Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111771
Jianjin Guo , Chi-Tang Ho , Naisheng Bai
This comprehensive study utilized response surface methodology (RSM) to optimize extraction conditions for total flavonoids and phenols from F. mandshurica. Optimal conditions for flavonoids were 75 % ethanol, 63 °C, and 84 min, yielding 14.98 ± 0.13 mg/g. For phenols, it was 70 % ethanol, 66 °C, and 87 min, resulting in 26.04 ± 0.22 mg/g. UPLC-Q-TOF-MS/MS identified 68 constituents in F. mandshurica, categorized into groups. HPLC-DAD established a method for quantitative analysis of 12 target compounds. Geographical distribution analysis highlighted the northeast region as the main production area. Fingerprinting of 30 samples and multivariate analysis identified five active compounds. Hierarchical cluster analysis (HCA) showed differences in active compounds based on origin. In vitro antidiabetic evaluation demonstrated α-glucosidase inhibitory effects. Molecular docking studies were conducted between 12 active compounds and the antidiabetic-related protein 8A27. Esculetin had the highest binding affinity. The study examined extraction methods, analyzed samples, and explored antidiabetic effects, providing data support and insights for F. mandshurica as a natural industrial product and for extracts and active compounds as antidiabetic sources.
{"title":"Utilizing HPLC-DAD, multivariate analysis, molecular docking, and in vitro validation methods to investigate phenolic compounds with potential antidiabetic properties in Fraxinus mandshurica","authors":"Jianjin Guo , Chi-Tang Ho , Naisheng Bai","doi":"10.1016/j.microc.2024.111771","DOIUrl":"10.1016/j.microc.2024.111771","url":null,"abstract":"<div><div>This comprehensive study utilized response surface methodology (RSM) to optimize extraction conditions for total flavonoids and phenols from <em>F. mandshurica</em>. Optimal conditions for flavonoids were 75 % ethanol, 63 °C, and 84 min, yielding 14.98 ± 0.13 mg/g. For phenols, it was 70 % ethanol, 66 °C, and 87 min, resulting in 26.04 ± 0.22 mg/g. UPLC-Q-TOF-MS/MS identified 68 constituents in <em>F. mandshurica</em>, categorized into groups. HPLC-DAD established a method for quantitative analysis of 12 target compounds. Geographical distribution analysis highlighted the northeast region as the main production area. Fingerprinting of 30 samples and multivariate analysis identified five active compounds. Hierarchical cluster analysis (HCA) showed differences in active compounds based on origin. In <em>vitro</em> antidiabetic evaluation demonstrated α-glucosidase inhibitory effects. Molecular docking studies were conducted between 12 active compounds and the antidiabetic-related protein 8A27. Esculetin had the highest binding affinity. The study examined extraction methods, analyzed samples, and explored antidiabetic effects, providing data support and insights for <em>F. mandshurica</em> as a natural industrial product and for extracts and active compounds as antidiabetic sources.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111771"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142322050","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111759
Chan Huang, Le Liang, Yong-qing Liu, Mei Han, Xue-lin Wang, Xiao-hua Cai, Guang-long Zou
Designing versatile carbon quantum dots (CDs) with excellent sensitivity and unique function as efficient fluorescent probe for detection of specific substance from cheap and readily available substrates is still a crucial challenge. A novel nitrogen-sulfur doped carbon dots (N, S-CDs) with blue-green fluorescent emission derived from lactose and 4-amino-3-hydroxy-1-naphthalenesulfonic acid (AHNS) was facilely synthesized by one-step hydrothermal process. The obtained N, S-CDs with graphene structure exhibited good water solubility, excellent biocompatibility, satisfactory stability and striking optical properties. The surface of N, S-CDs is modified by various functional groups which are helpful to combine with Ga3+ in the form of complexes N, S-CDs-Ga3+ to considerably enhance the fluorescence emission peak of N, S-CDs, further improving the selectivity and sensitivity of Ga3+ detection with the detection limit of 0.133 μM. At the meantime, N, S-CDs can cause yellow fluorescence quenching of riboflavin (VB2) with the detection limit of 0.121 μM under the concentration range from 1.000-20.000 μM. The possible mechanism is the functional groups at the surface of N, S-CDs combined with the hydroxyl, amino and carbonyl group of VB2 by protonation and hydrogen bonds. Further investigations for practical applications demonstrated that N, S-CDs has good prospects in Ga3+ananlysis and detection of VB2 in food. Moreover, N, S-CDs can be used to determine whether there is Ga3+ in transferrin, which can indirectly inhibit the growth of cancer cells through the influence on transporting iron ion. Therefore, it is profitable for preliminary diagnosis and treatment of cancer cells in the field of biomedicine.
