快速协同浊点萃取-高效液相色谱法测定水中4种苯酚类化合物  

Rapid Synergy Cloud Point Extraction-High Performance Liquid Chromatography for Determination of Four Phenolic Compounds in Water

作　　者：杨晓颖 姜勋 罗幸玲 叶小华 王梅 YANG Xiaoying;JIANG Xun;LUO Xingling;YE Xiaohua;WANG Mei(School of Public Health,Guangdong Pharmaceutical University,Guangzhou 510310)

机构地区：[1]广东药科大学公共卫生学院,广东广州510310

出　　处：《分析科学学报》2022年第6期729-735,共7页Journal of Analytical Science

基　　金：广州市科技计划项目(No.202002030409);广东药科大学“创新强校工程”(No.2020KZDZX1122,2019GCZX012)。

摘　　要：建立了水中4种极性苯酚类化合物对苯二酚、间苯二酚、邻苯二酚和苯酚的快速协同浊点萃取-高效液相色谱(RS-CPE-HPLC)检测新方法。实验以乙腈作协同诱导剂,磷酸三丁酯(TBP)为络合剂,仲醇聚氧乙烯醚15-S-7(Tergitol 15-S-7)为萃取剂,在室温下1 min内即可同时完成对4种极性苯酚类化合物的萃取,同时优化了乙腈用量、表面活性剂用量、络合剂用量、溶液pH、电解质浓度等影响因素。在最优条件下,4种目标物在0.1~191μg/L浓度范围内呈良好线性关系(r≥0.9996),方法的检出限在0.02~0.04μg/L,精密度良好(相对标准偏差≤2.58%,n=6),富集倍数为8.68~9.96,萃取率为86.8%~99.6%。同时将建立的方法应用于实际环境水样中4种苯酚类化合物的测定,样品加标回收率在93.9%~107%之间。该方法前处理简便、快速,经济环保,萃取率高,重现性好,可作为水中4种苯酚类化合物的有效检测方法。A new rapid synergistic-cloud point extraction-high performance liquid chromatographic(RS-CPE-HPLC)method was developed for the determination of four polar phenolic compounds(hydroquinone,resorcinol,catechol and phenol)in water.The extraction of the four polar phenols was accomplished simultaneously within 1 min at room temperature by using acetonitrile as the co-induction agent,tributyl phosphate(TBP)as the complexing agent and secondary alcohol ethoxylate 15-S-7(Tergitol 15-S-7)as the extractant.Under the optimal conditions,the four target compounds were extracted simultaneously.The method showed good linearity(r≥0.9996)in the concentration range of 0.1-191μg/L,high sensitivity(LOD≤0.04μg/L),good precision(RSD≤2.58%,n=6)with enrichment factors of 8.68-9.96 and extraction efficiency of 86.8%-99.6%.The developed method was applied to the determination of four phenolic compounds in real environmental water samples,and the spiked recoveries were in the range of 93.9%-107%.The method is simple,rapid,economical and environmentally friendly,and can be used as an effective method for the determination of the four phenolic compounds in water.

关 键 词：快速协同浊点萃取 乙腈 酚类化合物 环境水样 高效液相色谱法 

分 类 号：O657.72[理学—分析化学]