{"title":"An injection filling method for packing chromatography devices","authors":"Raja Ghosh, Justin Bernar","doi":"10.1016/j.chroma.2025.465913","DOIUrl":"10.1016/j.chroma.2025.465913","url":null,"abstract":"<div><div>An injection filling method for packing resin media in a chromatography device for protein separation is discussed in this paper. The method is first demonstrated by packing anion exchange resin within a cuboid chromatography device and a squat column, both having 7.5 mL bed volume. The method is further demonstrated by packing size exclusion chromatography media in a 50 mL cuboid chromatography device. Overall, the packing method is simple and is less demanding in terms of requirement for operator skill and experience. The devices packed using the injection filling method had excellent separation efficiency attributes. Flow through and eluted protein peaks obtained using a device with an intentional minor indentation on the inner surface of the chromatography device showed pre-peaks (or fronting) and these peaks were wider than those obtained with a device without such an indentation. Surface imperfections had a greater impact on eluted peaks than on flow-through peaks. Size exclusion chromatography experiment carried out at high flow rates showed that protein separation obtained with the 50 mL cuboid device packed using the injection filling method was superior to that obtained with a conventional 50 mL column packed with the same media. At a high flow rate. the resin-bed within the column compacted very significantly while no such compaction was observed in the cuboid device.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465913"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143738638","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}
Eun Jae Kim , Eunjung Kwon , Seo Jung Oh , Mi Ran Choi , Sang-Rae Lee , Byung Hwa Jung , Wonwoong Lee , Jongki Hong
{"title":"Thermal transformation of CBD, CBDA, and Δ9-THC during e-cigarette vaping: Identification of conversion products by GC–MS","authors":"Eun Jae Kim , Eunjung Kwon , Seo Jung Oh , Mi Ran Choi , Sang-Rae Lee , Byung Hwa Jung , Wonwoong Lee , Jongki Hong","doi":"10.1016/j.chroma.2025.465909","DOIUrl":"10.1016/j.chroma.2025.465909","url":null,"abstract":"<div><div>The use of electronic cigarettes (e-cigarettes) has gained popularity worldwide for reducing the unpleasant odors and flavors of smoking marijuana. However, due to the high vaporization temperature of the heating coil in e-cigarettes, cannabinoids could be converted into secondary cannabinoid products, potentially causing unintended psychological and harmful effects. A lab-built impinger and aerosol collection device was prepared to study the thermal transformation of cannabinoids during e-cigarette vaping, optimizing collection conditions according to variations in coil wattage, cartridge oil, and collection solvents. Thermal conversion of individual cannabidiolic acid (CBDA), cannabidiol (CBD), and Δ<sup>9</sup>-tetrahydrocannabinol (Δ<sup>9</sup>-THC) in e-cartridge liquid was performed with increasing coil power from 45 W to 105 W. Collected aerosol solution was derivatized with trimethylsilyl reagents and analyzed by gas chromatography-mass spectrometry (GC-MS) scan mode. Thermal vaping profiles of individual authentic cannabinoids were studied according to the variation of coil power of the e-cigarette. During the CBDA vaping process of the e-cigarette, most of the acidic CBDA was converted to neutral CBD through thermal decarboxylation and further degraded to produce several thermal products. Several interesting psychoactive Δ<sup>8</sup>-iso and Δ<sup>9</sup>-THC isomers, and cannabichromene (CBC) and CBD quinone (CBDQ) were observed from the vaping process of CBDA and CBD. In the case of Δ<sup>9</sup>-THC vaping, psychoactive hexahydrocannabinol (HHC) derivatives and cannabinol (CBN), were produced <em>via</em> thermal reduction and oxidation. These thermal products were identified by comparing retention times and mass spectra of authentic standards and interpreting their mass spectra. The amounts of most thermal products were increased with increasing coil power from 45 W to 105 W. In contrast, potentially harmful CBDQ was found to be highest amount at 45 W and decreased with increasing coil power. From the profile data and identification results, thermal transformation pathways of cannabinoids during the vaping process are proposed. This study will provide important information on the formation mechanism of thermal conversion products and basic guidance for risk assessment of <em>Cannabis</em> oil vaping by e-cigarette.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465909"},"PeriodicalIF":3.8,"publicationDate":"2025-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143725127","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}
