Journal of Chromatography A最新文献

{"title":"Fabrication and evaluation of a dual-zwitterionic functionalized hydrophilic monolith for chromatographic separation","authors":"Liang Lai ,&nbsp;Hongying Lan ,&nbsp;Hui Huang ,&nbsp;Tong Li ,&nbsp;Kesara Ar-sanork ,&nbsp;Jia-Huan Qu ,&nbsp;Dongsheng Xu ,&nbsp;Zhengjin Jiang","doi":"10.1016/j.chroma.2025.465917","DOIUrl":"10.1016/j.chroma.2025.465917","url":null,"abstract":"<div><div>In this study, the chromatographic performance of a novel dual-zwitterionic hydrophilic stationary phase were investigated. Three zwitterionic HILIC monoliths were prepared using 3-(4-((methacryloyloxy)methyl)-1-methylpiperidin-1-ium-1-yl)propane-1-sulfonate (MAMMPS), 2-methacryloyloxyethyl phosphorylcholine (MPC), and a combination of MAMMPS and MPC (1:1, molar ratio) with <em>N,N'</em>-methylenebisacrylamide (MBA), separately. The monoliths exhibited good repeatability and stability. A high column efficiency of 120,000 plates/m was reached on the novel dual-zwitterionic functionalized poly(MAMMPS@MPC-<em>co</em>-MBA) monolith. Through the analysis and testing with different standards, the poly(MAMMPS@MPC-<em>co</em>-MBA) monolith exhibited the strongest retention capacity for negatively charged benzoic acid derivatives due to its high hydrophilicity and weak electronegativity. In contrast, the poly(MPC-<em>co</em>-MBA) monolith, functionalized with a single zwitterion, facilitated electrostatic interactions with negatively charged analytes. Baseline separation was achieved on all three monoliths for selected nucleobases, nucleosides, phenol derivatives, and amine compounds. However, their retention strength was mainly related to the hydrophilicity of the stationary phases, while hydrogen bonding and electrostatic interactions played secondary roles. Among the monoliths, the poly(MAMMPS-<em>co</em>-MBA) monolith demonstrated the best separation for neutral, acidic, and alkaline compounds. These findings offer valuable insights for the future selection and application of dual-zwitterionic HILIC monoliths for chromatographic separations.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1751 ","pages":"Article 465917"},"PeriodicalIF":3.8,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143785293","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":"Development of a highly sensitive field-amplified capillary electrophoresis tandem triple quadrupole mass spectrometry for the quantification of trace methamphetamine in sewage","authors":"Yanping Wei ,&nbsp;Yujie Zhang ,&nbsp;Yueting Hu ,&nbsp;Fan Shui ,&nbsp;Jia Tang ,&nbsp;Yiyang Yu ,&nbsp;Guocan Zheng ,&nbsp;Jing Zeng","doi":"10.1016/j.chroma.2025.465920","DOIUrl":"10.1016/j.chroma.2025.465920","url":null,"abstract":"<div><div>Accurate quantification of trace levels of illicit drugs in wastewater, such as methamphetamine (MAMP), is crucial for sewage epidemiology. In this study, we developed a novel method that integrates field-amplified sample injection capillary electrophoresis with triple quadrupole mass spectrometry (FASI-CE-QQQ MS). This method enables simultaneous on-line preconcentration and separation, coupled with highly sensitive detection. Validation demonstrated excellent linearity within the range of 1 to 200 ng/L (R² = 0.9996), a limit of detection (LOD) of 0.1 ng/L (S/<em>N</em> = 12.3), high accuracy (RE &lt; 6.4 %) and precision (RSD &lt; 11.4 %). It was successfully applied to quantify MAMP in two unknown water samples, yielding average concentrations of 3.70 ng/L and 84.73 ng/L, respectively. These results were consistent with those obtained from an interlaboratory comparison exercise across China using on-line solid-phase extraction coupled with ultra-high performance liquid chromatography tandem triple quadrupole mass spectrometry (on-line SPE-UHPLC-QQQ MS). Finally, a comprehensive comparison between the newly developed FASI-CE-QQQ MS and the on-line SPE-UHPLC-QQQ MS methods revealed that the FASI-CE-QQQ MS offers significant advantages in terms of sensitivity, rapidity, and reduced solvent and sample consumption, making it a promising approach for the accurate determination of trace drugs in water.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465920"},"PeriodicalIF":3.8,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747596","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":"Ion exchange- and enrichment-based technology applied to large-scale plasma proteomic analysis of breast cancer neoadjuvant chemotherapy","authors":"Xiaozhen Cui ,&nbsp;Zhihua Zhong ,&nbsp;Sen Xu ,&nbsp;Yini Pan ,&nbsp;Xi Wang ,&nbsp;Luobin Zhang ,&nbsp;An He ,&nbsp;Xueting Ye ,&nbsp;Hua Cao ,&nbsp;Weibing Zhang ,&nbsp;Ruijun Tian","doi":"10.1016/j.chroma.2025.465914","DOIUrl":"10.1016/j.chroma.2025.465914","url":null,"abstract":"<div><div>Mass spectrometry (MS) based proteomics provides unbiased quantification of all proteins in plasma, which can dynamically reflect