Microchemical Journal最新文献

Effect of different solvents on biological attributes of olive leaves extracts of newly cultivated varieties:GC–MS based investigations

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-06 DOI: 10.1016/j.microc.2025.113281

Sami Ullah , Muhammad Azhar Iqbal

This study investigates the optimal solvents for extraction of bioactives from olive leaves, analyzing the yield, phenolic and flavonoid content, antioxidant, thrombolytic, antimicrobial activities, and chemical profiles of extracts from three olive varieties: Kalamata, Sikitita, and Chietina. During ultrasonic-assisted extraction, the highest extract yield (472.96 mg/g) was achieved with water, while the lowest (224.31 mg/g) antioxidant extract yield was obtained with absolute methanol. On the other hand, aqueous ethanolic extracts (AEEs) demonstrated the highest total phenolics (28.17 mg GAE/g DW) and flavonoids (170.67 mg RE/g DW) contents, along with significant antioxidant activities as measured by 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and ferric reducing antioxidant power (FRAP) assays. Gas chromatography–mass spectrometry (GC–MS) analysis of these extracts revealed the presence of high-valuebioactive compounds such as oleic acid, β-sitosterol, and 2-methoxy-4-vinylphenol, known for their health benefits. Moreover, hemolytic and thrombolytic activities revealed the safer and health-promoting potential of tested extracts. Carbohydrate analysis identified glucose as the most abundant sugar, while organic acid profiling highlighted tartaric acid as predominant. The AEEs extracts were the most effective against Gram-positive pathogens, particularly Staphylococcus aureus, but were less effective against Gram-negative bacteria. These findings highlight the importance of solvent choice in maximizing the extraction of bioactives and suggest the potential of olive leaf extracts for developing nutraceuticals and functional foods.

{"title":"Effect of different solvents on biological attributes of olive leaves extracts of newly cultivated varieties:GC–MS based investigations","authors":"Sami Ullah , Muhammad Azhar Iqbal","doi":"10.1016/j.microc.2025.113281","DOIUrl":"10.1016/j.microc.2025.113281","url":null,"abstract":"<div><div>This study investigates the optimal solvents for extraction of bioactives from olive leaves, analyzing the yield, phenolic and flavonoid content, antioxidant, thrombolytic, antimicrobial activities, and chemical profiles of extracts from three olive varieties: Kalamata, Sikitita, and Chietina. During ultrasonic-assisted extraction, the highest extract yield (472.96 mg/g) was achieved with water, while the lowest (224.31 mg/g) antioxidant extract yield was obtained with absolute methanol. On the other hand, aqueous ethanolic extracts (AEEs) demonstrated the highest total phenolics (28.17 mg GAE/g DW) and flavonoids (170.67 mg RE/g DW) contents, along with significant antioxidant activities as measured by 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and ferric reducing antioxidant power (FRAP) assays. Gas chromatography–mass spectrometry (GC–MS) analysis of these extracts revealed the presence of high-valuebioactive compounds such as oleic acid, <em>β</em>-sitosterol, and 2-methoxy-4-vinylphenol, known for their health benefits. Moreover, hemolytic and thrombolytic activities revealed the safer and health-promoting potential of tested extracts. Carbohydrate analysis identified glucose as the most abundant sugar, while organic acid profiling highlighted tartaric acid as predominant. The AEEs extracts were the most effective against Gram-positive pathogens, particularly <em>Staphylococcus aureus</em>, but were less effective against Gram-negative bacteria. These findings highlight the importance of solvent choice in maximizing the extraction of bioactives and suggest the potential of olive leaf extracts for developing nutraceuticals and functional foods.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113281"},"PeriodicalIF":4.9,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561759","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}

引用次数: 0

A SERS-Fluorescence dual-mode fiber sensor for monitoring in FRET system

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-05 DOI: 10.1016/j.microc.2025.113259

Zhihan Zheng , Yan Liu , Minglu Li , Huifang Chen , Shen Chen , Chengqi Lin , Xiaowei Jiang , Huihuang Lin , Simin Hong , Neil G.R. Broderick , Ben Xu , Juan Kang , Chunliu Zhao , Yi Wang

