【摘要】 邻苯二甲酸酯(Phthalate Esters, PAEs)作为常见的塑化剂，广泛用于食品包装材料，易迁移至人体造成潜在危害。因此，建立快速、灵敏的检测方法具有重要意义。固相微萃取(Solid Phase Microextraction, SPME)是一种高效的样品前处理技术，其性能核心取决于萃取涂层材料，开发新型高效、耐用的SPME涂层已成为研究重点。共价有机框架(COF)材料在萃取分离领域展现出巨大潜力。构建一种不锈钢纤维与三嗪COF-TZ-DBd的新型复合涂层，以期提升SPME涂层性能，从而为痕量污染物的灵敏检测提供可靠方法。首先采用两步电化学刻蚀法制得沟槽表面不锈钢纤维(Gully-like Surface Stainless Steel Fibers, GS-SSF)，再通过原位物理涂敷方式将三嗪COF-TZDBd与沟槽状表面嵌合制备固相微萃取(SPME)涂层。在不锈钢纤维(GS-SSF)的沟槽中原位物理涂敷了采用水热合成法合成的三嗪COF-TZ-DBd涂层。将所制备的纤维作为直接SPME吸附剂，结合气相色谱(Gas Chromatography, GC)技术建立了瓶装茶饮料中邻苯二甲酸酯(PAEs)的检测方法。该方法相关系数(R2)均高于0.990 1,检出限(S/N=3)LODs为0.10μg·L-1～0.44μg·L-1，富集因子(Enrichment Factors, EFs)为154～2 185，同一根萃取纤维5日间萃取效率相对标准偏差(Relative Standard Deviation, RSDs)为1.7%～7.6%，三根萃取纤维日内萃取效率相对标准偏差(Relative Standard Deviation, RSDs)为1.3%～8.9%。在对瓶装茶饮料中PAEs的加标回收实验中，加标回收率为93.21%～101.71%。更多还原

【Abstract】 Phthalate esters(PAEs), widely used as plasticizers in food packaging materials, can migrate and pose potential health risks. Therefore, establishing rapid and sensitive detection methods is of great significance. Solid-phase microextraction(SPME), as an efficient sample pretreatment technique, relies on its extraction coating material as the performance core, making the development of novel, high-efficiency, and durable SPME coatings a key research focus.Covalent organic framework(COF) materials have shown significant potential in extraction and separation applications.This study constructs a novel composite coating integrating stainless-steel fibers with a triazine-based COF(COF-TZ-DBd),aiming to enhance the performance of the SPME coating, thereby providing a reliable method for the sensitive detection of trace pollutants. A triazine-based covalent organic framework(COF-TZ-DBd) coating, synthesized via a hydrothermal method, was immobilized in situ onto a grooved stainless steel fiber(GS-SSF) through physical coating. The GS-SSF substrate was first fabricated using a two-step electrochemical etching process, and the COF-TZ-DBd coating was subsequently integrated into the micro-grooved surface via in situ physical deposition to prepare the solid-phase microextraction(SPME) coating. The prepared fiber was employed as a direct SPME adsorbent, and an analytical method for the determination of phthalate esters(PAEs) in bottled tea beverages was established by coupling with gas chromatography(GC). The method exhibited correlation coefficients(R2) above 0.990 1, limits of detection(LODs, S/N = 3)ranging from 0.10 to 0.44 μg·L-1, and enrichment factors(EFs) between 154 and 2185. The intra-day relative standard deviations(RSDs) for three individual fibers ranged from 1.3% to 8.9%, while the inter-day RSDs over five days for a single fiber were between 1.7% and 7.6%. In the spiked recovery tests of PAEs in bottled tea beverages, the recoveries obtained were 93.21%-101.71%.更多还原