基于共价有机骨架涂层的搅拌棒吸附萃取/高效液相色谱测定环境水样中的多环芳烃  

Determination of Polycyclic Aromatic Hydrocarbons in Environmental Water by HPLC with Stir Bar Adsorption Extraction Based on Covalent Organic Framework Coating

作　　者：刘海霞[1,2] 杨彩玲 饶红红[1,2] 刘芳 张丽[1] 赵国虎 LIU Hai-xia;YANG Cai-ling;RAO Hong-hong;LIU Fang;ZHANG Li;ZHAO Guo-hu(School of Chemistry and Chemical Engineering,Lanzhou City University,Lanzhou 730070,China;Provincial Key Laboratory of Gansu Higher Education for City Environmental Pollution Control,Lanzhou 730070,China)

机构地区：[1]兰州城市学院化学工程学院,甘肃兰州730070 [2]“城市环境污染控制”甘肃省高校省级重点实验室,甘肃兰州730070

出　　处：《分析测试学报》2023年第12期1573-1579,共7页Journal of Instrumental Analysis

基　　金：甘肃省自然科学基金项目(20JR5RA208,21JR7RA538);甘肃省高等学校科研项目(2021B-280)。

摘　　要：以刻蚀不锈钢丝(ESSW)为搅拌棒基体,用1,3,5-三(4-氨苯基)苯(TPB)和2,5-二乙烯基-1,4-苯二甲醛(DVA)两种单体,制备了一种分散良好的共价有机骨架涂层(TPB-DVA-COF)搅拌棒,结合高效液相色谱-紫外检测器(HPLC-UV)建立了环境水样中6种多环芳烃(PAHs)的分析方法。通过扫描电镜(SEM)、透射电镜(TEM)、傅里叶变换红外光谱(FTIR)等对涂层进行了表征,优化了离子强度、萃取温度、搅拌速率、萃取时间等条件。在优化条件下,菲、荧蒽和芘在0.20~200μg/L,[艹屈]、苯并[b]荧蒽和苯并[a]芘在0.05~200μg/L范围内与色谱峰面积呈良好的线性关系,相关系数(r)不小于0.9985,富集倍数最高可达到225倍,检出限(LOD,S/N=3)为0.007~0.150μg/L,同一根搅拌棒的相对标准偏差为3.8%~6.1%,样品加标回收率为87.1%~104%。结果表明,该方法可以成功地应用于实际环境水样中PAHs的准确和高灵敏检测。1,3,5-Tri(4-aminophenyl)benzene(TPB)and 2,5-divinyl-1,4-phenyldiformalde⁃hyde(DVA)were adopted as monomers to prepare a homogeneous covalent organic framework(TPBDVA-COF)coated stir bar.The stir bar combined with high performance liquid chromatography was used for the extraction and detection of six polycyclic aromatic hydrocarbons(PAHs)in environmental water samples.Scanning electron microscopy(SEM),transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FTIR)were performed to characterize the material to confirm successful preparation of TPB-DVA-COF.Meanwhile,a series of experimental parameters includ⁃ing ion strength,extraction temperature,stirring rate,extraction time and desorption time were op⁃timized.Under the optimized conditions,there were good linear relationships for phenanthrene(Phe),fluoranthene(Fla)and pyrene(Pyr)in the range of 0.20-200μg/L,chrysene(Chr),ben⁃zofluoranthrene(B[b]f)and benzopyren(B[a]p)in the range of 0.05-200μg/L,with the correla⁃tion coefficients(r)not less than 0.9985,and enrichment factor could be reached 225 folds.The limits of detection(LODs,S/N=3)were in the range of 0.007-0.150μg/L,and the relative stan⁃dard deviations(RSDs)were in the range of 3.8%-6.1%for one bar(n=5),respectively.In the case of real samples analyses,the spiked recoveries were 87.1%-104%.The results showed that the de⁃veloped method could be successfully applied to the accurate and highly sensitive detection of PAHs in actual environmental water samples.

关 键 词：共价有机骨架材料 搅拌棒吸附萃取 高效液相色谱 多环芳烃 环境水样 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]