Journal of Chromatography A最新文献

Application of Physics-Informed Neural Networks to predict concentration profiles in gradient liquid chromatography

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-03-03 DOI: 10.1016/j.chroma.2025.465831

Filip Rękas , Marcin Chutkowski , Krzysztof Kaczmarski

Chromatography is one of the key methods in the analysis of mixture compositions, in the testing of chemical purity, as well as in the production of highly pure compounds. For this reason, it finds an important place in many industries. Currently, one of the most widely used techniques is gradient liquid chromatography (GLC), which offers improved elution ability of the analytes. Experimental determination of optimal separation parameters with GLC is tedious, hence various numerical methods are used to optimize these processes. Recently, Physics-Informed Neural Networks (PINNs) have emerged as an alternative to classical numerical methods since they can also serve as a tool for solving partial differential equations (PDEs). The main concept of the PINN, apart from the ability to detect hidden and complex relationships between variables through machine learning, is to reach consistency with the governing physical laws by using a loss function that takes PDEs into account, which allows to obtain the results with better accuracy. In the paper, two PINN models are proposed, based on datasets obtained from numerical solutions of the equilibrium dispersive (ED) chromatography column model. After training and testing phases, the models are able to predict the concentration profiles under linear and nonlinear GLC conditions with more than satisfactory accuracy. The first model (model A1) was tested under linear GLC conditions, with variable inlet concentration or injection time, while the second model (model A2) was validated both under linear and nonlinear GLC modes and with variable axial dispersion and mass transport resistances.

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引用次数: 0

Effect of magnetized solvent on the porosity of magnetic graphene oxide@zirconium-based metal-organic framework sorbent for efficient extraction of remdesivir

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-03-02 DOI: 10.1016/j.chroma.2025.465839

Maryam Asefi, Amirhassan Amiri, Mostafa Gholizadeh

In this study, the effect of magnetized solvent on the synthesis and properties of magnetic graphene oxide@UiO-66 (MGO@UiO-66) nanocomposite as sorbent was investigated. The prepared sorbent was used for the magnetic solid-phase extraction (MSPE) of remdesivir drug from water and plasma samples. The extracted remdesivir was quantitatively determined by high-performance liquid chromatography with a photodiode array detector (HPLC-PDA). The MGO@UiO-66 sorbents were characterized using various techniques such as Fourier-transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), Brauer-emmett-teller analysis (BET), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating-sample magnetometry. The optimization of extraction parameters such as desorption solvent and its volume, sorbent amount, pH, desorption conditions, and extraction time were investigated and studied. Under the optimized conditions, the calibration plot for remdesivir was linear within the range of 0.1–300 ng mL⁻¹ and limits of detection (0.03 ng mL^–1). The MSPE-HPLC-PDA method showed good extraction recovery and relative standard deviations (RSD%) in the range of 95.5–99.5 % and 3.8–4.7 %, respectively. Furthermore, the method that was effectively utilized to analyze remdesivir in water and plasma samples, resulted in relative recoveries ranging from 95.5 % to 99.3 %.

{"title":"Effect of magnetized solvent on the porosity of magnetic graphene oxide@zirconium-based metal-organic framework sorbent for efficient extraction of remdesivir","authors":"Maryam Asefi, Amirhassan Amiri, Mostafa Gholizadeh","doi":"10.1016/j.chroma.2025.465839","DOIUrl":"10.1016/j.chroma.2025.465839","url":null,"abstract":"<div><div>In this study, the effect of magnetized solvent on the synthesis and properties of magnetic graphene oxide@UiO-66 (MGO@UiO-66) nanocomposite as sorbent was investigated. The prepared sorbent was used for the magnetic solid-phase extraction (MSPE) of remdesivir drug from water and plasma samples. The extracted remdesivir was quantitatively determined by high-performance liquid chromatography with a photodiode array detector (HPLC-PDA). The MGO@UiO-66 sorbents were characterized using various techniques such as Fourier-transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), Brauer-emmett-teller analysis (BET), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating-sample magnetometry. The optimization of extraction parameters such as desorption solvent and its volume, sorbent amount, pH, desorption conditions, and extraction time were investigated and studied. Under the optimized conditions, the calibration plot for remdesivir was linear within the range of 0.1–300 ng mL<sup>−1</sup> and limits of detection (0.03 ng mL<sup>–1</sup>). The MSPE-HPLC-PDA method showed good extraction recovery and relative standard deviations (RSD%) in the range of 95.5–99.5 % and 3.8–4.7 %, respectively. Furthermore, the method that was effectively utilized to analyze remdesivir in water and plasma samples, resulted in relative recoveries ranging from 95.5 % to 99.3 %.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465839"},"PeriodicalIF":3.8,"publicationDate":"2025-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143548476","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