individual health states in real time. However, large-scale proteomics studies are constrained by the excessive dynamic range of plasma proteome and low throughput. Herein, two kinds of magnetic metal-organic frameworks (MOFs) modified with ion exchange functional groups (denoted as MHP-UiO-66-SAX and MHP-HKUST-1-SCX) were designed and fabricated to exhibit large protein adsorption capability, which were combined with an automated Liquid-handling System, thus realizing in-depth, high-throughput and automated proteomics studies. The constructed workflow could automatically complete the sample preparation before MS within only six hours and nearly a thousand protein groups per sample could be quantified. In the cohort study of nearly one hundred breast cancer neoadjuvant chemotherapy (NC) plasma samples, two differentially expressed proteins previously reported as biomarkers were related with the pathological complete response (PCR) of the breast cancer, demonstrating the feasibility of the developed technology for preparing large-scale clinical samples and exhibiting the potential application in monitoring the effect of chemotherapy.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465914"},"PeriodicalIF":3.8,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143783028","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":"Model-based analysis of a hydrophobic interaction chromatography for antibody-drug conjugate purification","authors":"Tobias Hahn ,&nbsp;Fara Lyu ,&nbsp;Pia Graf ,&nbsp;Steve Richter ,&nbsp;Jorge Gandarilla ,&nbsp;Dean Clyne ,&nbsp;Lei Cao ,&nbsp;Chen Wang","doi":"10.1016/j.chroma.2025.465916","DOIUrl":"10.1016/j.chroma.2025.465916","url":null,"abstract":"<div><div>Antibody-drug conjugates (ADCs) are a class of biopharmaceutical drugs designed as a targeted therapy for treating cancer while sparing healthy cells. ADCs are complex molecules composed of an antibody linked to a biologically active cytotoxic drug. The drug-to-antibody ratio (DAR), which represents the number of drugs conjugated to an antibody, is an important quality attribute of ADCs. The conjugation process typically yields a complex DAR profile, which requires further purification to remove undesired DAR species. Separation of DAR species post conjugation reaction can be achieved using hydrophobic interaction chromatography (HIC). HIC utilizes the hydrophobicity differences of different drug-loaded ADCs to separate them by reversible interaction between the proteins and the hydrophobic stationary phase. The buffer greatly influences the binding interaction between hydrophobic proteins and a HIC resin, but the process is also sensitive to variations in temperature, resin attributes, and the solid-liquid ratio of the column. A mechanistic model that captures these critical process parameters and material and column properties was established from calibration studies using multiple well-characterized HIC columns and resin lots. This model enabled in-silico characterization of the HIC process and facilitated understanding of unexpected process performance observations. It revealed the importance of controlling resin-specific hydrophobic capacity to minimize the DAR separation variations. It led to identifying an effective process control strategy to ensure a consistent DAR profile.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465916"},"PeriodicalIF":3.8,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747594","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":"Off-line in-tube solid-phase microextraction of some herbicides based on poly(styrene-divinylbenzene) coated Fe3O4 nanoparticles","authors":"Maedeh Saadat ,&nbsp;Yadollah Yamini ,&nbsp;Nasser Nikfarjam ,&nbsp;Hanieh Kefayati","doi":"10.1016/j.chroma.2025.465910","DOIUrl":"10.1016/j.chroma.2025.465910","url":null,"abstract":"<div><div>Triazines are a class of persistent micropollutants in environmental areas with high toxicity. Because of their general usage and poisonous and stability of their deteriorated products, extraction and determination trace amounts of triazines are important. Off-line in-tube solid phase microextraction efficiently used for extraction of trace amounts of analytes. In addition, magnetic field was used to keep the nanoparticles in the tube and also to enhance preconcentration of the analytes. Magnetic nanoparticles can be utilized as a reusable sorbent with high surface area, strong interaction, chemical stability and high selectivity.