{"title":"Preparation and multipurpose applications of nitrogen-sulfur doped carbon dots fluorescent probe for Ga3+ and riboflavin (VB2) detection","authors":"Chan Huang, Le Liang, Yong-qing Liu, Mei Han, Xue-lin Wang, Xiao-hua Cai, Guang-long Zou","doi":"10.1016/j.microc.2024.111759","DOIUrl":"10.1016/j.microc.2024.111759","url":null,"abstract":"<div><div>Designing versatile carbon quantum dots (CDs) with excellent sensitivity and unique function as efficient fluorescent probe for detection of specific substance from cheap and readily available substrates is still a crucial challenge. A novel nitrogen-sulfur doped carbon dots (N, S-CDs) with blue-green fluorescent emission derived from lactose and 4-amino-3-hydroxy-1-naphthalenesulfonic acid (AHNS) was facilely synthesized by one-step hydrothermal process. The obtained N, S-CDs with graphene structure exhibited good water solubility, excellent biocompatibility, satisfactory stability and striking optical properties. The surface of N, S-CDs is modified by various functional groups which are helpful to combine with Ga<sup>3+</sup> in the form of complexes N, S-CDs-Ga<sup>3+</sup> to considerably enhance the fluorescence emission peak of N, S-CDs, further improving the selectivity and sensitivity of Ga<sup>3+</sup> detection with the detection limit of 0.133 μM. At the meantime, N, S-CDs can cause yellow fluorescence quenching of riboflavin (VB<sub>2</sub>) with the detection limit of 0.121 μM under the concentration range from 1.000-20.000 μM. The possible mechanism is the functional groups at the surface of N, S-CDs combined with the hydroxyl, amino and carbonyl group of VB<sub>2</sub> by protonation and hydrogen bonds. Further investigations for practical applications demonstrated that N, S-CDs has good prospects in Ga<sup>3+</sup>ananlysis and detection of VB<sub>2</sub> in food. Moreover, N, S-CDs can be used to determine whether there is Ga<sup>3+</sup> in transferrin, which can indirectly inhibit the growth of cancer cells through the influence on transporting iron ion. Therefore, it is profitable for preliminary diagnosis and treatment of cancer cells in the field of biomedicine.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111759"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142357868","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111760
Thi–Dan Thach , Le–Kim–Thuy Nguyen , T. Duy–Nguyen Nguyen , T. My–Thao Nguyen , Van–Su Dang , Dinh Tri Mai , Van–Dung Le , Chi–Hien Dang , Quynh Nguyen Nhu Le , Phuong Thuy Viet Nguyen , Minh Nam Nguyen , Van Kieu Thuy Nguyen , Nguyen–Nguyen Pham–Tran , Thanh–Danh Nguyen
In this study, four novel triphenylpyrazoline 4-toluenesulfonylureas (PYSUs) were synthesized to develop potential anticancer drugs and fluorescent probes for the detection of F− ions. The compounds were synthesized via a two-step microwave-assisted method. The antiproliferative activity of the PYSUs was tested against two cancer cell lines: HepG2 and MDA-MB-231. Among the compounds, 3a exhibited strong activity against both cell lines, while 3b showed strong activity against MDA-MB-231 cells but weaker inhibition of HepG2 cells. Furthermore, compound 3b was identified as the best fluorescent probe, with an increase in emission intensity in the presence of F− ions from tetrabutylammonium fluoride (TBAF). In DMSO, the emission wavelength was found to be 518 nm (green) with an excitation wavelength of 469 nm. The limit of detection (LOD) was calculated to be 0.269 mM in the linear range of 5–10 mM. The interaction mechanism between F− ions and compound 3b was further explored via DFT/TDDFT calculations. Additionally, fluorescent imaging of TBAF-incubated MDA-MB-231 and HepG2 cells confirmed the potential of PYSUs as fluorescent sensors for F− ions in living cancer cells.
