Journal of Chromatography A最新文献

{"title":"Untargeted analysis of psilocybin and non-psilocybin mushrooms using liquid chromatography quadrupole time of flight mass spectrometry","authors":"Sabrina Islam ,&nbsp;Tiffany Liden ,&nbsp;Roman Goff ,&nbsp;Kevin A. Schug","doi":"10.1016/j.chroma.2025.466009","DOIUrl":"10.1016/j.chroma.2025.466009","url":null,"abstract":"<div><div>Psilocybin mushrooms, particularly those containing the psychoactive compounds psilocybin and psilocin, have attracted recent attention due to their potential therapeutic use for the treatment of psychological disorders. To use psilocybin mushrooms in a clinical context, it is important to understand their chemical composition more fully. An untargeted analysis using liquid chromatography (LC) quadrupole time-of-flight mass spectrometry was performed to explore the chemical diversity of various species of psilocybin mushrooms (PM) relative to edible non-psilocybin mushrooms (NPM). The analysis was performed using reversed phase LC with electrospray ionization in data independent acquisition mode. The study revealed the presence of several classes of compounds and their derivatives. The data was analyzed using multiple statistical methods. Principal component analysis showed that the psilocybin mushrooms and non-psilocybin mushrooms are compositionally very different from each other. These findings contribute to a deeper understanding of the chemical complexity of psilocybin mushrooms and lay groundwork for future research into their potential applications in medicine and psychology.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466009"},"PeriodicalIF":3.8,"publicationDate":"2025-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143901939","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}

{"title":"Supramolecular deep eutectic solvents applied in analytical studies: A review","authors":"Jingyan Chen,&nbsp;Jeongmi Lee","doi":"10.1016/j.chroma.2025.466007","DOIUrl":"10.1016/j.chroma.2025.466007","url":null,"abstract":"<div><div>Deep eutectic solvents (DESs) have gained widespread application as green solvents in analytical chemistry due to their low volatility, nonflammability, ease of synthesis, and biodegradability. Recently, a new subclass of DESs, known as supramolecular deep eutectic solvents (SUPRADESs), has emerged. SUPRADESs are non-covalent eutectic mixtures formed by self-assembled hydrogen-bonding interactions between components, including macrocyclic compounds such as cyclodextrins. They have attracted increasing attention in analytical studies owing to the intrinsic properties of DESs in combination with the host–guest inclusion capabilities of macrocyclic compounds. This review provides an overview of SUPRADESs from their development history and classification based on their type (binary SUPRADES and ternary SUPRADES). It also reviews recent advancements in their applications to analytical studies, such as sample pretreatment and separation methods, by categorizing them based on their specific roles (extraction solvent, desorption agent, sorbent material or sorbent modifier, and chiral selector). Compared to conventional solvents and DESs, SUPRADESs have demonstrated improved extraction and desorption efficiencies, enhanced enantioseparation performance, or better analyte stability. Finally, the limitations (e.g., high viscosity and lack of rational selection strategy) and future perspectives of the SUPRADES are briefly discussed to provide a valuable outlook for further applications of SUPRADESs in analytical studies.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466007"},"PeriodicalIF":3.8,"publicationDate":"2025-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143910965","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}

{"title":"Generic gradient elution RPLC analyses","authors":"Leonid M. Blumberg ,&nbsp;Gert Desmet","doi":"10.1016/j.chroma.2025.465999","DOIUrl":"10.1016/j.chroma.2025.465999","url":null,"abstract":"<div><div>Optimal flow rate (<em>F</em>_opt) in reversed phase LC (RPLC) analysis using the same column with the same solvent at the same pressure substantially depend on the molecular weight (<em>M</em>) of the solutes in the sample. The same is true for the optimal mixing rate (<em>R_ϕ</em>_,opt) – the temporal rate of changing the solvent composition at the column inlet – in gradient elution RPLC. General equations describing the dependence of <em>F</em>_opt and <em>R_ϕ</em>_,opt on <em>M</em> in columns of an arbitrary internal support structure (packed, open, pillar array, etc.) are developed and treated herein as equations for constructing generic RPLC analyses. As an example, parameters of generic analyses of the samples with molecular weights 300, 3000 and 30,000 in packed columns with 1.25 µm, 2.5 µm and 5 µm particles at 400 bar, 800 bar and 1500 bar pressures at optimal and suboptimal flow of water/ACN and water/MeOH solvents are tabulated. Kinetic performance advantages of ACN vs. MeOH as well as the advantages of using <em>F</em>_opt are quantified.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465999"},"PeriodicalIF":3.8,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143903920","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}