In a complex Förster resonance energy transfer (FRET) system, it is necessary to monitor the composition change, chemical structural construction or intermolecular interactions. The fluorescence detecting method is not sufficient to supply such information. In this paper, a dual-mode fiber sensor for monitoring in FRET system is proposed. SERS and fluorescence detection can be realized with only one fiber probe. The sensor was designed on separated regions for each mode detections. The sensing capacities was tested, the lowest LOD was calculated to be 1.38 × 10⁻¹⁴ M in SERS detections. A FRET system was simulated with Rhodamine 6G (R6G) and Rhodamine B (RhB). There are FRET, spectra overlap, and competition on substrate between the two dyes, which makes the mixture a typical and complex FRET system. With the proposed sensor, the fluorescence intensity change was monitored, at the same time, a small portion of R6G (1/500 in high concentration and 1/10⁵ in low concentration) in the mixture be recognized with SERS detection. We further detected the illegal addition of Rhodamine in commercially available 100 % orange juice. Even when fluorescence could not detect it, R6G could still be effectively detected by SERS method at a concentration of 10⁻¹⁰ M. By the help of this dual-mode sensing device, the process of chemical reaction in FRET system could be monitored, and more widely applications of FRET technique could be realized.

{"title":"A SERS-Fluorescence dual-mode fiber sensor for monitoring in FRET system","authors":"Zhihan Zheng , Yan Liu , Minglu Li , Huifang Chen , Shen Chen , Chengqi Lin , Xiaowei Jiang , Huihuang Lin , Simin Hong , Neil G.R. Broderick , Ben Xu , Juan Kang , Chunliu Zhao , Yi Wang","doi":"10.1016/j.microc.2025.113259","DOIUrl":"10.1016/j.microc.2025.113259","url":null,"abstract":"<div><div>In a complex Förster resonance energy transfer (FRET) system, it is necessary to monitor the composition change, chemical structural construction or intermolecular interactions. The fluorescence detecting method is not sufficient to supply such information. In this paper, a dual-mode fiber sensor for monitoring in FRET system is proposed. SERS and fluorescence detection can be realized with only one fiber probe. The sensor was designed on separated regions for each mode detections. The sensing capacities was tested, the lowest LOD was calculated to be 1.38 × 10<sup>−14</sup> M in SERS detections. A FRET system was simulated with Rhodamine 6G (R6G) and Rhodamine B (RhB). There are FRET, spectra overlap, and competition on substrate between the two dyes, which makes the mixture a typical and complex FRET system. With the proposed sensor, the fluorescence intensity change was monitored, at the same time, a small portion of R6G (1/500 in high concentration and 1/10<sup>5</sup> in low concentration) in the mixture be recognized with SERS detection. We further detected the illegal addition of Rhodamine in commercially available 100 % orange juice. Even when fluorescence could not detect it, R6G could still be effectively detected by SERS method at a concentration of 10<sup>−10</sup> M. By the help of this dual-mode sensing device, the process of chemical reaction in FRET system could be monitored, and more widely applications of FRET technique could be realized.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113259"},"PeriodicalIF":4.9,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561825","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}

引用次数: 0

Biphasic electrochemical immunoassay based on tyramine-DNA cascade signal amplification for detection of interleukin-8 in human saliva samples

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113240

Tao Wang , Cheng Zhang , Huajuan Ye , Han Jie , Yu Qiu , Ning Li , Junyang Zhuang

Oral cancer poses a significant global public health challenge. The sensitive detection of salivary biomarkers, such as interleukin-8 (IL-8), holds promise for the early diagnosis of oral cancer. In this work, we developed a novel biphasic electrochemical immunoassay (BEIA) method for highly sensitive IL-8 detection in human saliva samples by integrating the conventional immunoassay method with homogeneous electrochemical sensing model. The recognition of IL-8 is achieved through a sandwich immunoreaction on the surface of magnetic beads (MBs). Subsequently, tyramide signal amplification (TSA) is performed to capture a large number of trigger DNA probes on MBs. These trigger DNA probes then initiate an exonuclease III-assisted signal amplification (EASA) reaction, resulting in the hydrolysis of numerous methylene blue (MB)-labeled signal DNA strands and release of MB into solution phase. The electrochemical signal of MB in solution phase is then monitored on an indium tin oxide (ITO) electrode using square wave voltammetry (SWV). With the introduction of TSA-EASA cascade signal amplification, IL-8 can be detected with high sensitivity. The developed method demonstrates a good linear relationship with IL-8 in the concentration range of 1.0 pg mL⁻¹ to 1000 pg mL⁻¹ and achieves a detection limit of 0.28 pg mL⁻¹ (S/N = 3). Additionally, the developed method exhibits high selectivity and can accurately determine IL-8 levels in clinical salivary samples, offering a promising alternative for point-of-care testing and early-stage diagnosis of oral cancer. Furthermore, the method can be easily adapted for the detection of other targets through the simple substitution of antibody pairs.

