Se pu = Chinese journal of chromatography最新文献

{"title":"[Research progress on sample pretreatment technology for the analysis of new pollutants in food using composite covalent organic framework materials].","authors":"Ze-Yi Sun, Guang-Nian Yuan, Yuan-Ye Niu, Ji-Ping Ma","doi":"10.3724/SP.J.1123.2025.08002","DOIUrl":"10.3724/SP.J.1123.2025.08002","url":null,"abstract":"<p><p>New pollutants are recently identified or recognized chemical substances. They pose risks to ecosystems or human health. Many are not yet regulated or lack effective control measures. These pollutants show biological toxicity， environmental persistence， and bioaccumulation. They threaten human health. In recent years， their detection frequency in food has increased. Efficient detection technologies are urgently needed. Sample pretreatment is key for analyzing new pollutants in food. The core of pretreatment lies in the preparation and selection of adsorbent materials. Covalent organic frameworks （COFs） are porous crystalline materials. They are formed by light elements linked through covalent bonds. COFs have highly ordered crystal structures. Their pore sizes can be adjusted. Surface properties are functionalizable. They show excellent chemical and thermal stability. Composite covalent organic framework materials combine COFs with other materials. This is achieved through physical or chemical methods. The composites exhibit synergistic effects. They retain the unique properties of both COFs and the other materials. This article reviews common sample pretreatment techniques for new pollutants in food. These include solid-phase extraction （SPE）， solid-phase microextraction （SPME）， stir bar sorptive extraction （SBSE）， dispersive solid-phase extraction （DSPE）， and magnetic solid-phase extraction （MSPE）. SPE is a chromatographic technique. It removes impurities from solid or liquid samples. It also enriches target compounds. SPE offers high enrichment factors and low solvent use. It is easy to automate. SPME balances samples between solid and liquid phases. It integrates sampling， extraction， and concentration. SPME uses little or no solvent. It is simple and automatable. It can be coupled with other techniques online. SBSE evolved from SPME. It has a larger stationary phase volume and higher capacity. SBSE uses a stir bar with a magnetic core. The bar is coated with an extraction layer. Stirring ensures full contact with analytes. SBSE is solvent-free or uses minimal solvent. It is accurate， fast， and easy to automate. DSPE disperses adsorbents into sample matrices. It increases contact area between adsorbents and analytes. DSPE simplifies sample processing. It avoids sample loss. MSPE uses magnetic or magnetizable materials as adsorbents. It captures target analytes efficiently. MSPE is simple to prepare and separate. Pipette-tip-SPE （PT-SPE） is a newer technique. It packs adsorbents into pipette tips. PT-SPE is flexible， low-cost， and needs small sample volumes. This article details types of composite COF materials. These include magnetic COF （MCOF）， sponge-COF， molecularly imprinted polymer-COF （MIP-COF）， metal-organic framework-COF （MOF-COF）， and electrospun-COF. MCOF combines COFs with magnetic nanoparticles. It enables quick separation under a magnetic field. Sponge-COF grows COFs on sponge fibers. It enhances adsorption capacity and mas","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"731-740"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352146/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414417","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}

{"title":"[Exploring the mechanism of action of <i>Synotis solidaginea</i> in treating acute eczema based on ultra performance liquid chromatography-linear trap quadrupole-Orbitrap mass spectrometry， network pharmacology and animal experiments].","authors":"Ci-Zhen Danzeng, Xin-Chen Fu, Pai-Er Luo, Ya-Chun Luo, Mei-Juan Shao, Shu-Ya Xie, Hao-Yu Ge, Xi-Fan Peng, Zha-Xi Pubu, Zhi-Hong Yan","doi":"10.3724/SP.J.1123.2025.10013","DOIUrl":"10.3724/SP.J.1123.2025.10013","url":null,"abstract":"&lt;p&gt;&lt;p&gt;This study employed an integrated strategy combining ultra performance liquid chromatography-linear trap quadrupole-Orbitrap mass spectrometry （UPLC-LTQ-Orbitrap-MS）， network pharmacology， molecular docking simulations， and in vivo animal experimentation to systematically analyze the active components of &lt;i&gt;Synotis&lt;/i&gt;&lt;i&gt;solidaginea&lt;/i&gt; （&lt;i&gt;S. solidaginea&lt;/i&gt;） and to elucidate its underlying therapeutic mechanism in the treatment of acute eczema. Initially， the UPLC-LTQ-Orbitrap-MS method was utilized to perform a comprehensive chemical profiling of &lt;i&gt;S. solidaginea&lt;/i&gt; extract. Based on accurate mass， multistage fragmentation spectra， and cross-validation with literature