Green synthesis of magnetic aromatic polyamide composites via mechanochemical ball milling with a deep eutectic system for the magnetic solid-phase extraction of antibiotics from water

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-03-01 DOI: 10.1016/j.chroma.2025.465830

Wuxia Ge , Yumei Chen , Xinru Ding , Wentao Bi , David Da Yong Chen

Magnetic aromatic polyamide (MAPA) composites were synthesized using a green mechanochemical ball milling process and used for magnetic solid-phase extraction (MSPE) and detection of trace level fluoroquinolone antibiotics (FQs) from water samples. The formation of MAPAs was facilitated by deep eutectic systems (DESys) created from magnetic beads and organic monomers during ball milling. A comprehensive study was conducted to investigate the kinetics, thermodynamics, and mechanisms of MAPA adsorption of ciprofloxacin hydrochloride (CIP) and ofloxacin (OFL) from water. The maximum adsorption capacities for CIP and OFL were found to be 151.5 mg/g and 164.1 mg/g, respectively. Additionally, the recyclability and selective adsorption capabilities of MAPAs were evaluated. MAPAs were subsequently used for MSPE of CIP and OFL in water samples. Both UV–Vis spectrometry and HPLC methods can be used for analysis, the MSPE-HPLC method showed superior linearity for CIP (0.06–1500 μg/L) and OFL (1–1200 μg/L), with R² values of 0.9995 and 0.9999, and limit of detection (LOD) as low as 0.006 μg/L and 0.02 μg/L, respectively. Both analytical methods are highly effective and practical for use with real water samples. MAPA used for MSPE offer a promising green approach for detecting antibiotic contamination in aquatic ecosystems.

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引用次数: 0

An quality evaluation method based on three-dimensional integration and machine learning: Advanced data processing

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-28 DOI: 10.1016/j.chroma.2025.465826

Jianglei Zhang, Yu Ren, Jin Zeng, Liuwei Zhang, Ming Cai, Lili Lan, Guoxiang Sun

This study presents an innovative approach for the quality evaluation of traditional Chinese medicine (TCM) by integrating three-dimensional (3D) data processing with machine learning, aimed at enhancing the efficiency and accuracy of HPLC-DAD data analysis. Through 3D data integration, multi-dimensional signals from the time and wavelength domains are transformed into two-dimensional data, simplifying the analytical process while ensuring precise quantification of component contents. Building on this foundation, dynamic time warping (DTW) and correlation optimized warping (COW) algorithms were applied to effectively resolve retention time drift across different sample batches, achieving both global and local alignment of chromatographic peak shapes. A Binary Evaluation System (BES), incorporating macro qualitative similarity (S_m) and macro quantitative similarity (P_m), was employed to provide a comprehensive assessment of the quality of TCM samples. Additionally, machine learning models such as Multiple Linear Regression (MLR), Decision Tree Regression (DTR), and Random Forest Regression (RFR) were introduced to further improve the automation and accuracy of the evaluation system. In the analysis of 20 Scutellaria baicalensis samples, the method demonstrated a prediction error range of ±0.2 % for Baicalin content. This approach not only enhances data processing efficiency and reduces experimental resource consumption but also provides a robust theoretical and technical foundation for TCM quality assessment. Ultimately, the results of this study confirm the broad applicability of 3D integration and machine learning in TCM quality control, offering innovative technical support for the modernization of TCM quality evaluation systems.

