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ISSN:1004-4957

CN:44-1318/TH

Administrator: Guangdong Academy of Sciences

Sponsors: Institute of Analysis,Guangdong Academy of Sciences (Guangzhou Center for Analytical and Testing of China) ; China Association for Instrumental Analysis

Editor-in-Chief: Academician Jiang Guibin

Publication Frequency: Monthly

Tel: 020-87684776

Address: No.100, Xianlie Zhong Road, Guangzhou

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Volume 45 期 3,2026 2026年第45卷第3期
  • Special Column on Environmental Monitoring and Health

    拉萨市PM2.5中糖类化合物研究取得新进展,专家通过一年观测分析其组成、季节变化及来源,发现生物质燃烧是主要来源,且存在明显季节差异,为大气污染源解析提供新依据。

    LI Jia-di, LIU Jun-wen, QIU Cheng, ZHANG Zhi-sheng, LI Jun, ZHANG Gan

    DOI:10.12452/j.fxcsxb.25111701
    摘要:Sugar compounds are important organic tracers for atmospheric pollution sources. However,their characteristics and origins in PM2.5 in high-altitude cities remain poorly understood. Based on a one-year observation campaign in urban Lhasa(elevation:3 650 m),this study analyzed the composition,seasonal variation and sources of sugar compounds in PM2.5. The annual average concentration of total sugars was(260.6±379.6) ng·m-3,dominated by levoglucosan(180.3±307.8) ng·m-3,indicating biomass burning as the primary source. Total sugar concentrations exhibited a distinct“winter-high,summer-low”pattern,with anhydrosugars accounting for over 90% of total sugars in winter,highlighting the influence of heating activities. Monosaccharides were primarily attributed to pollen emissions,while sugar alcohols mainly originated from fungal spores; however,both showed significant positive correlations with anhydrosugars(p<0.05),suggesting that biomass burning also contributed to their presence. Furthermore,certain sugar alcohols(e.g.,arabitol and mannitol) were significantly correlated with monosaccharides(p<0.05),reflecting source complexity. Combined with diagnostic ratios—levoglucosan/mannosan(L/M:8.8±2.6),mannosan/galactosan(M/G:4.0±1.4),and levoglucosan/potassium(L/K⁺:0.49±0.54)—and local fuel usage patterns,biomass burning sources were identified as softwood,herbaceous materials,crop residues,and yak dung. These sources exhibited pronounced seasonal variations:softwood dominated in winter;contributions from crop residues and herbaceous materials increased in summer and autumn;mixed sources characterized spring; and yak dung combustion likely occurred year-round.  
    关键词:Lhasa;PM2.5;sugar compounds;biomass burning;source   
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    专家提出多维校正与三维荧光法结合策略,研究荧蒽荧光特性及定量,克服基体效应,为多环芳烃类有机污染物检测提供理论依据。

    WANG You, TANG Wen-tao, LIU Jia-xin, ZHOU Chen, LI Yuan, AN Rong, MENG Wei, QING Xiang-dong