and reference standards， 59 constituents were unambiguously or tentatively identified. Subsequently， a network pharmacology framework was established to predict the potential pharmacological mechanisms of the identified compounds. Among the characterized constituents， seven bioactive ingredients-namely isorhamnetin， kaempferol， luteolin， quercetin， myricetin， betaine， and rosmarinic acid-were selected as the primary active components based on their relative abundance and favorable oral bioavailability and drug-likeness properties as predicted by the Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform （TCMSP）. The corresponding potential protein targets of these seven compounds were systematically screened using the TCMSP database and the SwissTargetPrediction tool， resulting in the identification of 192 component-associated targets after the removal of duplicate entries. Concurrently， a comprehensive collection of disease-associated targets was curated for acute eczema. By querying the GeneCards database and the Online Mendelian Inheritance in Man （OMIM） database with the keyword \"acute eczema\"， a total of 2 214 distinct therapeutic targets relevant to the pathogenesis and progression of the dermatological condition were retrieved. Through the construction of a Venn diagram to map the component-related targets onto the disease-specific target set， a core network comprising 75 overlapping targets was identified as the potential therapeutic intersection through which &lt;i&gt;S. solidaginea&lt;/i&gt; exerts its pharmacological effects against acute eczema. To further investigate the functional interactions and biological significance of these 75 intersecting proteins， a protein-protein interaction （PPI） network was constructed using the STRING database （version 12.0） and subsequently visualized and topologically analyzed using Cytoscape 3.10.1 software. Network topological analysis， specifically evaluating the degree centrality， betweenness centrality， and closeness centrality， highlighted SRC proto-oncogene tyrosine-protein kinase and matrix metalloproteinase 9 （MMP9） as the most prominent hub nodes within the network， suggesting their pivotal roles in mediating the therapeutic activity. Furthermore， Gene Ontology （GO） functional annotation and Kyoto Encyc","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"741-763"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352153/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414267","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}

{"title":"[Design and practice of instrumental analysis experiment： determination of borneol and camphor in <i>Chrysanthemum</i> by multiple headspace extraction-gas chromatography- mass spectrometry].","authors":"Hui-Xiang Li, Wen-Tao Jiang, Li-Hang Zhou, Han Zheng, Sha-Sha Liu, Jie Lei","doi":"10.3724/SP.J.1123.2025.09030","DOIUrl":"10.3724/SP.J.1123.2025.09030","url":null,"abstract":"<p><p>On the basis of previous experiments and research projects， this study developed an undergraduate instrumental analysis experiment by expanding the functionality of existing instruments. The primary objective was to enhance awareness among both instructors and students regarding the importance of sample pretreatment. Using <i>Chrysanthemum</i> as the analytical sample， an analytical method for determining the content of camphor and borneol was established based on multiple headspace extraction-gas chromatography-mass spectrometry （MHE-GC-MS）. By systematically optimizing key parameters such as headspace equilibration temperature and time， the optimal pretreatment conditions were determined as an equilibration temperature of 100 ℃ and an equilibration time of 20 min. Method validation demonstrated that both the liquid and solid external standard methods exhibit good linear relationships， correlation coefficients （<i>R</i>²） ranging from 0.981 2 to 0.999 2. Using the established method， the measured contents of camphor and borneol in <i>Chrysanthemum</i> were 0.917 4 mg/g and 0.944 2 mg/g， respectively. These results are significantly higher than those obtained by traditional hydrodistillation-solvent extraction， reflecting the near-complete extraction advantage of MHE. As a comprehensive inquiry-based teaching project， this experiment has been successfully integrated into the instrumental analysis laboratory course， effectively cultivating students' comprehensive practical skills and scientific thinking in method development， condition optimization， and data processing. The proposed teaching method does not require additional experimental reagents and demonstrates good universality， extendibility， and promotability， providing valuable insights for the reform of instrumental analysis laboratory teaching.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"821-826"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352150/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414315","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}

