最新刊期
卷 44 ， 期 1 ， 2025
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摘要：Protein phosphorylation and glycation are two of the most prevalent post-translational modification processes of proteins. Phosphoproteins and glycoproteins play an important role in the cell life cycle and are also of great significance for the early diagnosis of clinical diseases. However，due to the low content of them and large matrix interference in biological samples，finding an appropriate method for the separation and enrichment of phosphoproteins and glycoproteins is one of the decisive steps in proteomics research. Magnetic solid phase extraction（MSPE） is a solid phase extraction（SPE） technology with magnetic nanoparticles as adsorbent. Compared with conventional SPE，MSPE has the merits of simple operation and environmental friendliness，with its materials easy to recycle. Therefore MSPE has been widely applied for the separation and enrichment of phosphoproteins/peptides and glycoproteins/peptides before analysis. In this article，the MSPE materials used for separation and enrichment of phosphoproteins and glycoproteins in recent five years are systematically summarized and reviewed，and the future development trend of such materials is prospected and discussed.关键词：phosphoproteins;glycoproteins;magnetic solid phase extraction;magnetic nanoparticles611|1089|0更新时间：2025-10-13 -
摘要：Emerging contaminants（ECs） have attracted much attention in many countries because of their environmental persistence，bioaccumulation，biotoxicity and trace amounts in the environment. Therefore，the highly sensitive detection of ECs in environmental，food，and biological samples is essential. The traditional sample pretreatment technology still exists shortcomings such as consuming time，large amount of adsorbent and the poor analysis accuracy of unstable pollutants. Hence，it is urgent to develop and design new materials with high selectivity and high mass transfer efficiency as adsorbent of pretreatment technology to achieve the highly selective and sensitive detection of ECs. Covalent organic frameworks（COFs），especially its functionalized COFs materials，are widely used for the detection of ECs due to their advantages of the large specific surface area，designable structure，stability and abundant building elements. Based on this，the synthetic strategies of functionalized COFs materials and their applications as adsorbents of sample pretreatment for the analysis of ECs in environmental，food and biological samples were reviewed in this paper. Finally，the development tendency of such materials in the future were prospected.关键词：emerging contaminants;functionalized COFs materials;sample pretreatment techniques584|1352|0更新时间：2025-10-13 -
摘要：Electromembrane extraction（EME） is a green and efficient microextraction technique，which has been widely applied in all kinds of fields including food analysis，environmental analysis and forensic toxicological analysis in recent years due to the advantages of high selectivity，sufficient sample clean-up capability，and simple in operation. This review summarized the research progress in EME for the separation of drugs-of-abuse over the past five years，with a particular emphasis on its application in extracting and enriching abused drugs from various biological matrices，and paid special attention to the separation performance of EME for illicit drugs，new psychoactive substances（NPS），and addictive pharmaceuticals. Furthermore，this review also examined the challenges faced by EME in its routine application within the field of forensic science and provided a prospective outlook on the future development directions of EME.关键词：electromembrane extraction;forensic toxicological analysis;sample preparation;drugs-of-abuse;hair;saliva625|529|0更新时间：2025-10-13 -
