Journal of chromatography open最新文献

Semi-preparative on-line supercritical fluid extraction-supercritical fluid chromatography for solid-state injection and purification

Journal of chromatography open

Pub Date : 2025-02-06 DOI: 10.1016/j.jcoa.2025.100206

Quentin Gros, Yusuke Masuda, Yoshiyuki Watabe, Hidetoshi Terada

Thanks to the versatility and low viscosity of sub/supercritical fluids, supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) are attractive to extract and separate molecules in a quick and efficient way. By coupling both techniques, on-line SFE-SFC becomes even more versatile and can extract, separate, and detect molecules in a single approach. When used at semi-preparative (semi-prep.) scale, on-line SFE-SFC can also be an interesting tool to perform solid-state injection and simplify sample pretreatment before purification. The aim of this publication is to examine the possibilities offered by semi-prep. on-line SFE-SFC for solid-state injection and determine the key parameters for method development, using ibuprofen as a case study. First, solubility changes of ibuprofen in a pressurized carbon dioxide (CO₂)/methanol mixture were investigated, revealing a favorable solubility at 20 % of co-solvent. Then, an SFC method was developed at analytical scale and scaled up to semi-prep. SFC. This method allowed the separation of ibuprofen from structurally related compounds in less than 3 min, using a Shim-pack UC PolyVP column and 30 % of MeOH in pressurized CO₂. After that, the effect of co-solvent ratio and extraction duration on semi-prep. on-line SFE-SFC solid-state injection was investigated. With an appropriate static extraction using 20 % of co-solvent for 1 min followed by a dynamic extraction with 5 % of co-solvent over 4 min, it was possible to inject and purify 500 mg of solid-state ibuprofen in 10 min. Finally, the methodology was applied to 2.5 g of sample, demonstrating its suitability for larger solid-state injection.

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引用次数: 0

Evaluation of trap discs for root exudate eco-friendly sampling using rhizoboxes: Application to untargeted screening of organic compounds by gas chromatography hyphenated with high resolution mass spectrometry

Journal of chromatography open

Pub Date : 2025-02-05 DOI: 10.1016/j.jcoa.2025.100205

Victoria Bohm , Estelle Forey , Matthieu Chauvat , Pascal Cardinael , Valerie Peulon-Agasse

In the present paper, an unusual sampling method, called EcoRoot, was investigated for sampling directly in soil, root exudates of Poa annua L., belonging to the Poaceae family. Using a rhizobox, sorption filters were placed directly onto roots to serve as traps for root exudates. Various trap compositions, namely, cellulose nitrate, glass microfiber and nylon, were evaluated for their ability to adsorb/desorb a standard mixture of known exuded compounds and for recovery yield. Cellulose nitrate supports exhibited better yields for compounds known to be exudated by plants of the Poaceae family. Then, two crucial parameters were investigated: the contact and extraction times. The most suitable methodology for extracting the target compounds was a cellulose nitrate support with a contact time of 60 min and 30 min in an ultrasonic bath using a mixture H₂O/MeOH. Soil and root sampling was carried out under the optimized conditions. Then, silylation of extracts was performed, and GC-HRMS was used to demonstrate that this sampling method could be used to efficiently trap compounds from soil and roots. Moreover, among the 6,136 compounds detected in extracts, 516 appeared to be specific to root exudates. This Ecoroot methodology allows root exudates to be collected in conditions as close as possible to natural growth environment, limiting the environmental impact with a 0.59 score (AGREEprep) compared to hydroponic methods. Ecoroot offers interesting perspectives for studying root exudate metabolome and their temporal and spatial dynamics in the rhizosphere, with important issues in both Ecology and Plant biology.