{"title":"Novel sulfonylurea fluorescence probes for antiproliferative activity, detection and imaging of fluoride ions in living cells","authors":"Thi–Dan Thach , Le–Kim–Thuy Nguyen , T. Duy–Nguyen Nguyen , T. My–Thao Nguyen , Van–Su Dang , Dinh Tri Mai , Van–Dung Le , Chi–Hien Dang , Quynh Nguyen Nhu Le , Phuong Thuy Viet Nguyen , Minh Nam Nguyen , Van Kieu Thuy Nguyen , Nguyen–Nguyen Pham–Tran , Thanh–Danh Nguyen","doi":"10.1016/j.microc.2024.111760","DOIUrl":"10.1016/j.microc.2024.111760","url":null,"abstract":"<div><div>In this study, four novel triphenylpyrazoline 4-toluenesulfonylureas (PYSUs) were synthesized to develop potential anticancer drugs and fluorescent probes for the detection of F<sup>−</sup> ions. The compounds were synthesized via a two-step microwave-assisted method. The antiproliferative activity of the PYSUs was tested against two cancer cell lines: HepG2 and MDA-MB-231. Among the compounds, <strong>3a</strong> exhibited strong activity against both cell lines, while <strong>3b</strong> showed strong activity against MDA-MB-231 cells but weaker inhibition of HepG2 cells. Furthermore, compound <strong>3b</strong> was identified as the best fluorescent probe, with an increase in emission intensity in the presence of F<sup>−</sup> ions from tetrabutylammonium fluoride (TBAF). In DMSO, the emission wavelength was found to be 518 nm (green) with an excitation wavelength of 469 nm. The limit of detection (LOD) was calculated to be 0.269 mM in the linear range of 5–10 mM. The interaction mechanism between F<sup>−</sup> ions and compound 3b was further explored via DFT/TDDFT calculations. Additionally, fluorescent imaging of TBAF-incubated MDA-MB-231 and HepG2 cells confirmed the potential of PYSUs as fluorescent sensors for F<sup>−</sup> ions in living cancer cells.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111760"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142326391","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111768
Xiao-Dong Sun , Min Zhang , Huan Liang , Shuo Zhang , Peng-Jiao Wang , Xiu-Li Gao
The commercial value of cinnamon depends largely on its geographical origin. This study proposed high-performance liquid chromatography-diode array detection (HPLC-DAD) fingerprints combined with chemometrics to identify geographical origins of cinnamons. Alternating trilinear decomposition (ATLD) algorithm was applied to extract meaningful chemical information from the HPLC fingerprint data. Then, non-targeted HPLC fingerprints and chemical component information were used as chemical descriptors to distinguish geographical origins using principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA)/N-way partial least squares-discriminant analysis (NPLS-DA). Satisfactory classification results were acquired for each discriminant model and the correct classification rates (CCRs) of training and test sets were 100%. Moreover, four characteristic variables were screened by variable importance in projection (VIP) method, three of which were reasonably identified as cinnamic acid, cinnamaldehyde and 2-methoxycinnamaldehyde, which can be regarded as potential markers to distinguish cinnamon from different geographical origins. The results indicated that HPLC-DAD fingerprints combined with chemometrics can be a promising means to identify the geographical origins and screen potential markers of cinnamon samples, especially in the absence of high-cost and sophisticated analytical instrumentals (e.g., high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy). This work can help to prevent cinnamon fraud practices and maintain the normal order of the cinnamon market.