摘要：Cyclodextrin（CD） is a type of cyclic oligosaccharide comprising glucose molecules，and it possesses a large ring cavity that is hydrophilic on the exterior and hydrophobic on the interior，enabling it to encapsulate a diverse range of guest molecules. Cyclodextrin-containing polymers（CDPs） are defined as a polymer derivative containing multiple cyclodextrin units constructed by chemical bonding of cyclodextrin molecules，which not only preserves the envelope recognition capabilities of cyclodextrin，but also exhibits enhanced mechanical strength，stability，and chemical adaptability as a polymeric entity. CDPs have a wide range of potential applications in sample pretreatment，their selective adsorption and separation，efficient removal of contaminants，and reproducible and environmentally friendly properties provide strong support for their applications in environmental protection，food safety and other fields. This paper presents a generalization of the synthesis methods of different CDPs and their applications in the field of sample preparation for food analysis，by combining with solid-phase microextraction，magnetic solid-phase extraction，stir bar extraction and other techniques. CDPs are able to effectively separate and enrich target analytes，including pesticide residues，food additives and natural flavour components，in food. Additionally，it offers a summary of the current development status and future development trends of CDPs.关键词：cyclodextrin;cyclodextrin polymers;sample pretreatment;food analysis;selective adsorption501|659|0更新时间：2025-10-13 -
摘要：Direct analysis in real time mass spectrometry（DART-MS） is widely used in food analysis，forensic science，pharmaceutical analysis，clinical science，environmental science and other fields，as it requires no or minimal sample preparation and can perform in-situ ionization and direct sample analysis. Although the quantitative results of DART-MS have been reported to be comparable to those of liquid/gas chromatography-mass spectrometry，the detection performance of trace analytes is still an important issue. To obtain more accurate quantitative results，a series of sample pretreatment technologies have been developed to be combined with DART-MS. In this review，the general principle of DART-MS is introduced，followed by its applications in different research fields that do not require sample pretreatment. Sample pretreatment technologies coupling with DART-MS，including solid-phase extraction（SPE），solid-phase microextraction（SPME），solid-phase mesh enhanced sorption from headspace（SPMESH），dispersive solid-phase extraction（DSPE），dispersive micro solid-phase extraction（DMSPE），mechanochemical extraction（MCE），microwave-assisted extraction（MAE） and thermal desorption（TD） are further summarized and commented. The possible optimizations in the future are also proposed in this review，hoping to provide great insight into the applications of direct sample analysis by DART-MS and the development of sample pretreatment technologies coupling with DART-MS.关键词：mass spectrometry;direct analysis in real time;direct sample analysis;sample pretreatment technology680|612|0更新时间：2025-10-13 -
摘要：As industrial development advances，the intensification of heavy metal and radioactive substance pollution has coincided with a growing demand for rare metals. Consequently，it is essential to implement a process of separation and enrichment of metals. Covalent organic frameworks（COFs），which are distinguished by large specific surface area，high porosity，high crystallinity，and adjustable pore size，have emerged as promising materials for metal separation and enrichment. The selectivity of COFs for specific metal ions can be enhanced through the incorporation of tailored functional groups. Furthermore，the robust covalent bonds within COFs contributes to their stability in harsh environments. Given the above，this paper offers a comprehensive overview of the application of COFs in metal separation and enrichment in recent years. It focuses on the diverse connection modes of COFs and their associated separation，enrichment，and adsorption mechanisms in precious metals，heavy metals，rare earth elements，and radioactive elements. Finally，the article addresses presents a comprehensive analysis of the challenges associated with the practical application of COFs for the separation and enrichment of metals，while also offering insights for future research.关键词：covalent organic frameworks;separation;enrichment;metal579|1156|0更新时间：2025-10-13 -