{"title":"Evaluation of trap discs for root exudate eco-friendly sampling using rhizoboxes: Application to untargeted screening of organic compounds by gas chromatography hyphenated with high resolution mass spectrometry","authors":"Victoria Bohm , Estelle Forey , Matthieu Chauvat , Pascal Cardinael , Valerie Peulon-Agasse","doi":"10.1016/j.jcoa.2025.100205","DOIUrl":"10.1016/j.jcoa.2025.100205","url":null,"abstract":"<div><div>In the present paper, an unusual sampling method, called EcoRoot, was investigated for sampling directly in soil, root exudates of <em>Poa annua L.,</em> belonging to the Poaceae family. Using a rhizobox, sorption filters were placed directly onto roots to serve as traps for root exudates. Various trap compositions, namely, cellulose nitrate, glass microfiber and nylon, were evaluated for their ability to adsorb/desorb a standard mixture of known exuded compounds and for recovery yield. Cellulose nitrate supports exhibited better yields for compounds known to be exudated by plants of the Poaceae family. Then, two crucial parameters were investigated: the contact and extraction times. The most suitable methodology for extracting the target compounds was a cellulose nitrate support with a contact time of 60 min and 30 min in an ultrasonic bath using a mixture H<sub>2</sub>O/MeOH. Soil and root sampling was carried out under the optimized conditions. Then, silylation of extracts was performed, and GC-HRMS was used to demonstrate that this sampling method could be used to efficiently trap compounds from soil and roots. Moreover, among the 6,136 compounds detected in extracts, 516 appeared to be specific to root exudates. This Ecoroot methodology allows root exudates to be collected in conditions as close as possible to natural growth environment, limiting the environmental impact with a 0.59 score (AGREEprep) compared to hydroponic methods. Ecoroot offers interesting perspectives for studying root exudate metabolome and their temporal and spatial dynamics in the rhizosphere, with important issues in both Ecology and Plant biology.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100205"},"PeriodicalIF":0.0,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143386385","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Identifying skin surface chemicals as potential tuberculosis diagnostic biomarkers using ultra performance liquid chromatography-high resolution mass spectrometry

Journal of chromatography open

Pub Date : 2025-02-02 DOI: 10.1016/j.jcoa.2025.100204

Madelien Wooding, Kornelis van Pletzen, Yvette Naudé

Tuberculosis (TB) remains a significant cause of morbidity and mortality globally, despite its preventability and curability. Early and accurate diagnosis of active TB is essential for enhancing patient care, improving outcomes, and interrupting the transmission cycles of Mycobacterium tuberculosis (M.tb). Metabolomics proves to be an emerging area of study for the development of a non-invasive approach to TB diagnostics.. High-resolution mass spectrometry combined with ion mobility spectrometry enhances the confidence in identifying and annotating biological markers during metabolomic research. This study outlines an analytical workflow encompassing sample preparation through to multivariate analyses for detecting potential TB diagnostic biomarkers. A custom-designed wearable polydimethylsiloxane (PDMS) sampler was employed as a passive sampling device, effectively concentrating chemical compounds from the skin surface. The sampler was directly desorbed into solvent within an LC vial, streamlining the extraction-to-analysis process. Utilising accurate mass and collision cross sections (CCS), fourteen biomarkers were tentatively identified, demonstrating the ability to differentiate TB patients from control groups. Receiver operating characteristic (ROC) analysis yielded an area under the curve (AUC) of 0.911. Among these, para-aminobenzoic acid (PABA) emerged as a promising biomarker for TB, achieving a specificity of 1, sensitivity of 0.9, and an AUC of 0.961. Method limits of detection for the 1-hour non-invasive skin sampling method ranged from 6 (PABA) to 172 ng (phenylalanine) for a calibration working range of 10 – 800 ng with a R² of ≥ 0.99. These first results demonstrate the potential of using skin surface compounds in TB diagnostics.

{"title":"Identifying skin surface chemicals as potential tuberculosis diagnostic biomarkers using ultra performance liquid chromatography-high resolution mass spectrometry","authors":"Madelien Wooding, Kornelis van Pletzen, Yvette Naudé","doi":"10.1016/j.jcoa.2025.100204","DOIUrl":"10.1016/j.jcoa.2025.100204","url":null,"abstract":"<div><div>Tuberculosis (TB) remains a significant cause of morbidity and mortality globally, despite its preventability and curability. Early and accurate diagnosis of active TB is essential for enhancing patient care, improving outcomes, and interrupting the transmission cycles of <em>Mycobacterium tuberculosis</em> (<em>M.tb</em>). Metabolomics proves to be an emerging area of study for the development of a non-invasive approach to TB diagnostics.. High-resolution mass spectrometry combined with ion mobility spectrometry enhances the confidence in identifying and annotating biological markers during metabolomic research. This study outlines an analytical workflow encompassing sample preparation through to multivariate analyses for detecting potential TB diagnostic biomarkers. A custom-designed wearable polydimethylsiloxane (PDMS) sampler was employed as a passive sampling device, effectively concentrating chemical compounds from the skin surface. The sampler was directly desorbed into solvent within an LC vial, streamlining the extraction-to-analysis process. Utilising accurate mass and collision cross sections (CCS), fourteen biomarkers were tentatively identified, demonstrating the ability to differentiate TB patients from control groups. Receiver operating characteristic (ROC) analysis yielded an area under the curve (AUC) of 0.911. Among these, para-aminobenzoic acid (PABA) emerged as a promising biomarker for TB, achieving a specificity of 1, sensitivity of 0.9, and an AUC of 0.961. Method limits of detection for the 1-hour non-invasive skin sampling method ranged from 6 (PABA) to 172 ng (phenylalanine) for a calibration working range of 10 – 800 ng with a R<sup>2</sup> of ≥ 0.99. These first results demonstrate the potential of using skin surface compounds in TB diagnostics.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100204"},"PeriodicalIF":0.0,"publicationDate":"2025-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168832","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Comprehensive characterization and identification of chemical constituents of Pingwei Powder by ultra high performance liquid chromatography tandem quadrupole-time-of-flight tandem mass spectrometry