{"title":"Biphasic electrochemical immunoassay based on tyramine-DNA cascade signal amplification for detection of interleukin-8 in human saliva samples","authors":"Tao Wang , Cheng Zhang , Huajuan Ye , Han Jie , Yu Qiu , Ning Li , Junyang Zhuang","doi":"10.1016/j.microc.2025.113240","DOIUrl":"10.1016/j.microc.2025.113240","url":null,"abstract":"<div><div>Oral cancer poses a significant global public health challenge. The sensitive detection of salivary biomarkers, such as interleukin-8 (IL-8), holds promise for the early diagnosis of oral cancer. In this work, we developed a novel biphasic electrochemical immunoassay (BEIA) method for highly sensitive IL-8 detection in human saliva samples by integrating the conventional immunoassay method with homogeneous electrochemical sensing model. The recognition of IL-8 is achieved through a sandwich immunoreaction on the surface of magnetic beads (MBs). Subsequently, tyramide signal amplification (TSA) is performed to capture a large number of trigger DNA probes on MBs. These trigger DNA probes then initiate an exonuclease III-assisted signal amplification (EASA) reaction, resulting in the hydrolysis of numerous methylene blue (MB)-labeled signal DNA strands and release of MB into solution phase. The electrochemical signal of MB in solution phase is then monitored on an indium tin oxide (ITO) electrode using square wave voltammetry (SWV). With the introduction of TSA-EASA cascade signal amplification, IL-8 can be detected with high sensitivity. The developed method demonstrates a good linear relationship with IL-8 in the concentration range of 1.0 pg mL<sup>−1</sup> to 1000 pg mL<sup>−1</sup> and achieves a detection limit of 0.28 pg mL<sup>−1</sup> (S/N = 3). Additionally, the developed method exhibits high selectivity and can accurately determine IL-8 levels in clinical salivary samples, offering a promising alternative for point-of-care testing and early-stage diagnosis of oral cancer. Furthermore, the method can be easily adapted for the detection of other targets through the simple substitution of antibody pairs.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113240"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561757","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}

引用次数: 0

Qualitative and quantitative comparison of compounds in different parts of Thalictrum foliolosum DC using UPLC-PDA/UHPLC-QTOF-IMS

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113244

Pooja Bhatt , Shinde Bhagatsing Devidas , Km Swati , Parul , Nitisha Sendri , Pamita Bhandari

Thalictrum foliolosum is least explored species of the Thalictrum genus. This plant is known for its immense utility in traditional folk medicine. Different parts of the plant hold various ethnomedicinal values that are yet to be explored from a phytochemical perspective. The current study primarily aimed to investigate and compare the diversity of metabolites in root and aerial parts (stems and leaves) of T. foliolosum. For this, a UPLC-PDA-based analytical approach has been employed for the estimation of five isoquinoline alkaloids [magnoflorine (8), thalidasine (18), jatrorrhizine (19), palmatine (20), and berberine (21)] in different extracts and fractions of the plant. Quantitative results revealed that roots contain the highest content of targeted alkaloids. The UPLC method showed ideal linearity (r² ≥ 0.999), quantification limit (0.13–0.51 μg/mL), detection limit (0.039–0.156 μg/mL), precision (intra-day RSDs < 0.33 %, and inter-day RSDs < 1.98 %), and accuracy (83.68 –104.13 %). Extensive metabolite profiling through UHPLC-QTOF-IMS tentatively identified 25 alkaloids while METLIN database identified 268, 104, and 102 metabolites of various classes in leaves, stems, and roots, respectively. This study is the first to offer thorough metabolite profiling in the plant. GC–MS-based targeted profiling showed the highest content of methyl palmitate (roots and leaves) and hexadecanoic acid (stems and leaves). The statistical evaluation of targeted and untargeted metabolites highlighted similarities and variances among the roots, stems, and leaves. Conclusively, these findings provide new insights into the metabolite distribution in T. foliolosum and underscore its potential for use in the pharmaceutical sector.

