manjunatha","doi":"10.1007/s00706-024-03248-7","DOIUrl":"https://doi.org/10.1007/s00706-024-03248-7","url":null,"abstract":"<p>In the present study, electrochemical sensing electrode based on uniform poly(arginine)-modified carbon nanotube paste electrode (PAMCNTPE) is introduced for concurrent determination of caffeic acid and paracetamol. Scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS) were used to characterize the surface of the sensor. In addition, cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to investigate the performance of PAMCNTPE. The redox optimum current of caffeic acid was increased dramatically at the PAMCNTPE surface alongside bare carbon nanotube paste electrode (BCNTPE) and their overpotentials decreased. SEM images shows the morphological differences between bare and modified electrode which shows the evidence of modification. The effects of pH, polymerization cycle, and potential were investigated on the electrochemical redox response of caffeic acid based on response surface methodology. In addition, scan rate technique showed the process is adsorption controlled. Under the optimized conditions, linear response was obtained over the range of 10–200 μM, and also, detection limits were found to be 0.13 μM by DPV method on the surface of PAMCNTPE. The PAMCNTPE showed good stability, reproducibility, and repeatability as well as high recovery. The practical application of the PAMCNTPE was demonstrated by measuring the concentration of caffeic acid in apple juice as real sample. The proposed technique is simple, rapid, and cost-effective, serving as an important analytical tool for quality control in the pharmaceutical industry.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"33 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932448","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}
This paper presents the development of spectrofluorimetric and smartphone-based detection methods for gentamicin determination using fluorescamine as a reagent. The research included selecting excitation (415 nm) and emission (489 nm) wavelengths, reaction time, and conditions like reagent concentration, and pH of the reaction medium. Moreover, the optimal operating parameters of the smartphone camera, like ISO, white balance, camera shutter, and RGB model channel were selected. Analytical parameters of the developed spectrofluorimetric and smartphone-based methods were estimated including the linear range: 0.04–15.00 mg dm−3 and 0.18–1.20 mg dm−3, respectively, limits of detection and quantification: 0.01 and 0.04 mg dm−3, and 0.06 and 0.18 mg dm−3, respectively, and precision (CV, n = 6): 5.2% and 2.8%, respectively. The proposed approaches were successfully applied to determine gentamicin in pharmaceutical samples. The obtained results were consistent with values declared by manufacturers and satisfactory recovery values, 93.2–113.6% were obtained for both spectrofluorimetric and smartphone-based methods. The developed fluorimetric method with smartphone-based detection provides a low limit of detection specific to spectrofluorimetric methods whereas the measurement system is a simple, easily accessible, compact, and low-cost device. Hence, it can become a competitive alternative to other gentamicin determination methods.
{"title":"Spectrofluorimetric and smartphone-based detection methods for determination of gentamicin","authors":"Karol Kubacki, Karolina Mermer, Justyna Paluch, Magdalena Bąk, Kamil Strzelak, Joanna Kozak","doi":"10.1007/s00706-024-03244-x","DOIUrl":"https://doi.org/10.1007/s00706-024-03244-x","url":null,"abstract":"<p>This paper presents the development of spectrofluorimetric and smartphone-based detection methods for gentamicin determination using fluorescamine as a reagent. The research included selecting excitation (415 nm) and emission (489 nm) wavelengths, reaction time, and conditions like reagent concentration, and pH of the reaction medium. Moreover, the optimal operating parameters of the smartphone camera, like ISO, white balance, camera shutter, and RGB model channel were selected. Analytical parameters of the developed spectrofluorimetric and smartphone-based methods were estimated including the linear range: 0.04–15.00 mg dm<sup>−3</sup> and 0.18–1.20 mg dm<sup>−3</sup>, respectively, limits of detection and quantification: 0.01 and 0.04 mg dm<sup>−3</sup>, and 0.06 and 0.18 mg dm<sup>−3</sup>, respectively, and precision (<i>CV</i>, <i>n</i> = 6): 5.2% and 2.8%, respectively. The proposed approaches were successfully applied to determine gentamicin in pharmaceutical samples. The obtained results were consistent with values declared by manufacturers and satisfactory recovery values, 93.2–113.6% were obtained for both spectrofluorimetric and smartphone-based methods. The developed fluorimetric method with smartphone-based detection provides a low limit of detection specific to spectrofluorimetric methods whereas the measurement system is a simple, easily accessible, compact, and low-cost device. Hence, it can become a competitive alternative to other gentamicin determination methods.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"5 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141968755","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 : 2024-08-06DOI: 10.1007/s00706-024-03245-w
Tomáš Lener, Karel Nesměrák
One of the fundamental parameters of drugs and pharmaceutical products is, in addition to their physiological effects, also their shelf-life. Even pharmaceuticals are subject to the effects of time, which gradually degrades and deteriorates them. This results in a reduction or even a serious change in the effects, or the development of toxicity. Therefore, the determination of the shelf-life of any drug or pharmaceutical product is of paramount importance. Unused drugs or pharmaceutical products after the expiry date have to be disposed of in a costly manner, which means financial losses and also imposes an unnecessary burden on the environment. There has recently been considerable discussion about the possible extension of the shelf-life of pharmaceuticals. The results of analyses of the historical remains of pharmaceuticals play an important role in this discussion. Therefore, an overview of recent results in this field is given here. In the first part, the review focuses on historical medicinal preparations (from antiquity to the early 19th century), which represent interesting, valuable, and often unique material for the study of the stability of medicinal substances over a long period (despite the uncertainty we have about their initial composition). The second part of the review gives an overview of articles on the stability of modern medicinal products, mostly already industrially produced.
{"title":"Long-term stability or degradation of drugs and pharmaceutical products: state-of-the-art","authors":"Tomáš Lener, Karel Nesměrák","doi":"10.1007/s00706-024-03245-w","DOIUrl":"https://doi.org/10.1007/s00706-024-03245-w","url":null,"abstract":"<p>One of the fundamental parameters of drugs and pharmaceutical products is, in addition to their physiological effects, also their shelf-life. Even pharmaceuticals are subject to the effects of time, which gradually degrades and deteriorates them. This results in a reduction or even a serious change in the effects, or the development of toxicity. Therefore, the determination of the shelf-life of any drug or pharmaceutical product is of paramount importance. Unused drugs or pharmaceutical products after the expiry date have to be disposed of in a costly manner, which means financial losses and also imposes an unnecessary burden on the environment. There has recently been considerable discussion about the possible extension of the shelf-life of pharmaceuticals. The results of analyses of the historical remains of pharmaceuticals play an important role in this discussion. Therefore, an overview of recent results in this field is given here. In the first part, the review focuses on historical medicinal preparations (from antiquity to the early 19th century), which represent interesting, valuable, and often unique material for the study of the stability of medicinal substances over a long period (despite the uncertainty we have about their initial composition). The second part of the review gives an overview of articles on the stability of modern medicinal products, mostly already industrially produced.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"22 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141932468","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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