Pub Date : 2024-07-25DOI: 10.1007/s00706-024-03237-w
Paweł Stelmaszczyk, Katarzyna Białkowska, Karolina Sekuła, Roman Stanaszek, Renata Wietecha-Posłuszny
This study investigates the electrochemical behavior of ketamine using an in-lab fabricated screen-printed electrode system and explores its potential application in quantitative analysis. Cyclic voltammetry and differential pulse voltammetry (DPV) experiments were employed to characterize the oxidation behavior of ketamine. Systematic optimization of DPV parameters, including pulse amplitude, pulse width, potential step, potential, and time accumulation for analyte preconcentration resulted in the selection of optimal conditions for quantitative analysis. The developed DPV method exhibited excellent linearity (R2 = 0.996) over the concentration range of 50–500 µM, with a limit of detection of 15 µM and a limit of quantification of 50 µM. Authentic samples analysis demonstrated the utility of the proposed sensor for quantitative analysis of ketamine in pharmaceutical products and seized drug samples. Overall, the developed sensor offers a promising tool for the rapid and accurate analysis of ketamine in various samples with potential applications in on-site forensic analysis.
{"title":"Screen-printed electrode-based sensor for rapid ketamine determination: optimization and on-site application for seized drugs analysis","authors":"Paweł Stelmaszczyk, Katarzyna Białkowska, Karolina Sekuła, Roman Stanaszek, Renata Wietecha-Posłuszny","doi":"10.1007/s00706-024-03237-w","DOIUrl":"https://doi.org/10.1007/s00706-024-03237-w","url":null,"abstract":"<p>This study investigates the electrochemical behavior of ketamine using an in-lab fabricated screen-printed electrode system and explores its potential application in quantitative analysis. Cyclic voltammetry and differential pulse voltammetry (DPV) experiments were employed to characterize the oxidation behavior of ketamine. Systematic optimization of DPV parameters, including pulse amplitude, pulse width, potential step, potential, and time accumulation for analyte preconcentration resulted in the selection of optimal conditions for quantitative analysis. The developed DPV method exhibited excellent linearity (R<sup>2</sup> = 0.996) over the concentration range of 50–500 µM, with a limit of detection of 15 µM and a limit of quantification of 50 µM. Authentic samples analysis demonstrated the utility of the proposed sensor for quantitative analysis of ketamine in pharmaceutical products and seized drug samples. Overall, the developed sensor offers a promising tool for the rapid and accurate analysis of ketamine in various samples with potential applications in on-site forensic analysis.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141784889","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 : 2024-07-24DOI: 10.1007/s00706-024-03234-z
Sathish Reddy, R. B. Raghavendra, R. Yashwanth, B. Nandana, K. J. Abhishek, M. Madesh Kumar, K. N. Harish, Mohan Kumar, G. K. Jayaprakash
Environmental and public health risks may arise from the presence of antibiotic residues, and specifically chloramphenicol in food samples. Therefore, it is quite important for researchers to detect chloramphenicol. In this work, PDA@CuFe2O4 nanoparticles were synthesized and characterizsed. The PDA@CuFe2O4 nanoparticles that had been prepared were used to create PDA@CuFe2O4/GCE, which was then used to detect chloramphenicol electrochemically in a 0.1 M phosphate buffer solution (pH 7). The study focused on the electrochemical properties, including changes in scan rate, sensing, and pH influence. Compared to the unmodified electrode, the PDA@CuFe2O4/GCE electrode exhibits better sensing properties. The advantage of the PDA@CuFe2O4/GCE electrode is that it shows unique electrochemical sensing toward individual and chloramphenicol detection; for instance, it has a low detection of 0.12µM for chloramphenicol detection and a high sensitivity of 16.25A µM−1 cm−2 for chloramphenicol detection.