{"title":"[Simultaneous determination of five common pyrethroid metabolites in urine using liquid-liquid extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Xiao-Mei Zhang, Xiang-Juan Meng, Yue Hu, Xiao-Dong Liu","doi":"10.3724/SP.J.1123.2025.10017","DOIUrl":"10.3724/SP.J.1123.2025.10017","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Pyrethroids are extensively employed in agricultural pest management and household sanitation practices. However， their widespread use has raised concerns as they pose a multitude of health risks to humans. Consequently， the development of precise， highly sensitive， and efficient biomonitoring techniques for evaluating internal exposure levels of pyrethroids across different populations has emerged as a paramount goal in the field of environmental exposure and health effect research. This study developed a method using ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） for the simultaneous determination of five common pyrethroid metabolites in urine， with sample pretreatment involving hydrochloric acid hydrolysis and liquid-liquid extraction. The method was optimized for mass spectrometric acquisition parameters and liquid chromatography separation conditions. Chromatographic separation was successfully accomplished utilizing a BEH C&lt;sub&gt;18&lt;/sub&gt; column （100 mm×2.1 mm，1.7 μm）. Mass spectrometric data were acquired in negative ion mode under multiple reaction monitoring （MRM） conditions. Among the analytes， &lt;i&gt;trans&lt;/i&gt;-3-（2，2-dichlorovinyl）-2，2-dimethylcyclopropanecarboxylic acid （&lt;i&gt;trans&lt;/i&gt;-DCCA） and &lt;i&gt;cis&lt;/i&gt;-3-（2，2-dichlorovinyl）-2，2-dimethylcyclopropanecarboxylic acid （&lt;i&gt;cis&lt;/i&gt;-DCCA） are isomers， as are 2-phenoxybenzoic acid （2-PBA） and 3-phenoxybenzoic acid （3-PBA）， and they share identical MS acquisition parameters. Identification was based on reference standards and retention times. The mobile phase consisted of 0.1% acetic acid in water （A） and acetonitrile （B）. The gradient elution program was as follows： 0-0.5 min， 10%B； 0.5-4.5 min， 10%B-70%B； 4.5-5 min， 70%B-100%B； 5-7 min， 100%B； 7-8 min， 100%B-10%B； 8-10 min， 10%B. The optimization of urine sample pretreatment conditions was divided into two parts： hydrolysis and extraction. Using the recoveries of target analytes as the evaluation metric， parameters including the dosage of hydrolysis reagent， hydrolysis temperature and duration， as well as the type， dosage， and extraction time of the extraction solvent were systematically optimized. The optimized pretreatment protocol is delineated as follows： Initially， 40 µL of the 2-PBA internal standard working solution was precisely added to 1 mL of urine sample， followed by thorough mixing to ensure homogeneity. Subsequently， 150 µL of hydrochloric acid （2 mol/L） was introduced to facilitate hydrolysis， which was allowed to proceed at ambient room temperature for a duration of 30 min. Finally， extraction was carried out using 2 mL of ethyl acetate， accompanied by vigorous shaking for 30 min to maximize extraction efficiency. Following centrifugation， the organic phase was separated， evaporated to near dryness， and reconstituted with 1.0 mL of acetonitrile prior to instrumental analysis. The matrix effects were evaluated using pure solvent and matrix-matched standards. Among the five analytes， three exhibi","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"777-784"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352147/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414433","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}

{"title":"[Value assignment technology for 1，3-oleic-2-palmitic triglyceride purity reference material].","authors":"Xin-Yu Wang, Ying Wang, Meng-Qian Xu, Xia Zhou, Hong-Tao Chu, Qing-He Zhang, Xiu-Qin Li","doi":"10.3724/SP.J.1123.2025.10031","DOIUrl":"10.3724/SP.J.1123.2025.10031","url":null,"abstract":"&lt;p&gt;&lt;p&gt;1，3-Oleic-2-palmitic triglyceride （OPO） has received widespread attention as a nutritional fortifier allowed to be added to infant formulas， and there is an urgent need to develop high-purity certified reference material （CRM） to meet the metrological traceability requirements of relevant tests. Value assignment methods for pure materials are a key technical challenge in the development of high-purity CRMs. The commonly used mass balance （MB） method indirectly determines the purity of the material by subtracting impurities， which involves the accurate quantification of structurally similar impurities， moisture， volatile solvents， and non-volatile impurities. Among these steps， the separation and analysis of structurally similar impurities of