共价有机骨架磁固相萃取-气相色谱法测定15种邻苯二甲酸酯

Determination of 15 kinds of phthalate esters by covalent organic framework magnetic solid-phase extraction-gas chromatography

中文关键词:  邻苯二甲酸酯  磁性固相萃取  气相色谱法  共价有机骨架

英文关键词:phthalate esters  magnetic solid phase extraction  gas chromatography  covalent organic framework

中文摘要:

      目的 建立磁共价有机骨架材料TpPa-1/Fe3O4固相萃取与气相色谱法(gas chromatography, GC)联用技术测定样品中15种邻苯二甲酸酯(phthalate esters, PAEs)的分析方法。方法 将TpPa-1与Fe2+、Fe3+在碱性条件下合成TpPa-1/Fe3O4, 经过磁固相萃取过程将PAEs吸附, 并使用甲醇洗脱, 上机检测, 外标法定量。结果 15种PAEs的检出限为0.313~5.198 μg/L(S/N=3)。PAEs的日内和日间相对标准偏差(relative standard deviations, RSDs)值分别小于6.6%和7.8%。该方法已成功应用于碳酸饮料和环境水样中痕量PAEs的测定, 回收率在89.1%~103.6%之间, RSD小于7.9%。结论 本研究提供了一种简单快速的共价有机骨架(covalent organic frameworks, COFs)材料的磁化方法, 可应用于食品样品前处理中富集和分离PAEs。

英文摘要:

      Objective To establish a method for the determination of 15 kinds of phthalate esters (PAEs) in samples by solid phase extraction of covalent organic framework magnetic solid TpPa-1/Fe3O4 and gas chromatography (GC). Methods TpPa-1/Fe3O4 was synthesized with Fe2+, Fe3+ and TpPa-1 under alkaline conditions. The PAEs were adsorbed by magnetic solid phase extraction and eluted with methanol, quantified by external standard method and then detected by GC. Results The limit of detections of 15 PAEs were 0.313-5.198 μg/L (S/N=3). The intra-day and inter-day relative standard deviations (RSDs) of the PAEs were less than 6.6% and 7.8%, respectively. The developed method was successfully applied for the determination of trace PAEs in carbonated drinks and tap water with recoveries ranging from 89.1% to 103.6% and RSDs were less than 7.9%. Conclusions This is a simple and rapid magnetization method for covalent organic frameworks (COFs) materials, which is expected to be used to enrich and separate PAEs in food sample pretreatment.