{"title":"An quality evaluation method based on three-dimensional integration and machine learning: Advanced data processing","authors":"Jianglei Zhang, Yu Ren, Jin Zeng, Liuwei Zhang, Ming Cai, Lili Lan, Guoxiang Sun","doi":"10.1016/j.chroma.2025.465826","DOIUrl":"10.1016/j.chroma.2025.465826","url":null,"abstract":"<div><div>This study presents an innovative approach for the quality evaluation of traditional Chinese medicine (TCM) by integrating three-dimensional (3D) data processing with machine learning, aimed at enhancing the efficiency and accuracy of HPLC-DAD data analysis. Through 3D data integration, multi-dimensional signals from the time and wavelength domains are transformed into two-dimensional data, simplifying the analytical process while ensuring precise quantification of component contents. Building on this foundation, dynamic time warping (DTW) and correlation optimized warping (COW) algorithms were applied to effectively resolve retention time drift across different sample batches, achieving both global and local alignment of chromatographic peak shapes. A Binary Evaluation System (BES), incorporating macro qualitative similarity (<strong><em>S</em></strong><sub>m</sub>) and macro quantitative similarity (<strong><em>P</em></strong><sub>m</sub>), was employed to provide a comprehensive assessment of the quality of TCM samples. Additionally, machine learning models such as Multiple Linear Regression (MLR), Decision Tree Regression (DTR), and Random Forest Regression (RFR) were introduced to further improve the automation and accuracy of the evaluation system. In the analysis of 20 Scutellaria baicalensis samples, the method demonstrated a prediction error range of ±0.2 % for Baicalin content. This approach not only enhances data processing efficiency and reduces experimental resource consumption but also provides a robust theoretical and technical foundation for TCM quality assessment. Ultimately, the results of this study confirm the broad applicability of 3D integration and machine learning in TCM quality control, offering innovative technical support for the modernization of TCM quality evaluation systems.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1747 ","pages":"Article 465826"},"PeriodicalIF":3.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143551529","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

Automation and miniaturization of solid-phase extraction for high-throughput analysis of cyanotoxins

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-28 DOI: 10.1016/j.chroma.2025.465828

Tommy Melzer , Thomas Wichard , Robert Möller , Nico Ueberschaar , Georg Pohnert

We present a resource-efficient method for automated sample preparation, designated to facilitate high-throughput analysis of microcystins and nodularin-R. These cyanotoxins, commonly associated with harmful algal blooms, are monitored to ensure the safety of drinking water and recreational water bodies. The method utilizes a liquid handling platform to flexibly process between 1 and 96 samples within one hour for subsequent LC-MS analysis, requiring only 5 mL of sample for triplicate analysis. By miniaturizing solid-phase extraction into a 96-well format, the protocol reduces transfer volumes, and solvent consumption and has the potential to decrease the use of plastic materials. This approach is suitable for both high-throughput analyses and long-term monitoring studies, and it has been successfully applied to diverse water sources, including river, lake, pond, and HPLC-grade water. The method demonstrates excellent accuracy, with results meeting recommended guidelines. As proof of concept, it was applied to quantify cyanotoxins in two lake water samples and a laboratory culture of Microcystis aeruginosa.

{"title":"Automation and miniaturization of solid-phase extraction for high-throughput analysis of cyanotoxins","authors":"Tommy Melzer , Thomas Wichard , Robert Möller , Nico Ueberschaar , Georg Pohnert","doi":"10.1016/j.chroma.2025.465828","DOIUrl":"10.1016/j.chroma.2025.465828","url":null,"abstract":"<div><div>We present a resource-efficient method for automated sample preparation, designated to facilitate high-throughput analysis of microcystins and nodularin-R. These cyanotoxins, commonly associated with harmful algal blooms, are monitored to ensure the safety of drinking water and recreational water bodies. The method utilizes a liquid handling platform to flexibly process between 1 and 96 samples within one hour for subsequent LC-MS analysis, requiring only 5 mL of sample for triplicate analysis. By miniaturizing solid-phase extraction into a 96-well format, the protocol reduces transfer volumes, and solvent consumption and has the potential to decrease the use of plastic materials. This approach is suitable for both high-throughput analyses and long-term monitoring studies, and it has been successfully applied to diverse water sources, including river, lake, pond, and HPLC-grade water. The method demonstrates excellent accuracy, with results meeting recommended guidelines. As proof of concept, it was applied to quantify cyanotoxins in two lake water samples and a laboratory culture of <em>Microcystis aeruginosa</em>.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465828"},"PeriodicalIF":3.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143548475","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}

引用次数: 0

Smart proteolytic samplers for liquid chromatography-mass spectrometry protein quantification: Assessing trypsin immobilization via divinyl sulfone or periodate functionalization

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-27 DOI: 10.1016/j.chroma.2025.465825