摘要：Hydrogen bonding was usually the main mechanism for molecularly imprinted polymers to recognize template molecules. Due to the interference of many influencing factors such as water molecules，efficient identification of analytes in water environment has always been a major challenge for molecularly imprinted techniques. Surface-imprinted microspheres had the characteristics of large surface area and easy modification，which could be flexibly applied to meet the needs of various aqueous sample pretreatments，which was one of the effective methods to overcome the difficulties of aqueous phase identification. This paper reviewed various preparation strategies for aqueous-phase recognition of surface-imprinted microspheres and their representative applications in recent years，including surface-imprinted microspheres with different substrates，hydrophilic recognition，non-hydrogen-bonded synergistic recognition，and those based on special components. Various interfering factors and their regulatory strategies in the recognition of molecules in aqueous media were discussed in depth on the aspects of forces and recognition mechanisms. The application of surface-imprinted microspheres in the pretreatment of aqueous samples was further presented. Finally，the challenges and future research trends of surface-imprinted microspheres in the field of aqueous sample pretreatment were discussed.关键词：surface-imprinted microspheres;aqueous recognition;sample pretreatment;preparation strategy448|446|1更新时间：2025-10-13 -
摘要：Lipids are essential not only as major components of cell membranes but also in various biological processes，such as energy storage and signal transduction. Due to its high sensitivity，accuracy，and rapid analytical capabilities，mass spectrometry（MS） has become a core technology for lipid analysis，particularly in structural characterization. However，the structural diversity and high similarity of lipids present significant challenges for their qualitative and quantitative analysis using MS. Chemical derivatization techniques，by modifying lipid structures，can enhance ionization efficiency and improve the sensitivity and selectivity of MS detection，thus facilitating effective lipid structure identification and quantification. In recent years，the combination of chemical derivatization and MS has been widely applied in lipid analysis. This review summarizes the research progress of MS techniques based on chemical derivatization in resolving the structural characterization of lipids，improving detection sensitivity and quantitative accuracy，and coupling with advanced mass spectrometry over the last decade.关键词：lipids;chemical derivatization;mass spectrometry;structural characterization545|653|1更新时间：2025-10-13 -
摘要：Metal-organic frameworks（MOFs） and covalent organic frameworks（COFs） possess exceptional attributes，notably their remarkably extensive specific surface areas and adjustable pore sizes，which greatly facilitate the selective enrichment and separation of target compounds. These unique properties have exhibited considerable potential in the field of active components derived from traditional Chinese medicine（TCM）. This review elucidates the prevalent methodologies for synthesizing MOFs and COFs，and delves into their applications，alongside composite materials，in the selective enrichment and chromatographic separation of active ingredients from a diverse array of Chinese medicinal matrices. Moreover，it examines the future prospects of these materials in identifying active components of TCM through the perspective of network pharmacology，providing valuable insights for the exploration and development of novel organic framework materials within the domain of efficacious constituents in TCM.关键词：metal-organic frameworks;covalent organic frameworks;active ingredients of TCM;selective enrichment;chromatographic separation999|1102|0更新时间：2025-10-13 -
摘要：Microfluidic paper-based analytical devices（μPADs） are straightforward，portable testing platforms based on paper materials that demonstrate significant potential for applications in domains such as clinical diagnosis，food quality control，and environmental monitoring. As a rapid detection platform，μPADs need to complete the sample pre-treatment process in addition to the rapid quantification of the target. In recent years，scientists have developed a variety of sample pre-treatment methods based on paper-based chips for the analysis of targets in different samples. Due to the strong compatibility of paper，enhancing the sample pre-treatment function of paper-based chips and linking them with various rapid detection methods can greatly expand the application areas of μPADs. This paper presents a summary of the sample pretreatment methods that including the paper-based chips with self-driving and the paper-based chips with external driving combined self-driving. It also outlines the research progress of paper-based chips in target analytes separation and enrichment，and discusses the advantages and limitations of various paper-based chips pre-treatment methods. Furthermore，this paper looks at the direction of μPADs，which need to be developed commercially to meet the testing needs of various industries，in addition to continuously improving sample preprocessing capabilities to expand their application in sample preparation.关键词：rapid analysis;microfluidic paper-based analytical devices;separation;driving;pre-preparation515|585|0更新时间：2025-10-13 -