    DOI:10.12452/j.fxcsxb.25111103
    摘要:Fluoranthene(FLU) is a persistent organic pollutant ubiquitously present in environment. This work proposed an integrated strategy combining alternating multi-linear decomposition-based multi-way calibration with three-dimensional fluorescence for studying the fluorescence spectral characteristics and accurate quantitative analysis of FLU in different environmental samples. First,fluorescence data arrays of FLU in synthetic water samples under different pH conditions were analyzed using alternating trilinear decomposition(ATLD),augmented ATLD(AATLD) and alternating quadrilinear decomposition(AQLD),respectively. The results revealed that when pH changed from 3.0 to 9.0,the FLU excitation spectrum underwent distortion,with its maximum excitation wavelength exhibiting a blue shift,while the emission spectrum remained unchanged. The average recoveries(ARs) of FLU obtained by AATLD and AQLD were(99.8±6.6)% and(100±7.2)%,respectively,which were superior to the result of ATLD((103±7.7)%). Subsequently,ATLD was employed to explore the fluorescence spectral characteristics and contents of FLU in different matrices(tap water,lake water,river water and soil). It was found that matrix effects did not alter the FLU spectral shape resolved by ATLD,but severely impaired the quantitative ability of ATLD. Finally,multi-way fluorescence data arrays incorporating pH variations and matrix interferences were constructed and subsequently resolved using AQLD and extended AQLD(AAQLD). The achieved ARs for FLU were(107±12.4)% and(99.7±9.5)% for AQLD and AAQLD,respectively. These approaches effectively mitigated matrix effects,yielding satisfactory outcomes. Additionally,two sustainability assessment tools(AGREE and MA) evaluated the developed methodologies,both achieving scores exceeding 80.0%,confirming excellent analytical performance. This study comprehensively demonstrated the“higher-order advantage”inherent in multi-may calibration,which enabled rapid and accurate cross-matrix quantification of FLU by overcoming matrix heterogeneity. It thereby established a theoretical foundation for expedited detection of polycyclic aromatic hydrocarbons(PAHs) pollutants in diverse environmental matrices.  
    关键词:alternating multilinear decomposition;three-dimensional fluorescence;fluoranthene;multi-way calibration;PAHs   
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    该研究基于超高效液相色谱 - 线性离子阱 - 高场轨道阱回旋共振质谱仪,建立了一种快速分析灰尘中 5 种环三磷腈类化合物的方法,为灰尘样品中 CTPs 的快速检测提供新方案。

    WANG Guo-pu, CUI Jun-tao, ZENG Xiang-ying, YU Zhi-qiang

    DOI:10.12452/j.fxcsxb.25121102
    摘要:The ultra-high performance liquid chromatography coupled with Orbitrap Fusion TMS(UHPLC-Orbitrap Fusion TMS) is a powerful tool for identification of trace pollutants in complex matrices because of its ultrahigh resolution and mass accuracy. In this study,a sensitive analytical method for the determination of five cyclotriphosphazenes(CTPs) in dust has been developed using UHPLC-Orbitrap Fusion TMS. Based on investigation of different solvent with varied pH,a mixture of acetonitrile,dichloromethane,and methyl tert-butyl ether(2∶2∶1,by volume,containing 1% ammonia) was selected as extraction solvent. Two key instrument parameters,automatic gain control(AGC) and maximum ion injection time(ITmax),were optimized as AGC target 5e5 and ITmax 300 ms,respectively. Determination and quantification of CTPs were performed in selected ion monitoring(SIM) mode,using an Xbridge BEH C8 column(4.6 mm× 250 mm,5 μm),with water(5 mmol/L ammonium acetate solution-0.3% ammonia) and methanol as mobile phase. Under the optimized condition,CTPs exhibited good linearity relationship within the range of 0.01-1 μg/L(with linear correlation coefficients>0.99) and sensitive detection of limits in the range of 0.011-0.14 ng/g. Acceptable recoveries were achieved at 72.7%-94.3% with relative standard deviations of 1.1%-5.4%,for low,medium,and high standards of spiked concentrations. The results indicated that CTPs could be extracted from dust and quantified sensitively without any clean-up procedure.  
    关键词:cyclotriphosphazenes;ultra-high performance liquid chromatography;high-resolution mass spectrometry;lithium-ion batteries;flame retardants   
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    镧系生物基多孔配位聚合物(Ln-BCPs)在重金属离子吸附与检测领域取得新进展,研究团队通过后合成策略构建了新型材料Tb-Asp-CP,实现了对Pb(Ⅱ)的高选择性吸附和高灵敏检测,为开发高性能重金属离子吸附和检测材料提供了新思路和理论依据。