Noor Al-Rubaye , Ago Mrsa , Manuel Ramirez Garrastacho , Trine Grønhaug Halvorsen , Léon Reubsaet

In this report we try to answer the question if smart proteolytic samplers can be used for LC-MS based quantitative determination of proteins from paper. Production of smart proteolytic samplers is a two-stage process: In the first stage cellulose is functionalized while in the second stage trypsin is covalently bound. Two functionalization strategies, divinyl sulfone - and periodate functionalization, were compared under various conditions. The divinyl sulfone functionalization in combination with trypsin immobilization is here described for the first time. This functionalization chemistry shows to be equally successful as the periodate functionalization. Using Whatman Grade CF12 paper, it appears that smart proteolytic samplers with high tryptic activity can be produced. These have the capability to produce tryptic peptides with good linearity in buffered solutions: up to 0.998 for BSA (using HLVDEPQNLIK as signature peptide and IO₄-functionalization) and 0.990 for Cytochrome C (using MIFAGIK as signature peptide and IO₄-functionalization). The reproducibility in complex biological samples is acceptable (<20 % average RSD for divinyl sulfone functionalized paper) when internal correction is carried out. Overall, smart proteolytic samplers can be used for reliable LC-MS based determination of proteins when the correct proteotypic peptides are chosen.

{"title":"Smart proteolytic samplers for liquid chromatography-mass spectrometry protein quantification: Assessing trypsin immobilization via divinyl sulfone or periodate functionalization","authors":"Noor Al-Rubaye , Ago Mrsa , Manuel Ramirez Garrastacho , Trine Grønhaug Halvorsen , Léon Reubsaet","doi":"10.1016/j.chroma.2025.465825","DOIUrl":"10.1016/j.chroma.2025.465825","url":null,"abstract":"<div><div>In this report we try to answer the question if smart proteolytic samplers can be used for LC-MS based quantitative determination of proteins from paper. Production of smart proteolytic samplers is a two-stage process: In the first stage cellulose is functionalized while in the second stage trypsin is covalently bound. Two functionalization strategies, divinyl sulfone - and periodate functionalization, were compared under various conditions. The divinyl sulfone functionalization in combination with trypsin immobilization is here described for the first time. This functionalization chemistry shows to be equally successful as the periodate functionalization. Using Whatman Grade CF12 paper, it appears that smart proteolytic samplers with high tryptic activity can be produced. These have the capability to produce tryptic peptides with good linearity in buffered solutions: up to 0.998 for BSA (using HLVDEPQNLIK as signature peptide and IO<sub>4</sub>-functionalization) and 0.990 for Cytochrome C (using MIFAGIK as signature peptide and IO<sub>4</sub>-functionalization). The reproducibility in complex biological samples is acceptable (<20 % average RSD for divinyl sulfone functionalized paper) when internal correction is carried out. Overall, smart proteolytic samplers can be used for reliable LC-MS based determination of proteins when the correct proteotypic peptides are chosen.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1747 ","pages":"Article 465825"},"PeriodicalIF":3.8,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143527238","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}

引用次数: 0

An overview of hydrophobic deep eutectic solvents driven liquid-phase extraction: Applications and prospects

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-26 DOI: 10.1016/j.chroma.2025.465824

Xinxin Zheng , Fan Yin , Gang Gong , Xinger Zhang , Sile He , Weiyang Tang , Xiao-Hong Wei

Deep eutectic solvents (DESs) are a type of emerging green solvent. They are simple to prepare, cost-effective, highly atom-efficient, exhibit extremely low toxicity, and are biodegradable. Since their discovery, DESs have attracted significant interest from the scientific community across various fields. In recent years, these solvents have been extensively studied by researchers as extraction media. Hydrophobic deep eutectic solvents (hDESs) first appeared in the literature in 2015 and represent a group of DESs that meet the requirements of green chemistry. hDESs have great potential in the fields of separation and extraction and are considered effective alternatives to replace hydrophilic DESs and other hydrophobic organic solvents for the extraction of lipophilic natural products. This review summarizes pioneering and innovative work on hDESs, including the latest research progress regarding their applications, extraction techniques, and recycling methods. It also highlights issues that need to be addressed in the future. The results of hDESs in natural product extraction and the extraction of other compounds have revealed their significant potential as alternative green solvents in industrial separation processes.