the main component are the key to MB method. Owing to the lack of ultraviolet/fluorescence chromophores， OPO cannot be effectively detected by liquid chromatography with terminal absorption （190-210 nm）； this technique lacks sufficient sensitivity for low-level related impurities. Therefore， with a universal detector， this study established a high performance liquid chromatography-charged aerosol detector （HPLC-CAD） method for the analysis of structural analogue impurities in OPO， and applied the mass balance method to certify the purity of the reference material. On the other hand， based on quantitative nuclear magnetic resonance （qNMR） technology， a qNMR purity assignment method for OPO purity was established by optimizing key parameters such as NMR internal standards and quantitative peaks. In the mass balance method， an HPLC-CAD was selected as the core technique for quantifying trace structurally similar impurities of OPO. The chromatographic conditions were as follows： Nova Pak C8 column （150 mm×3.9 mm， 4 μm）， acetonitrile-isopropanol （90∶10， volume ratio） at a flow rate of 1.0 mL/min， sample dissolved in &lt;i&gt;n&lt;/i&gt;-hexane-isopropanol （1∶1， volume ratio） at a mass concentration of 2.0 mg/mL with an injection volume of 5 μL. Under these conditions， four structurally related trace impurities were baseline-separated and accurately quantified. Method validation showed that in the mass concentration range of 0.001-0.025 mg/mL， good linear relationship was obtained （&lt;i&gt;R&lt;/i&gt;²=0.999 1）. The limits of detection （LOD） and quantification （LOQ） were 0.000 5 mg/mL and 0.001 mg/mL， respectively， meeting the requirements for quantitative analysis. Six replicate measurements gave an average total impurity content of 1.23% （standard deviation 0.03%）， corresponding to an OPO main component content of 98.77%. In addition， Karl Fischer coulometric titration was used to determine moisture content， headspace gas chromatography-flame ionization detection （HS-GC-FID） was used to analyze residual volatile organic solvents （VOC）， and thermogravimetric analysis was used to determine non-volatile impurities. The purity of OPO was calculated as 98.51% by subtracting related impurities， moisture， VOC and non-volatile residues. ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"785-794"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352152/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414512","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}

{"title":"[Innovation in experimental teaching practice based on miniature mass spectrometer： from mass spectrometry principles to applications].","authors":"Lan Li, Jie Hong, Xin-Hui Yu, Pei-Feng Gao, Yan-Bing Zhai","doi":"10.3724/SP.J.1123.2025.06022","DOIUrl":"10.3724/SP.J.1123.2025.06022","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Mass spectrometer is an important component of the instrumental analysis courses in higher education. However， conventional commercial mass spectrometers usually lead to an imbalance between theory and practice in teaching， because of their characteristics of large size， high price and complicated operations， which makes it difficult to establish a direct link between instrument structure and detection principles. The miniature mass spectrometer shares the same core principles as commercial mass spectrometers. Equipped with an atmospheric pressure ionization （API） source， it significantly reduces sample preparation requirements， and enables rapid analysis of complex samples. The unique capability of the linear ion trap mass analyzer to scan， store， and eject ions enables a dramatic reduction in instrument size. The miniature ion funnel transmission technology and atmospheric pressure continuous sampling interface ensure high repeatability and rapid analysis， allowing compatibility with various atmospheric pressure ion sources for diverse sample types. In terms of performance， the miniature mass spectrometer has a mass-to-charge （&lt;i&gt;m/z&lt;/i&gt;） scan range of 50-2 000， and supports tandem mass spectrometry （MS&lt;i&gt;ⁿ&lt;/i&gt;）， enabling structural analysis of common organic compounds and rapid testing of complex samples. Therefore， the miniature mass spectrometer becomes an ideal tool for experimental teaching. This teaching course has developed a \"three-dimensional integrated\" teaching system aimed at enhancing students' knowledge， abilities， and literacy. Firstly， students disassemble key components of the instrument such as the ion source， ion funnel and trap to understand how they work together to achieve sample ionization， transmission， and acquisition. Mass calibration and full scan test help students master the basic operation. By adjusting the radio frequency （RF） voltage parameters， students could observe the impact of different parameters on the