{"title":"Geographical origin identification of cinnamon using HPLC-DAD fingerprints and chemometrics","authors":"Xiao-Dong Sun , Min Zhang , Huan Liang , Shuo Zhang , Peng-Jiao Wang , Xiu-Li Gao","doi":"10.1016/j.microc.2024.111768","DOIUrl":"10.1016/j.microc.2024.111768","url":null,"abstract":"<div><div>The commercial value of cinnamon depends largely on its geographical origin. This study proposed high-performance liquid chromatography-diode array detection (HPLC-DAD) fingerprints combined with chemometrics to identify geographical origins of cinnamons. Alternating trilinear decomposition (ATLD) algorithm was applied to extract meaningful chemical information from the HPLC fingerprint data. Then, non-targeted HPLC fingerprints and chemical component information were used as chemical descriptors to distinguish geographical origins using principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA)/N-way partial least squares-discriminant analysis (NPLS-DA). Satisfactory classification results were acquired for each discriminant model and the correct classification rates (CCRs) of training and test sets were 100%. Moreover, four characteristic variables were screened by variable importance in projection (VIP) method, three of which were reasonably identified as cinnamic acid, cinnamaldehyde and 2-methoxycinnamaldehyde, which can be regarded as potential markers to distinguish cinnamon from different geographical origins. The results indicated that HPLC-DAD fingerprints combined with chemometrics can be a promising means to identify the geographical origins and screen potential markers of cinnamon samples, especially in the absence of high-cost and sophisticated analytical instrumentals (e.g., high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy). This work can help to prevent cinnamon fraud practices and maintain the normal order of the cinnamon market.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111768"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142326389","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111770
Nerea Núñez , Javier Saurina , Oscar Núñez
The importance of monitoring the presence of bioactive compounds as food attributes for sample classification and characterization is increasing. In this study, targeted Liquid Chromatography coupled with High-Resolution Mass Spectrometry (LC-HRMS) was employed to analyze the chemical profile of polyphenolic compounds as the source of information for the characterization and classification of 306 commercial coffee samples. Coffee holds a distinguished position as one of the most widely popular beverages globally but also one of the most easily adulterated. Regrettably, in recent times, instances of coffee adulteration have been on the rise. Consequently, implementing rigorous quality control measures for coffee becomes imperative to guarantee its quality. The results obtained in this work confirm that the proposed chemical profiles serve as excellent descriptors for sample characterization and classification through the implementation of principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA), achieving classification rates higher than 83.3% in PLS-DA validation. Moreover, the proposed LC-HRMS polyphenolic approach was employed to identify and measure adulteration levels in coffee samples using partial least squares (PLS) regression with prediction errors below 7.8%.
{"title":"Polyphenolic profiling of coffee beverages by Liquid Chromatography-High-Resolution mass Spectrometry for classification and characterization","authors":"Nerea Núñez , Javier Saurina , Oscar Núñez","doi":"10.1016/j.microc.2024.111770","DOIUrl":"10.1016/j.microc.2024.111770","url":null,"abstract":"<div><div>The importance of monitoring the presence of bioactive compounds as food attributes for sample classification and characterization is increasing. In this study, targeted Liquid Chromatography coupled with High-Resolution Mass Spectrometry (LC-HRMS) was employed to analyze the chemical profile of polyphenolic compounds as the source of information for the characterization and classification of 306 commercial coffee samples. Coffee holds a distinguished position as one of the most widely popular beverages globally but also one of the most easily adulterated. Regrettably, in recent times, instances of coffee adulteration have been on the rise. Consequently, implementing rigorous quality control measures for coffee becomes imperative to guarantee its quality. The results obtained in this work confirm that the proposed chemical profiles serve as excellent descriptors for sample characterization and classification through the implementation of principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA), achieving classification rates higher than 83.3% in PLS-DA validation. Moreover, the proposed LC-HRMS polyphenolic approach was employed to identify and measure adulteration levels in coffee samples using partial least squares (PLS) regression with prediction errors below 7.8%.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111770"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142326390","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111756
Xin Zhang , Qianyue Jia , Yuewu Shi , Zhiying Gao , Amr Amin , Yingqiu Xie , Yong Li
Ribonuclease H (RNase H) plays a crucial role in a variety of cellular processes and is emerging as an essential therapeutic target for many diseases. Various methods have been constructed to assay RNase H activity, but these methods are either time-consuming or have poor sensitivity. In this study, we developed a novel strategy that combined a specially designed DNA/RNA chimeric substrate with exponential amplification reaction (EXPAR) for rapid and sensitive detection of RNase H activity. In the presence of RNase H, the RNA strand of the DNA/RNA heteroduplex was specifically degraded, forming a 3′-hydroxyl group in the locking primer for recognition and extension by DNA polymerase. This ultimately triggered EXPAR and produced a large number of single-stranded DNA, which was monitored in real-time with fluorescent dye. Under optimized conditions, the proposed strategy can detect as low as 6 × 10−10 U/μL of RNase H, which was at least 1000 times more sensitive than several reported methods. Furthermore, we demonstrated the usage of this method for RNase H inhibitor analysis and practical application in complex biological samples, including serum and tumor cell extracts. Therefore, these results suggested that the developed method is a promising tool for highly sensitive detection of RNase H and RNase H-associated disease diagnosis.
