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苯基丙基功能化杂化溶胶-凝胶增强铝带作为薄膜微萃取装置,用于痕量定量分析液态食品中的八种多氯联苯。

Phenyl propyl functionalized hybrid sol-gel reinforced aluminum strip as a thin film microextraction device for the trace quantitation of eight PCBs in liquid foodstuffs.

机构信息

Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.

Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.

出版信息

Talanta. 2019 Jul 1;199:547-555. doi: 10.1016/j.talanta.2019.02.095. Epub 2019 Feb 28.

Abstract

In the present study, a low-cost, convenient and reliable thin film coating was developed as the extraction phase. The new sorbent was obtained by chemical bond formation between the hybrid sol-gel precursors and aluminum strip substrate in the first step and subsequent functionalization by phenyl propyl groups. The surface properties of the synthesized sorbent were characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Eight polychlorinated biphenyl (PCB) homologs were effectively extracted by using the self-made device in thin film microextraction (TFME) set-up followed by gas chromatography-mass spectrometry (GC-MS) determination. The influencing factors, including extraction and desorption solvent, desorption solvent volume, extraction and desorption time, extraction temperature, agitation speed, salt addition, and matrix effect were investigated. Under the optimized conditions, the limits of detection (at S/N ratio of 3) were found to be 1-3 ng L and the linearity was in the range of 10-1000 ng L. The method precision values calculated as relative standard deviations (RSDs%), were in the range of 6.8-11.0% (intra-day), and 9.0-12.4% (inter-day). This work was successfully applied to enrichment and trace levels determination of PCB congeners in orange juice, cola drink, milk, beer, and honey. The evaluations also showed satisfactory recoveries (70.6-103.5%) for different spiked real samples.

摘要

在本研究中,开发了一种低成本、方便且可靠的薄膜涂层作为萃取相。新的吸附剂是通过在第一步中将杂化溶胶-凝胶前体与铝带基底之间形成化学键,以及随后用苯基丙基官能化而获得的。通过傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)和能谱(EDS)对合成的吸附剂的表面性质进行了表征。使用自制的装置,通过薄膜微萃取(TFME)装置有效地提取了八种多氯联苯(PCB)同系物,然后通过气相色谱-质谱(GC-MS)测定。研究了萃取和洗脱溶剂、洗脱溶剂体积、萃取和洗脱时间、萃取温度、搅拌速度、加盐和基质效应等影响因素。在优化条件下,检测限(信噪比为 3)为 1-3ng/L,线性范围为 10-1000ng/L。方法精密度(以相对标准偏差(RSD)%表示)为 6.8-11.0%(日内)和 9.0-12.4%(日间)。该方法成功应用于橙汁、可乐饮料、牛奶、啤酒和蜂蜜中 PCB 同系物的富集和痕量测定。评估还表明,对于不同添加的实际样品,回收率令人满意(70.6-103.5%)。

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