</div><div>A novel approach was introduced using a magnetic nanocomposite of cross-linked poly(styrene-divinylbenzene) for the in-tube solid-phase microextraction of triazine herbicides. The prepared material was characterized using various techniques. High performance liquid chromatography-ultraviolet detection was used to separate and determine the analytes. The effects of pH (6), extraction time (20 min), type and volume of elution solvent (500 µL methanol) and extraction flow rate (2 mL min^-1), desorption flow rate (50 µL min^-1) and salt addition (15%) and applying magnetic field on the extraction efficiency of the triazines were investigated. Under optimum conditions, calibration curves were found to be linear in the range of 0.3-500 µg L⁻¹ for cyanazine, simazine, and propazine with a coefficient of determination (R²) of 0.9951, 0.9984, and 0.9984, respectively. The LODs were 0.1 µg L⁻¹ for all of the analytes. The method was successfully used for the extraction and determination of triazine herbicides in fruit juice samples.</div><div>Magnetic nano particles illustrate minimum back pressure in tube due to elimination of filters, high surface-to-volume ratio and lot of active sites favorable for the adsorption of the analytes. Despite the limitations imposed by the chemical conditions of extraction on the application of nanoparticles and polymeric sorbents, variables such as pH, concentration, and surface charges do not influence the magnetic interactions of MNPs. By applying magnetic field, the magnetic nature of the analytes is effective on the preconcentration of them.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465910"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143747597","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":"An injection filling method for packing chromatography devices","authors":"Raja Ghosh,&nbsp;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}

{"title":"Study of the aberrant retention behavior of a semi-crystalline polyamide in reversed-phase liquid chromatography","authors":"Jordy D. Kruijswijk ,&nbsp;Stefan Wijker ,&nbsp;Harry J.A. Philipsen ,&nbsp;Peter J. Schoenmakers ,&nbsp;Govert W. Somsen","doi":"10.1016/j.chroma.2025.465887","DOIUrl":"10.1016/j.chroma.2025.465887","url":null,"abstract":"<div><div>The elution behavior of semi-crystalline polyamides (PAs) in reversed-phase liquid chromatography (RPLC) was examined. RPLC of the aliphatic polyamide 4,6 (PA46) yielded a single broad peak. However, the partly aromatic polyamide X (PAX) displayed a deviating elution profile, encompassing early- and late-eluting portions, which changed in relative abundance when varying injection and gradient conditions. These bands were suspected to be due to formation of amorphous and crystalline phases, respectively. RPLC fractions of the PAs were subjected to the same RPLC system and to size-exclusion chromatography. The presumed amorphous PAX portion showed two bands in RPLC, suggesting that (largely) amorphous and crystalline phases are formed upon sample injection. Differential scanning calorimetry (DSC) demonstrated that reducing the crystallinity of PAX decreased the relative abundance of the late-eluting fraction, approaching the behavior of aliphatic polyamides. X-ray diffraction and static-light-scattering analyses confirmed the semi-crystallinity of the two solid PA samples. Although both small particles and larger aggregates were observed in solution, these findings could not be correlated to the differences in elution profile of the PAs. Cloud-point measurements indicated that the solubility of both PA46 and PAX was almost independent of temperature. Strikingly, at low column temperatures (i.e. below the depressed melting point), PAX eluted as a single broad PAX peak. To conclude, the semi-crystallinity of PAX influences its RPLC-elution behavior, and by ensuring complete dissolution of the crystalline phase useful chemical information can be extracted from the obtained chromatograms.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1750 ","pages":"Article 465887"},"PeriodicalIF":3.8,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143759299","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":"Thermal transformation of CBD, CBDA, and Δ9-THC during e-cigarette vaping: Identification of conversion products by GC–MS","authors":"Eun Jae Kim ,&nbsp;Eunjung Kwon ,&nbsp;Seo Jung Oh ,&nbsp;Mi Ran Choi ,&nbsp;Sang-Rae Lee ,&nbsp;Byung Hwa Jung ,&nbsp;Wonwoong Lee ,&nbsp;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 Δ⁹-tetrahydrocannabinol (Δ⁹-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 Δ⁸-iso and Δ⁹-THC isomers, and cannabichromene (CBC) and CBD quinone (CBDQ) were observed from the vaping process of CBDA and CBD. In the case of Δ⁹-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}

{"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 ,&nbsp;Gerardo Álvarez-Rivera ,&nbsp;Miguel Herrero ,&nbsp;Alejandro Cifuentes ,&nbsp;Karem Henriquez-Aedo ,&nbsp;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}

{"title":"In situ immobilization of covalent organic frameworks on diatomaceous earth for pipette-tip solid-phase microextraction","authors":"Zhihao Li ,&nbsp;Dihong Zhong ,&nbsp;Haipeng Lin ,&nbsp;Peiyin Li ,&nbsp;Yongyi Li ,&nbsp;Qingmei Huang ,&nbsp;Lingzhi Yang ,&nbsp;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}