{"title":"Quantitative analysis of odor-causing compounds in technical lignins by static headspace-gas chromatography with calibration by standard addition","authors":"S. Carter Fox","doi":"10.1016/j.chroma.2025.465991","DOIUrl":"10.1016/j.chroma.2025.465991","url":null,"abstract":"<div><div>The odor of lignin derived from industrial wood pulping is an obstacle to incorporating it into industrial processes to make value-added products from this renewable resource. However, the molecular cause of the odors remains poorly understood. This is in part due to a lack of analytical methods capable of accurately quantifying odor-causing volatile chemicals in lignin. In this research, a procedure was developed to quantify volatile compounds in lignin using a standard addition protocol to calibrate chromatographic data generated by static headspace gas chromatography/mass spectrometry. Lignin samples were equilibrated at 150 °C for 1 h prior to sampling for analysis. It was found that performing the headspace analysis at this temperature, above the glass transition temperature of the lignin, was critical to obtaining accurate results. Alternatively, the sample equilibration temperature could be lowered if the lignin was sufficiently dissolved in a solvent or softened by a plasticizer. In contrast, heating dry lignin at a temperature below its glass transition temperature does not result in full equilibration of present volatile compounds between the bulk sample and the vapor phase. These findings will help improve objective analysis of odor from lignin and aid in the development of processes to better control lignin odor.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465991"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143895393","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}

{"title":"Analysis of neutral per- and polyfluoroalkyl substances (PFAS) by gas chromatography ‒ high resolution mass spectrometry (GCHRMS)","authors":"Yelena Sapozhnikova,&nbsp;Kevin Stroski","doi":"10.1016/j.chroma.2025.465989","DOIUrl":"10.1016/j.chroma.2025.465989","url":null,"abstract":"<div><div>Most of the studies on per- and polyfluoroalkyl substances (PFAS) to date encompass water soluble and ionic PFAS analyzed by liquid chromatography ̶ mass spectrometry, yet analytical methods and information on the occurrence of neutral PFAS are lacking. To this aim, we developed a new method for analysis of forty neutral PFAS using gas chromatography (GC) ̶ Orbitrap mass spectrometry with electron ionization (EI). Analytes were comprised of 29 fluorotelomer alcohols, 6 fluorotelomer acrylates and methacrylates, 3 perfluoroalkane sulfonamides and 2 perfluoroalkane sulfonamido alcohols. Gas chromatographic separation was developed on two GC phases: a standard non-polar (5 % diphenyl and 95 % dimethyl polysiloxane) and a mid-polar (6 % cyanopropylphenyl, 94 % dimethylpolysiloxane). A custom-made high-resolution mass spectral (HRMS) library was developed and used to evaluate PFAS accuracy of identification. Overall, 85 % of PFAS were correctly identified. A quantitative method was developed and evaluated for sensitivity, linearity, reproducibility, and ion interferences. Method sensitivity varied for different PFAS from 1 to 50 ppb based on the lowest calibrated levels. The developed method was utilized for analysis of PFAS in paper-based food contact materials after developing and evaluating the extraction protocol. Method applicability was demonstrated by analyzing paper-based food packaging samples, where 6:2 fluorotelomer alcohol was detected and measured at levels up to 351 ng/g. The developed GC<img>HRMS method can be utilized for identification and measurement of neutral PFAS in various matrices, including food, dust, food contact materials, textiles and others.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465989"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143881874","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}