{"title":"Qualitative and quantitative comparison of compounds in different parts of Thalictrum foliolosum DC using UPLC-PDA/UHPLC-QTOF-IMS","authors":"Pooja Bhatt , Shinde Bhagatsing Devidas , Km Swati , Parul , Nitisha Sendri , Pamita Bhandari","doi":"10.1016/j.microc.2025.113244","DOIUrl":"10.1016/j.microc.2025.113244","url":null,"abstract":"<div><div><em>Thalictrum foliolosum</em> is least explored species of the <em>Thalictrum</em> genus. This plant is known for its immense utility in traditional folk medicine. Different parts of the plant hold various ethnomedicinal values that are yet to be explored from a phytochemical perspective. The current study primarily aimed to investigate and compare the diversity of metabolites in root and aerial parts (stems and leaves) of <em>T. foliolosum</em>. For this, a UPLC-PDA-based analytical approach has been employed for the estimation of five isoquinoline alkaloids [magnoflorine (<strong>8</strong>), thalidasine (<strong>18</strong>), jatrorrhizine (<strong>19</strong>), palmatine (<strong>20</strong>), and berberine (<strong>21</strong>)] in different extracts and fractions of the plant. Quantitative results revealed that roots contain the highest content of targeted alkaloids. The UPLC method showed ideal linearity (<em>r</em><sup>2</sup> ≥ 0.999), quantification limit (0.13–0.51 μg/mL), detection limit (0.039–0.156 μg/mL), precision (intra-day RSDs < 0.33 %, and inter-day RSDs < 1.98 %), and accuracy (83.68 –104.13 %). Extensive metabolite profiling through UHPLC-QTOF-IMS tentatively identified 25 alkaloids while METLIN database identified 268, 104, and 102 metabolites of various classes in leaves, stems, and roots, respectively. This study is the first to offer thorough metabolite profiling in the plant. GC–MS-based targeted profiling showed the highest content of methyl palmitate (roots and leaves) and hexadecanoic acid (stems and leaves). The statistical evaluation of targeted and untargeted metabolites highlighted similarities and variances among the roots, stems, and leaves. Conclusively, these findings provide new insights into the metabolite distribution in <em>T. foliolosum</em> and underscore its potential for use in the pharmaceutical sector.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113244"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561756","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}

引用次数: 0

Gold nanoparticle-based electrochemical immunosensor for the detection of Russell’s viper venom using IgY antibodies

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113247

S. Janani , Ankit Choraria , KV Ashok Raj , S. Rajeswari , R. Sivasubramanian , A. Michael , R. Selvakumar

In this study, we have developed for the first time a sensitive electrochemical immunosensor by electrostatically immobilizing IgY antibodies onto the citrate capped gold nanoparticle (ctAuNP) functionalized glassy carbon electrode (GCE) for the detection of Russell’s Viper (RV) venom in human blood and serum. Initially, the ctAuNP was prepared by a simple citrate reduction method. Simultaneously a novel approach of preparing RV IgY antibodies was raised in immunized chicken for this study. The ctAuNP-IgY modified electrode was characterized using cyclic voltammetry (CV) and the sensing was carried out using electrochemical impedance spectroscopy (EIS). The Nyquist plot was recorded for different concentrations of RV venom using signals produced during antigen–antibody interactions. The presence of ctAuNP helps in the adsorption of antibodies and also enhances the conductivity of the sensor. The limit of detection (LOD) was estimated to be 0.74 µg/mL with a linear range from 3.34 to 6.68 µg/mL of RV venom. The sensor was tested in both human serum and blood samples which showed a satisfactory recovery percentage ranging from 87.3 % to 110.4 % and 84.6 % to 108.5 % respectively. Stability studies showed that the surface-modified electrode retained 87 % of the initial sensitivity after storage at 4 °C for one week.

