Microchemical Journal最新文献_第8页

A protocol for synthesizing reference materials for multi-isotope analysis via high-temperature and high-pressure sintering: A demonstration with Ti-Hf in rutile

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-05 DOI: 10.1016/j.microc.2025.113238

Deyi Peng, Zhian Bao, Lei Kang, Xiaojuan Nie, Kaiyun Chen, Yan Zhang, Honglin Yuan

Multi-isotope tracers are vital in exploring complex systems and processes in environmental science, archaeology, and Earth sciences. Laser ablation multiple-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS), as a robust technique for such isotope analyses, offers high spatial resolution to identify micro-regional isotopic heterogeneity. However, high-precision in-situ isotope measurements typically necessitate the use of matrix-matched reference materials to correct for matrix effects, instrumental bias, and fractionation induced by laser ablation. Natural minerals with homogeneous multi-isotopic compositions are extremely rare and inadequate to fully meet diverse experimental requirements. This study proposes a robust synthesis protocol to make matrix-matched reference materials tailored for in-situ multi-isotope analysis via LA-MC-ICP-MS. This protocol integrates elemental doping (ED) with high-temperature and high-pressure (HTHP) techniques, offering a versatile approach to prepare solid reference materials tailored for multiple isotopes of interest. To validate the reliability of this method, a HfO₂-doped rutile (NWU-RT) was synthesized for Ti-Hf isotope determination. Comprehensive in-situ analyses demonstrate that NWU-RT exhibits exceptional homogeneity in Ti and Hf isotopes. The mean δ⁴⁹Ti_OL-Ti value is 0.42 ± 0.12 ‰ (2SD, n = 666), with a ¹⁷⁶Hf/¹⁷⁷Hf isotopic ratio of 0.282265 ± 0.000071 (2SD, n = 561), aligning with results obtained from SN-MC-ICP-MS. Reproducibility tests involving six batches of NWU-RT synthesized under identical experimental conditions over a year confirm the significant potential of the ED-HTHP method for synthesizing reliable solid reference materials for in-situ multi-isotope measurements using LA-MC-ICP-MS.

{"title":"A protocol for synthesizing reference materials for multi-isotope analysis via high-temperature and high-pressure sintering: A demonstration with Ti-Hf in rutile","authors":"Deyi Peng, Zhian Bao, Lei Kang, Xiaojuan Nie, Kaiyun Chen, Yan Zhang, Honglin Yuan","doi":"10.1016/j.microc.2025.113238","DOIUrl":"10.1016/j.microc.2025.113238","url":null,"abstract":"<div><div>Multi-isotope tracers are vital in exploring complex systems and processes in environmental science, archaeology, and Earth sciences. Laser ablation multiple-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS), as a robust technique for such isotope analyses, offers high spatial resolution to identify micro-regional isotopic heterogeneity. However, high-precision in-situ isotope measurements typically necessitate the use of matrix-matched reference materials to correct for matrix effects, instrumental bias, and fractionation induced by laser ablation. Natural minerals with homogeneous multi-isotopic compositions are extremely rare and inadequate to fully meet diverse experimental requirements. This study proposes a robust synthesis protocol to make matrix-matched reference materials tailored for in-situ multi-isotope analysis via LA-MC-ICP-MS. This protocol integrates elemental doping (ED) with high-temperature and high-pressure (HTHP) techniques, offering a versatile approach to prepare solid reference materials tailored for multiple isotopes of interest. To validate the reliability of this method, a HfO<sub>2</sub>-doped rutile (NWU-RT) was synthesized for Ti-Hf isotope determination. Comprehensive in-situ analyses demonstrate that NWU-RT exhibits exceptional homogeneity in Ti and Hf isotopes. The mean δ<sup>49</sup>Ti<sub>OL-Ti</sub> value is 0.42 ± 0.12 ‰ (2SD, n = 666), with a <sup>176</sup>Hf/<sup>177</sup>Hf isotopic ratio of 0.282265 ± 0.000071 (2SD, n = 561), aligning with results obtained from SN-MC-ICP-MS. Reproducibility tests involving six batches of NWU-RT synthesized under identical experimental conditions over a year confirm the significant potential of the ED-HTHP method for synthesizing reliable solid reference materials for in-situ multi-isotope measurements using LA-MC-ICP-MS.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113238"},"PeriodicalIF":4.9,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143578702","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

A spherical nucleic acid-based colorimetric and fluorescent dual-responsive sensor for rapid and sensitive detection of neomycin in environmental water samples

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113252

Yinghua Zhu , Youduo Zhao , Jingjing Deng , Tianshu Zhou

The widespread application of neomycin (NEO) has raised pollution problem caused by the accumulation of its residues, which poses potential risk to human health and ecological safety. Therefore, the development of sensitive and reliable approaches is crucial for detecting and monitoring low levels of NEO in complex samples. In this study, an innovative spherical nucleic acid (SNA) based sensor was designed for the selective detection of NEO. The colorimetric response was attributed to hydrogen bonding, electrostatic interaction, and coordination between the SNA and NEO. Meanwhile, the fluorescence of FAM-labeled SNA was quenched by NEO due to fluorescence resonance energy transfer (FRET) effect. By integrating visual colorimetry and fluorescence analysis, the dual-responsive sensor enabled rapid, selective, and sensitive determination of NEO, with detection limits of 40.0 nM and 3.3 nM, respectively. Furthermore, the SNA exhibited good salt tolerance, maintaining stability without aggregation even in high-salt conditions. The average recoveries for detecting NEO in water samples analysis ranged from 97.6 % to 108.7 %, confirming its reliability and accuracy in practical applications. This work provides an effective strategy for NEO detection and expands the potential applications of SNA in environmental monitoring and pollution control.