Jessy Pavón-Pérez , Gerardo Álvarez-Rivera , Miguel Herrero , Alejandro Cifuentes , Karem Henriquez-Aedo , Mario Aranda-Bustos
{"title":"Comparison of triple quadrupole and hybrid quadrupole-time-of-flight mass analyzers for LC-MS/MS determination of casein and ovalbumin in wines","authors":"Jessy Pavón-Pérez , Gerardo Álvarez-Rivera , Miguel Herrero , Alejandro Cifuentes , Karem Henriquez-Aedo , Mario Aranda-Bustos","doi":"10.1016/j.chroma.2025.465906","DOIUrl":"10.1016/j.chroma.2025.465906","url":null,"abstract":"<div><div>Casein and ovalbumin are commonly used as fining agents in the winemaking process to remove undesirable compounds like polymeric phenols. Since these proteins can trigger allergenic reactions in susceptible individuals, their presence must be declared on the label. Mass spectrometry (MS) using triple quadrupole (QqQ) analyzer under Multiple Reaction Monitoring (MRM) mode is one of the most used techniques for targeted proteomic analysis. However, recent advances in hybrid mass analyzers like quadrupole-time-of-flight analyzers (QTOF) have proved their potential for quantitative analysis. The objective of the present work was to perform a comprehensive analytical comparison of QqQ and QTOF performance for casein and ovalbumin quantification in wines. The performances of both analyzers were compared through the evaluation of fourteen wine samples applying isotope dilution analysis. Target proteins were determined employing <em>bottom-up</em> approach studying the resulting peptides from trypsin digestion. Results showed that QTOF analysis allowed the detection of 12, 6, and 4 more transitions than QqQ for α-casein, β-casein and ovalbumin, respectively. Instead, QqQ showed detection (LOD) and quantification limits (LOQ) 10-fold and 20-fold lower than QTOF for casein and ovalbumin, respectively. Sample analysis by QqQ revealed that 93 % of samples had detectable levels of casein and/or ovalbumin and 64 % showed higher levels than the EU limit for declaration. Overall, even when QqQ is the gold standard for accurate quantification, our results suggest the use of QTOF is a proper alternative for casein and ovalbumin determination in wines considering the higher number of transitions identified with a fit-of-purpose LOD and LOQ.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465906"},"PeriodicalIF":3.8,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143725126","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}
Zhihao Li , Dihong Zhong , Haipeng Lin , Peiyin Li , Yongyi Li , Qingmei Huang , Lingzhi Yang , Xueji Zhang
{"title":"In situ immobilization of covalent organic frameworks on diatomaceous earth for pipette-tip solid-phase microextraction","authors":"Zhihao Li , Dihong Zhong , Haipeng Lin , Peiyin Li , Yongyi Li , Qingmei Huang , Lingzhi Yang , Xueji Zhang","doi":"10.1016/j.chroma.2025.465893","DOIUrl":"10.1016/j.chroma.2025.465893","url":null,"abstract":"<div><div>Solid-phase microextraction (SPME) is essential for analyzing ultra-low concentration samples, such as trace drugs and environmental pollutants. Among various formats, pipette tip-based SPME (PT-SPME) stands out for its advantages in efficiency, automation, and flexibility. However, PT-SPME faces challenges such as material loss, high synthesis costs, and environmental impact. To address these issues, we developed a novel PT-SPME device by synthesizing Schiff-base covalent organic frameworks (COFs) <em>in situ</em> on diatomaceous earth (DE), which served as both a matrix and support. This approach significantly improved stability and reduced COFs consumption by 93.7 %. The DE@COFs were packed into pipette tips with a sandwich-like structure and used to extract polycyclic aromatic hydrocarbons (PAHs), with detection achieved through high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD). The method exhibited excellent sensitivity, with limits of detection (LODs) ranging from 2.05 to 52.5 pg/mL and limits of quantification (LOQs) from 15.0 to 159 pg/mL. It also demonstrated high accuracy, with recoveries between 87.05 % and 115.86 %, and strong repeatability, making it suitable for trace pollutant analysis in complex matrices This cost-effective and environmentally friendly PT-SPME system enhances extraction efficiency while reducing material usage, providing a practical and innovative solution for trace pollutant analysis in pharmaceutical and environmental applications.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465893"},"PeriodicalIF":3.8,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143715978","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}