核糖核酸酶 H（RNase H）在多种细胞过程中发挥着至关重要的作用，正在成为许多疾病的重要治疗靶点。目前已经构建了多种方法来检测 RNase H 的活性，但这些方法要么耗时长，要么灵敏度低。在这项研究中，我们开发了一种新策略，将专门设计的 DNA/RNA 嵌合底物与指数扩增反应（EXPAR）相结合，快速灵敏地检测 RNase H 的活性。在 RNase H 的存在下，DNA/RNA 异源双链的 RNA 链被特异性降解，在锁定引物中形成一个 3′-羟基，供 DNA 聚合酶识别和延伸。这最终触发了 EXPAR，产生了大量单链 DNA，并用荧光染料对其进行实时监测。在优化的条件下，所提出的策略可以检测到低至 6 × 10-10 U/μL 的 RNase H，其灵敏度比已报道的几种方法至少高出 1000 倍。此外，我们还展示了该方法在 RNase H 抑制剂分析中的应用，以及在复杂生物样本（包括血清和肿瘤细胞提取物）中的实际应用。因此，这些结果表明，所开发的方法在高灵敏度检测 RNase H 和 RNase H 相关疾病诊断方面是一种很有前途的工具。
{"title":"Highly sensitive detection of RNase H via a novel DNA/RNA heteroduplex combining isothermal exponential amplification strategy","authors":"Xin Zhang , Qianyue Jia , Yuewu Shi , Zhiying Gao , Amr Amin , Yingqiu Xie , Yong Li","doi":"10.1016/j.microc.2024.111756","DOIUrl":"10.1016/j.microc.2024.111756","url":null,"abstract":"<div><div>Ribonuclease H (RNase H) plays a crucial role in a variety of cellular processes and is emerging as an essential therapeutic target for many diseases. Various methods have been constructed to assay RNase H activity, but these methods are either time-consuming or have poor sensitivity. In this study, we developed a novel strategy that combined a specially designed DNA/RNA chimeric substrate with exponential amplification reaction (EXPAR) for rapid and sensitive detection of RNase H activity. In the presence of RNase H, the RNA strand of the DNA/RNA heteroduplex was specifically degraded, forming a 3′-hydroxyl group in the locking primer for recognition and extension by DNA polymerase. This ultimately triggered EXPAR and produced a large number of single-stranded DNA, which was monitored in real-time with fluorescent dye. Under optimized conditions, the proposed strategy can detect as low as 6 × 10<sup>−10</sup> U/μL of RNase H, which was at least 1000 times more sensitive than several reported methods. Furthermore, we demonstrated the usage of this method for RNase H inhibitor analysis and practical application in complex biological samples, including serum and tumor cell extracts. Therefore, these results suggested that the developed method is a promising tool for highly sensitive detection of RNase H and RNase H-associated disease diagnosis.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111756"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142317843","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-24DOI: 10.1016/j.microc.2024.111753
Helí Potes-Rodríguez , Juan Manuel Marchante-Gayón , Pablo Rodríguez-González , Ana V. Filgueiras , Lucia Viñas , Begoña Pérez-Fernández , Rubén Moreno-González , Cristina López-Galindo , Juan Antonio Campillo González , J. Ignacio García Alonso
The use of organotin compounds, especially tributyltin (TBT), on ships as anti-fouling agent was banned in 1999 by the International Maritime Organization (IMO) due to their risk for the marine environment. Unfortunately, butylated organotin compounds have remained in the environment due to their high stability, accumulating in marine sediments. Current European legislation requires the continuous monitoring of the levels of organotin compounds in coastal marine sediments. Therefore, the aim of this work was the development and application of a fast and reliable analytical methodology that could be easily implemented for a routine basis to quantify the levels of TBT and its degradation products dibutyltin (DBT) and monobutyltin (MBT) in marine sediments at the low ng/g levels dry weight (d.w.). The technique chosen was Gas Chromatography coupled to electron ionization and tandem Mass Spectrometry after ethylation of the organotin compounds. Extraction of the organotin compounds from the sediment was carried out by 1:3 mixture of methanol and acetic acid. Quantification was carried out by Isotope Dilution Mass Spectrometry (IDMS) using 119Sn-labelled compounds. The detection limits which can be reached for TBT, DBT and MBT were 0.3, 0.3 and 0.1 ng·g−1 d.w. respectively. Validation was carried out with three reference materials (BCR-462, BCR-646 and PACS-2) with satisfactory results. Relative standard deviations were, in all cases, less than 5 % for all compounds. The method was applied to the first monitorization of 87 coastal marine sediments covering the whole Spanish maritime waters. TBT was identified in 13 % of the samples analyzed in the Mediterranean Sea and in 6 % of the samples from the Atlantic Ocean. The implication of the results for coastal monitoring is also discussed.
