羟基七元瓜环固相微萃取测定环境水体中的硝基苯酚异构体  

Determination of Nitrophenol Isomers in Environmental Water by Solid-phase Microextraction Based on Monohydroxy-Cucurbit[7]uril

作　　者：赵雨璇 董南[1] 董美玉 ZHAO Yuxuan;DONG Nan;DONG Meiyu(School of Chemistry and Chemical Engineering,Guizhou University,Guiyang 550025,China)

机构地区：[1]贵州大学化学与化工学院,贵州贵阳550025

出　　处：《贵州大学学报（自然科学版）》2022年第3期46-51,共6页Journal of Guizhou University:Natural Sciences

基　　金：国家自然科学基金资助项目(21665005);贵州省科技计划资助项目(黔科合基础-zk[2021]一般054)。

摘　　要：以单羟基七元瓜环(Q[7]-OH)和端羟基聚二甲基硅氧烷(OH-PDMS)为固定相,利用溶胶-凝胶方法制备了PDMS/Q[7]-OH的固相微萃取搅拌棒(stir-bar sorptive extraction,SBSE),建立了SBSE-高效液相色谱(high performance liquid chromatography,HPLC)-二极管阵列检测器(diode-array detector,DAD)对环境水样中3种硝基苯酚异构体同时检测的分析方法。方法对萃取时间、溶液的pH值、盐离子浓度、解吸溶剂和解吸时间进行了优化。在优化条件下,SBSE-HPLC-DAD测定硝基苯酚异构体的线性范围为0.01~10.00 mg/L,相关系数均大于0.9997,检测限在0.002~0.006 mg/L范围内,日内及日间精密度的相对标准偏差在2.9%~7.5%之间(C=0.8 mg/L),3个加标浓度的平均相对回收率在71.5%~116.8%范围内。方法灵敏、简便,可满足环境水样中硝基苯酚异构体同时测定的要求。Stir-bar sorptive extraction(SBSE)based on PDMS/Q[7]-OH was prepared by sol-gel method using hydroxyl-terminated polydimethylsiloxane(OH-PDMS)and monohydroxy-cucurbit[7]uril(Q[7]-OH)as stationary.A SBSE-High performance liquid chromatography with diode array detector(HPLC/DAD)method was developed for the simultaneous determination of three nitrophenol isomers in environmental water samples.The extraction time,pH value of solution,the concentration of salt ions,desorption solvent and desorption time were optimized.Under optimal conditions,the linear range of three nitrophenol isomers determined by SBSE-HPLC-DAD was between 0.01 mg/L and 10.00 mg/L,and the correlation coefficient were all greater than 0.9997.The limits of detection of the proposed method were in the range of 0.002-0.006 mg/L.The mean relative recoveries at three spiked levels ranged from 71.5%to 116.8%,with intra-precision and inter-precision both in the range of 2.9%-7.5%.The proposed method is simple and sensitive,and it is suitable for the simultaneous analysis of phenols in environmental water.

关 键 词：单羟基取代七元瓜环 固相微萃取小棒 硝基苯酚异构体 高效液相色谱 环境水样 

分 类 号：O69[理学—化学] O657.72