experimental results. Secondly， selected ion monitoring and tandem MS analysis help enhance students' data analysis skills and further develop their abilities in structural confirmation of compounds with MS. Lastly， pharmaceutical ingredient analysis， blood drug testing and multi-component screening of traditional Chinese medicine comprehensively demonstrate the wide applications of MS in scientific research and daily life， aiming to cultivate students' research thinking and problem-solving abilities. The gradient experiments （from basic calibration to advanced MS &lt;i&gt;&lt;sup&gt;n&lt;/sup&gt;&lt;/i&gt; ） combined with practical applications have effectively driven the implementation of the offline teaching course. The suggested experimental class hours are 12， covering pre-class preparation， in-class hands-on practice， data acquisition， and post-class summary. Practice has demonstrated that this integrated \"structure-principle-application\" teaching model effectively bridges the knowledge chain from theoretical learning t","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"834-842"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352154/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414400","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}

{"title":"[\"I love the lab\" research training： a cationic covalent organic framework aerogel for organic dye removal].","authors":"Yun-Meng Li, Hong-Yi Li, Dong-Xiao Cao, An-Na Tang, De-Ming Kong","doi":"10.3724/SP.J.1123.2025.10018","DOIUrl":"10.3724/SP.J.1123.2025.10018","url":null,"abstract":"<p><p>Methyl orange （MO） is a typical water-soluble azo organic dye. It is commonly used as an acid-base indicator in basic experiments and as a common organic dye in industrial production. It has strong polluting effects on water bodies. If azo dyes are accidentally ingested， the azo bond is cleaved by azoreductase， generating highly toxic aromatic amines that pose potential carcinogenic risks. Ionic covalent organic frameworks （ICOFs） are novel materials derived from covalent organic frameworks， featuring charged structures on their frameworks and pores. ICOFs exhibit excellent adsorption performance in aqueous solutions. Their high surface area and abundant porous channels facilitate rapid diffusion of pollutants into the inner structure， enabling effective pollutant adsorption. Eggplant is a sustainable biomass material with regular vertical macropores， which can be used as a substrate. This experiment employed an in-situ solvothermal method to prepare a highly efficient adsorbent monolithic material of eggplant composite aerogel （EP@PDA-TGDha COF）. It is applied to organic dye wastewater treatment. Developing this experiment as an undergraduate teaching module of \"I love the laboratory\" helps cultivate and enhance students' abilities in sample pretreatment， material synthesis， structural and property characterization， and practical sample analysis. Students enter the research group offline， experience the academic atmosphere， keep abreast of cutting-edge research， taking the crucial first step in their academic journey. Through the \"I Love the Lab\" research training program， students significantly enhance their professional knowledge， experimental skills， and research-oriented thinking abilities. It also fosters students' environmental protection awareness and enables them to apply their knowledge and skills to environmental conservation.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"812-820"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352151/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414290","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}

{"title":"[Determination of 29 per- and polyfluoroalkyl substances and 22 organophosphate esters and diester metabolites in human serum by high-throughput solid-phase extraction- ultra performance liquid chromatography- high resolution mass spectrometry].","authors":"Shi-Qi Zhao, Hao Ding, Xu-Wenqi Zhang, Min-Min Hou, Ting-Ting Zhou, Ya-Li Shi, Ya-Qi Cai","doi":"10.3724/SP.J.1123.2025.07008","DOIUrl":"10.3724/SP.J.1123.2025.07008","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Monitoring pollutants in human blood is a crucial basis for assessing human exposure levels and health risks. Per- and polyfluoroalkyl substances （PFAS）， organophosphate esters （OPEs）， and their diester metabolites （di-OPEs） are widespread environmental co-contaminants with significant toxic effects， making it crucial to monitor their internal human exposure levels. However， existing studies have predominantly investigated these substances in isolation， lacking comprehensive research that simultaneously quantifies PFAS， OPEs， and di-OPEs in human serum. Based on the pretreatment method of 96-well solid phase extraction columns， this study compared three extraction columns and optimized the pretreatment steps to establish an ultra performance liquid chromatography-high resolution mass spectrometry （UPLC-HRMS） method for 29 PFAS， 17 OPEs， and 5 di-OPEs in human serum samples. Phree PLR 96-Wellplate was used as a cleanup plate. 