College of Science, Hebei Agricultural University, Baoding 071001, China.
College of Science, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2021 Mar 29;1641:461972. doi: 10.1016/j.chroma.2021.461972. Epub 2021 Feb 10.
Design and synthesis of novel coatings for solid phase microextraction (SPME) is urgently needed for sample pretreatment. In this study, three hypercrosslinked polymers (HCPs) were constructed by the facile Friedel-Crafts alkylation reactions between tetraphenylethylene (TPE) and 1,4-bis(chloromethyl)benzene (BCMB), 4,4'-bis(chloromethyl)-1,1'-biphenyl (BCMBP), and cyanuric chloride (CC), respectively. The newly-synthesized HCPs were employed as SPME coatings for the extraction of phthalate esters (PAEs). Various parameters influencing the SPME efficiencies, including extraction time and temperature, ionic strength, stirring rate, desorption temperature and time were optimized. Under the optimal conditions, low limits of detection (0.003-0.033 μg L ), wide linearity (0.01-10 μg L ) and good repeatability (4.1-9.3%) were achieved. The HCPs-based SPME method was successfully applied for the determination of eight PAEs in environmental water and bottled water samples with recoveries from 75.3% to 116%. This method provides a good alternative for monitoring trace level of PAEs in water samples.
用于固相微萃取(SPME)的新型涂层的设计和合成对于样品预处理是迫切需要的。在本研究中,通过四苯乙烯(TPE)与 1,4-双(氯甲基)苯(BCMB)、4,4'-双(氯甲基)-1,1'-联苯(BCMBP)和三聚氯氰(CC)之间的简便 Friedel-Crafts 烷基化反应,分别构建了三种超交联聚合物(HCPs)。新合成的 HCPs 被用作 SPME 涂层,用于提取邻苯二甲酸酯(PAEs)。优化了影响 SPME 效率的各种参数,包括萃取时间和温度、离子强度、搅拌速度、解吸温度和时间。在最佳条件下,实现了低检测限(0.003-0.033 μg L-1)、宽线性范围(0.01-10 μg L-1)和良好的重复性(4.1-9.3%)。基于 HCPs 的 SPME 方法成功应用于环境水样和瓶装水样中 8 种 PAEs 的测定,回收率为 75.3%-116%。该方法为监测水样中痕量 PAEs 提供了一种很好的选择。