Journal of chromatography open

Pub Date : 2025-01-09 DOI: 10.1016/j.jcoa.2025.100203

Tongyan Zhu , Na Li , Chunying Zhao , Jianwei Liu , Yuling Liu , Jianhui Chen , Yuxin Dong , Yuxuan Tian , Xia Hong , Hui Xiong

Pingwei Powder, a basic traditional Chinese medicine (TCM) prescription, was used for treating the chronic colitis, liver cirrhosis, and acute gastritis, etc. However, its systematic chemical characteristics has not been reported, which hinders the interpretation of its therapeutic mechanism, and quality control.

To develop a powerful ultra high performance liquid chromatography tandem quadrupole-time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS)-based method for the systematic chemical characterisation of Pingwei Powder, providing a basis for further research on pharmacological substance basis, and quality control of Pingwei Powder. UHPLC-Q-TOF-MS was used to detect a wide range of chemical substances in Pingwei Powder, and the obtained spectral data were imported into PeakView 1.2 software for data processing. Subsequently, the chemical substances in Pingwei Powder were identified by comparison with reference standards, literatures, and the built-in database of SCIEX OS 2.2 software. Finally, the chemical profile of Pingwei Powder was acquired, and 329 chemical components in Pingwei Powder were identified for the first time, mainly including flavonoids, terpenoids, organic acids, alkaloids, phenylpropanoids. Of note, 48 were from Atractylodis Rhizoma, 37 were from Magnoliae Officinalis Cortex, 72 were from Citri Reticulatae Pericarpium, 80 were from Glycyrrhizae Radix et Rhizoma, 32 were from Ginger, 60 were from Ziziphus jujuba. A scientifically efficient and credible method for obtaining the comprehensive chemical profile of Pingwei Powder based on UHPLC-Q-TOF-MS was developed for the first time, providing a basis for further research on pharmacological substance basis, and quality control of Pingwei Powder.

{"title":"Comprehensive characterization and identification of chemical constituents of Pingwei Powder by ultra high performance liquid chromatography tandem quadrupole-time-of-flight tandem mass spectrometry","authors":"Tongyan Zhu , Na Li , Chunying Zhao , Jianwei Liu , Yuling Liu , Jianhui Chen , Yuxin Dong , Yuxuan Tian , Xia Hong , Hui Xiong","doi":"10.1016/j.jcoa.2025.100203","DOIUrl":"10.1016/j.jcoa.2025.100203","url":null,"abstract":"<div><div>Pingwei Powder, a basic traditional Chinese medicine (TCM) prescription, was used for treating the chronic colitis, liver cirrhosis, and acute gastritis, etc. However, its systematic chemical characteristics has not been reported, which hinders the interpretation of its therapeutic mechanism, and quality control.</div><div>To develop a powerful ultra high performance liquid chromatography tandem quadrupole-time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS)-based method for the systematic chemical characterisation of Pingwei Powder, providing a basis for further research on pharmacological substance basis, and quality control of Pingwei Powder. UHPLC-Q-TOF-MS was used to detect a wide range of chemical substances in Pingwei Powder, and the obtained spectral data were imported into PeakView 1.2 software for data processing. Subsequently, the chemical substances in Pingwei Powder were identified by comparison with reference standards, literatures, and the built-in database of SCIEX OS 2.2 software. Finally, the chemical profile of Pingwei Powder was acquired, and 329 chemical components in Pingwei Powder were identified for the first time, mainly including flavonoids, terpenoids, organic acids, alkaloids, phenylpropanoids. Of note, 48 were from Atractylodis Rhizoma, 37 were from Magnoliae Officinalis Cortex, 72 were from Citri Reticulatae Pericarpium, 80 were from Glycyrrhizae Radix et Rhizoma, 32 were from Ginger, 60 were from Ziziphus jujuba. A scientifically efficient and credible method for obtaining the comprehensive chemical profile of Pingwei Powder based on UHPLC-Q-TOF-MS was developed for the first time, providing a basis for further research on pharmacological substance basis, and quality control of Pingwei Powder.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100203"},"PeriodicalIF":0.0,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168831","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of miniaturized autonomous and versatile gas chromatograph for Volatile Organic Compounds monitoring using Nano-Gravimetric-Detector