300 µL of 1% formic acid in acetonitrile， 100 µL of the serum sample， and internal standards were added to the cleanup device in sequence. After standing for 5 minutes， the 96-well plate positive pressure device was used to press the mixture into the 96-well collection plate. Finally， the sample was eluted with 100 µL of 1% formic acid in acetonitrile. The eluate was collected and concentrated for the detection of PFAS， OPEs， and di-OPEs by UPLC-HRMS. PFAS and OPEs were detected using an Acclaim RSLC 120 C18 column， while di-OPEs were detected using an Acquity UPLC BEH C18 column. Both were subjected to gradient elution with methanol and 5 mmol/L ammonium acetate in water as the mobile phases. Sample ionization was performed using a heated electrospray ionization source （H-ESI）. PFAS and di-OPEs were analyzed in negative ion mode， while OPEs were analyzed in positive ion mode. Data acquisition was conducted in full-scan/data-dependent tandem mass spectrometry （Full MS/ddMS&lt;sup&gt;2&lt;/sup&gt;） mode. Quantification was achieved using the internal standard calibration method to ensure measurement accuracy. The results showed that under the optimized conditions， the target compounds had good linear relationships in the range of 0.05-50 ng/mL （&lt;i&gt;R&lt;/i&gt;&lt;sup&gt;2&lt;/sup&gt; &gt; 0.99）， and the method detection limits （MDLs） of 29 PFAS， 17 OPEs and 5 di-OPEs were 0.000 120-0.274 ng/mL， 0.011 0-0.250 ng/mL， and 0.012 0-0.220 ng/mL， respectively， and the spiked recoveries were between 45.9% and 147.8%. The relative standard deviations （RSDs） were 1.2%-29.0%. Most PFAS and di-OPEs had matrix enhancement effects， and most OPEs had matrix inhibition effects. Among them， hexafluoropropylene oxide dimer acid （GenX） （196.5%） and trimethylphenyl phosphate （TMPP） （54.6%） had significant matrix enhancement and inhibition effects， respectively， which could be corrected with appropriate internal standards. The recoveries of these two substances after correction were 127.3% and 78.7%， respectively， which met the analysis requirements. The proposed approach of","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"764-776"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352148/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414279","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}

{"title":"[Case-based teaching with both positive and negative examples in undergraduate analytical chemistry laboratory： determination of six nitrogen-containing pesticides in environmental samples by solid-phase microextraction-high performance liquid chromatography].","authors":"Jie Zhang, Xin-Zhong Zhang, Zhen Zhang, Jing-Wei Liu, Xue-Mei Wang","doi":"10.3724/SP.J.1123.2025.10005","DOIUrl":"10.3724/SP.J.1123.2025.10005","url":null,"abstract":"<p><p>In analytical chemistry， separation and enrichment steps serve not only as critical stages in the analytical workflow， but also as core technologies that determine the accuracy， reliability， and applicability of analytical methods. However， in conventional experimental instruction， this step is frequently overlooked owing to time constraints and an overemphasis on instrumental techniques， leading to fragmented knowledge structures and hindering the development of integrated analytical thinking that connects theory with practice. To address this issue， this study， based on the \"knowledge-ability-practice\" three-dimensional integrated teaching objective， innovatively establishes a \"positive-negative case-based teaching\" model， using the solid-phase microextraction （SPME） of six nitrogen-containing pesticides from environmental water samples as the instructional case. By comparing fibers coated with non-polar polydimethylsiloxane （PDMS） and strongly polar polyacrylate （PA）， and employing high performance liquid chromatography with ultraviolet detection （HPLC-UV）， this study systematically investigates the matching relationship between analyte polarity and coating properties. In the positive case， the PDMS coating demonstrates superior extraction performance for weakly polar pesticides based on the \"like dissolves like\" principle， with a linear coefficient of determination <i>R</i>²≥0.993 7 and detection limits ranging from 0.019 to 0.17 μg/L. In contrast， in the negative case， the PA coating shows weaker extraction efficiency due to differences in the extraction mechanism， yielding detection limits between 0.066 to 1.069 μg/L. Based on spiked recovery tests conducted on actual river water samples from Lanzhou （recoveries： 81.5% to 117%）， a multi-dimensional