{"title":"Isotope dilution gas chromatography coupled to electron ionization and tandem mass spectrometry for the determination of butyltin compounds in the Spanish coastal marine sediments","authors":"Helí Potes-Rodríguez , Juan Manuel Marchante-Gayón , Pablo Rodríguez-González , Ana V. Filgueiras , Lucia Viñas , Begoña Pérez-Fernández , Rubén Moreno-González , Cristina López-Galindo , Juan Antonio Campillo González , J. Ignacio García Alonso","doi":"10.1016/j.microc.2024.111753","DOIUrl":"10.1016/j.microc.2024.111753","url":null,"abstract":"<div><div>The use of organotin compounds, especially tributyltin (TBT), on ships as anti-fouling agent was banned in 1999 by the International Maritime Organization (IMO) due to their risk for the marine environment. Unfortunately, butylated organotin compounds have remained in the environment due to their high stability, accumulating in marine sediments. Current European legislation requires the continuous monitoring of the levels of organotin compounds in coastal marine sediments. Therefore, the aim of this work was the development and application of a fast and reliable analytical methodology that could be easily implemented for a routine basis to quantify the levels of TBT and its degradation products dibutyltin (DBT) and monobutyltin (MBT) in marine sediments at the low ng/g levels dry weight (d.w.). The technique chosen was Gas Chromatography coupled to electron ionization and tandem Mass Spectrometry after ethylation of the organotin compounds. Extraction of the organotin compounds from the sediment was carried out by 1:3 mixture of methanol and acetic acid. Quantification was carried out by Isotope Dilution Mass Spectrometry (IDMS) using <sup>119</sup>Sn-labelled compounds. The detection limits which can be reached for TBT, DBT and MBT were 0.3, 0.3 and 0.1 ng·g<sup>−1</sup> d.w. respectively. Validation was carried out with three reference materials (BCR-462, BCR-646 and PACS-2) with satisfactory results. Relative standard deviations were, in all cases, less than 5 % for all compounds. The method was applied to the first monitorization of 87 coastal marine sediments covering the whole Spanish maritime waters. TBT was identified in 13 % of the samples analyzed in the Mediterranean Sea and in 6 % of the samples from the Atlantic Ocean. The implication of the results for coastal monitoring is also discussed.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111753"},"PeriodicalIF":4.9,"publicationDate":"2024-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142357864","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-23DOI: 10.1016/j.microc.2024.111707
Dipakkumar Bariya, Satyendra Mishra
Amines are ubiquitous in biological world, yet are toxic and harmful in nature. To preserve the quality and safety of these packaged meals, it’s critical to identify biogenic amines that are emitted from spoiled meat, fish, or dairy products. To this endeavour, herein we report bile acid based triazole derivative with phenothiazine that are capable of sensing various amines by rapid change of fluorescence colour or intensity. The triazole derivatives exhibit a multiphase sensing platform by effectively sensing amine vapours or solutions in both solid and solution phases. Probes in the vapour state exhibit very quick interaction to primary amines (26 s for CTPTZ) and strong sensitivity to putrescine, which is a common example of biogenic amines (BAs). We have employed our unique sensing triazole derivative as a spoilage indication for meat. It detects biogenic amines from spoiled food and produces an optical response. Significant changes in both visual and luminescent were noted within 4–18 h of packaging at room temperature (∼25 °C). The rapid response that biogenic amines provide to these molecular sensors makes them highly promising for applications in the food packaging industry, medical diagnostics, and other sensory devices.