João P.P. Saavedra , A. Rita Silva-Santos , Sofia O.D. Duarte , Ana M. Azevedo
{"title":"Scalable purification of bacteriophages preparations","authors":"João P.P. Saavedra , A. Rita Silva-Santos , Sofia O.D. Duarte , Ana M. Azevedo","doi":"10.1016/j.chroma.2025.465890","DOIUrl":"10.1016/j.chroma.2025.465890","url":null,"abstract":"<div><div>The use of bacteriophages to treat bacterial infections, known as phage therapy, has regained interest due to the rise of antibiotic-resistant bacteria. To make phage therapy more widely available, scalable purification methods that can adequately remove endotoxins, proteins and host cell DNA must be implemented. This is particularly important when considering intravenous (IV) administration, since the presence of these impurities is highly controlled by regulatory agencies. This work aimed at developing a purification workflow amenable to large-scale manufacturing, centred on the use anion-exchange chromatography (AEC). Lytic phage T4 and <em>Escherichia coli</em> K12 were used as the infection agent and host, respectively. Since endotoxins and phages are negatively charged, the use of an alkaline phosphatase (AP) prior to AEC was investigated to reduce their net negative charge and allow an efficient separation during chromatography. AP was used at 20 or 200 U/mL, and different AEC ligands and stationary phases were tested. H-bond chromatography (without enzymatic treatment) was exploited as well. Final phage titres up to 1.26 × 10<sup>11</sup> PFU/mL (plaque forming units) and global recoveries up to 45.1 % were obtained. The highest removal of endotoxins (98.8 %) was obtained after treatment with 20 U/mL of AP, followed by AEC with a quaternary amine packed-bed column. Virtually all proteins and DNA were removed in all workflows. Some of the obtained phage preparations would be suitable for IV administration, regarding endotoxin content. These results demonstrate that an enzymatic treatment in combination with AEC is a promising and scalable alternative to current phage purification techniques.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465890"},"PeriodicalIF":3.8,"publicationDate":"2025-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143715977","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}
Junlian Wang , Xiumin Yang , Chengqiang Hu , Ruiyi Sun , Guodong Xu
{"title":"Adsorption and separation of zirconium and hafnium from sulfate media by a conveniently synthesized (2,4,4-trimethylpentyl)(2-methylpropyl)phosphinic acid functionalized Merrifield Resin: A combined study of experiments and DFT calculations","authors":"Junlian Wang , Xiumin Yang , Chengqiang Hu , Ruiyi Sun , Guodong Xu","doi":"10.1016/j.chroma.2025.465894","DOIUrl":"10.1016/j.chroma.2025.465894","url":null,"abstract":"<div><div>A novel extractive resin grafting (2-methylpropyl)(2,4,4-trimethylpentyl)phosphinic acid groups through N atoms (marked as Mer-N-POOH-272), which is superior to most of the reported resins for hafnium(Hf) selective separation from zirconium (Zr), was synthesized and structurally characterized by FT-IR, SEM-EDS and XPS. The adsorption and separation behaviors of Mer-N-POOH-272 for Zr and Hf in sulphate media were investigated. The desorption behaviors of the adsorbed Zr and Hf by HCl, H<sub>2</sub>SO<sub>4</sub>, NaOH and Na<sub>2</sub>CO<sub>3</sub> solutions were studied. Density functional theory (DFT) calculations were conducted to reveal the adsorption mechanism. Mer-N-POOH-272 preferentially adsorbs Hf over Zr in H<sub>2</sub>SO<sub>4</sub> media, and the maximum Zr/Hf separation factor (<em>β</em><sub>Hf/Zr</sub>) reached to 6.5 <span><math><mo>±</mo></math></span> 0.3. The Zr and Hf adsorption by Mer-N-POOH-272 fit pseudo-first kinetic model and Langmuir isothermal adsorptionc model. It is the intraparticle diffusion that probably determines the adsorption rate. The Zr and Hf adsorptions onto Mer-N-POOH-272 belong to monolayer adsorption, and their experimental maximum adsorption amounts were 16.8 <span><math><mo>±</mo></math></span> 0.8 mg/g and 29.2 ± 1.0 mg/g, respectively. Sulfuric acid solution of 4.5 mol/L selectively desorbed the adsorbed Zr, and NaOH and Na<sub>2</sub>CO<sub>3</sub> solutions of ≥ 1.0 mol/L efficiently desorbed the left Hf. The DFT calculations show it is the two O atoms of -POOH in Mer-N-POOH-272 that probably interact with Zr or Hf ions during adsorption in H<sub>2</sub>SO<sub>4</sub> media, and Hf has lower adsorption energy than Zr, which explains the selectivity of Mer-N-POOH-272.