摘要：Intercellular heterogeneity has been demonstrated to exist in various organisms and their development. Conventionally，the average results obtained from measurements of population cells cannot used to analyze the cellular heterogeneity，so it is important to study the physiological state of single cell at the level of single cells. As proteins are the main carriers of life activities，the analysis of single-cell proteomics is of great significance for the accurate study of the relationship between signal molecules and related signal pathways. Traditional techniques such as immunofluorescence are limited by the binding specificity，availability of antibodies and the analysis of pre-selected proteins. In this paper，the commonly used methods of single-cell proteomics based on mass spectrometry in recent years are reviewed. According to different analytical strategies，they are divided into three methods：bottom-up，top-down and native proteomics. Then the development of protein sample pretreatment is also discussed. Finally，the challenges and development of single-cell proteomics research based on mass spectrometry are summarized and prospected.关键词：mass spectrometry（MS）;proteomics;single cell;sample pretreatment600|823|0更新时间：2025-10-13
Reviews
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摘要：To determine the total isoflavones（ISF），most analytical methods have focused on the three aglycone ISFs and three basic glucoside ISFs due to the unavailability of reference standards for malonyl- and acetyl- glucosides，and resulted in bias. Hence，an ultra performance liquid chromatography UPLC） method was developed that allows the quantitation of all 12 ISFs using only 3 isoflavone standards. All glucoside ISFs，including daidzin，malonyl and acetyl daidzin，glycitin，malonyl and acetyl glycitin，genistin，malonyl and acetyl genistin，were converted into only 3 aglycone ISFs via alkaline methanol extraction and enzymatic hydrolysis. The malonyl glucosides and acetyl glucosides in sample were firstly hydrolyzed to their corresponding glucoside forms in alkaline methanol，the produced glucosides were further hydrolyzed by a β-glucosidase from almonds，and the sugar moieties from glucoside were removed. The released and original existed aglycone units were concentrated by polyamide through a dispersive solid-phase extraction，and determined by UPLC. All 3 aglycone ISFs（daidzein，glycitein and genistein） were separated in a reversed-phase C18 column（2.1 mm i.d.×50 mm，1.8 µm）. The mobile phase，mixed acetonitrile and phosphoric acid aqueous solution was employed to enable a 3 min of isocratic elution. All linearity correlation coefficients（r2） were higher than 0.999，and the recoveries were between 94.3% and 102% with relative standard deviations（RSD，n=6） less than 5.0%，that demonstrated precise and accurate results in the determination of total ISFs. To determine the total ISFs by simply summing the concentrations of the aglycon ISF will mitigate the pressure from interference，deviation and cost on test. In addition，based on the mechanisms of absorption and metabolism，using aglycone（free） forms to quantitate total ISFs is expected to present actual bioactivity of the phytoestrogens，this will avoid overestimate isoflavone levels or intake by simply adding of free and glucoside forms of isoflavone concentrations.关键词：isoflavone;polyamide（PA）;dispersive solid-phase extraction（d-SPE）;β-glucosidase;ultra performance liquid chromatography（UPLC）502|404|0更新时间：2025-10-13 -