{"title":"A spherical nucleic acid-based colorimetric and fluorescent dual-responsive sensor for rapid and sensitive detection of neomycin in environmental water samples","authors":"Yinghua Zhu , Youduo Zhao , Jingjing Deng , Tianshu Zhou","doi":"10.1016/j.microc.2025.113252","DOIUrl":"10.1016/j.microc.2025.113252","url":null,"abstract":"<div><div>The widespread application of neomycin (NEO) has raised pollution problem caused by the accumulation of its residues, which poses potential risk to human health and ecological safety. Therefore, the development of sensitive and reliable approaches is crucial for detecting and monitoring low levels of NEO in complex samples. In this study, an innovative spherical nucleic acid (SNA) based sensor was designed for the selective detection of NEO. The colorimetric response was attributed to hydrogen bonding, electrostatic interaction, and coordination between the SNA and NEO. Meanwhile, the fluorescence of FAM-labeled SNA was quenched by NEO due to fluorescence resonance energy transfer (FRET) effect. By integrating visual colorimetry and fluorescence analysis, the dual-responsive sensor enabled rapid, selective, and sensitive determination of NEO, with detection limits of 40.0 nM and 3.3 nM, respectively. Furthermore, the SNA exhibited good salt tolerance, maintaining stability without aggregation even in high-salt conditions. The average recoveries for detecting NEO in water samples analysis ranged from 97.6 % to 108.7 %, confirming its reliability and accuracy in practical applications. This work provides an effective strategy for NEO detection and expands the potential applications of SNA in environmental monitoring and pollution control.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113252"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143578778","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

Deep learning meets visualization: A novel method for particle size monitoring in fluidized bed coating

IF 4.9 2区化学 Q1 CHEMISTRY, ANALYTICAL

Microchemical Journal

Pub Date : 2025-03-04 DOI: 10.1016/j.microc.2025.113256

Liang Zhong , Lele Gao , Lian Li , Wenping Yin , Lei Nie , Hengchang Zang

The accurate monitoring of particle size distribution (PSD) is essential for ensuring the quality of oral solid dosage forms during fluidized bed coating. Here, a novel deep learning visualization framework was developed to predict and visualize PSD values of pellets based on near-infrared spectroscopy (NIRS). A multi-head self-attention convolutional neural network (MHSA-CNN) was designed to extract local spatial features as well as global contextual information from spectra. Bayesian optimization was employed to fine-tune the hyperparameters of the MHSA-CNN, thereby ensuring optimal model performance. Comparative analyses demonstrated that the proposed MHSA-CNN outperformed traditional CNN and partial least squares (PLS) methods in predicting PSD values, highlighting its robustness and accuracy. To further refine the network architecture, conventional method and uniform manifold approximation and projection (UMAP) were utilized to visualize the feature representations of the MHSA-CNN across different layers. The visualizations provided critical insights into the relationship between layer-wise feature transformations and PSD values prediction, facilitating iterative optimization of the MHSA-CNN structure by adjusting the number of layers. This systematic approach not only enhanced the predictive accuracy of the model but also provided a deeper understanding of the network’s inner workings.

{"title":"Deep learning meets visualization: A novel method for particle size monitoring in fluidized bed coating","authors":"Liang Zhong , Lele Gao , Lian Li , Wenping Yin , Lei Nie , Hengchang Zang","doi":"10.1016/j.microc.2025.113256","DOIUrl":"10.1016/j.microc.2025.113256","url":null,"abstract":"<div><div>The accurate monitoring of particle size distribution (PSD) is essential for ensuring the quality of oral solid dosage forms during fluidized bed coating. Here, a novel deep learning visualization framework was developed to predict and visualize PSD values of pellets based on near-infrared spectroscopy (NIRS). A multi-head self-attention convolutional neural network (MHSA-CNN) was designed to extract local spatial features as well as global contextual information from spectra. Bayesian optimization was employed to fine-tune the hyperparameters of the MHSA-CNN, thereby ensuring optimal model performance. Comparative analyses demonstrated that the proposed MHSA-CNN outperformed traditional CNN and partial least squares (PLS) methods in predicting PSD values, highlighting its robustness and accuracy. To further refine the network architecture, conventional method and uniform manifold approximation and projection (UMAP) were utilized to visualize the feature representations of the MHSA-CNN across different layers. The visualizations provided critical insights into the relationship between layer-wise feature transformations and PSD values prediction, facilitating iterative optimization of the MHSA-CNN structure by adjusting the number of layers. This systematic approach not only enhanced the predictive accuracy of the model but also provided a deeper understanding of the network’s inner workings.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"212 ","pages":"Article 113256"},"PeriodicalIF":4.9,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143578699","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