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465894"},"PeriodicalIF":3.8,"publicationDate":"2025-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143734506","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}
Xiong Liu , He Zhang , Wei Zhou , Yuying Zhou , Yuexin Zhang , Xiaoliang Cao , Muqing Liu , Yingzi Peng
{"title":"Machine learning for predicting retention times of chiral analytes chromatographically separated by CMPA technique","authors":"Xiong Liu , He Zhang , Wei Zhou , Yuying Zhou , Yuexin Zhang , Xiaoliang Cao , Muqing Liu , Yingzi Peng","doi":"10.1016/j.chroma.2025.465896","DOIUrl":"10.1016/j.chroma.2025.465896","url":null,"abstract":"<div><div>Chiral mobile phase additive (CMPA) technique is an attractive method for chromatographic enantioseparation of chiral analytes. However, establishing chromatographic separation and analysis methods for given chiral analytes often requires extensive trial-and-error experiments, leading to time-consuming processes with high experimental costs. To address this challenge, machine learning (ML) was employed for the prediction of retention times of <em>R</em> and <em>S</em>-analytes to facilitate chromatographic enantioseparation. In this study, the enantiomeric retention times of chiral analytes enantioseparated by HPLC using cyclodextrin derivatives as CMPA were recorded, and the molecular descriptors of both the chiral analytes and the CMPA were calculated. Subsequently, several algorithms were employed for model development, with the coefficient of determination (<em>R</em><sup>2</sup>) serving as the metric to assess the precision of these models. The findings indicate that the CatBoost model works well in predicting retention times and separability of chiral analytes. This study provides a rapid and efficient method to facilitate the development of CMPA technique.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465896"},"PeriodicalIF":3.8,"publicationDate":"2025-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143704437","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}
Mathias B. Jørgensen , Jimi B. Dan , Kristian R. Nielsen , Tore Vulpius , Jan H. Christensen
{"title":"Real-time monitoring of contaminants of emerging concern in effluent wastewater with dynamic headspace gas chromatography mass spectrometry analysis","authors":"Mathias B. Jørgensen , Jimi B. Dan , Kristian R. Nielsen , Tore Vulpius , Jan H. Christensen","doi":"10.1016/j.chroma.2025.465895","DOIUrl":"10.1016/j.chroma.2025.465895","url":null,"abstract":"<div><div>Wastewater treatment plants are a major source of contamination, introducing pharmaceuticals, pesticides, and combustion products into aquatic environments. Currently, real-time monitoring of parameters such as nitrate and ammonia enables automatical control of these plants. In this paper we present the implementation and development of a dynamic headspace gas chromatography mass spectrometry method for real-time monitoring of contaminants of emerging concern in effluent wastewater. We observed a clear relation between polarity, water solubility, and analytical sensitivity, with the lowest sensitivity for the most polar compounds. Limits of quantification ranged from 15 to 3000 ng L<sup>-1</sup> in full scan mode depending on the physico-chemical properties of the internal standards. Both the proprietary software MassHunter and open-source software PARADISe were used for non-target screening. Both software solutions were in general able to identify similar compound structures and sample time profiles using the specified data processing methods. The identified non-target compounds were typically semipolar aromatic compounds such as fuel-related compounds, transformation products from biological wastewater treatment, and compounds such as the UV blocker benzophenone and the odorant amberonne.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465895"},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143715980","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}