{"title":"Insights into shell formation mechanism and semi-scale preparation of radially porous SiO2@SiO2 core-shell microspheres in a biphasic system for fast separation in ultra-performance liquid chromatography","authors":"Changwei Tang,&nbsp;Changle Li,&nbsp;Zilong Yang,&nbsp;Jiawei Liu,&nbsp;Quan Bai","doi":"10.1016/j.chroma.2025.465990","DOIUrl":"10.1016/j.chroma.2025.465990","url":null,"abstract":"<div><div>The biphasic method is commonly used to prepare SiO₂@SiO₂ core-shell microspheres (CSSMs) with pores perpendicular to the surface of the SiO₂ core. However, this method often results in incomplete shell coverage during scale-up preparation, which severely hinders the commercial application of this method. In this paper, the formation mechanism of the silica shell layer during the preparation of CSSMs using the biphasic method was investigated. The degree of interface disturbance in the biphasic system was found to affect the type and size distribution of emulsion droplets containing TEOS. Mild disturbance led to small O/W emulsion droplets around 2 μm in size, while strong disturbance resulted in both small O/W emulsion droplets around 2 μm and larger W/O/W emulsion droplets larger than 5 μm in the aqueous phase. Due to their mass differences, the droplets exhibit distinct inertial motion in the reaction system, leading to different wetting behaviors on the SiO₂ core surface. Specifically, the larger 5 μm droplets can partially wet the SiO₂ core interface when the silicate oligomer density on the droplet surface is low and hydrophobicity is high, whereas the smaller 2 μm droplets only wet the SiO₂ core interface when the silicate oligomer density is high and hydrophilicity is strong. When both droplet sizes coexist in the aqueous phase and participate in interfacial wetting, the residues with varying silicate oligomer densities further hydrolyze and condense, leading to shell structures with varying integrity. By reducing the stirrer diameter and agitation speed to maintain weak interfacial disturbance and generate only approximately 2 μm emulsion droplets, this study successfully resolved the issue of incomplete shell coverage during scale-up, achieving a CSSMs yield of 50 g. Furthermore, CSSMs modified with C18 were employed as the stationary phase in reversed phase liquid chromatography (RPLC) for the fast separation of small molecules and peptides. The superior separation efficiency indicates that the biphasic method has the potential to be utilized in the large-scale production of CSSMs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465990"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143881875","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}

{"title":"Influence of descriptor database selection on modeling retention factors in capillary micellar and microemulsion electrokinetic chromatography using the solvation parameter model","authors":"Sanka N. Atapattu ,&nbsp;Colin F. Poole","doi":"10.1016/j.chroma.2025.465992","DOIUrl":"10.1016/j.chroma.2025.465992","url":null,"abstract":"<div><div>Abraham's solvation parameter model has been widely used to model retention in capillary micellar and microemulsion electrokinetic chromatography systems. To fit or predict retention factors in separation systems experimentally determined compound descriptors are required. These are typically obtained from two sources: the Abraham and Wayne State University (WSU) compound descriptor databases. Alternatively, compound descriptors can be estimated from molecular structures using computational, machine learning, and group contribution approaches without having to resort to experimental methods for compounds without assigned values in either database. Here, we compare descriptor quality for the Abraham and WSU experimental compound descriptor databases as well as computational approaches using group contribution and machine learning approaches for modelling retention in capillary micellar and microemulsion electrokinetic chromatography systems. It is shown that the WSU compound descriptor database affords a more accurate description for the retention of varied compounds while descriptors based on a machine learning approach more accurately modeled retention factors than a group contribution approach. Model standard errors and coefficients of determination for WSU descriptors varied from 0.046 to 0.116 and 0.976 to 0.996, respectively, while Abraham descriptors varied from 0.048 to 0.166 and 0.953 to 0.995, respectively. Model standard errors and coefficients of determination for machine learning descriptors ranged from 0.086 to 0.116 and 0.979 to 0.981, respectively, whereas group contribution descriptors ranged from 0.090 to 0.181 and 0.942 to 0.979, respectively. Descriptor quality is important when modeling retention in capillary micellar and microemulsion electrokinetic chromatography systems.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465992"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143886691","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}