{"title":"Gold nanoparticle-based electrochemical immunosensor for the detection of Russell’s viper venom using IgY antibodies","authors":"S. Janani , Ankit Choraria , KV Ashok Raj , S. Rajeswari , R. Sivasubramanian , A. Michael , R. Selvakumar","doi":"10.1016/j.microc.2025.113247","DOIUrl":"10.1016/j.microc.2025.113247","url":null,"abstract":"<div><div>In this study, we have developed for the first time a sensitive electrochemical immunosensor by electrostatically immobilizing IgY antibodies onto the citrate capped gold nanoparticle (ctAuNP) functionalized glassy carbon electrode (GCE) for the detection of Russell’s Viper (RV) venom in human blood and serum. Initially, the ctAuNP was prepared by a simple citrate reduction method. Simultaneously a novel approach of preparing RV IgY antibodies was raised in immunized chicken for this study. The ctAuNP-IgY modified electrode was characterized using cyclic voltammetry (CV) and the sensing was carried out using electrochemical impedance spectroscopy (EIS). The Nyquist plot was recorded for different concentrations of RV venom using signals produced during antigen–antibody interactions. The presence of ctAuNP helps in the adsorption of antibodies and also enhances the conductivity of the sensor. The limit of detection (LOD) was estimated to be 0.74 µg/mL with a linear range from 3.34 to 6.68 µg/mL of RV venom. The sensor was tested in both human serum and blood samples which showed a satisfactory recovery percentage ranging from 87.3 % to 110.4 % and 84.6 % to 108.5 % respectively. Stability studies showed that the surface-modified electrode retained 87 % of the initial sensitivity after storage at 4 °C for one week.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113247"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561758","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}

引用次数: 0

Deep learning assisted ATR-FTIR and Raman spectroscopy fusion technology for microplastic identification

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113224

Haoze Li , Shihan Xu , Jiahao Teng , Xiangheng Jiang , Han Zhang , Yazhou Qin , Yingsheng He , Li Fan

Microplastics, recognized as persistent environmental pollutants, have garnered significant global attention due to their widespread distribution and resistance to degradation. Accurate identification and classification of microplastics are crucial for monitoring pollution levels and assessing potential health risks. In this study, we employed Raman spectroscopy and Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) to analyze eight types of microplastics, establish a spectroscopic database. Additionally, we developed a one-dimensional convolutional neural network (1D-CNN) model that incorporates an embedded multi-head attention mechanism for the classification of eight kinds of microplastics. The recognition accuracy is 73% for ATR-FTIR and 75% for Raman. In order to overcome the shortcomings of single spectral data, a three-level data fusion classification and recognition algorithm were developed to leverage the complementary strengths of ATR-FTIR and Raman spectroscopy. The classification accuracies achieved by the low-level, mid-level, and high-level fusion models were 88%, 97%, and 99%, respectively. We further investigate the model’s applicability to real samples, by conduct spiked tests across three different media (milk, coke and tap water). The data obtained from these tests served as an external validation set to assess the model’s generalization ability. Notably, the recognition accuracy of the high-level fusion model exceeds 98% in all three spiked media. This study provides a more robust and effective method for the accurate classification and identification of microplastic.

{"title":"Deep learning assisted ATR-FTIR and Raman spectroscopy fusion technology for microplastic identification","authors":"Haoze Li , Shihan Xu , Jiahao Teng , Xiangheng Jiang , Han Zhang , Yazhou Qin , Yingsheng He , Li Fan","doi":"10.1016/j.microc.2025.113224","DOIUrl":"10.1016/j.microc.2025.113224","url":null,"abstract":"<div><div>Microplastics, recognized as persistent environmental pollutants, have garnered significant global attention due to their widespread distribution and resistance to degradation. Accurate identification and classification of microplastics are crucial for monitoring pollution levels and assessing potential health risks. In this study, we employed Raman spectroscopy and Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) to analyze eight types of microplastics, establish a spectroscopic database. Additionally, we developed a one-dimensional convolutional neural network (1D-CNN) model that incorporates an embedded multi-head attention mechanism for the classification of eight kinds of microplastics. The recognition accuracy is 73% for ATR-FTIR and 75% for Raman. In order to overcome the shortcomings of single spectral data, a three-level data fusion classification and recognition algorithm were developed to leverage the complementary strengths of ATR-FTIR and Raman spectroscopy. The classification accuracies achieved by the low-level, mid-level, and high-level fusion models were 88%, 97%, and 99%, respectively. We further investigate the model’s applicability to real samples, by conduct spiked tests across three different media (milk, coke and tap water). The data obtained from these tests served as an external validation set to assess the model’s generalization ability. Notably, the recognition accuracy of the high-level fusion model exceeds 98% in all three spiked media. This study provides a more robust and effective method for the accurate classification and identification of microplastic.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113224"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547966","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}

