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在钛纤维上原位生长共价有机框架用于蔬菜中 11 种邻苯二甲酸酯的顶空固相微萃取。

In situ growth of covalent organic framework on titanium fiber for headspace solid-phase microextraction of 11 phthalate esters in vegetables.

机构信息

State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122, China.

State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122, China.

出版信息

Food Chem. 2020 Jul 15;318:126507. doi: 10.1016/j.foodchem.2020.126507. Epub 2020 Feb 27.

DOI:10.1016/j.foodchem.2020.126507
PMID:32145544
Abstract

Vegetables are easily contaminated by phthalate esters (PAEs) from the environment, agricultural films and fertilizers, affecting human health. In this paper, titanium dioxide (TiO) nanotube arrays were prepared by electrochemical anodic oxidation on the surface of titanium wire. Covalent organic framework of TpBD was in situ bonded to the titanium wire via TiO nanotube arrays using monomers of 1,3,5-trimethylphloroglucinol (Tp) and benzidine (BD). The fabricated TpBD-TiO coated titanium wire was used as the solid-phase microextraction fiber to extract 11 PAEs in vegetable samples. Coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS), the limits of detection for PAEs were from 0.001 (di-n-butyl phthalate) to 0.430 (butyl benzyl phthalate) μg/L (S/N = 3) and enrichment factors were between 226 (dimethyl phthalate) and 2154 (di-n-butyl phthalate). Our fabricated TpBD-TiO fiber can be used at least 150 times without significant loss of extraction efficiency (<4.8%). Quantitative determination of PAEs in vegetable samples (tomato, lettuce, cucumber) was achieved by standard addition.

摘要

蔬菜很容易被环境、农用薄膜和肥料中的邻苯二甲酸酯(PAEs)污染,从而影响人类健康。在本文中,通过在钛丝表面进行电化学阳极氧化,制备了二氧化钛(TiO)纳米管阵列。通过 TiO 纳米管阵列,单体 1,3,5-均三甲苯(Tp)和联苯二胺(BD)原位键合到钛丝上,形成共价有机框架 TpBD。制备的 TpBD-TiO 涂层钛丝用作固相微萃取纤维,用于提取蔬菜样品中的 11 种邻苯二甲酸酯。与气相色谱-串联质谱(GC-MS/MS)联用,PAEs 的检测限从 0.001(邻苯二甲酸二丁酯)到 0.430(邻苯二甲酸丁基苄基酯)μg/L(S/N=3),富集因子在 226(邻苯二甲酸二甲酯)到 2154(邻苯二甲酸二丁酯)之间。我们制备的 TpBD-TiO 纤维在没有明显萃取效率损失(<4.8%)的情况下,至少可以使用 150 次。通过标准加入法对蔬菜样品(番茄、生菜、黄瓜)中的邻苯二甲酸酯进行定量测定。

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