摘要：Lead isotope ratios for national soil reference materials was accurately determinated by using multiple collectors inductively coupled plasma mass spectrometry（MC-ICP-MS）. The fractionation properties of MC-ICP-MS in the determination of lead isotope was studied，which exhibits mass-independent fractionation. The Baxter and the standard-sample bracketing（SSB） method were used to corrected the mass-dependent fractionation and mass-independent fractionation in the instrument.The lead isotope ratio of the NIST SRM 981 standard solution which was corrected has high accuracy and precision. The lead isotope ratio of three national soil reference materials（GBW07564，GBW07406a，GBW07980） were determined using MC-ICP-MS，and the soil was digested by microwave and purified. The recovery was more than 98%，and the blank of the whole process was less than 0.22 ng. The lead isotope ratio of GBW07564 is 19.960 3±0.030 3 for 206Pb/204Pb，15.767 5±0.006 1 for 207Pb/204Pb，and 39.086 8±0.026 4 for 208Pb/204Pb（n=9，2SD）；the lead isotope ratio of GBW07 406a is 18.802 4±0.001 8 for 206Pb/204Pb，15.744 2±0.002 5 for 207Pb/204Pb，and 39.194 3±0.008 6 for 208Pb/204Pb（n=9，2SD）；the lead isotope ratio of GBW07 980 is 18.614 2±0.005 7 for 206Pb/204Pb，15.737 8±0.004 4 for 207Pb/204Pb，and 38.962 9±0.015 3 for 208Pb/204Pb（n=9，2SD）. The 206Pb/207Pb of these soil reference materials are 1.265 9±0.001 4，1.194 2±0.000 1，1.182 8±0.000 1（n=9，2SD），and the 208Pb/206Pb are 1.958 2±0.001 8，2.084 5±0.000 3，2.093 2±0.000 2（n= 9，2 SD），respectively. These values are roughly within the range of natural soil lead isotopes 206Pb/207Pb（more than 1.17） and 208Pb/206Pb（less than 2.11）. These samples are easily obtainable，and their chemical and lead isotope compositions are uniform，making them suitable as isotope soil reference materials for monitoring the reliability of soil lead isotope chemistry and mass spectrometry analysis data.关键词：soil reference materials;lead isotopes;MC-ICP-MS;Baxter;the standard-sample bracketing（SSB） method;mass-independent fractionation485|538|0更新时间：2025-10-13 -
摘要：Hydroxyapatite modified bamboo shoot shell biochar（BS-HAP） with porous structure and hydrophilic phosphate group was synthesized from bamboo shoot shell to adsorb uranyl ions（UO22+） in wastewater. The porous structure of BS-HAP can effectively increase the contact area with UO22+ and promote the adsorption process of UO22+. The phosphate groups in BS-HAP can provide binding sites for the chemisorption of UO22+，which makes BS-HAP excellent adsorption properties for UO22+. At the same time，the ion exchange between Ca²+ and UO22+ and the electrostatic interaction between biochar and UO22+ synergistically promote the adsorption of UO22+ by BS-HAP. Under acidic conditions，the adsorption capacity of BS-HAP for UO22+ is 815.2 mg·g-1. BS-HAP not only has strong adsorption capacity for UO22+，but also has good selectivity and stability. Even under multiple recycling and actual wastewater treatment conditions，BS-HAP can still maintain the efficient removal capacity for UO22+. BS-HAP provides an effective method for the treatment of uranium containing wastewater，which is of great significance for promoting the development of green and sustainable wastewater treatment technology.关键词：bamboo shoot shell;biochar;hydroxyapatite;uranyl ion;adsorption614|375|0更新时间：2025-10-13 -
摘要：In order to clarify the differences of volatile components in different batch of breakable capsule flavor，a solid phase microextraction arrow and gas chromatography-mass spectrometry（SPME-Arrow/GC-MS） method was established by investigating the type of SPME Arrow，sodium chloride contenet，extraction temperature，equilibrium time and extraction time. The volatile and semi-volatile components in different batch of breakable capsule flavor were analyzed by this method，and the significant differential compounds were analyzed by principal component analysis（PCA），orthogonal partial least squares-discrimination analysis（OPLS-DA） and F-test. The results showed that，the optimized extraction conditions of SPME arrow were DVB/CAR/PDMS，sodium chloride for 2.0 g，equilibrium for 50 min and extraction for 40 min at 60 ℃. Through spectral library retrieval combined with retention index assisted qualitative analysis，a total of 96 volatile and semi-volatile components were identified. The number of peaks with a relative standard deviation of less than 10% of the target compounds intra-day relative standard deviations（RSDs） accounted for 92.7% of the total peaks. It indicates that the method has good repeatability. A total of 17 potential differential compounds were analyzed from different batches of breakable capsule flavor. Through the F-test，10 significant differential compounds were identified，which were α-pinene，limonene，eucalyptol，isopulegol，menthone （including isomers），neoisomenthol，neomenthyl acetate，glycerol tricaprylate and dioctanoic acid monodecanoic acid glyceride. This method can effectively distinguish the internal component differences of different batches of bead samples，and has the characteristics of accuracy，reliability and strong visualization. It can provide technical support for sensory quality inspection of bead products.关键词：SPME-Arrow;GC-MS;multivariable statistics;breakable capsule flavor;differential compounds510|567|0更新时间：2025-10-13 -
