中空聚合物纳米球（hps）作为固相萃取（SPE）尿液中反式、反式粘膜酸的可重复使用吸附剂

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B Pub Date : 2025-05-28 DOI:10.1016/j.jchromb.2025.124674

Nematullah Kurd , Abbas Afkhami , Hanieh Ganji

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引用次数: 0

摘要

在本工作中，制备了中空聚合物纳米球（hps），并将其作为可重复使用的吸附剂应用于固相萃取（SPE）中，以提取和测定尿液样本中的反式，反式粘膜酸（tt-MA），作为低水平苯暴露的潜在生物标志物。在水热条件下，采用弱酸-碱组装法合成了具有可控尺寸和功能壳的HPSs。空心纳米球可以作为储层或纳米反应器，其功能壳不仅为反应提供了较大的表面积，而且通过其丰富的官能团易于螯合目标化合物。通过与高效液相色谱（HPLC-UV）分析仪的耦合，对样品体积、样品流速、洗脱量、样品pH、洗涤溶剂类型、洗脱溶剂类型等影响提取性能的主要因素进行了评价和优化。在pH为7、进样量为2 ml、流速为1 ml/min、去离子水/甲醇（9,1 v/v）为洗涤溶剂、乙醇/乙酸3% （8,2 v/v）为洗脱溶剂的条件下，hps吸附剂对尿液中tt-MA的回收率最高。采用0.1、25、50 μg/ml 3种浓度对优化方法进行了验证，验证了优化方法的日内重现性和日重现性(RSD <；7.7%)。良好的线性范围(r 2 >；低检出限（0.05 μg/ml）。在质量控制（QC）浓度下，加样尿液中tt-MA的回收率大于96%，证明了高效液相色谱-固相萃取法对苯暴露人群尿液样品分析的适用性。

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Hollow polymer nanospheres (HPSs) as reusable adsorbent for solid-phase extraction (SPE) of trans, trans-muconic acid from urine samples

In the present work, hollow polymer nanospheres (HPSs) were prepared and applied as reusable adsorbent in solid-phase extraction (SPE) to extract and determine trans, trans- muconic acid (tt-MA) from urine samples as a potential biomarker of low-level exposure to benzene. HPSs with controllable size and functional shells were synthesized through weak acid-base assembly under hydrothermal conditions. Hollow nanospheres can act as a storage reservoir or a nanoreactor, the functional shell not only provides a significant surface area for reactions, but also easily chelates target compounds through the abundant functional groups present in it. The main factors affecting the extraction performance, including sample volume, sample flow rate, elution volume, sample pH, type of washing solvent, and type of elution solvent, were evaluated and optimized through coupling to a high-performance liquid chromatography (HPLC-UV) analyzer. The highest recovery rate of tt-MA from urine with HPSs adsorbent was obtained at pH 7, sample volume 2 ml, sample flow rate 1 ml/min, deionized water/methanol (9,1 v/v) as washing solvent, and ethanol/acetic acid 3 % (8,2 v/v) as elution solvent. The optimized method was validated using three concentrations of 0.1, 25, and 50 μg/ml, and its within-day and day-to-day reproducibility was confirmed (RSD < 7.7 %). A good linear range (r ² > 0.99) and low limits of detection (0.05 μg/ml) were obtained as well. The recovery of tt-MA from spiked urine samples in the quality control (QC) concentrations was more than 96 %, demonstrating the HPS-SPE method's applicability in the analysis of urine samples of benzene-exposed people.

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来源期刊

Journal of Chromatography B 医学-分析化学

CiteScore

5.60

自引率

3.30%

发文量

306

审稿时长

44 days

期刊介绍： The Journal of Chromatography B publishes papers on developments in separation science relevant to biology and biomedical research including both fundamental advances and applications. Analytical techniques which may be considered include the various facets of chromatography, electrophoresis and related methods, affinity and immunoaffinity-based methodologies, hyphenated and other multi-dimensional techniques, and microanalytical approaches. The journal also considers articles reporting developments in sample preparation, detection techniques including mass spectrometry, and data handling and analysis. Developments related to preparative separations for the isolation and purification of components of biological systems may be published, including chromatographic and electrophoretic methods, affinity separations, field flow fractionation and other preparative approaches. Applications to the analysis of biological systems and samples will be considered when the analytical science contains a significant element of novelty, e.g. a new approach to the separation of a compound, novel combination of analytical techniques, or significantly improved analytical performance.