引用次数: 0

Monolithic capillary columns based on methacryl-substituted polyhedral oligomeric silsesquioxane and sulfobetaine methacrylates synthesized in the wide-bore capillary: Evaluation and application in liquid chromatography

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113239

Dana Moravcová, Josef Planeta, Zuzana Gogaľová, Jozef Šesták, Matej Ščepán, Pavel Karásek, Michal Roth

The protocol for preparation of methacryl-substituted polyhedral oligomeric silsesquioxane-based monolithic stationary phases containing zwitterionic sulfobetaine monomers in 450 µm i.d. fused silica capillaries is presented. The monolithic columns were evaluated by scanning electron microscopy, inverse size-exclusion chromatography, and isocratic HPLC separation of model compounds. Nature of zwitterionic sulfobetaine monomers has distinct impact on the structure of the final monolithic material as well as on its polarity and separation ability. The columns are suitable for multimodal chromatography as confirmed by their capability to separate compounds over a wide range of polarities (alkylbenzenes, phenolics, aromatic carboxylic acids, a mixture of purine-, pyrimidine-bases, nucleosides, and 2-deoxynucleosides). The critical mobile phase composition for the transition from hydrophilic interaction liquid chromatography to reversed-phase mode is around 84 % of acetonitrile which confirms the prevailing non-polar nature of formed monoliths. The proposed preparation protocol allowed preparation of stable columns whose efficiency reached the minimal height of the theoretical plate 6–10 µm which decreased by less than 12 % during the two months of everyday use.

{"title":"Monolithic capillary columns based on methacryl-substituted polyhedral oligomeric silsesquioxane and sulfobetaine methacrylates synthesized in the wide-bore capillary: Evaluation and application in liquid chromatography","authors":"Dana Moravcová, Josef Planeta, Zuzana Gogaľová, Jozef Šesták, Matej Ščepán, Pavel Karásek, Michal Roth","doi":"10.1016/j.microc.2025.113239","DOIUrl":"10.1016/j.microc.2025.113239","url":null,"abstract":"<div><div>The protocol for preparation of methacryl-substituted polyhedral oligomeric silsesquioxane-based monolithic stationary phases containing zwitterionic sulfobetaine monomers in 450 µm i.d. fused silica capillaries is presented. The monolithic columns were evaluated by scanning electron microscopy, inverse size-exclusion chromatography, and isocratic HPLC separation of model compounds. Nature of zwitterionic sulfobetaine monomers has distinct impact on the structure of the final monolithic material as well as on its polarity and separation ability. The columns are suitable for multimodal chromatography as confirmed by their capability to separate compounds over a wide range of polarities (alkylbenzenes, phenolics, aromatic carboxylic acids, a mixture of purine-, pyrimidine-bases, nucleosides, and 2-deoxynucleosides). The critical mobile phase composition for the transition from hydrophilic interaction liquid chromatography to reversed-phase mode is around 84 % of acetonitrile which confirms the prevailing non-polar nature of formed monoliths. The proposed preparation protocol allowed preparation of stable columns whose efficiency reached the minimal height of the theoretical plate 6–10 µm which decreased by less than 12 % during the two months ofeveryday use.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113239"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561826","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}

引用次数: 0

Single-electrode electrochemiluminescence immunoarray combined with smartphone for high-throughput detection of heart-type fatty acid binding protein

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113249

Mingquan Guo , Yifeng Pan , Dexin Du , Liangbiao Wang , Wei Nie

Acute myocardial infarction (AMI) is a cardiovascular disease with high fatality and acute morbidity. The timely diagnosis and treatment are vital for improving recovery of AMI patients. Heart-type fatty acid binding protein (h-FABP) is an important biomarker for early assessment and exclusion of AMI. Herein, we developed single-electrode electrochemiluminescence (ECL) immunoarray for high throughput and portable detection of h-FABP. This ECL immunoarray was fabricated by successively assembling ECL nanocomposites and h-FABP conjugated gold nanoparticles on the surface of indium tin oxide microchips electrodes and the bovine serum albumin was used in blocking nonspecific binding sites, which can be used for detection of h-FABP. In the presence of h-FABP, the ECL intensity increased with increasing concentration. Thus, a high throughput and portable immunoarray was established for the determination of h-FABP with a linear dynamic range from 0.1 to 1000 pg/mL and a detection limit of 0.09 pg/mL, which exhibited excellent performance compared with other ECL methods. Moreover, the developed ECL immunoarray was used in detecting the h-FABP in clinical sample of human serum, which demonstrated good recoveries in the range of 92.20 %∼108.00 %. Therefore, the proposed ECL immunoarray can effectively handle the determination of clinical samples, which was promising for using the early screening or exclusion for AMI at home or in an ambulance due to portable detection based on smartphone. This strategy is very promising to effectively reduce fatality and acute morbidity of AMI patients.

