微波萃取高效液相色谱-冷原子荧光光谱法测定沉积物中甲基汞和无机汞  

Determination of Methylmercury and Inorganic Mercury in Sediments by High Performance Liquid Chromatography Hyphenated to Cold Vapor Generation Atomic Fluorescence Spectrometry Following a Microwave-Assisted Extraction

作　　者：冷庚[1] 王俊伟[2] 万旭[2] 钱蜀 但德忠[1] 

机构地区：[1]四川大学建筑与环境学院,成都610065 [2]四川省环境监测中心站,成都610041

出　　处：《分析化学》2012年第2期191-195,共5页Chinese Journal of Analytical Chemistry

基　　金：国家环境保护部基金(No.1030);四川省环境保护厅基金(No.08H1164)资助项目

摘　　要：建立了微波萃取高效液相色谱-冷原子荧光光谱法(MAE-HPLC-CVAFS)测定沉积物中甲基汞(MeHg+)和无机汞(Hg2+)的方法。以0.1%(V/V)2-巯基乙醇为萃取剂,用于沉积物样品中汞形态的萃取,在80℃下萃取8 min,萃取液直接注入HPLC-CVAFS系统分析。在优化条件下,MeHg+和Hg2+的检出限分别为0.58和0.48 ng/g;加标回收率分别为96.2%和95.8%;RSD(n=6)分别为5.7%和4.1%。对标准参考物质(IAEA-405和ERM-CC580)的分析结果与推荐值一致。本方法简单、快速、准确、检出限低,抗干扰能力强,具有很好的实用性和推广价值。A high performance liquid chromatography（HPLC） coupled with cold vapor generation atomic fluorescence spectrometry method（CVAFS） has been developed for the separation and determination of methylmercury（MeHg＋） and inorganic mercury（Hg2＋） in sediment samples.The previous extraction of samples was carried out at a temperature of 80 ℃ for 8 min by using 0.1%（V/V） 2-mercaptoethanol as the extractant.The separation and determination of mercury species were achieved by direct injecting the extractant to HPLC-CVAFS system.Under the optimized conditions,the limit of detection was 0.58 ng/g for MeHg＋ and 0.48 ng/g for Hg2＋.The average recoveries were 96.2% and 95.8% for MeHg＋ and Hg2＋,respectively,by spiking three concentration levels of mercury species into samples.The proposed method was validated for the determination of certified reference material IAEA-405 and ERM-CC580,and the analytical results were in good agreement with the certified values.The proposed method was simple,rapid,accurate,no interference and suitable for the determination of methylmercury and inorganic mercury in sediment samples.

关 键 词：汞 形态分析 微波辅助萃取 高效液相色谱 冷原子荧光光谱 

分 类 号：O657.31[理学—分析化学]