Journal of chromatography open

Pub Date : 2024-12-31 DOI: 10.1016/j.jcoa.2024.100202

Malak Rizk-Bigourd , Cécile Gaimoz , Eric Colinet , Jean-Pierre Pineau , Vincent Guerreni , Vivien Tranier , Fabrice Bertrand , David Coscia , Anaïs Feron , Michel Cabane , Cyril Szopa , Patrice Coll , Agnès Borbon , François Ravetta

Environmental monitoring and air quality survey during long-term field campaign tests, especially in low-accessibility or extreme environments, requires robust, standalone and autonomous analyzer with low gas consumption and minimal human intervention. The current states of art emphasize the need to develop miniaturized GC based on novel detectors that offers the best compromise between carrier gas consumption, detection limits and panel of measured VOCs. This work presents the development and optimization of MAVERIC, a miniaturized and autonomous Gas Chromatograph system coupled to an innovative Nano Gravimetric Detector (NGD) based on NEMS (nano-electromechanical-system) resonator. A homemade software is developed to control the instrument as well as the electronics modules. The system operates at low flow rate (2 mL.min⁻¹) of helium used as carrier gas, and allows the measurements of VOCs from C₆ to C₁₀ in less than 30 min. A mixture of isoprene, benzene, toluene and α-pinene is used to optimize experimental conditions. Under optimal conditions, the detection limit, the stability, the repeatability and the linearity of the analytical system are assessed. A detection limit of sub-ppb to few ppt level was determined for C₆ and C₉ compounds, respectively. The lowest detection limit corresponds to the highest molecular weight compounds due to NGD sensitivity at ambient temperature. The system is standalone, portable, robust and equipped with 4G connection that allows remote control of the instrument and easy data export. It is very adapted for a long period field campaign test, environmental monitoring and air quality survey outdoors and in low-accessibility or extreme environments.

{"title":"Development of miniaturized autonomous and versatile gas chromatograph for Volatile Organic Compounds monitoring using Nano-Gravimetric-Detector","authors":"Malak Rizk-Bigourd , Cécile Gaimoz , Eric Colinet , Jean-Pierre Pineau , Vincent Guerreni , Vivien Tranier , Fabrice Bertrand , David Coscia , Anaïs Feron , Michel Cabane , Cyril Szopa , Patrice Coll , Agnès Borbon , François Ravetta","doi":"10.1016/j.jcoa.2024.100202","DOIUrl":"10.1016/j.jcoa.2024.100202","url":null,"abstract":"<div><div>Environmental monitoring and air quality survey during long-term field campaign tests, especially in low-accessibility or extreme environments, requires robust, standalone and autonomous analyzer with low gas consumption and minimal human intervention. The current states of art emphasize the need to develop miniaturized GC based on novel detectors that offers the best compromise between carrier gas consumption, detection limits and panel of measured VOCs. This work presents the development and optimization of MAVERIC, a miniaturized and autonomous Gas Chromatograph system coupled to an innovative <em>Nano Gravimetric Detector (</em>NGD) based on NEMS (nano-electromechanical-system) resonator. A homemade software is developed to control the instrument as well as the electronics modules. The system operates at low flow rate (2 mL.min<sup>−1</sup>) of helium used as carrier gas, and allows the measurements of VOCs from C<sub>6</sub> to C<sub>10</sub> in less than 30 min. A mixture of isoprene, benzene, toluene and α-pinene is used to optimize experimental conditions. Under optimal conditions, the detection limit, the stability, the repeatability and the linearity of the analytical system are assessed. A detection limit of sub-ppb to few ppt level was determined for C<sub>6</sub> and C<sub>9</sub> compounds, respectively. The lowest detection limit corresponds to the highest molecular weight compounds due to NGD sensitivity at ambient temperature. The system is standalone, portable, robust and equipped with 4G connection that allows remote control of the instrument and easy data export. It is very adapted for a long period field campaign test, environmental monitoring and air quality survey outdoors and in low-accessibility or extreme environments.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100202"},"PeriodicalIF":0.0,"publicationDate":"2024-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168829","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of a transportable High-Performance Liquid Chromatograph with Ultraviolet detection and a method for the rapid analysis of 13 carbonyl compounds hydrazones