{"title":"Polydopamine-wrapped copper ferrite nanoparticle electrochemical sensor for detection of chloramphenicol","authors":"Sathish Reddy, R. B. Raghavendra, R. Yashwanth, B. Nandana, K. J. Abhishek, M. Madesh Kumar, K. N. Harish, Mohan Kumar, G. K. Jayaprakash","doi":"10.1007/s00706-024-03234-z","DOIUrl":"https://doi.org/10.1007/s00706-024-03234-z","url":null,"abstract":"<p>Environmental and public health risks may arise from the presence of antibiotic residues, and specifically chloramphenicol in food samples. Therefore, it is quite important for researchers to detect chloramphenicol. In this work, PDA@CuFe<sub>2</sub>O<sub>4</sub> nanoparticles were synthesized and characterizsed. The PDA@CuFe<sub>2</sub>O<sub>4</sub> nanoparticles that had been prepared were used to create PDA@CuFe<sub>2</sub>O<sub>4</sub>/GCE, which was then used to detect chloramphenicol electrochemically in a 0.1 M phosphate buffer solution (pH 7). The study focused on the electrochemical properties, including changes in scan rate, sensing, and pH influence. Compared to the unmodified electrode, the PDA@CuFe<sub>2</sub>O<sub>4</sub>/GCE electrode exhibits better sensing properties. The advantage of the PDA@CuFe<sub>2</sub>O<sub>4</sub>/GCE electrode is that it shows unique electrochemical sensing toward individual and chloramphenicol detection; for instance, it has a low detection of 0.12µM for chloramphenicol detection and a high sensitivity of 16.25A µM<sup>−1</sup> cm<sup>−2</sup> for chloramphenicol detection.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141784890","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 : 2024-07-24DOI: 10.1007/s00706-024-03232-1
Kateřina Černá, Petr Kozlík
Triazoles serve as crucial intermediates in the production of ribavirin, a drug utilized for treating hepatitis C, respiratory syncytial virus (RSV) infections, and viral hemorrhagic fevers. In this study, we developed a rapid and straightforward method employing high-performance liquid chromatography with UV detection to determine triazoles used in these intermediates' synthesis. We compared several recently developed LC mixed-mode stationary phases with the classical C18 stationary phase. Using an Astra DM column with a multimodal stationary phase enabled rapid separation of all analytes within 3.2 min, surpassing the separation achieved with a C18 stationary phase. Our developed method demonstrated excellent linearity within a concentration range of 1 (2.5)–200 µg cm−3, with acceptable accuracy and precision levels within 1 and 5%, respectively. These results indicate that the optimized method is suitable for routine analysis of pertinent substances involved in the synthesis process, particularly when determining all ribavirin intermediates is necessary.
{"title":"Chromatographic method for rapid determination of triazoles in ribavirin intermediates synthesis: stationary phase comparison","authors":"Kateřina Černá, Petr Kozlík","doi":"10.1007/s00706-024-03232-1","DOIUrl":"https://doi.org/10.1007/s00706-024-03232-1","url":null,"abstract":"<p>Triazoles serve as crucial intermediates in the production of ribavirin, a drug utilized for treating hepatitis C, respiratory syncytial virus (RSV) infections, and viral hemorrhagic fevers. In this study, we developed a rapid and straightforward method employing high-performance liquid chromatography with UV detection to determine triazoles used in these intermediates' synthesis. We compared several recently developed LC mixed-mode stationary phases with the classical C18 stationary phase. Using an Astra DM column with a multimodal stationary phase enabled rapid separation of all analytes within 3.2 min, surpassing the separation achieved with a C18 stationary phase. Our developed method demonstrated excellent linearity within a concentration range of 1 (2.5)–200 µg cm<sup>−3</sup>, with acceptable accuracy and precision levels within 1 and 5%, respectively. These results indicate that the optimized method is suitable for routine analysis of pertinent substances involved in the synthesis process, particularly when determining all ribavirin intermediates is necessary.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"35 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141784786","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 : 2024-07-24DOI: 10.1007/s00706-024-03233-0
Lucie Pražáková, Jan Fischer, Andrew Taylor, Anna Kubíčková
The effect of the boron content doped in the diamond electrode on the oxidative degradation behaviour of the active pharmaceutical ingredient abacavir was investigated. The characteristics of five working boron-doped diamond electrodes, differing in a B/C doping ratio of 500 ppm, 1000 ppm, 2000 ppm, 4000 ppm, and 8000 ppm, were studied. The oxidative degradation of the substance abacavir was studied in a batch cell. The degradation took place under potentiostatic electrolysis at potentials from +0.6 V to +3.7 V. The boron level has a significant effect on the oxidative degradation of the substance at potentials greater than +2.0 V only. Liquid chromatography coupled with mass spectrometry was employed to verify the generation of two primary degradation by-products, namely OP1 (m/z = 319.20) and OP2 (m/z = 247.19). The relative amounts of these degradation products showed variability depending on the diamond electrode used, which was conditioned by different B/C ratios.