{"title":"Determination of carboxyatractyloside, the main toxic component of Xanthium strumarium L., and alkaloid toxins in soybean by liquid chromatography tandem mass spectrometry","authors":"Ádám Tölgyesi, Attila Cseh, Andrea Simon","doi":"10.1016/j.chroma.2025.465897","DOIUrl":"10.1016/j.chroma.2025.465897","url":null,"abstract":"<div><div>The presence of carboxyatractyloside (CAT) in <em>Xanthium strumarium</em> L. (cocklebur weed) presents a high risk for both human and animal health. In this paper, we report a liquid chromatography tandem mass spectrometric (LC-MS/MS) method for the determination of CAT in soybean intended for animal feed. The herein described approach involves a fast sample preparation utilising QuEChERS extraction followed by dSPE clean-up. The optimised mobile phase composition flowing through an HPLC column packed with C18 fused-core particles consisted of alkaline conditions (pH = 8.8) in the aqueous eluent and pure methanol as the organic modifier. In this manner, it was also suitable for the analysis of tropane and ergot alkaloids together with CAT, which was attempted for the first time and may improve the analysis efficiency and reduce costs. During the method validation the matrix effect was also investigated, which clearly showed that matrix-matched calibration or standard addition is needed for appropriate quantification, mainly at low levels. The recoveries were between 94 % and 115 %, and the RSD % varied from 2.0 % to 7.3 %. The limits of quantification for alkaloids and CAT were 1 µg/kg and 100 µg/kg, respectively. The method implementation in other LC-MS/MS instruments was also tested. Finally, the validated method was successfully applied on soybean samples naturally contaminated with cocklebur.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465897"},"PeriodicalIF":3.8,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143697177","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}
Jin Liu , Wei Pan , Suzhen Li , Yuanjun Nie , Xinyuan Bi , Xu Jing , Li Li
{"title":"Green solvent-based high-throughput dispersive liquid-liquid microextraction for detecting strobilurin fungicides in environmental water samples","authors":"Jin Liu , Wei Pan , Suzhen Li , Yuanjun Nie , Xinyuan Bi , Xu Jing , Li Li","doi":"10.1016/j.chroma.2025.465888","DOIUrl":"10.1016/j.chroma.2025.465888","url":null,"abstract":"<div><div>A green solvent-based high-throughput dispersive liquid-liquid microextraction (HTDLLME) method has been developed as an environmentally friendly, straightforward, and efficient sample pretreatment technique. Six batches of extractant (eucalyptol) and dispersant (γ-valerolactone) mixtures were simultaneously injected into six samples and uniformly dispersed using electric 12-channel pipettes, achieving rapid extraction. The extractant and dispersant are sustainable, renewable, and non-toxic, eliminating the need for harmful solvents. The rapid dispersion and spontaneous separation of the extractant do not require auxiliary devices or demulsifiers, aside from the electric 12-channel pipettes. The combined use of electric 12-channel pipettes and deep-well plates increased pretreatment throughput, enabled semi-automatic operation, and improved overall efficiency. UHPLC-MS/MS was selected as the detector to ensure the sensitivity of the proposed method. Under optimal extraction conditions, the linear range was 0.002–0.2 μg L<sup>–1</sup>. The limit of detection and limit of quantification were 0.001 μg L<sup>–1</sup> and 0.002 μg L<sup>–1</sup>, respectively. The intra-day and inter-day relative standard deviations ranged from 2.4 % to 5.5 % and 1.5 % to 5.8 %, respectively. The green solvent-based HTDLLME-UHPLC-MS/MS method achieved rapid detection of SFs in different environmental samples, with extraction recoveries of 81.1 %–105.8 %. Greenness and blueness evaluation tools confirmed the environmental friendliness and practicality of the method. The green solvent-based HTDLLME approach provides a sustainable, straightforward, and practical solution for processing multiple samples simultaneously, supporting effective environmental monitoring.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1749 ","pages":"Article 465888"},"PeriodicalIF":3.8,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143697587","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}