    GAO Run, DING Xin-er, YANG Zi-hao, XU Fei, WU Xiu-xiu, HAO Li-ling, CAO Hui

    DOI:10.12452/j.fxcsxb.25110310
    摘要:Biofunctionalized porous lanthanide coordination polymer(Ln-BCPs) have recently gained increasing attention for heavy metal ion adsorption and detection,owing to their tunable pore structures,abundant functional groups,and distinct photochemical properties. In this study,a novel material,Tb-Asp-CP,was constructed for the highly selective adsorption and sensitive detection of Pb(Ⅱ) by incorporating L-aspartic acid(L-Asp) into a Tb-based framework through post-synthetic modification. The recognition and binding mechanisms of Tb-Asp-CP toward Pb(Ⅱ) were elucidated through a combination of experimental analysis and quantum chemical calculations. Density functional theory(DFT) calculations revealed that L-Asp coordinates with Pb(Ⅱ) predominantly through its carboxyl oxygen and amino nitrogen atoms,with electrostatic interactions contributing up to 95.03% of the binding energy. The adsorption behavior of Tb-Asp-CP towards Pb(Ⅱ) was well-described by the Langmuir isotherm and pseudo-second-order kinetic models,indicating a monolayer chemisorption process controlled by the interface reaction. The material exhibited a maximum adsorption capacity of 478 mg/g for Pb(Ⅱ) at pH 4.0 and 25 ℃,which is better than that of many previously reported Ln-BCPs. Furthermore,Tb-Asp-CP demonstrated excellent selectivity toward Pb(Ⅱ) in the presence of competing metal ions(Ni²⁺,Cr³⁺,Cu²⁺,Zn²⁺,etc.),with selectivity coefficients ranging from 3.03 to 32.54. Moreover,the material maintained 71.8% of its adsorption capacity after five adsorption-desorption cycles,indicating strong reusability. For detection applications,Tb-Asp-CP exhibited sensitive fluorescence responses toward Pb(Ⅱ),with a linear range of 0.01-5.0 mg/L(r²=0.996) and a low detection limit of 3.19 μg/L. Spike recovery experiments using vegetable samples yielded recoveries of 86.9%-108% with relative standard deviations(RSDs) of 2.9%-8.3%,confirming its practical applicability. Electrostatic potential(ESP) analysis revealed the presence of an “oxygen-rich cavity” formed by multiple carboxyl oxygen atoms from H₄btec and L-Asp,serving as the primary binding site for Pb(Ⅱ). Frontier molecular orbital(FMO) analysis showed that the Tb-Asp-CP-Pb(Ⅱ) complex possesses a narrow HOMO-LUMO energy gap(0.057 eV),which facilitates electron transfer and stabilizes the coordination structure. Upon the adsorption of Pb(Ⅱ) within these cavities,the energy transfer from the ligand to the central Tb³⁺ ion is likely impeded by a photoinduced electron transfer(PET) process,thereby enabling the highly sensitive detection of Pb(Ⅱ). Overall,this work provides a feasible post-synthetic modification strategy for constructing biofunctionalized Ln-BCPs. The excellent Pb(Ⅱ) adsorption and fluorescence detection performance of Tb-Asp-CP offers valuable insights and theoretical guidance for the development of high-efficiency materials for heavy metal remediation and food safety monitoring.  
    关键词:porous coordination polymers;amino acid functionalization;lead ions;adsorption mechanism;detection   
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    介绍了其在环境检测领域的研究进展,相关专家建立了水环境中108种半挥发性有机污染物筛查与定量一体化分析方法,为环境损害案件中污染物快速筛查和定量分析提供有效解决方案。

    GUO Yi-ting, ZHU Jun, LI Ya-jun, HAN Dong, LIU Xi, YANG Rui-qin, GUO Hong-ling

    DOI:10.12452/j.fxcsxb.25082904
    摘要:An integrated analytical method for the screening and quantification of 108 semi-volatile organic pollutants in aquatic environments was established using gas chromatography-tandem mass spectrometry(GC-MS/MS). This study investigated the impact of various types of diversion liners on the detection outcomes of target analytes,optimized the extraction solvents,and established optimal analytical conditions for measurement. Following dichloromethane liquid-liquid extraction of water samples,the optimized GC-MS/MS method demonstrated excellent linearity(r²>0.99) for all 108 target compounds within their respective concentration ranges. The method exhibited detection limits(LODs) of 0.001-1 μg/L,quantification limits(LOQs) of 0.002-2 μg/L,spiked recoveries of 77.8%-118%,relative standard deviations(RSDs) of 1.7%-12%,and matrix effects ranging from 79.7% to 129%. Application to eight electroplating wastewater samples(primarily containing copper,nickel,and zinc plating effluents) detected 25 semi-volatile organic pollutants at concentrations ranging from 1.78 μg/L to 30.53 mg/L. This method offers comprehensive compound coverage,rapid analysis,low detection limits,high precision,and excellent accuracy,making it particularly suitable for rapid screening and quantitative analysis of pollutants in environmental damage assessment cases.  
    关键词:GC-MS/MS;semi-volatile organic compounds;environmental damage litigation cases;liquid-liquid extraction   
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    专家建立了超高效液相色谱 - 串联质谱测定大气 PM2.5 中 16 种硝基酚类物质的分析方法,为大气棕碳污染溯源及健康风险评估提供技术支撑。