evaluation system of \"knowledge internalization， competency enhancement， and practical literacy\" is established accordingly. Teaching feedback demonstrates that the students show a marked improvement in their understanding of the core principles， and their innovative thinking and problem-solving skills are effectively cultivated. The \"contrasting-case-based\" pedagogical approach effectively bridges theory and experiment while stimulating students' investigative thinking. The study provides a replicable and scalable practical model for the reform of analytical chemistry experimental teaching， which holds significant value in cultivating high-caliber talents with rational method selection and problem-solving abilities.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 6","pages":"713-720"},"PeriodicalIF":0.0,"publicationDate":"2026-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13237627/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148166409","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}

{"title":"[Preparation of mesoporous covalent organic framework core-shell stationary phase and its application in the analysis of astragaloside Ⅳ content in <i>Astragalus</i>].","authors":"Xing-Yun Zhao, Jiang-Yan Jin, Xiao-Jian Liu, Li-Juan Yan, Si-Yu Yang, Zhen-Wei Zhang, Li-Yun Zhang, Rong-Fang Wu","doi":"10.3724/SP.J.1123.2025.09020","DOIUrl":"10.3724/SP.J.1123.2025.09020","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Quality control of traditional Chinese medicine （TCM） has always been a key and challenging issue in the field of its modernization research. This has posed a high demand for advanced separation materials due to the complex compositions. Covalent organic framework materials （COFs） are a new class of porous crystalline materials composed of multidentate organic units connected by covalent bonds. They have demonstrated significant application value in areas such as catalysis and chromatographic analysis. This study focused on developing a novel core-shell-type chromatographic stationary phase using 2，4，6-tris（4-aminophenyl）-1，3，5-triazine （TAPT） and 1，4-benzenedicarboxaldehyde （TA） as building units. The TAPT-TA-COF@SiO&lt;sub&gt;2&lt;/sub&gt; core-shell composite materials were successfully prepared on the surface of silica microspheres using a multi-step polymerization strategy， in which the SiO&lt;sub&gt;2&lt;/sub&gt; cores were fabricated using the polymerization-induced colloidal aggregation （PICA） method. The imine-linked TAPT-TA-COF@SiO&lt;sub&gt;2&lt;/sub&gt; core-shell stationary phase was subjected to comprehensive physicochemical characterization and chromatographic evaluation experiments. The analytical techniques employed included scanning electron microscopy （SEM）， transmission electron microscopy （TEM）， energy dispersive spectroscopy analysis （EDS）， nitrogen adsorption-desorption isotherms， Fourier transform infrared spectroscopy （FT-IR）， and powder X-ray diffraction （PXRD）. The systematic characterization results clearly indicate that the prepared stationary phase exhibits excellent monodispersity， and the COF layer is uniformly coated on the surface of the SiO₂ core. TEM characterization demonstrated that the thickness of the COF materials on the surface of SiO&lt;sub&gt;2&lt;/sub&gt; is approximately 110 nm. Furthermore， FT-IR spectra were collected and the results demonstrated that the characteristic stretching vibrations at 3 209， 2 927， and 1 515 cm&lt;sup&gt;-1&lt;/sup&gt;， attributed to N-H， C-H， and C=N stretching， confirm the condensation reaction between TAPT and TA. In the XRD pattern， the peaks observed at 16.6°， 18.9°， 25.2° and 27.5° were attributed to the COF material and were consistent with previous reports， thereby confirming the successful synthesis of this derivative. The N&lt;sub&gt;2&lt;/sub&gt; adsorption-desorption isotherm analysis confirmed that the material possesses a typical mesoporous structure. Its specific surface area and pore size distribution are similar to those of the original porous SiO₂ microspheres， subsequently providing a structural basis for efficient chromatographic mass transfer kinetics. In addition， the chromatographic performance was investigated. And it was confirmed that the stationary phase was effectively used for the separation of representative neutral polar or non-polar compounds such as benzenes， alkylbenzenes， phthalate esters， formamides， and aniline mixtures. These compounds are separated due to hydrophobic interactions， &lt;i&gt;π-π&lt;/i&gt; interac","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 6","pages":"639-649"},"PeriodicalIF":0.0,"publicationDate":"2026-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13237632/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148166043","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}