{"title":"An overview of hydrophobic deep eutectic solvents driven liquid-phase extraction: Applications and prospects","authors":"Xinxin Zheng , Fan Yin , Gang Gong , Xinger Zhang , Sile He , Weiyang Tang , Xiao-Hong Wei","doi":"10.1016/j.chroma.2025.465824","DOIUrl":"10.1016/j.chroma.2025.465824","url":null,"abstract":"<div><div>Deep eutectic solvents (DESs) are a type of emerging green solvent. They are simple to prepare, cost-effective, highly atom-efficient, exhibit extremely low toxicity, and are biodegradable. Since their discovery, DESs have attracted significant interest from the scientific community across various fields. In recent years, these solvents have been extensively studied by researchers as extraction media. Hydrophobic deep eutectic solvents (hDESs) first appeared in the literature in 2015 and represent a group of DESs that meet the requirements of green chemistry. hDESs have great potential in the fields of separation and extraction and are considered effective alternatives to replace hydrophilic DESs and other hydrophobic organic solvents for the extraction of lipophilic natural products. This review summarizes pioneering and innovative work on hDESs, including the latest research progress regarding their applications, extraction techniques, and recycling methods. It also highlights issues that need to be addressed in the future. The results of hDESs in natural product extraction and the extraction of other compounds have revealed their significant potential as alternative green solvents in industrial separation processes.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465824"},"PeriodicalIF":3.8,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143562415","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

Preparation of boric acid functionalized hyper-crosslinked polymer for efficient extraction of phenylurea herbicides from lake water, green tea drink and tomato samples

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-26 DOI: 10.1016/j.chroma.2025.465823

Zichen Zhao , Ruiyang Ma , Juntao Wang , Qing Zhang , Miao Jing , Chun Wang , Qiuhua Wu , Zhi Wang

A boric acid functionalized hyper-crosslinked polymer (HCP), designated as NPCBA/TBM-HCP, was successfully synthesized via Friedel-Crafts reaction by copolymerizing N-phenylcarbazole-2-boronic acid (NPCBA) and 2,4,6-Tris(bromomethyl)mesitylene (TBM). The NPCBA/TBM-HCP showed a large surface area and a good adsorption property for phenylurea herbicides (PUHs). A method with NPCBA/TBM-HCP based solid phase extraction and high-performance liquid chromatographic detection was developed for the simultaneous analysis of PUHs in lake water, green tea drink and tomato samples. Under the optimized experimental conditions that the amount of the NPCBA/TBM-HCP was 30 mg, sample solution was 100 mL, sample loading rate was 4 mL min^-1, and eluent was 0.3 mL acetonitrile, the linear response for the PUHs was in the range of 0.06–80.0 ng mL^-1, 0.6–80.0 ng mL^-1 and 0.9–200 ng g^-1 for lake water, green tea drink and tomato samples, respectively, with a good linearity (the coefficients of determination (r²) ≥ 0.9916). The detection limits (S/N = 3) for lake water, green tea drink and tomato samples were 0.02–0.03 ng mL^-1, 0.2 ng mL^-1 and 0.3–0.5 ng g^-1, respectively. The method recoveries for spiked samples were 80.0 %-119.1 % and RSDs were lower than 9.9 % for the determination. The method provides a new and feasible approach for the determination of phenylurea herbicide in real samples.