    XUE Ya-wei, GAO Yuan, YE Jian-bo, LU Run, THAM Yee-jun

    DOI:10.12452/j.fxcsxb.25102902
    摘要:An analytical method for the determination of 16 nitrophenols(including typical species such as 4-nitrophenol,4-nitrocatechol,and 3-nitrosalicylic acid) in PM2.5 sample was established by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methodological validation showed that the 16 nitrophenols exhibited good linearity in the range of 0.4-60 μg/L(r²>0.99). Based on a sampling volume of 54 m3 for actual samples,the method detection limits(LODs) ranged from 0.018 5 to 0.074 6 ng/m³,and the lower limits of quantification(LOQs) were from 0.073 9 to 0.298 2 ng/m³. At three spiking levels(low,medium,and high),the average recoveries were 87.4%-118%,and the relative standard deviations(RSDs,n=6) were not more than 15%. When this method was applied to the analysis of fine particles from DaWanShan Island(DWS) in Zhuhai,the total concentration of the 16 nitrophenols ranged from 0.60 to 88.57 ng/m3,among which 5-nitrosalicylic acid(accounting for 27.32%),4-nitrophenol(accounting for 25.86%),and 4-nitrocatechol(accounting for 17.69%) were the main components. This method is suitable for the detection of trace nitrophenols in the complex matrix of atmospheric fine particles and can provide technical support for the source tracing of atmospheric brown carbon pollution and health risk assessment.  
    关键词:ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);fine particles;nitrophenol compounds;air pollution   
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    专家建立了高效液相色谱 - 串联质谱测定尿中二氯乙酸和三氯乙酸的快速检测方法,为四氯乙烷职业中毒临床检验提供技术支持。

    SUN Jin-ying, TAN Cheng-long, WEI Hui-wei, ZHANG Hao-ling, ZHANG Ying, TANG Liang, ZHENG Quan-dong

    DOI:10.12452/j.fxcsxb.25081201
    摘要:A rapid detection method using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established for determining dichloroacetic acid(DCA) and trichloroacetic acid(TCA) in urine of occupationally exposed individuals to 1,1,2,2-tetrachloroethane. The urine samples were acidified by adding hydrochloric acid solution,followed with sodium chloride being added and shaking. Subsequently DCA and TCA were extracted with ethyl acetate. The upper extract was concentrated to near dryness using nitrogen blowing,and then redissolved with 15% acetonitrile solution. After being filtered through a microporous membrane,they were injected into the instrument. Chromatographic separation was achieved using a Waters HSS T3(2.1 mm×100 mm,1.8 μm) column,with acetonitrile-0.1% acetic acid aqueous solution as the mobile phase for gradient elution. Electrospray ionization(ESI) source and multiple reaction monitoring(MRM) mode were employed. Quantification was performed using the matrix-matched curve external standard method. Both DCA and TCA exhibited linear relationships within the mass concentration range of 2.0-100 µg/L,with linear correlation coefficients(r) higher than 0.999. The limits of detection(LODs) and the limits of quantitation(LOQs) were calculated to be 0.2 µg/L and 1.0 µg/L,respectively. The recoveries at low,medium and high spiked concentration levels ranged from 75.3% to 104%. The average recoveries of DCA and TCA were 91.1% and 86.1%,respectively,with relative standard deviations(RSDs) ranging from 2.1% to 9.5%. The established analytical procedure was employed for urine DCA and TCA level investigating of the general population,routine occupational population,and occupational poisoning patients. The method is simple,rapid and highly sensitive,providing a technical reference for biological monitoring and clinical testing of occupational poisoning in occupationally exposed individuals to 1,1,2,2-tetrachloroethane.  
    关键词:1,1,2,2-tetrachloroethane;high performance liquid chromatography-tandem mass spectrometry;dichloroacetic acid;trichloroacetic acid;occupational poisoning   
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