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氨基功能化 SBA-15 用于分散固相萃取 QuEChERS 法分析环境中的微污染物。

Amino groups modified SBA-15 for dispersive-solid phase extraction in the analysis of micropollutants by QuEchERS approach.

机构信息

Department of Chemistry, University of Turin, Via P. Giuria 7, 10125 Turin, Italy.

Department of Applied Science and Technology, DISAT, Polytechnic of Turin, Corso Duca degli Abruzzi 24, 10129 Turin, Italy.

出版信息

J Chromatogr A. 2021 May 24;1645:462107. doi: 10.1016/j.chroma.2021.462107. Epub 2021 Mar 26.

DOI:10.1016/j.chroma.2021.462107
PMID:33857677
Abstract

In the analysis of contaminants in food products, sample preparation is performed by proper adsorbents, whose choice is crucial to eliminate matrix interference. In this work we modified SBA-15 adsorbents by functionalization with (3-aminopropyl)-triethoxysilane (SBA-15-APTES) and N-[3-(trimethoxysilyl)propyl]aniline (SBA-15-AN) aiming to use them for the first time in the clean-up step of a QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction of micropollutants from strawberry, a sugar rich fruit. After physico-chemical characterization by nitrogen adsorption, infrared spectroscopy and thermogravimetric analysis, the adsorption capabilities of SBA-15 sorbents and possible interaction mechanisms were studied at different pH (2.1-8.5) for glucose, sucrose and fructose at concentrations characteristic of those found in strawberries. The performance of the two SBA-15 sorbents was compared with that of commercial PSA (primary secondary amine), usually proposed in QuEChERS protocols. Both SBA-15 materials exhibit up to 30% higher adsorption than PSA, suggesting their possible QuEChERS application. Synthesized SBA-15 adsorbents were hence used as innovative dispersive sorbents in the QuEChERS extractions of 13 PAHs and 14 PCBs from strawberry. For PCBs, SBA-15-AN provides better matrix removal than PSA and comparable extraction recoveries around 90%. For PAHs, the use of SBA-15-AN has the advantage of lower relative standard deviation (7%) than PSA (19%).

摘要

在食品污染物分析中,通过适当的吸附剂进行样品制备,选择合适的吸附剂对于消除基质干扰至关重要。在这项工作中,我们通过(3-氨丙基)三乙氧基硅烷(SBA-15-APTES)和 N-[3-(三甲氧基硅基)丙基]苯胺(SBA-15-AN)对 SBA-15 进行了功能化修饰,旨在首次将其用于从草莓中提取微污染物的 QuEChERS(快速、简单、廉价、有效、坚固和安全)萃取的净化步骤中,草莓是一种含糖量高的水果。通过氮气吸附、红外光谱和热重分析进行物理化学表征后,研究了 SBA-15 吸附剂的吸附能力以及在不同 pH(2.1-8.5)下葡萄糖、蔗糖和果糖的可能相互作用机制,这些浓度特征与草莓中的浓度相似。两种 SBA-15 吸附剂的性能与 QuEChERS 协议中通常提出的商用 PSA(伯仲胺)进行了比较。两种 SBA-15 材料的吸附能力均比 PSA 高 30%,这表明它们可能在 QuEChERS 中得到应用。因此,合成的 SBA-15 吸附剂被用作 QuEChERS 从草莓中提取 13 种多环芳烃和 14 种多氯联苯的新型分散吸附剂。对于 PCB,SBA-15-AN 比 PSA 提供更好的基质去除效果,萃取回收率约为 90%。对于 PAHs,使用 SBA-15-AN 的优点是相对标准偏差(7%)低于 PSA(19%)。

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