摘要：Excessive pesticide residues in food pose a potential threat to biodiversity and human health. Solid phase extraction（SPE）technology is widely used in the extraction of pesticides， and the core of this method is the selection of adsorbent materials. Covalent organic frameworks（COFs） have attracted significant attention in sample pretreatment due to their unique advantages. The structure of COFs determines the material's adsorption performance，which plays a crucial role in improving pesticide extraction efficiency. In this study， six COFs with different structural properties （grafting different functional groups onto the same parent material， possessing different charged properties and conjugated structures）were prepared. To facilitate experimentation without altering the structure of the COFs，they were formulated into COFs-sodium alginate hydrogels（CACPs）. A CACPs-dispersed solid-phase extraction（CACPs-dSPE） method was established to compare the extraction effects of different CACPs for carbamate，triazole，and triazine pesticides. Scanning electron microscopy，Fourier transform infrared spectroscopy，X-ray crystal diffraction and other methods were used to characterise the morphology，structures and properties of the series of COFs as well as the series of CACPs. The extraction effect was investigated by CACPs-dSPE combined with high performance liquid chromatography（HPLC）or ultraviolet-visible spectrophotometry（UV-Vis）. By combining theoretical calculations to simulate the binding of COFs with the analyte， this study explores the adsorption mechanism of different CACPs on carbamate， triazole， and triazine pesticides. The results showed that the optimal adsorption performance of CACPs for different types of pesticides varied，which was coordinately determined by the nature of their porous structure（specific surface area，pore size） and the intrinsic structure of the loaded COFs（size of conjugated structure，grafted groups）. The CACPs prepared by COFs with large conjugated structures and grafted hydroxyl groups were most favourable for the adsorption of three types of pesticides，with Dt-TAPB-CACPs showing the best extraction effect，providing theoretical guidance for the selection and design of adsorption materials in the process of pesticide extraction.关键词：pesticide residue;covalent organic frameworks;COFs-alginate hydrogel;dispersive solid phase extraction（dSPE）;adsorption mechanism487|402|0更新时间：2025-10-13 -
摘要：The immobilized metal ion affinity chromatography（IMAC） theory was employed to design and synthesize a poly（VIM-co-DVB）-Cu2+ monolithic column. The poly（VIM-co-DVB） matrix monolithic column was initially prepared via thermally initiated polymerization of 1-vinylimidazole（VIM） and divinylbenzene（DVB），and Cu2+ was immobilized directly on the matrix monolithic column through a post-modification multi-step method. The extraction conditions of the affinity monolithic columns were optimized. Under the optimal conditions，the poly（VIM-co-DVB）-Cu2+ monolithic column was applied for capillary microextraction（CME） of microcystins（MCs） prior to high performance liquid chromatography-mass spectrometry（HPLC-MS） analysis in both tap water and lake water samples. The detection limits of MCs ranged from 0.89 to 1.23 ng/L，with recoveries between 80.0% and 105%，and the relative standard deviations（RSDs） were not more than 6.8%. The validated CME/HPLC-MS methodology exhibits exceptional sensitivity and accuracy，making it a valuable tool for the monitoring and analysis of MCs in environmental waters.关键词：microcystins（MCs）;immobilized metal affinity monolithic columns;capillary microextraction（CME）;high performance liquid chromatography-mass spectrometry（HPLC-MS）427|355|0更新时间：2025-10-13 -