{"title":"Fluorescent-based bile acid triazole-phenothiazine derivatives: Multiphase detection of biogenic amines and application in spoiled foods","authors":"Dipakkumar Bariya, Satyendra Mishra","doi":"10.1016/j.microc.2024.111707","DOIUrl":"10.1016/j.microc.2024.111707","url":null,"abstract":"<div><div>Amines are ubiquitous in biological world, yet are toxic and harmful in nature. To preserve the quality and safety of these packaged meals, it’s critical to identify biogenic amines that are emitted from spoiled meat, fish, or dairy products. To this endeavour, herein we report bile acid based triazole derivative with phenothiazine that are capable of sensing various amines by rapid change of fluorescence colour or intensity. The triazole derivatives exhibit a multiphase sensing platform by effectively sensing amine vapours or solutions in both solid and solution phases. Probes in the vapour state exhibit very quick interaction to primary amines (26 s for CTPTZ) and strong sensitivity to putrescine, which is a common example of biogenic amines (BAs). We have employed our unique sensing triazole derivative as a spoilage indication for meat. It detects biogenic amines from spoiled food and produces an optical response. Significant changes in both visual and luminescent were noted within 4–18 h of packaging at room temperature (∼25 °C). The rapid response that biogenic amines provide to these molecular sensors makes them highly promising for applications in the food packaging industry, medical diagnostics, and other sensory devices.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111707"},"PeriodicalIF":4.9,"publicationDate":"2024-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142322201","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-23DOI: 10.1016/j.microc.2024.111691
Ana Torres-Agullo, Romà Tauler, Silvia Lacorte
The global use of phthalate esters (PAEs) in plastic production entails a need for developing effective remediation strategies to minimize exposure and health risks. In this study, pyrolysis degradation processes are evaluated for 17 different PAEs that were analyzed by high-resolution gas chromatography-mass spectrometry (Pyr-GC-Orbitrap-MS) at different temperatures (300 °C, 400 °C, 500 °C, 600 °C, 700 °C, 800 °C) both in electron ionization (EI) and positive chemical ionization (PCI) mode. All the analytical data generated have been processed with the Regions of Interest Multivariate Curve Resolution (ROIMCR) chemometrics method. A preliminary selection of the Mass Spectrometry Regions of Interest (ROIs) coupled to a bilinear factor decomposition method (MCR-ALS) allowed the identification of 4 principal components, which were used to define the thermal degradation process. ROIMCR method is a powerful tool for non-targeted analysis which allows the resolution of the elution and spectral profiles of the different constituents present in the analyzed samples, which were confirmed using PCI. Moreover, ROIMCR was used to resolve and identify the different products generated during the studied degradation processes. As a result, 10 new thermal degradation products were identified in the analysis of the different sample sets. Finally, the degradation efficiencies higher than 99.8 % were obtained for all the PAEs at 800 °C, except for benzoic acid-benzyl ester, whose removal efficiency decreased to 94.8 %. As phthalates are widespread and toxic compounds for the environment and for humans, there is a need for new remediation technologies. This study provides new knowledge to understand their elimination through thermal processes. We combine mass spectrometric data with powerful chemometric processing to determine the removal efficiency, to understand the degradation process and to identify the degradation compounds formed through thermal decomposition.
{"title":"Exploring the pyrolytic degradation of seventeen phthalate esters using the non-targeted regions of interest-multivariate curve resolution (ROIMCR) chemometric method","authors":"Ana Torres-Agullo, Romà Tauler, Silvia Lacorte","doi":"10.1016/j.microc.2024.111691","DOIUrl":"10.1016/j.microc.2024.111691","url":null,"abstract":"<div><div>The global use of phthalate esters (PAEs) in plastic production entails a need for developing effective remediation strategies to minimize exposure and health risks. In this study, pyrolysis degradation processes are evaluated for 17 different PAEs that were analyzed by high-resolution gas chromatography-mass spectrometry (Pyr-GC-Orbitrap-MS) at different temperatures (300 °C, 400 °C, 500 °C, 600 °C, 700 °C, 800 °C) both in electron ionization (EI) and positive chemical ionization (PCI) mode. All the analytical data generated have been processed with the Regions of Interest Multivariate Curve Resolution (ROIMCR) chemometrics method. A preliminary selection of the Mass Spectrometry Regions of Interest (ROIs) coupled to a bilinear factor decomposition method (MCR-ALS) allowed the identification of 4 principal components, which were used to define