Journal of chromatography open

Pub Date : 2024-12-24 DOI: 10.1016/j.jcoa.2024.100201

Audrey Grandjean , Anaïs Becker , Mathilde Mascles , Franck Amiet , Jean-Philippe Amiet , Damien Bazin , Stéphane Le Calvé

In environments with elevated air pollution, highly reactive aldehydes pose significant health concerns. This study proposes a simultaneous analysis of 13 carbonyl compounds, according to the ISO 16,000–3 reference method, adapted for a novel transportable High-Performance Liquid Chromatograph (HPLC) system. The transportable HPLC system consists of a reinforced analytical suitcase and a computer suitcase, each equipped with spring systems to fortify them against impact. The system features a straightforward isocratic pump, ensuring reliability and ease of operation, while sample delivery is managed by a piston pump coupled to a multiplexing valve. Derived carbonyl compounds with 2,4-dinitrophenylhydrazine were separated in isocratic mode using water and acetonitrile with a reverse-phase column in less than 20 min. Out of the 13 hydrazones, only 2-butanone-2,4-DNPH (BO-DNPH) and butanal-2,4-DNPH (BA-DNPH) were fully coeluted, and separation of the other critical pairs containing 3 and 4 carbons was achieved. The method was applied to the transportable HPLC equipped with a UV or light-emitting diode (LED) detector. These results were compared with the ones obtained on two benchtop laboratory HPLCs equipped with a diode array detector (DAD). The limit of detection (LOD) for the hydrazones of the carbonyl compounds ranged from 0.12 to 0.38 mg L^–1 with the UV detector and 0.45 to 1.04 mg L^–1 with the LED detector. Precision was determined from consecutive injections of the analytes to yield RSD<11.5% (UV) and RSD<14.1% (LED). Performances were close to that of the laboratory HPLCs, either in sensitivity, resolution, or repeatability with overall more accurate and robust results with the UV than with the LED detector. Despite the LED system not fully meeting the standard method requirements with linearities correlation coefficients lower than 0.999, both systems and methods were validated for the isocratic analysis of hydrazones for aldehydes and ketones quantification. An additional comparison was made with the literature regarding both the isocratic method developed and the transportable system.

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引用次数: 0

Weak to strong ion-pair gradients to expand the selectivity of oligonucleotide separations in reversed phase liquid chromatography - A proof of concept

Journal of chromatography open

Pub Date : 2024-12-22 DOI: 10.1016/j.jcoa.2024.100200

Szabolcs Fekete , Mateusz Imiolek , Matthew Lauber

This study introduces a novel ion-pair reversed-phase liquid chromatography (IP-RPLC) method using a dual gradient approach to enhance the separation of oligonucleotides. By combining a weak ion-pairing (IP) agent in the starting (weaker) mobile phase with a strong IP agent in the final (stronger) mobile phase, this method widens the elution window, improving the resolution and selectivity for complex ON mixtures. The approach outperforms traditional single IP systems, particularly in separating sequence and size variants of ONs. Experimental results demonstrate that the weak-to-strong gradient yields better peak separation and higher selectivity compared to conventional methods. This innovative gradient strategy, combined with concave gradients, offers significant potential for optimizing ON separations in the development of oligonucleotide-based therapeutics.