Graphical abstract
研究了掺入金刚石电极中的硼含量对活性药物成分阿巴卡韦氧化降解行为的影响。研究了五种硼掺杂金刚石电极的特性，它们的硼/碳掺杂比分别为 500 ppm、1000 ppm、2000 ppm、4000 ppm 和 8000 ppm。在批处理池中研究了阿巴卡韦物质的氧化降解。降解是在电位为 +0.6 V 至 +3.7 V 的恒电位电解条件下进行的。只有在电位大于 +2.0 V 时，硼含量才会对该物质的氧化降解产生显著影响。采用液相色谱-质谱法验证了两种主要降解副产物的生成，即 OP1（m/z = 319.20）和 OP2（m/z = 247.19）。这些降解产物的相对数量随所使用的金刚石电极（以不同的 B/C 比值为条件）的不同而变化。
{"title":"Boron-doped diamond electrodes: examining the effect of doping level on the degradation of pharmaceuticals","authors":"Lucie Pražáková, Jan Fischer, Andrew Taylor, Anna Kubíčková","doi":"10.1007/s00706-024-03233-0","DOIUrl":"https://doi.org/10.1007/s00706-024-03233-0","url":null,"abstract":"<p>The effect of the boron content doped in the diamond electrode on the oxidative degradation behaviour of the active pharmaceutical ingredient abacavir was investigated. The characteristics of five working boron-doped diamond electrodes, differing in a B/C doping ratio of 500 ppm, 1000 ppm, 2000 ppm, 4000 ppm, and 8000 ppm, were studied. The oxidative degradation of the substance abacavir was studied in a batch cell. The degradation took place under potentiostatic electrolysis at potentials from +0.6 V to +3.7 V. The boron level has a significant effect on the oxidative degradation of the substance at potentials greater than +2.0 V only. Liquid chromatography coupled with mass spectrometry was employed to verify the generation of two primary degradation by-products, namely OP1 (<i>m/z</i> = 319.20) and OP2 (<i>m/z</i> = 247.19). The relative amounts of these degradation products showed variability depending on the diamond electrode used, which was conditioned by different B/C ratios.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"18 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141784784","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 : 2024-07-24DOI: 10.1007/s00706-024-03229-w
Hemn A. H. Barzani, Hoshyar Saadi Ali, Yavuz Yardım
This research paper presents an electroanalytical investigation utilizing voltammetry to quantify the antidiabetic drug linagliptin with an unmodified boron-doped diamond electrode. Using cyclic voltammetry, linagliptin exhibited a single, distinct, irreversible oxidation peak at around + 1.03 V (vs. Ag/AgCl) in a 0.1 mol dm−3 phosphate buffer solution at pH 7.4. The square-wave voltammetry technique achieved acceptable linearity at approximately + 0.94 V in PBS (pH 7.4). The methodology demonstrated linearity within the concentration range of 1.0 and 50.0 μg cm−3 (equivalent to 2.1 × 10–6–1.1 × 10–4 mol dm−3) and yielded a limit of detection of 0.28 μg cm−3 (equivalent to 5.9 × 10–7 mol dm−3). The investigation of the proposed method's applicability was ultimately conducted through the sensing of linagliptin in drug formulations. The established methodologies can serve as viable alternatives to other analytical techniques due to their cost-effectiveness, user-friendliness, efficiency, and ability to yield reliable and repeatable results.