摘要：In this study，on-line solid phase extraction（SPE） based on quinolinecarboxylic acid-linked covalent organic framework（QCA-COF） microsphere was developed. On-line SPE coupled with high performance liquid chromatography（HPLC） was used for the determination of four aflatoxins（AFs） in food samples and Chinese medicinal herbs，including AFB1，AFB2，AFG1 and AFG2. QCA-COF microsphere was successfully synthesized via the Doebner multicomponent reaction. For this process，1，3，5-tris（4-aminophenyl）benzene，4，4’-biphenyldicarboxaldehyde and pyruvic acid were used as the synthetic monomer under the catalysis of sulfamic acid. QCA-COF microsphere was characterized by scanning electron microscope，Fourier transform infrared spectroscopy，powder X-ray diffraction，and N2 adsorption-desorption isotherms. The results showed that micro-sized QCA-COF microsphere was obtained in a solution of 1，4-dioxane-acetonitrile（1∶4，volume ratio）. The structure of QCA-COF has aromatic rings，pyridine groups and —COOH groups，which permits multiple binding interactions with aflatoxins. Based on their binding groups，QCA-COF exhibited excellent on-line SPE capability compared to the commercial materials，such as C18，PSA and GCB. The extraction parameters of the adsorption and elution processes were optimized in detail，including flow rates of loading，eluting solvent，volume of eluting solvent，and flow rates of elution. The optimal conditions were shown as follows：loading flow rate，0.4 mL·min-1；eluting solvent，300 μL of 0.1% acetic acid in methanol；elution flow rate，0.2 mL·min-1. Under the optimized conditions，the developed on-line SPE coupled with HPLC method provided good recovery（82.5%-105%），good precision（4.3%-10%，n=6），and low limit of detection（0.024-0.030 ng·g-1）. The introduced method was successfully used to analyze four AFs in peanuts，wheat，orange peel，almonds and cassia seed.关键词：aflatoxins;on-line solid phase extraction;covalent organic framework;high performance liquid chromatography461|315|1更新时间：2025-10-13 -
摘要：A rapid extraction and desorption strategy for the detection of seven volatile aromatic hydrocarbons and their derivatives in soil has been developed utilizing a graphene oxide modified solid phase micro-extraction（GO@SPME）needle，in conjunction with gas chromatography（GC）coupled with a hydrogen flame ionization detector（FID）. The target compounds include toluene，chlorobenzene，ethylbenzene，paraxylene，orthoxylene，nitrobenzene and naphthalene. The influence of seven factors（extraction liquid volume，stirring rate，extraction temperature，salt addition，desorption temperature，extraction time and desorption time） on the extraction efficiency was systematically investigated to determine optimal experimental conditions. In the experimental process，we initially introduced deuterated toluene，which serves as an internal standard，to the soil sample to calibrate the systematic errors inherent in the analytical process. In addition，the organic compounds from the soil samples were extracted through methanol soaking，a step designed to separate the target compounds from the complex soil sample. Under optimal conditions，the target analytes were rapidly enriched using headspace solid phase micro-extraction technology. Finally，the enriched samples were analyzed using GC-FID and internal standard quantification was achieved by constructing a calibration curve，ensuring the precision and reliability of the analytical results. The findings indicate that rapid extraction and desorption are feasible within 15 seconds，with extraction taking 12 seconds and desorption requiring just 3 seconds. The linear relation of seven volatile aromatic hydrocarbons and their derivatives was good，with correlation coefficients（r²） not less than 0.998 9. The limits of detection（LODs，S/N=3） ranged from 1.71 to 11.60 μg/g，while the limits of quantification（LOQs，S/N=10） were from 5.70 to 38.67 μg/g. The average recoveries of the seven volatile aromatic hydrocarbons and their derivatives at three spiked levels of 60，120 and 180 μg/g，ranged from 87.3% to 109%. Concurrently，the relative standard deviations（RSDs）were not more than 12%. This method has simple and fast preprocessing，low cost，stable and reliable data，and is suitable for rapid detection of aromatic hydrocarbons in soil samples.关键词：aromatic hydrocarbons and their derivatives;graphene oxide;headspace solid phase micro-extraction（HS-SPME）;gas chromatography;rapid extraction-desorption strategy;soil630|258|0更新时间：2025-10-13 -