引用次数: 0

Evaluation of thermodynamic contributions to extraction of medical devices by organic solvents as a sample preparation step in chemical characterization of medical devices

Journal of chromatography open

Pub Date : 2024-12-18 DOI: 10.1016/j.jcoa.2024.100199

Jianwei Li

<div><div>The thermodynamic contribution to extraction of medical devices by organic solvents as a first sample preparation step in chemical characterization studies is evaluated by Abraham's solvation parameter model using five representative materials (low density polyethylene or LDPE, silicone, polyurethane or PU, polyoxymethylene or POM, and polyacrylate or PA) and ten solvents (methanol, ethanol, isopropanol, acetonitrile, ethylene glycol, acetone, butanone, hexane, olive oil, and triolein). The Abraham's model is used to predict the material-solvent partition system coefficients by the corresponding partition system constants and representative extractables. The partition system constants are indirectly derived by a “thermodynamic circle conversion” method, based on material-water partition systems and solvent- water partition systems or material-air partition systems and solvent-air water partition systems. The material-solvent partition coefficient, <span><math><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></math></span>=<span><math><mrow><msub><mi>C</mi><mi>M</mi></msub><mo>/</mo><msub><mi>C</mi><mrow><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></mrow></math></span>, defined as the concentration in the material phase divided by the concentration in the solvent phase, is used as the solvent extraction strength. <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values are predicted for all material-solvent pairs using the representative extractables, mostly from Wayne state university experimental descriptor database (WSUEDD). The predictive <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values of material-solvent pairs are considered as the upper bound, indicating the significance of partitioning effect in solvent extraction. The calculation results using water-based or air-based partition systems are also compared. The predictive results are discussed in relation to the solvent-material interaction or swelling as well. Several conclusions can be drawn from this study. First, the predictive consistency of two conversion systems (water-based or air-based) is established, indicating the accuracy and robustness of Abraham's model. Second, the predicted partition coefficients are confirmed by available experimental values (LDPE and silicone), and the predicted solvent extraction strengths are supported by available experimental extraction data. Third, the kinetic effect, rather than the thermodynamic effect, is the dominant extractables release process in sample preparation step of chemical characterization studies. The solvent sel

{"title":"Evaluation of thermodynamic contributions to extraction of medical devices by organic solvents as a sample preparation step in chemical characterization of medical devices","authors":"Jianwei Li","doi":"10.1016/j.jcoa.2024.100199","DOIUrl":"10.1016/j.jcoa.2024.100199","url":null,"abstract":"<div><div>The thermodynamic contribution to extraction of medical devices by organic solvents as a first sample preparation step in chemical characterization studies is evaluated by Abraham's solvation parameter model using five representative materials (low density polyethylene or LDPE, silicone, polyurethane or PU, polyoxymethylene or POM, and polyacrylate or PA) and ten solvents (methanol, ethanol, isopropanol, acetonitrile, ethylene glycol, acetone, butanone, hexane, olive oil, and triolein). The Abraham's model is used to predict the material-solvent partition system coefficients by the corresponding partition system constants and representative extractables. The partition system constants are indirectly derived by a “thermodynamic circle conversion” method, based on material-water partition systems and solvent- water partition systems or material-air partition systems and solvent-air water partition systems. The material-solvent partition coefficient, <span><math><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></math></span>=<span><math><mrow><msub><mi>C</mi><mi>M</mi></msub><mo>/</mo><msub><mi>C</mi><mrow><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub></mrow></math></span>, defined as the concentration in the material phase divided by the concentration in the solvent phase, is used as the solvent extraction strength. <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values are predicted for all material-solvent pairs using the representative extractables, mostly from Wayne state university experimental descriptor database (WSUEDD). The predictive <span><math><mrow><mi>log</mi><mo>(</mo><msub><mi>P</mi><mrow><mi>M</mi><mo>/</mo><mi>S</mi><mi>o</mi><mi>l</mi><mi>v</mi><mi>e</mi><mi>n</mi><mi>t</mi></mrow></msub><mo>)</mo></mrow></math></span> values of material-solvent pairs are considered as the upper bound, indicating the significance of partitioning effect in solvent extraction. The calculation results using water-based or air-based partition systems are also compared. The predictive results are discussed in relation to the solvent-material interaction or swelling as well. Several conclusions can be drawn from this study. First, the predictive consistency of two conversion systems (water-based or air-based) is established, indicating the accuracy and robustness of Abraham's model. Second, the predicted partition coefficients are confirmed by available experimental values (LDPE and silicone), and the predicted solvent extraction strengths are supported by available experimental extraction data. Third, the kinetic effect, rather than the thermodynamic effect, is the dominant extractables release process in sample preparation step of chemical characterization studies. The solvent sel","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100199"},"PeriodicalIF":0.0,"publicationDate":"2024-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Targeted proteomics for absolute quantification of glucose transporter 1 in mammalian brain cells using liquid chromatography-mass spectrometry