{"title":"Preparation of boric acid functionalized hyper-crosslinked polymer for efficient extraction of phenylurea herbicides from lake water, green tea drink and tomato samples","authors":"Zichen Zhao , Ruiyang Ma , Juntao Wang , Qing Zhang , Miao Jing , Chun Wang , Qiuhua Wu , Zhi Wang","doi":"10.1016/j.chroma.2025.465823","DOIUrl":"10.1016/j.chroma.2025.465823","url":null,"abstract":"<div><div>A boric acid functionalized hyper-crosslinked polymer (HCP), designated as NPCBA/TBM-HCP, was successfully synthesized via Friedel-Crafts reaction by copolymerizing N-phenylcarbazole-2-boronic acid (NPCBA) and 2,4,6-Tris(bromomethyl)mesitylene (TBM). The NPCBA/TBM-HCP showed a large surface area and a good adsorption property for phenylurea herbicides (PUHs). A method with NPCBA/TBM-HCP based solid phase extraction and high-performance liquid chromatographic detection was developed for the simultaneous analysis of PUHs in lake water, green tea drink and tomato samples. Under the optimized experimental conditions that the amount of the NPCBA/TBM-HCP was 30 mg, sample solution was 100 mL, sample loading rate was 4 mL min<sup>-1</sup>, and eluent was 0.3 mL acetonitrile, the linear response for the PUHs was in the range of 0.06–80.0 ng mL<sup>-1</sup>, 0.6–80.0 ng mL<sup>-1</sup> and 0.9–200 ng g<sup>-1</sup> for lake water, green tea drink and tomato samples, respectively, with a good linearity (the coefficients of determination (<em>r</em><sup>2</sup>) ≥ 0.9916). The detection limits (S/N = 3) for lake water, green tea drink and tomato samples were 0.02–0.03 ng mL<sup>-1</sup>, 0.2 ng mL<sup>-1</sup> and 0.3–0.5 ng g<sup>-1</sup>, respectively. The method recoveries for spiked samples were 80.0 %-119.1 % and RSDs were lower than 9.9 % for the determination. The method provides a new and feasible approach for the determination of phenylurea herbicide in real samples.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1747 ","pages":"Article 465823"},"PeriodicalIF":3.8,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143551527","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

Determination of perfluoroalkyl carboxylic acids in mice serum and tissue by dispersive solid-phase extraction based on fluorine-functionalized covalent organic frameworks coupled with UPLC-MS/MS 基于氟功能化共价有机框架的分散固相萃取-UPLC-MS/MS法测定小鼠血清和组织中的全氟烷基羧酸

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-25 DOI: 10.1016/j.chroma.2025.465820

Jinni Zhang , Songtao Li , Xiaojing Li , Canrong Chen , Wen Xie , Yanhui Zhong , Zian Lin , Zongwei Cai

Perfluoroalkyl carboxylic acids (PFCAs) are a class of persistent organic pollutants (POPs), which posed various hazards to organisms, including reproductive, developmental, neurological, and immunological toxicity. Consequently, developing an analytical method aimed at achieving highly sensitive detection of trace amounts of PFCAs in complex samples is clearly of great significance. Herein, the Fluorine-functionalized covalent organic framework (F-COF) was synthesized at ambient temperature, which has the advantages of high specific surface area (1297.7 m² g^-1), suitable selective adsorption pore size and good stability. Based on the multiple effects of suitable pore size, fluorine-fluorine interactions and hydrophobic interactions, F-COF exhibited high adsorption performance towards PFCAs. Accordingly, the method of F-COF-based dispersive solid-phase extraction (dSPE) coupled with UPLC-MS/MS was developed for the quantitative analysis of 5 PFCAs in complex biological samples. The results showed that the good linearity for the 5 PFCAs within the concentration ranges of 0.4 to 10⁴ ng L^-1, with correlation coefficients (r) all greater than 0.9993. The enrichment factors (EFs) ranged from 11.4 to 22.3 folds, and the limits of detection (LODs) were 0.11 to 0.17 ng L^-1. The established method provided a powerful tool for the enrichment and detection of PFCAs in mice serum and tissue. F-COF holds promising application prospects as a solid-phase extraction material for efficient enrichment separation and detection of PFCAs.

