Background

Edible oils are susceptible to contamination with polycyclic aromatic hydrocarbons (PAHs) throughout production, storage, and transportation processes due to their lipophilic nature. The necessity of quantifying PAHs present in complex oil matrices at trace levels, which bind strongly to impurities in oil matrices, poses a major challenge to the accurate quantification of these contaminants. Therefore, the development of straightforward and effective methods for the separation and enrichment of PAHs in oil samples prior to instrumental analysis is paramount to guaranteeing food safety.

Results

A pyrazine embedded hyper-crosslinked porous polymer, HCP_Pz-TPB, was synthesized via a Friedel-Crafts reaction, utilizing triphenylbenzene (TPB) as the monomer and 2,5-dibromomethylpyrazine as the cross-linking reagent. The material was combined with polydimethylsiloxane (PDMS) using the sol-gel method, and applied as a coating to a dumbbell-shaped stir bar prepared in-house. Using stir bar sorptive extraction (SBSE) combined with gas chromatography-mass spectrometry (GC-MS), 15 PAHs in edible oils were successfully quantified. Optimal conditions for the extraction of PAHs were experimentally investigated, with factors such as stirring rate, extraction time, extraction temperature, desorption solvent, and desorption time systematically optimized. The final method demonstrated a broad linear range (0.12–150 ng g⁻¹), and low limits of detection (0.04–0.28 ng g⁻¹). The recoveries of PAHs in real edible oil samples ranged from 83.14 % to 128.01 %, with relative standard deviations (RSDs) below 13.47 %.

Significance

This method simplifies PAH extraction by eliminating steps such as saponification, liquid-liquid extraction, drying, and re-dissolution, thus reducing potential analyte loss and errors associated with the inclusion of multiple pretreatment steps typical of conventional methods reported in the literature. Notably, the adsorbent materials prepared in this study can be reused up to 30 times, underscoring its sustainability. The proposed research broadens the diversity of coating choices for SBSE applications while offering a streamlined, cost-effective, and greener alternative for PAH determinations in edible oils via SBSE/GC-MS.

中文翻译：

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通过聚二甲基硅氧烷/吡嗪基超交联聚合物涂层搅拌棒吸附萃取后气相色谱-质谱检测，简单灵敏地监测食用油中的多环芳烃

 背景

由于其亲脂性，食用油在整个生产、储存和运输过程中容易受到多环芳烃 （PAH） 的污染。复杂油基质中存在的痕量多环芳烃必须与油基质中的杂质紧密结合，因此必须定量分析这些污染物的准确定量。因此，在仪器分析之前开发简单有效的方法来分离和富集油样中的 PAH 对于保证食品安全至关重要。

 结果

以三苯苯 （TPB） 为单体，以 2,5-二溴甲基吡嗪为交联剂，通过 Friedel-Crafts 反应合成了吡嗪包埋的高交联多孔聚合物 HCP_Pz-TPB。使用溶胶-凝胶法将该材料与聚二甲基硅氧烷 （PDMS） 结合，并作为涂层涂覆到内部制备的哑铃形搅拌棒上。采用搅拌棒吸附萃取 （SBSE） 结合气相色谱-质谱联用 （GC-MS） 技术，成功定量了食用油中 15 种 PAHs。实验研究了提取 PAHs 的最佳条件，系统优化了搅拌速率、提取时间、提取温度、解吸溶剂和解吸时间等因素。最终方法显示出较宽的线性范围 （0.12–150 ng ^g-1），检测限低 （0.04-0.28 ng ^g-1）。实际食用油样品中 PAHs 的回收率在 83.14 % 至 128.01 % 之间，相对标准偏差 （RSD） 低于 13.47 %。

 意义

该方法通过消除皂化、液-液萃取、干燥和再溶等步骤简化了 PAH 提取，从而减少了与包含文献中报道的常规方法典型的多个预处理步骤相关的潜在分析物损失和错误。值得注意的是，本研究中制备的吸附材料可以重复使用多达 30 次，强调了其可持续性。拟议的研究拓宽了 SBSE 应用的涂层选择多样性，同时为通过 SBSE/GC-MS 测定食用油中的 PAH 提供了一种简化、经济高效且更环保的替代方案。