Journal of chromatography open

Pub Date : 2024-12-14 DOI: 10.1016/j.jcoa.2024.100198

Yash Mehta , Dhavalkumar Patel , Iqra Pervaiz, Ulrich Bickel, Abraham Jacob Al-Ahmad

Glucose represents a major source of energy for mammalian brains. Its uptake is tributary to a functional glucose transporter (GLUT1) expression at the blood-brain barrier (BBB). However, detecting and quantifying GLUT1 at the protein level using antibodies-based methods can be challenging. In this study, we have described an analytical method (using liquid-chromatography mass-spectrometry (LC-MS/MS)) to provide a specific and absolute quantification of GLUT1 in human and non-human cells.

We identified a specific peptide signature for GLUT1 (TFDEIASGFR), with a retention time of 1.53 min with three distinct MRM transitions (571.8 > 894.3, 571.8 > 537.2 and 571.8 > 650.3 m/z ratios respectively). Following optimization, we compared the GLUT1 protein expression of our method versus immunoblot and concluded that our method was superior in terms of sensitivity (LLOQ=0.78ng/mL vs. 3.125μg/lane), better dynamic range (0.78–200ng/mL versus 3.125–25μg/lane) and better linearity (R2 = 0.999 versus R2 = 0.929) than the immunoblots counterpart. Furthermore, we used such a method to provide absolute GLUT1 quantification in various brain endothelial cells, showing differences in protein expression. Finally, we also used this method to assess changes in GLUT1 protein levels during the differentiation of induced pluripotent stem cells (iPSCs) into astrocyte-like cells (iAstros) and brain microvascular endothelial cell-like cells (iBMECs). Taken together, we have developed and optimized a proteomic method for the absolute quantification of GLUT1 in mammalian cells, which allows an alternative method for protein quantification independent of the antibody-based ones.

{"title":"Targeted proteomics for absolute quantification of glucose transporter 1 in mammalian brain cells using liquid chromatography-mass spectrometry","authors":"Yash Mehta , Dhavalkumar Patel , Iqra Pervaiz, Ulrich Bickel, Abraham Jacob Al-Ahmad","doi":"10.1016/j.jcoa.2024.100198","DOIUrl":"10.1016/j.jcoa.2024.100198","url":null,"abstract":"<div><div>Glucose represents a major source of energy for mammalian brains. Its uptake is tributary to a functional glucose transporter (GLUT1) expression at the blood-brain barrier (BBB). However, detecting and quantifying GLUT1 at the protein level using antibodies-based methods can be challenging. In this study, we have described an analytical method (using liquid-chromatography mass-spectrometry (LC-MS/MS)) to provide a specific and absolute quantification of GLUT1 in human and non-human cells.</div><div>We identified a specific peptide signature for GLUT1 (TFDEIASGFR), with a retention time of 1.53 min with three distinct MRM transitions (571.8 > 894.3, 571.8 > 537.2 and 571.8 > 650.3 m/z ratios respectively). Following optimization, we compared the GLUT1 protein expression of our method versus immunoblot and concluded that our method was superior in terms of sensitivity (LLOQ=0.78ng/mL vs. 3.125μg/lane), better dynamic range (0.78–200ng/mL versus 3.125–25μg/lane) and better linearity (R2 = 0.999 versus R2 = 0.929) than the immunoblots counterpart. Furthermore, we used such a method to provide absolute GLUT1 quantification in various brain endothelial cells, showing differences in protein expression. Finally, we also used this method to assess changes in GLUT1 protein levels during the differentiation of induced pluripotent stem cells (iPSCs) into astrocyte-like cells (iAstros) and brain microvascular endothelial cell-like cells (iBMECs). Taken together, we have developed and optimized a proteomic method for the absolute quantification of GLUT1 in mammalian cells, which allows an alternative method for protein quantification independent of the antibody-based ones.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100198"},"PeriodicalIF":0.0,"publicationDate":"2024-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168828","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Extraction of estrogenic hormones in wastewater samples by using rotating disk and modified clays with ionic liquids

Journal of chromatography open

Pub Date : 2024-12-04 DOI: 10.1016/j.jcoa.2024.100194

Carlos Andrés López-Vargas , Pablo Richter , Milton Rosero-Moreano

Both synthetic and natural hormones—17α-ethinylestradiol (EE2), 17β-estradiol (E2), and estriol (E3)—are present in wastewater samples in concentrations typically expressed in ng l^-1. These concentrations are significant, as the presence of such hormones in water sources poses risks to both living organisms and the environment. Steroidal hormones from human sources are categorized as emerging pollutants and endocrine-disrupting compounds (EDCs), which constitute a health hazard.