{"title":"Electroanalytical sensing of antidiabetic drug linagliptin by using square-wave voltammetry on the boron-doped diamond electrode","authors":"Hemn A. H. Barzani, Hoshyar Saadi Ali, Yavuz Yardım","doi":"10.1007/s00706-024-03229-w","DOIUrl":"https://doi.org/10.1007/s00706-024-03229-w","url":null,"abstract":"<p>This research paper presents an electroanalytical investigation utilizing voltammetry to quantify the antidiabetic drug linagliptin with an unmodified boron-doped diamond electrode. Using cyclic voltammetry, linagliptin exhibited a single, distinct, irreversible oxidation peak at around + 1.03 V (vs. Ag/AgCl) in a 0.1 mol dm<sup>−3</sup> phosphate buffer solution at pH 7.4. The square-wave voltammetry technique achieved acceptable linearity at approximately + 0.94 V in PBS (pH 7.4). The methodology demonstrated linearity within the concentration range of 1.0 and 50.0 μg cm<sup>−3</sup> (equivalent to 2.1 × 10<sup>–6</sup>–1.1 × 10<sup>–4</sup> mol dm<sup>−3</sup>) and yielded a limit of detection of 0.28 μg cm<sup>−3</sup> (equivalent to 5.9 × 10<sup>–7</sup> mol dm<sup>−3</sup>). The investigation of the proposed method's applicability was ultimately conducted through the sensing of linagliptin in drug formulations. The established methodologies can serve as viable alternatives to other analytical techniques due to their cost-effectiveness, user-friendliness, efficiency, and ability to yield reliable and repeatable results.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"43 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141784785","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 : 2024-07-01DOI: 10.1007/s00706-024-03226-z
Tomáš Lener, Martin Štícha, Karel Nesměrák
In this work, more than 200-year-old historical remains of liquorice root powder and a current liquorice root as a reference material were analyzed by HPLC–MS/MS to confirm the botanical authenticity of the historical material by comparing the results obtained. Combining extraction with different solvents with HPLC–MS/MS successfully identified nine chemotaxonomic markers in the historical material, thus confirming its identity as liquorice. In the current reference material, 32 chemotaxonomic markers of liquorice were successfully identified. Therefore, several liquorice-specific compounds in the historical remains analyzed were shown to have degraded over time. In addition, possible fragmentation mechanisms for five liquorice-specific compounds that have not been previously published in the literature were proposed.
{"title":"HPLC–MS/MS authentication of the eighteenth century liquorice drug remains and mass spectrometry of selected liquorice-specific compounds","authors":"Tomáš Lener, Martin Štícha, Karel Nesměrák","doi":"10.1007/s00706-024-03226-z","DOIUrl":"https://doi.org/10.1007/s00706-024-03226-z","url":null,"abstract":"<p>In this work, more than 200-year-old historical remains of liquorice root powder and a current liquorice root as a reference material were analyzed by HPLC–MS/MS to confirm the botanical authenticity of the historical material by comparing the results obtained. Combining extraction with different solvents with HPLC–MS/MS successfully identified nine chemotaxonomic markers in the historical material, thus confirming its identity as liquorice. In the current reference material, 32 chemotaxonomic markers of liquorice were successfully identified. Therefore, several liquorice-specific compounds in the historical remains analyzed were shown to have degraded over time. In addition, possible fragmentation mechanisms for five liquorice-specific compounds that have not been previously published in the literature were proposed.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"165 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141508461","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 : 2024-06-17DOI: 10.1007/s00706-024-03225-0
Karel Nesměrák, Karel Kudláček, Jakub Hraníček, Jacopo La Nasa, Erika Ribechini, Maria Perla Colombini
An array of analytical techniques (GC–MS, SPME–GC–MS, RP–HPLC–MS, FIA–MS, HPLC–UV, ICP–MS) was used to study the molecular composition of six ointment residues from the first third of the twentieth century. The objectives of the study were (i) to validate the applicability of a previously proposed strategy for the identification of lipids and active pharmaceutical ingredients in remains of historical pharmaceuticals and (ii) to shed light on early twentieth-century pharmaceutical practice. Although no further information on the composition of the samples studied was available (all were marked by a period pharmacist with the general label “Ointment” only), it was possible to identify the likely lipidic ointment bases as well as quantify the main likely active substances in all samples. This allowed us to partially reconstruct the composition of each ointment and to estimate its original purpose.