摘要：In this work，MIL-101@MF composites were created by employing polyvinylidene fluoride（PVDF） as a cross-linking agent to fix the metal-organic framework（MOF） Fe-MIL-101 on melamine foam（MF）. Using the MIL-101@MF composites as adsorbents in the pipette-tip，a high performance MIL-101@MF with pipette-tip solid-phase extraction（PT-SPE） method was established.The antibiotic residues of chloramphenicol（CAP），thiamphenicol（TAP） and florfenicol（FF） in eggs were determined using this PT-SPE method combined with liquid chromatography tandem mass spectrometry（LC-MS/MS）. The morphology，crystal structure and functional groups of MIL-101@MF composites were characterized using scanning electron microscopy（SEM），powder X-ray diffraction analysis（XRD） and fourier transform-infrared spectroscopy（FTIR）. These methods showed that the MOF Fe-MIL-101 was successfully synthesized and well immobilized on melamine foam. PT-SPE parameters were optimized，including pH，salt concentration，elution solvents，elution volume，the number of extraction and elution cycles. Samples were extracted and cleaned up after PT-SPE，the target compounds were analyzed by a Waters C18（100 mm×2.1 mm，1.7 μm） column with 0.1% formic acid water（containing 5 mmol/L ammonium acetate）-acetonitrile as the mobile phase. The detection was carried out in the negative ion mode using multi-reaction monitoring（MRM）.The matrix standard curve combined with internal standard method was selected for the quantitative determination of chloramphenicols（CAP，TAP，FF） .The results showed that due to the co-existence of interactions such as electrostatic force，π-π action，and hydrogen bonding，the MIL-101@MF composites had a very high adsorption capacity for chloramphenicols. The extraction process could be finished quickly in less than 3 minutes. Moreover，even after 60 reuses，the material held its stability. Under the optimal conditions，the three targets showed good linearity in the mass concentration range of 0.1-10 μg/kg（r2＞0.999），and the limits of quantification（LOQs） were 0.1 μg/kg. The recoveries ranged from 78.2% to 108% with the relative standard deviations（RSDs） not more than 8.5%.The method was applied to determine 80 batches of egg samples，2.50% of TAP was detected between 0.21 and 1.2 µg/kg，while 8.75% of FF was detected between 0.47 and 4.2 µg/kg. Compared with other methods，the developed MIL-101@MF pipette-tip solid-phase extraction method is easy to operate，sensitive and accurate in quantification. It is expected to be applied in the pretreatment of multi-veterinary drug residues in animal foods. It can provide technical support for residue monitoring for safety of China's imported and exported food.关键词：metal-organic frameworks;melamine foam;pipette-tip solid-phase extraction;liquid chromatography-tandem mass spectrometry;egg;chloramphenicols538|402|0更新时间：2025-10-13 -
摘要：Metal-organic frameworks（MOFs），owing to their readily modifiable structural features and distinctive molecular sieve effects，enable efficient enrichment of target compounds，thereby exhibiting vast potential applications in fields such as environmental science，food safety and medicinal health. In this study，MOF-808 was as carriers to achieve enrichment and extraction of alkaloid bioactive components from Coptis chinensis（Huanglian）. Furthermore，we delved into the synergistic interactions during the extraction process of these alkaloids using MOFs in conjunction with low-co-solvent systems，based on their structural characteristics. By optimizing conditions such as incubation and extraction procedures，it achieved a remarkable recovery of 85.78% for jatrorrhizine from crude extracts of Huanglian. In addition，it boasted a wide linear range spanning from 0.1 to 300 µg·L-1，with ultra-low detection limits ranging from 0.02-0.05 µg·L-1 and relative standard deviations maintained within 0.40%-4.7%. Additionally，for jatrorrhizine，epiberberine，coptisine，palmatine and berberine in the Huanglian crude extract matrix，the spiked recoveries reached an impressive range of 69.7% to 128%. This approach efficiently and rapidly enriches and extracts alkaloid bioactive components from the Huanglian，thereby offering a novel perspective for the research on the selective extraction and enrichment of active ingredients in traditional Chinese medicines using MOFs materials.关键词：metal-organic framework;selective enrichment;chromatographic separation;active ingredients of alkaloids;Coptis chinensis419|326|0更新时间：2025-10-13
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