{"title":"Nontargeted screening strategy of chemical residues in animal-derived foods based on endogenous metabolite global annotation and interquartile range filtering by ultrahigh-performance liquid chromatography–high-resolution mass spectrometry","authors":"Wenying Liang ,&nbsp;Tiantian Chen ,&nbsp;Jun Yang ,&nbsp;Xinxin Wang ,&nbsp;Yujie Zhang ,&nbsp;Xin Lu ,&nbsp;Xinyu Liu ,&nbsp;Chunxia Zhao ,&nbsp;Guowang Xu","doi":"10.1016/j.chroma.2025.465986","DOIUrl":"10.1016/j.chroma.2025.465986","url":null,"abstract":"<div><div>Endogenous components and other experimental background information can interfere with the efficiency of nontargeted screening for unknown chemical residues in complex food matrices. In this study, a new nontargeted screening strategy of chemical residues in animal-derived foods was developed based on endogenous metabolite global annotation and interquartile range (IQR) filtering by ultrahigh-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS). First, endogenous metabolite global annotation was employed to eliminate the majority of endogenous components and their related ion peaks in food from the UHPLC-HRMS data. Second, IQR filtering was evaluated across multiple intercept values under different sample sizes and spiking concentrations based on 72 standards of chemical residues. The evaluation results indicated that chemical residues could be rapidly found after background interference was effectively removed when the sum of the third quartile and 20 times the interquartile range was used as intercept values. By integrating endogenous metabolite global annotation information with IQR filtering, this strategy achieved a total background interference filtering performance of &gt;95 %. Finally, this strategy was applied to screen 13 meat samples. Suspected chemical residues in meat samples were successfully found out and identified by endogenous metabolite global annotation and IQR filtering, and the overall capability for filtering background interference reached 93.1 %. The strategy effectively improved the efficiency of nontargeted screening for unknown chemical residues in animal-derived foods, which can provide a powerful tool for routine risk assessment of food safety.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465986"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143892175","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}

{"title":"Emission simulation using direct thermal extraction gas chromatography-mass spectrometry: Case study with curing of lignin-based binder","authors":"Daniil Salionov ,&nbsp;Miroslav Nikolic ,&nbsp;Marianne Glasius","doi":"10.1016/j.chroma.2025.465970","DOIUrl":"10.1016/j.chroma.2025.465970","url":null,"abstract":"<div><div>The transition towards using green construction materials represents a significant shift in the industry, aimed at reducing environmental impact and enhancing sustainability. A specific example of this is the development of lignin-based binders to produce insulation materials. Understanding and analyzing the process emission of novel binders can be crucial for sustainable production and legislative compliance. In this study a cost-effective and time-efficient laboratory method was developed to simulate emissions from the mineral wool curing process using direct thermal extraction gas chromatography mass spectrometry. Factors affecting the emissions of volatile organic compounds (VOC), such as flow, residence time, and the atmosphere (air or He) during the thermal desorption step, were investigated to identify the dominant factor influencing the chemical composition of emissions and to better replicate industrial processes. A laboratory method for binder impregnation was also developed to mimic factory-produced materials. Results showed that only the atmosphere significantly affects the chemical composition of emissions. The most abundant compounds in emissions were glycols, followed by aliphatic ketones, aldehydes (from mineral oil oxidation), and phenolic species (from lignin degradation). The VOC emissions from laboratory simulations closely matched those from industrial tests, particularly in an air atmosphere. This study establishes a method to evaluate the chemical composition of VOC emissions of novel lignin-based binders, facilitating a thorough analysis of their environmental effects.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465970"},"PeriodicalIF":3.8,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143892266","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}

{"title":"Construction of a natural puerarin-based green hypercrosslinked polymer fiber coating for the effective SPME of nitrobenzenes from environmental samples","authors":"Jiamiao Gao,&nbsp;Ruiyang Ma,&nbsp;Sijia Lv,&nbsp;Xiumin Yang,&nbsp;Zhi Wang","doi":"10.1016/j.chroma.2025.465987","DOIUrl":"10.1016/j.chroma.2025.465987","url":null,"abstract":"<div><div>Due to the potential hazardous effect caused by the possible nitrobenzenes (NBs) residues in environmental samples, the development of effective analytical methods for the quantification of NBs in some environmental samples becomes necessary in monitoring the environmental quality and protecting the public health. Herein, we developed a natural product-derived solid-phase microextraction (SPME) coating through a green synthesis of a natural puerarin-based hypercrosslinked polymer (Pue-HCP1) via Friedel-Crafts alkylation. Featuring abundant adsorption sites and suitable hydrophobicity, the Pue-HCP1-based fiber coating achieved the enrichment factors as high as 1112–6483 for the NBs. The coating also exhibited a good stability and durability. By integrating the SPME with gas chromatography-flame ionization detection, we developed a sensitive and reliable method for detecting NBs from environmental water and soil samples, with high sensitivity (limits of detection: 0.01–0.2 ng mL^-1 for water; 0.4–1.0 ng g^-1 for soil) and good accuracy (recoveries: 83.8%-115%).</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 465987"},"PeriodicalIF":3.8,"publicationDate":"2025-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143895391","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}