{"title":"The molecular composition of six ointment remains from the first third of the twentieth century determined by a multi-analytical approach","authors":"Karel Nesměrák, Karel Kudláček, Jakub Hraníček, Jacopo La Nasa, Erika Ribechini, Maria Perla Colombini","doi":"10.1007/s00706-024-03225-0","DOIUrl":"https://doi.org/10.1007/s00706-024-03225-0","url":null,"abstract":"<p>An array of analytical techniques (GC–MS, SPME–GC–MS, RP–HPLC–MS, FIA–MS, HPLC–UV, ICP–MS) was used to study the molecular composition of six ointment residues from the first third of the twentieth century. The objectives of the study were (i) to validate the applicability of a previously proposed strategy for the identification of lipids and active pharmaceutical ingredients in remains of historical pharmaceuticals and (ii) to shed light on early twentieth-century pharmaceutical practice. Although no further information on the composition of the samples studied was available (all were marked by a period pharmacist with the general label “Ointment” only), it was possible to identify the likely lipidic ointment bases as well as quantify the main likely active substances in all samples. This allowed us to partially reconstruct the composition of each ointment and to estimate its original purpose.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"50 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141529748","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 : 2024-06-04DOI: 10.1007/s00706-024-03223-2
K. P. Moulya, J. G. Manjunatha, Tahani Mazyad Almutairi, M. Nagaraja, B. Somashekara
This study offers a simple voltammetric method for quantifying hydroquinone using a poly(valine)-modified carbon paste electrode (PVLMCPE). Differential pulse voltammetry, cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy were utilized to assess the performance of the developed sensor. The oxidation peak current of hydroquinone at the PVLMCPE surface significantly increased in contrast to the bare carbon paste electrode, and overpotentials decreased. Using response surface methodology, a methodical investigation of the electrochemical response of hydroquinone electro-oxidation was carried out, taking potential, pH, polymerization cycle, and scan rate into consideration as important variables. At pH 6.5, phosphate buffer solution produced the best results. In perfect circumstances, the linear detection range showed a high correlation coefficient of 0.920, ranging from 20 to 150 μM. The results showed that the limit of detection and limit of quantification were 0.092 μM and 0.027 μM, respectively. A successful assessment of the results with those obtained using the official method was necessary for validation. Additionally, the created sensor demonstrated a remarkable sensitivity in detecting hydroquinone even in the presence of common interference molecules such as resorcinol. The modified electrode exhibits notable recovery rates and can be used for accurate determination of hydroquinone in real samples due to its broad linear range, high sensitivity, and excellent reproducibility.
{"title":"A new sensing platform based on poly(valine)-modified carbon paste electrode for the determination of hydroquinone and resorcinol","authors":"K. P. Moulya, J. G. Manjunatha, Tahani Mazyad Almutairi, M. Nagaraja, B. Somashekara","doi":"10.1007/s00706-024-03223-2","DOIUrl":"https://doi.org/10.1007/s00706-024-03223-2","url":null,"abstract":"<p>This study offers a simple voltammetric method for quantifying hydroquinone using a poly(valine)-modified carbon paste electrode (PVLMCPE). Differential pulse voltammetry, cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy were utilized to assess the performance of the developed sensor. The oxidation peak current of hydroquinone at the PVLMCPE surface significantly increased in contrast to the bare carbon paste electrode, and overpotentials decreased. Using response surface methodology, a methodical investigation of the electrochemical response of hydroquinone electro-oxidation was carried out, taking potential, pH, polymerization cycle, and scan rate into consideration as important variables. At pH 6.5, phosphate buffer solution produced the best results. In perfect circumstances, the linear detection range showed a high correlation coefficient of 0.920, ranging from 20 to 150 μM. The results showed that the limit of detection and limit of quantification were 0.092 μM and 0.027 μM, respectively. A successful assessment of the results with those obtained using the official method was necessary for validation. Additionally, the created sensor demonstrated a remarkable sensitivity in detecting hydroquinone even in the presence of common interference molecules such as resorcinol. The modified electrode exhibits notable recovery rates and can be used for accurate determination of hydroquinone in real samples due to its broad linear range, high sensitivity, and excellent reproducibility.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"67 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141257483","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 : 2024-05-29DOI: 10.1007/s00706-024-03210-7