{"title":"Single-electrode electrochemiluminescence immunoarray combined with smartphone for high-throughput detection of heart-type fatty acid binding protein","authors":"Mingquan Guo , Yifeng Pan , Dexin Du , Liangbiao Wang , Wei Nie","doi":"10.1016/j.microc.2025.113249","DOIUrl":"10.1016/j.microc.2025.113249","url":null,"abstract":"<div><div>Acute myocardial infarction (AMI) is a cardiovascular disease with high fatality and acute morbidity. The timely diagnosis and treatment are vital for improving recovery of AMI patients. Heart-type fatty acid binding protein (h-FABP) is an important biomarker for early assessment and exclusion of AMI. Herein, we developed single-electrode electrochemiluminescence (ECL) immunoarray for high throughput and portable detection of h-FABP. This ECL immunoarray was fabricated by successively assembling ECL nanocomposites and h-FABP conjugated gold nanoparticles on the surface of indium tin oxide microchips electrodes and the bovine serum albumin was used in blocking nonspecific binding sites, which can be used for detection of h-FABP. In the presence of h-FABP, the ECL intensity increased with increasing concentration. Thus, a high throughput and portable immunoarray was established for the determination of h-FABP with a linear dynamic range from 0.1 to 1000 pg/mL and a detection limit of 0.09 pg/mL, which exhibited excellent performance compared with other ECL methods. Moreover, the developed ECL immunoarray was used in detecting the h-FABP in clinical sample of human serum, which demonstrated good recoveries in the range of 92.20 %∼108.00 %. Therefore, the proposed ECL immunoarray can effectively handle the determination of clinical samples, which was promising for using the early screening or exclusion for AMI at home or in an ambulance due to portable detection based on smartphone. This strategy is very promising to effectively reduce fatality and acute morbidity of AMI patients.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113249"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143547965","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}

引用次数: 0

A validated method using RP-HPLC for the simultaneous quantification of creatine, creatinine, cholesterol, and hyaluronic acid across pharmaceutical, food, and biological matrices

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113242

Khaled Elgendy , Mounir Zaky , Dina Abdelaleem

This study presents a highly efficient, precise, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method that innovatively integrates the concurrent quantification of four important analytes: creatine, creatinine, cholesterol, and sodium hyaluronate into a single analytical procedure. The development of this integrated method marks a significant advancement over traditional approaches, which often require separate methods for each analyte. HPLC separation was achieved using a Hypersil C18 analytical column (150 mm x 4.6 mm, 5 μm) with a mobile phase consisting of 1 % triethanolamine and 80 % acetonitrile, at a flow rate of 1 mL/min and a detection wavelength of 200 nm at room temperature (25 °C). The method exhibited excellent retention times for creatine, creatinine, cholesterol, and sodium hyaluronate (3.155, 5.215, 2.194, and 3.106 min, respectively) and demonstrated a wide linearity range (25 to 80 µg/mL) with correlation coefficients exceeding 0.999 for all analytes. Validation results confirmed that the method meets the acceptance criteria of the ICH Q2 (R1) guidelines. This innovative approach offers a significant improvement in efficiency, reducing both time and resource consumption while maintaining high accuracy and reliability in simultaneous analysis. Hence it can be successfully used for routine analysis of Creatine, Creatinine, Cholesterol, and Hyaluronic acid in pharmaceutical formulations, food, and human body fluids.