the thermal degradation process. ROIMCR method is a powerful tool for non-targeted analysis which allows the resolution of the elution and spectral profiles of the different constituents present in the analyzed samples, which were confirmed using PCI. Moreover, ROIMCR was used to resolve and identify the different products generated during the studied degradation processes. As a result, 10 new thermal degradation products were identified in the analysis of the different sample sets. Finally, the degradation efficiencies higher than 99.8 % were obtained for all the PAEs at 800 °C, except for benzoic acid-benzyl ester, whose removal efficiency decreased to 94.8 %. As phthalates are widespread and toxic compounds for the environment and for humans, there is a need for new remediation technologies. This study provides new knowledge to understand their elimination through thermal processes. We combine mass spectrometric data with powerful chemometric processing to determine the removal efficiency, to understand the degradation process and to identify the degradation compounds formed through thermal decomposition.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111691"},"PeriodicalIF":4.9,"publicationDate":"2024-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142322052","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-23DOI: 10.1016/j.microc.2024.111710
Pawan Kumar Sada , Amanpreet Kaur Jassal , Amit Bar , Prabhat Kumar , S. Srikrishna , Sumit Kumar , Alok Kumar Singh , Youngil Lee , Laxman Singh , Abhishek Rai
A new rhodamine appended probe 3-allyl salicylaldehyde rhodamine hydrazone (RGAL) has been synthesized and thoroughly characterized using various spectroscopic techniques, as well as single crystal XRD. The optical properties of RGAL were investigated in 10 mM HEPES buffer in H2O:CH3CN (2:8, v/v, pH=7.2) in the presence of various cations. RGAL showed selectivity and sensitivity towards Cu2+ during absorption process and “turn on” behavior towards Fe3+ during emission study owing to the opening of a spirolactum ring. The detection limits for Cu2+ and Fe3+ ions using RGAL were determined to be 6.15 ppm and 4.75 ppm, respectively. The binding constant of RGAL with Cu2+ and Fe3+ ions was found to be 1.20 × 104 M−1 and 1.71 × 104 M−1, respectively. Hirshfeld surface and fingerprint analysis of RGAL provides the in-depth analysis of pairwise interaction between two atoms. Furthermore, the topological analysis of RGAL is performed using NCI, AIM, ELF and LOL analysis. The analysis provides information about O78-H79…N71 and C40-H41…O77 hydrogen bonding interactions in the monomer of RGAL whereas various inter- and intra- molecular interactions give strength to the dimer pattern of RGAL.
{"title":"Development of a new rhodamine 6G based probe and its application as an optical sensor of Cu2+ and Fe3+ ions: A comprehensive experimental and Theoretical studies","authors":"Pawan Kumar Sada , Amanpreet Kaur Jassal , Amit Bar , Prabhat Kumar , S. Srikrishna , Sumit Kumar , Alok Kumar Singh , Youngil Lee , Laxman Singh , Abhishek Rai","doi":"10.1016/j.microc.2024.111710","DOIUrl":"10.1016/j.microc.2024.111710","url":null,"abstract":"<div><div>A new rhodamine appended probe 3-allyl salicylaldehyde rhodamine hydrazone (<strong>RGAL</strong>) has been synthesized and thoroughly characterized using various spectroscopic techniques, as well as single crystal XRD. The optical properties of <strong>RGAL</strong> were investigated in 10 mM HEPES buffer in H<sub>2</sub>O:CH<sub>3</sub>CN (2:8, v/v, pH=7.2) in the presence of various cations. <strong>RGAL</strong> showed selectivity and sensitivity towards Cu<sup>2+</sup> during absorption process and “turn on” behavior towards Fe<sup>3+</sup> during emission study owing to the opening of a spirolactum ring. The detection limits for Cu<sup>2+</sup> and Fe<sup>3+</sup> ions using <strong>RGAL</strong> were determined to be 6.15 ppm and 4.75 ppm, respectively. The binding constant of <strong>RGAL</strong> with Cu<sup>2+</sup> and Fe<sup>3+</sup> ions was found to be 1.20 × 10<sup>4</sup> M<sup>−1</sup> and 1.71 × 10<sup>4</sup> M<sup>−1</sup>, respectively. Hirshfeld surface and fingerprint analysis of <strong>RGAL</strong> provides the in-depth analysis of pairwise interaction between two atoms. Furthermore, the topological analysis of <strong>RGAL</strong> is performed using NCI, AIM, ELF and LOL analysis. The analysis provides information about O78-H79…N71 and C40-H41…O77 hydrogen bonding interactions in the<!--> <!-->monomer of <strong>RGAL</strong> whereas various inter- and intra- molecular interactions give strength to the dimer pattern of <strong>RGAL</strong>.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"207 ","pages":"Article 111710"},"PeriodicalIF":4.9,"publicationDate":"2024-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142357858","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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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