多孔氮化硼掺杂聚吡咯-2,3,3-三甲基吲哚固相微萃取涂层的制备及多环芳烃的检测  

Preparation of porous boron nitride-doped polypyrrole-2,3,3-trimethylindole solid-phase microextraction coatingfor polycyclic aromatic hydrocarbon detection

作　　者：杜洁 孙鹏超[1,2] 张梦露 连泽特 原凤刚 王刚 DU Jie;SUN Pengchao;ZHANG Menglu;LIAN Zete;YUAN Fenggang;WANG Gang(Experimental Testing Research Institute of PetroChina Xinjiang Oilfield Company,Karamay 834000,China;China National Petroleum Corporation Key Laboratory for Exploration and Development of Conglomerate Oil and Gas Reservoirs,Karamay 834000,China;No.1 Petrol Factory of PetroChina Xinjiang Oilfield Company,Karamay 834000,China;No.1 Gas Factory of PetroChina Xinjiang Oilfield Company,Karamay 834000,China)

机构地区：[1]中国石油新疆油田分公司实验检测研究院,新疆克拉玛依834000 [2]中国石油天然气集团公司砾岩油气藏勘探开发重点实验室,新疆克拉玛依834000 [3]中国石油新疆油田分公司采油一厂,新疆克拉玛依834000 [4]中国石油新疆油田分公司采气一厂,新疆克拉玛依834000

出　　处：《色谱》2023年第9期789-798,共10页Chinese Journal of Chromatography

基　　金：国家自然科学基金(21275112).

摘　　要：多环芳烃(PAHs)是持久性有机污染物中的一种,大部分具有较强的致癌、致畸和致突变性,对生态环境和人类健康易造成严重威胁。由于环境样品基质复杂且其中PAHs含量低,因此在仪器分析之前需要对环境样品进行必要的前处理。萃取材料的特性是决定大部分前处理技术萃取效率的关键。基于此,本文以低成本且富含较多官能团的吡咯(py)、2,3,3-三甲基吲哚(2,3,3-TMe@In)为单体,多孔氮化硼为掺杂物,采用电化学循环伏安法制备出多孔氮化硼掺杂聚吡咯-2,3,3-三甲基吲哚(Ppy/P2,3,3-TMe@In/BN)复合涂层,通过扫描电子显微镜、热稳定性分析、傅里叶红外光谱等手段对Ppy/P2,3,3-TMe@In/BN进行表征,结果表明:该涂层呈现出多孔、多褶皱的枝状结构,该结构有利于增加涂层的比表面积,从而实现对PAHs的大量富集;在320℃解吸温度下,涂层材料的色谱基线基本稳定,表明该涂层具有良好的热稳定性。将其修饰在不锈钢丝表面制成固相微萃取涂层,结合气相色谱-氢火焰离子化检测器,对影响萃取和分离萘(NAP)、苊(ANY)、芴(FLU)3种PAHs的条件进行优化,建立了用于以上3种PAHs检测的分析方法。该方法具有检出限低(10.6~14.5 ng/L,S/N=3)、稳定性好、萃取效率高等优势。将该方法应用于2种环境水样中3种PAHs的检测,在水样1中检测到少量的ANY(1.39μg/L)。通过向2种水样中加入低(1μg/L)、中(10μg/L)、高(50μg/L)3个水平的标准溶液考察了该方法的可靠性,得到了满意的回收率(82.5%~113.9%)。实验结果表明,所建立的分析方法可实现对环境水样中这3种PAHs的有效检测。Most polycyclic aromatic hydrocarbons(PAHs),which are persistent organic pollutants,have strong carcinogenicity,teratogenicity,and mutagenicity,and pose serious threats to the ecological environment and human health.Owing to the complexity of the matrix and low PAH content of environmental samples,separating and enriching PAHs in environmental samples is necessary prior to their detection.Solid-phase microextraction(SPME)technology is commonly used to detect PAHs owing to its advantages of simple operation,online connection with other instruments,low solvent usage,and integrability of sampling separation,enrichment,and desorption.The extraction coating is the core of this technology,and the type and thickness of the coating are important factors affecting the sensitivity and accuracy of the analysis.Common commercial extraction coatings include polydimethylsiloxane and quartz fiber;however,these materials have a number of disadvantages,such as poor thermal stability and high cost.Several methods,including electrochemical,sol-gel,molecular imprinting,and other coating methods,have been developed to prepare SPME coatings.Electrochemical methods have attracted considerable attention because of their simplicity,short duration,and high coating stability.In the development of an electrochemical method,the selection of the conductive polymer is of particular importance.Polypyrroles(Ppy)are easily synthesized and have numerous advantages,such as good conductivity and stable chemical properties.Thus,their use as a substrate material for SPME coatings is beneficial for improving the overall stability of the coating.Copolymerization with other polymers can enhance the adsorption performance of such coatings via synergistic effects.When doped with inorganic materials with high thermal stability,the composite coating can exhibit high temperature resistance.In this study, a porous boron nitride-doped Ppy- 2,3,3- trimethylindole (Ppy/ P2,3,3- TMe@In/BN) composite was prepared as a new SPME copolymer coating to detect three PAHs

关 键 词：固相微萃取 气相色谱 循环伏安法 多环芳烃 环境水样 

分 类 号：O658[理学—分析化学]