{"title":"A validated method using RP-HPLC for the simultaneous quantification of creatine, creatinine, cholesterol, and hyaluronic acid across pharmaceutical, food, and biological matrices","authors":"Khaled Elgendy , Mounir Zaky , Dina Abdelaleem","doi":"10.1016/j.microc.2025.113242","DOIUrl":"10.1016/j.microc.2025.113242","url":null,"abstract":"<div><div>This study presents a highly efficient, precise, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method that innovatively integrates the concurrent quantification of four important analytes: creatine, creatinine, cholesterol, and sodium hyaluronate into a single analytical procedure. The development of this integrated method marks a significant advancement over traditional approaches, which often require separate methods for each analyte. HPLC separation was achieved using a Hypersil C18 analytical column (150 mm x 4.6 mm, 5 μm) with a mobile phase consisting of 1 % triethanolamine and 80 % acetonitrile, at a flow rate of 1 mL/min and a detection wavelength of 200 nm at room temperature (25 °C). The method exhibited excellent retention times for creatine, creatinine, cholesterol, and sodium hyaluronate (3.155, 5.215, 2.194, and 3.106 min, respectively) and demonstrated a wide linearity range (25 to 80 µg/mL) with correlation coefficients exceeding 0.999 for all analytes. Validation results confirmed that the method meets the acceptance criteria of the ICH Q2 (R1) guidelines. This innovative approach offers a significant improvement in efficiency, reducing both time and resource consumption while maintaining high accuracy and reliability in simultaneous analysis. Hence it can be successfully used for routine analysis of Creatine, Creatinine, Cholesterol, and Hyaluronic acid in pharmaceutical formulations, food, and human body fluids.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113242"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143562301","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}

引用次数: 0

Spectral and chromatographic fingerprint −based qualitative and quantitative evaluation strategy combined with chemometrics for quality control of functional red yeast

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113211

Ting Yang , Lan Xue , Xi Liu , Chunhui Hao , Dandan Gong , Guoxiang Sun

The red yeast has significant potential for application in the food industry and in the improvement of cardiovascular diseases. The objective of this study is to develop a rapid, accurate, and comprehensive quality control strategy. Functional and common red yeast were identified through Fourier Transform Infrared (FTIR) spectral fingerprinting combined with Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA). A quantitative prediction model for the indicator component, lovastatin, was constructed by integrating Ultraviolet (UV) spectral fingerprinting with Partial Least Squares (PLS) model. The FTIR and UV spectral quantized fingerprints (QFPs) of functional red yeast were obtained, thereby rendering the spectral information concise. The spectral QFPs were evaluated for qualitative and quantitative similarity by combining them with Systematically Quantified Fingerprint Method (SQFM), and the integration of evaluation results were obtained using the coefficient of variation weighted mean. The combination of High Performance Liquid Chromatography (HPLC) fingerprints and SQFM demonstrated the process stability of the production of functional red yeast into Xuezhikang capsules. This strategy innovatively integrates chemometrics, fingerprinting techniques, and similarity evaluation methods, offering a more efficient and comprehensive approach than traditional identification and quality control methods. It represents a novel paradigm for source-level quality control of functional red yeast.

{"title":"Spectral and chromatographic fingerprint −based qualitative and quantitative evaluation strategy combined with chemometrics for quality control of functional red yeast","authors":"Ting Yang , Lan Xue , Xi Liu , Chunhui Hao , Dandan Gong , Guoxiang Sun","doi":"10.1016/j.microc.2025.113211","DOIUrl":"10.1016/j.microc.2025.113211","url":null,"abstract":"<div><div>The red yeast has significant potential for application in the food industry and in the improvement of cardiovascular diseases. The objective of this study is to develop a rapid, accurate, and comprehensive quality control strategy. Functional and common red yeast were identified through Fourier Transform Infrared (FTIR) spectral fingerprinting combined with Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA). A quantitative prediction model for the indicator component, lovastatin, was constructed by integrating Ultraviolet (UV) spectral fingerprinting with Partial Least Squares (PLS) model. The FTIR and UV spectral quantized fingerprints (QFPs) of functional red yeast were obtained, thereby rendering the spectral information concise. The spectral QFPs were evaluated for qualitative and quantitative similarity by combining them with Systematically Quantified Fingerprint Method (SQFM), and the integration of evaluation results were obtained using the coefficient of variation weighted mean. The combination of High Performance Liquid Chromatography (HPLC) fingerprints and SQFM demonstrated the process stability of the production of functional red yeast into Xuezhikang capsules. This strategy innovatively integrates chemometrics, fingerprinting techniques, and similarity evaluation methods, offering a more efficient and comprehensive approach than traditional identification and quality control methods. It represents a novel paradigm for source-level quality control of functional red yeast.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113211"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561917","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}

引用次数: 0