André Culum, Herwig Prasch, Tobias Dorn, Roland Fischer, Ema Gardić, Franziska Schmutz, Magdalena Steinbrugger, Arnold E. Stütz, Patrick Weber, Tanja M. Wrodnigg, Martin Thonhofer
Herein, we present an alternative and elegant synthetic approach toward powerful β-glucosidase inhibitor isofagomine. Derivatizations of the ring nitrogen provided a selected set of N-modified isofagomine analogues. Biological evaluation of these compounds showed a remarkable change in potency as well as α/β-preference for various glycosidases from different sources when compared to the parent compound isofagomine. Overall, the conducted N-modification improved the potency against α-glucosidase from Saccharomyces cerevisiae (GH13). Coming along, significant diminished activities toward GH1 family β-glucosidases from three different sources have been observed for all tested derivatives. Moreover, and contrary to isofagomine, deactivations of β-galactosidase from Escherichia coli (GH2) as well as α-mannosidase from Canavalia ensiformis (GH38) have not been verified for this series of compounds.
{"title":"A remarkable change in inhibition potency and selectivity of isofagomine by simple N-modification","authors":"André Culum, Herwig Prasch, Tobias Dorn, Roland Fischer, Ema Gardić, Franziska Schmutz, Magdalena Steinbrugger, Arnold E. Stütz, Patrick Weber, Tanja M. Wrodnigg, Martin Thonhofer","doi":"10.1007/s00706-024-03210-7","DOIUrl":"https://doi.org/10.1007/s00706-024-03210-7","url":null,"abstract":"<p>Herein, we present an alternative and elegant synthetic approach toward powerful β-glucosidase inhibitor isofagomine. Derivatizations of the ring nitrogen provided a selected set of N-modified isofagomine analogues. Biological evaluation of these compounds showed a remarkable change in potency as well as α/β-preference for various glycosidases from different sources when compared to the parent compound isofagomine. Overall, the conducted N-modification improved the potency against α-glucosidase from <i>Saccharomyces cerevisiae</i> (GH13). Coming along, significant diminished activities toward GH1 family β-glucosidases from three different sources have been observed for all tested derivatives. Moreover, and contrary to isofagomine, deactivations of β-galactosidase from <i>Escherichia coli</i> (GH2) as well as α-mannosidase from <i>Canavalia ensiformis</i> (GH38) have not been verified for this series of compounds.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"27 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141165489","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 : 2024-05-28DOI: 10.1007/s00706-024-03214-3
Bogdan R. Brutiu, Le Tang, Daniel Kaiser, Nuno Maulide
A Brønsted acid-catalyzed regioselective intramolecular hydroalkoxylation is described. This reaction proceeds via a carbocation intermediate and enables the preparation of 1,1,1’-trisubstituted tetrahydropyran derivatives under mild conditions using catalytic triflic acid (TfOH) and hexafluoroisopropanol (HFIP) as a mediator.
{"title":"Tetrahydropyran synthesis mediated by catalytic triflic acid and hexafluoroisopropanol","authors":"Bogdan R. Brutiu, Le Tang, Daniel Kaiser, Nuno Maulide","doi":"10.1007/s00706-024-03214-3","DOIUrl":"https://doi.org/10.1007/s00706-024-03214-3","url":null,"abstract":"<p>A Brønsted acid-catalyzed regioselective intramolecular hydroalkoxylation is described. This reaction proceeds via a carbocation intermediate and enables the preparation of 1,1,1’-trisubstituted tetrahydropyran derivatives under mild conditions using catalytic triflic acid (TfOH) and hexafluoroisopropanol (HFIP) as a mediator.</p><h3 data-test=\"abstract-sub-heading\">Graphical abstract</h3>\u0000","PeriodicalId":19011,"journal":{"name":"Monatshefte für Chemie / Chemical Monthly","volume":"68 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141165473","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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