{"title":"Determination of perfluoroalkyl carboxylic acids in mice serum and tissue by dispersive solid-phase extraction based on fluorine-functionalized covalent organic frameworks coupled with UPLC-MS/MS","authors":"Jinni Zhang , Songtao Li , Xiaojing Li , Canrong Chen , Wen Xie , Yanhui Zhong , Zian Lin , Zongwei Cai","doi":"10.1016/j.chroma.2025.465820","DOIUrl":"10.1016/j.chroma.2025.465820","url":null,"abstract":"<div><div>Perfluoroalkyl carboxylic acids (PFCAs) are a class of persistent organic pollutants (POPs), which posed various hazards to organisms, including reproductive, developmental, neurological, and immunological toxicity. Consequently, developing an analytical method aimed at achieving highly sensitive detection of trace amounts of PFCAs in complex samples is clearly of great significance. Herein, the Fluorine-functionalized covalent organic framework (F-COF) was synthesized at ambient temperature, which has the advantages of high specific surface area (1297.7 m<sup>2</sup> g<sup>-1</sup>), suitable selective adsorption pore size and good stability. Based on the multiple effects of suitable pore size, fluorine-fluorine interactions and hydrophobic interactions, F-COF exhibited high adsorption performance towards PFCAs. Accordingly, the method of F-COF-based dispersive solid-phase extraction (dSPE) coupled with UPLC-MS/MS was developed for the quantitative analysis of 5 PFCAs in complex biological samples. The results showed that the good linearity for the 5 PFCAs within the concentration ranges of 0.4 to 10<sup>4</sup> ng L<sup>-1</sup>, with correlation coefficients (r) all greater than 0.9993. The enrichment factors (EFs) ranged from 11.4 to 22.3 folds, and the limits of detection (LODs) were 0.11 to 0.17 ng L<sup>-1</sup>. The established method provided a powerful tool for the enrichment and detection of PFCAs in mice serum and tissue. F-COF holds promising application prospects as a solid-phase extraction material for efficient enrichment separation and detection of PFCAs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1747 ","pages":"Article 465820"},"PeriodicalIF":3.8,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143527222","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

Use of Fisher's Ratio assisted multivariate curve resolution- alternating least squares for discovery-based analysis using ultrahigh pressure liquid chromatography-high resolution mass spectrometry

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-25 DOI: 10.1016/j.chroma.2025.465812

Brooke R. Baumgarten, Chris E. Freye

Non-targeted analysis of complex chemical mixtures can be difficult considering the convoluted nature of the matrix and the potential unknown chemical differences between samples or classes of samples. Ultrahigh pressure liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UHPLC-QTOF) is an ideal technique to probe chemical differences for a wide variety of samples. While UHPLC-QTOF can discover minute chemical differences down to low part per billion (ppb) concentrations with a high degree of confidence, the application of high-resolution mass spectrometry can yield massive amounts of information (∼ 10 gb per sample) that cannot be analyzed manually. Therefore, the application of chemometric techniques is mandatory for the interrogation of complex samples. Fisher's ratio (FR) assisted multivariate curve resolution-alternating least squares (MCR-ALS) was used to the discover and identify the chemical differences between two classes of materials: 1) a pond water matrix and 2) the matrix spiked with a pharmaceutical standard mix containing 17 compounds. Thirteen of the seventeen spiked compounds were discovered using FR analysis, and then five were successfully deconvoluted using MCR-ALS wherein the number of curves chosen were automatically determined using singular value decomposition (SVD). The use of an automated FR assisted MCR-ALS will aid in discovering trace levels of chemical components without the need for the researcher to provide potentially biased input which will aid in non-targeted workflow.

{"title":"Use of Fisher's Ratio assisted multivariate curve resolution- alternating least squares for discovery-based analysis using ultrahigh pressure liquid chromatography-high resolution mass spectrometry","authors":"Brooke R. Baumgarten, Chris E. Freye","doi":"10.1016/j.chroma.2025.465812","DOIUrl":"10.1016/j.chroma.2025.465812","url":null,"abstract":"<div><div>Non-targeted analysis of complex chemical mixtures can be difficult considering the convoluted nature of the matrix and the potential unknown chemical differences between samples or classes of samples. Ultrahigh pressure liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UHPLC-QTOF) is an ideal technique to probe chemical differences for a wide variety of samples. While UHPLC-QTOF can discover minute chemical differences down to low part per billion (ppb) concentrations with a high degree of confidence, the application of high-resolution mass spectrometry can yield massive amounts of information (∼ 10 gb per sample) that cannot be analyzed manually. Therefore, the application of chemometric techniques is mandatory for the interrogation of complex samples. Fisher's ratio (FR) assisted multivariate curve resolution-alternating least squares (MCR-ALS) was used to the discover and identify the chemical differences between two classes of materials: 1) a pond water matrix and 2) the matrix spiked with a pharmaceutical standard mix containing 17 compounds. Thirteen of the seventeen spiked compounds were discovered using FR analysis, and then five were successfully deconvoluted using MCR-ALS wherein the number of curves chosen were automatically determined using singular value decomposition (SVD). The use of an automated FR assisted MCR-ALS will aid in discovering trace levels of chemical components without the need for the researcher to provide potentially biased input which will aid in non-targeted workflow.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1747 ","pages":"Article 465812"},"PeriodicalIF":3.8,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143520423","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