分析化学Issue(7)：1033-1038,6.DOI:10.11895/j.issn.0253-3820.131030
低压液相色谱-原子荧光快速测定鱼肉和土壤样品中汞形态
Mercury Speciation Determination in Fish and Soil Samples Based on Low Pressure LC-AFS Combined with Rapid Sample Pretreatment
曹小丹 1秦德元 1郝伟 2焦晓琳2
作者信息
- 1. 北京吉天仪器有限公司，北京100015
- 2. 北京大学环境工程学院，北京100087
- 折叠
摘要
Abstract
The build-in low-pressure monolithic column combined with hydride generation atomic fluorescence spectrometry ( HG-AFS ) was employed for speciation analysis of fish meat. The sample pretreatment and separation approach could be accomplished within 30 min. The proper amount of fish sample was weighed and smashed into puree. The extraction solution composed of 10% HCl, 1% thiourea, and 0. 15% KCl was added before loaded into the automatic temperature controlled vertex system with 2000 r/min. The sample solution was separated through Merck monolithic column, with 3% ( V/V) acetonitrile, 30 mmol/L amonium acetate and 0. 03%(V/V) 2-mercaptoethanol (2-ME) as the eluent. The after-column eluent was digested by novel UV digestion device with pipeline sintered into the lamp, and then detected by hydrid-generation AFS. The rapid LC separation enabled fast mercury speciation of fish sample within 10 min. The different UV lamp digestion effects, eluent components, carrier gas, shield gas, lamp current, as well as PMT working power was optimized. Under the optimal conditions, the robust system achieved detection limits (DL) of 0. 15 μg/L and 0. 14 μg/L for methylmercury and HgⅡ, respectively. The RSD (n=7) was less than 5%, the linear correlation coefficient was 0 . 999 , and the matrix spiked recovery was in the range of 85%-110% for Hg speciation. This method was used for the determination of Hg speciation in fish and soil samples, and was proofed to be a reliable, easy approach for daily inspection.关键词
低压液相-原子荧光联用/整体柱/汞形态分析Key words
Low pressure liquid chromatography-hydride generation atomic fluorescence spectrometry combination/Monolithic column/Mercury speciation引用本文复制引用
曹小丹,秦德元,郝伟,焦晓琳..低压液相色谱-原子荧光快速测定鱼肉和土壤样品中汞形态[J].分析化学,2014,(7):1033-1038,6.
