Wang Zhuo, He Man, Chen Beibei, Hu Bin
Department of Chemistry, Wuhan University, Wuhan 430072, China.
Department of Chemistry, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2021 Dec 20;1660:462665. doi: 10.1016/j.chroma.2021.462665. Epub 2021 Nov 2.
Cyanuric chloride and 4,4'-diamino-p-terphenyl were adopted as monomers to synthesize poly (4,4'-diamino-p-terphenyl-triazine) (PDT) covalent organic polymer. PDT coated stir bar was prepared and evaluated for the extraction of five phthalate esters (PAEs) with relatively lower logP values (2.7-4.9), including diethyl phthalate, diallyl phthalate, dipropyl phthalate, benzylbutyl phthalate and dibutyl phthalate. It exhibited higher extraction recovery (> 65%) and faster extraction kinetics (50 min vs 240 min) for target PAEs over commercial polydimethylsiloxane coated stir bar. Based on the superior performance, PDT coated stir bar sorptive extraction was combined with high-performance liquid chromatography-diode array detection for trace analysis of five PAEs plasticizers. The limits of detection for target PAEs were 0.04-0.27 μg/L, with the enrichment factors of 54-80-fold. The potential of the method was demonstrated by detecting five target PAEs in Chinese liquor and mineral water samples. No target analytes were detected in Chinese liquor sample, and recoveries of 85.4-109% were obtained for target analytes in spiked liquor samples; trace diethyl phthalate (1.19-2.98 μg/L) and dibutyl phthalate (0.77-0.91 μg/L) were detected in two mineral water samples, with recoveries of 85.4-117% and 87.4-117% respectively in spiked mineral water samples.
采用三聚氯氰和4,4'-二氨基对三联苯作为单体合成聚(4,4'-二氨基对三联苯三嗪)(PDT)共价有机聚合物。制备了PDT涂层搅拌棒,并对其萃取5种logP值相对较低(2.7 - 4.9)的邻苯二甲酸酯(PAEs)进行了评估,包括邻苯二甲酸二乙酯、邻苯二甲酸二烯丙酯、邻苯二甲酸二丙酯、邻苯二甲酸苄基丁酯和邻苯二甲酸二丁酯。与市售聚二甲基硅氧烷涂层搅拌棒相比,它对目标PAEs表现出更高的萃取回收率(>65%)和更快的萃取动力学(50分钟对240分钟)。基于优异的性能,将PDT涂层搅拌棒吸附萃取与高效液相色谱 - 二极管阵列检测相结合,用于5种PAEs增塑剂的痕量分析。目标PAEs的检测限为0.04 - 0.27μg/L,富集倍数为54 - 80倍。通过检测白酒和矿泉水样品中的5种目标PAEs证明了该方法的潜力。白酒样品中未检测到目标分析物,加标白酒样品中目标分析物的回收率为85.4 - 109%;在两个矿泉水样品中检测到痕量邻苯二甲酸二乙酯(1.19 - 2.98μg/L)和邻苯二甲酸二丁酯(0.77 - 0.91μg/L),加标矿泉水样品中的回收率分别为85.4 - 117%和87.4 - 117%。