In this study, the Rotating Disk Sorption Extraction (RDSE) method was used with modified clays incorporating ionic liquids to detect estrogenic hormones in hospital wastewater treatment plant (HWWTP) samples. Sodium montmorillonite was modified to enhance its extractive capacity by intercalating ionic liquids ([C16MIM⁺][anion^-], where anion = Br^-, OH^-, or BF₄^-) between its interlayers. Following extraction, the concentrated analytes were measured using liquid chromatography coupled with photodiode array detection (HPLC-PDA). The method achieved absolute recoveries of 61 % for EE2, 41 % for E2, and 20 % for E3; these recoveries were lower than those obtained with a commercial C18 sorbent. However, the technique achieved enrichment factors of 13, 23, and 32 for E3, EE2, and E2, respectively. In wastewater, the intra-disk reproducibility (RSD) was below 12 %. The method also provided limits of detection and quantification in HWWTP samples of 0.18–0.42 ng mL^-1 for E3, 0.15–0.37 ng mL^-1 for E2, and 0.07–0.16 ng mL^-1 for EE2 when using the modified adsorbents. Average concentrations in hospital wastewater were measured at 4.30, 3.85, and 7.23 ng mL^-1 in the influent (before treatment) and 3.81, 1.33, and 4.00 ng mL^-1 in the effluent (after treatment) for E3, E2, and EE2, respectively.

{"title":"Extraction of estrogenic hormones in wastewater samples by using rotating disk and modified clays with ionic liquids","authors":"Carlos Andrés López-Vargas , Pablo Richter , Milton Rosero-Moreano","doi":"10.1016/j.jcoa.2024.100194","DOIUrl":"10.1016/j.jcoa.2024.100194","url":null,"abstract":"<div><div>Both synthetic and natural hormones—17α-ethinylestradiol (EE2), 17β-estradiol (E2), and estriol (E3)—are present in wastewater samples in concentrations typically expressed in ng <span>l</span><sup>-1</sup>. These concentrations are significant, as the presence of such hormones in water sources poses risks to both living organisms and the environment. Steroidal hormones from human sources are categorized as emerging pollutants and endocrine-disrupting compounds (EDCs), which constitute a health hazard.</div><div>In this study, the Rotating Disk Sorption Extraction (RDSE) method was used with modified clays incorporating ionic liquids to detect estrogenic hormones in hospital wastewater treatment plant (HWWTP) samples. Sodium montmorillonite was modified to enhance its extractive capacity by intercalating ionic liquids ([C16MIM<sup>+</sup>][anion<sup>-</sup>], where anion = Br<sup>-</sup>, OH<sup>-</sup>, or BF<sub>4</sub><sup>-</sup>) between its interlayers. Following extraction, the concentrated analytes were measured using liquid chromatography coupled with photodiode array detection (HPLC-PDA). The method achieved absolute recoveries of 61 % for EE2, 41 % for E2, and 20 % for E3; these recoveries were lower than those obtained with a commercial C18 sorbent. However, the technique achieved enrichment factors of 13, 23, and 32 for E3, EE2, and E2, respectively. In wastewater, the intra-disk reproducibility (RSD) was below 12 %. The method also provided limits of detection and quantification in HWWTP samples of 0.18–0.42 ng mL<sup>-1</sup> for E3, 0.15–0.37 ng mL<sup>-1</sup> for E2, and 0.07–0.16 ng mL<sup>-1</sup> for EE2 when using the modified adsorbents. Average concentrations in hospital wastewater were measured at 4.30, 3.85, and 7.23 ng mL<sup>-1</sup> in the influent (before treatment) and 3.81, 1.33, and 4.00 ng mL<sup>-1</sup> in the effluent (after treatment) for E3, E2, and EE2, respectively.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100194"},"PeriodicalIF":0.0,"publicationDate":"2024-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143168826","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0