Abstract

In this study, we report for the first time developing an analytical method based on three metal–organic frameworks (MOF) including UiO-66, UiO-66-NH₂ and UiO-66-NH₂ @ Fe₃O₄-SiO₂ in micro-extraction by packed sorbent (MEPS) extracting trans, trans-muconic acid (tt-MA) in urine. The FT-IR, XRD and FE-SEM techniques were used for characterization of the synthesized MOFs. The effects of some analytical parameters were investigated on the MEPS performance using central composite design by response surface methodology. The findings demonstrated that the sample volume and desorption cycles were the most important parameters for the extraction of tt-MA using UiO-MEPS procedure combined with high-performance liquid chromatography (HPLC). The limit of quantification (LOQ) of UiO-MEPS-HPLC procedure for UiO-66, UiO-66-NH₂ and UiO-66-NH₂ @ Fe₃O₄-SiO₂ core–shell was 0.005, 0.005 and 0.003 µg mL⁻¹, respectively. Under optimal conditions, the UiO-MEPS-HPLC method offered a good performance for extracting tt-MA from urine samples (UiO-66, UiO-66-NH₂ and UiO-66-NH₂ @ Fe₃O₄-SiO₂ core–shell: 86%, 0.95% and 98.5%, respectively, RSD < 3.54%). The results indicated that this technique was a sensitive, fast and reusable method and can be applied to extract and determine trace amounts of urinary tt-MA in the urine matrix.

Graphic abstract

中文翻译：

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锆基金属有机骨架在尿中反式，反粘康酸填充吸附剂微萃取中的应用

摘要

在这项研究中，我们首次报告了基于三种金属有机框架（MOF）的分析方法，包括UiO-66，UiO-66-NH ₂和UiO-66-NH ₂ @ Fe ₃ O ₄ -SiO ₂吸附吸附剂（MEPS）在微萃取中提取尿液中的反式，反粘康酸（tt-MA）。FT-IR，XRD和FE-SEM技术用于表征合成的MOF。通过响应面方法，采用中心复合设计，研究了一些分析参数对MEPS性能的影响。研究结果表明，样品体积和解吸循环是使用UiO-MEPS程序结合高效液相色谱（HPLC）萃取tt-MA的最重要参数。Fe ₃ O ₄ -SiO ₂核-壳的UiO-66，UiO-66-NH ₂和UiO-66-NH ₂的UiO-MEPS-HPLC方法的定量限（LOQ）为0.005、0.005和0.003 µg毫升^-1。在最佳条件下，UiO-MEPS-HPLC方法在从尿液样品（UiO-66，UiO-66-NH ₂和UiO-66-NH ₂ @ Fe ₃ O ₄ -SiO ₂核心）中提取tt-MA方面具有良好的性能。–壳：分别为86％，0.95％和98.5％，RSD <3.54％）。结果表明，该技术是一种灵敏，快速且可重复使用的方法，可用于提取和测定尿基质中的痕量尿tt-MA。

图形摘要