基于氨基功能化石墨烯磁性材料的磁固相萃取-高效液相色谱法分析海水中的氯酚类污染物  

Analysis of Chlorophenols in Seawater Samples by Amine-functional Magnetic Graphene Oxide-Based Magnetic Solid Phase Extraction Coupled with High Performance Liquid Chromatography

作　　者：孙美娜[1,2] 刘佰威 项奇 王春春[1] 毛时强 沈昊宇[1] 叶仙森[3] 

机构地区：[1]浙江大学宁波理工学院,浙江宁波315100 [2]浙江杭康检测技术有限公司,浙江杭州310011 [3]国家海洋局宁波海洋环境监测中心站,浙江宁波315012

出　　处：《分析科学学报》2017年第4期455-460,共6页Journal of Analytical Science

基　　金：浙江省自然科学基金(No.LY14B04003);宁波市自然科学基金(No.2014A610092);国家级大学生创新创业训练计划(No.201513022009);浙江省新苗计划(No.2015R401181)

摘　　要：本文采用氨基功能化石墨烯磁性材料富集海水中的5种氯酚类(CPs)污染物,建立了一种快速、高效、灵敏的磁固相萃取-高效液相色谱(MSPE-HPLC)法,用于其残留量的测定。实验优化了磁固相萃取的条件,考察了样品pH值、富集时间和洗脱剂的种类与用量等对CPs回收率的影响。样品经富集后在C8反相液相色谱柱(250×4.6mm i.d.,5μm)上分离,以体积比为70∶30的甲醇-5mmol/L NH_4Ac溶液为流动相,紫外检测波长为230nm。结果表明,5种CPs的富集倍数可达250倍;CPs浓度在1~2 000ng/L范围内呈现良好的线性关系,线性相关系数(R)均大于0.9995;平均回收率为92.6%~101.2%,相对标准偏差为0.6%~7.2%;检出限为0.15~1.06ng/L,定量限为0.5~3.2ng/L。采用本方法对5个实际海水样品中的CPs进行了定量检测,结果其中一种样品含有2,4,6-三氯苯酚,浓度为6.5ng/L。In this work,a rapid,sensitive and accurate method for the simultaneous determination of 5chlorophenols（CPs）in seawater samples by magnetic solid phase extraction-high performance liquid chromatography（MSPE-HPLC）was reported.The seawater samples were firstly enriched by aminefunctional magnetic graphene oxide materials（NH2-MGO）,then separated on a C8 analytical column（250×4.6mm i.d.,5.0μm）,with a methanol-5mmol/L NH4Ac（70∶30,V/V）solution eluting system and detected at 230 nm via UV detector.The results showed that the enrichment factor of the target CPs reached 250.Under the optimal condition,linear range were from 1to 2 000ng/L with correlation coefficients（R）higher than 0.9995 for the target chlorophenols.The recoveries were between 92.6%and 101.2% at the spiked levels with the relative standard deviations in the range of 0.6%-7.2%.The limits of detection were in the range of 0.15-1.06ng/L and the limits of quantification were between0.5-3.2ng/L.The developed method can be applied to the routine analysis of the chlorophenols in seawater samples.The present method has been applied for the determination of the CPs in 5real samples.The result showed that one of them was found to contain 6.5ng/L 2,4,6-TCP.

关 键 词：氨基功能化 石墨烯磁性材料 氯酚类污染物 海水 磁固相萃取 

分 类 号：O657.72[理学—分析化学]