高效液相色谱-原子荧光光谱法测定水产品中汞的形态
HPLC-AFS Determination of Species of Mercury in Aquatic Products
摘 要
提出了高效液相色谱与原子荧光光谱法联用测定水产品中3种汞化合物,即无机汞、甲基汞和乙基汞含量的方法。样品提取液过C18固相萃取柱净化,经C18色谱柱分离后,用原子荧光形态分析仪测定3种汞化合物的含量。无机汞、甲基汞和乙基汞的质量浓度在1.00~50.0 μg·L-1范围内与其荧光强度呈线性关系,无机汞和甲基汞的测定下限(10S/N)为0.03 mg·kg-1,乙基汞的测定下限为0.04 mg·kg-1。方法用于水产品分析,并进行加标回收试验,方法的回收率在73.3%~87.4%之间,测定值的相对标准偏差(n=6)在3.6%~9.1%之间。
汞
形态分析
高效液相色谱-原子荧光光谱法
Aquatic products
Mercury
Speciation analysis
HPLC-AFS
Abstract
A method of HPLC and AFS in hyphenation for the determination of the species of 3 mercury compounds in aquatic products was proposed. Sample of aquatic product was extracted with a solution containing thiourea, KCl and HCl, and the extract was cleaned up on C18 SPE column, and separated on C18 chromatographic column, and then determined by atomic fluorescence speciation analyzer. Linear relationships between values of fluorescence intensity and mass concentration of Hg2+, CH3Hg and CH3CH2Hg were kept in the same range from 1.00 to 50.0 μg · L-1, with lower determination of limits (10S/N) of 0.03 mg·kg-1 for Hg2+ and CH3Hg, and 0.04 mg·kg-1 for CH3CH2Hg. The proposed method was applied to the analysis of aquatic products, giving values of recovery obtained by standard addition method in the range of 73.3%-87.4% and RSD′s (n=6) in the range of 3.6%-9.1%.
中图分类号 O652.63 O657.31
所属栏目 工作简报
基金项目 浙江省科技计划项目(2012F30021);浙江省重点科技创新团队(2010R50028)
收稿日期 2012/6/6
修改稿日期
网络出版日期
作者单位点击查看
联系人作者梅光明(3057312@163.com)
备注梅光明(1984-),男,湖北黄冈人,工程师,硕士,研究方向为水产品质量安全及标准化。
引用该论文: MEI Guang-ming,GUO Yuan-ming,ZHU Jing-ping,CHEN Xue-chang,ZHANG Xiao-jun,LI Pei-pei,LIU Qin. HPLC-AFS Determination of Species of Mercury in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(7): 840～843
梅光明,郭远明,朱敬萍,陈雪昌,张小军,李佩佩,刘琴. 高效液相色谱-原子荧光光谱法测定水产品中汞的形态[J]. 理化检验－化学分册, 2013, 49(7): 840～843
被引情况:
【1】戴礼洪,刘潇威,王迪,蒋梦, "固相萃取-高效液相色谱-原子荧光光谱法联用测定水中无机汞(Ⅱ)及有机汞",理化检验－化学分册 51, 1178-1182(2015)
【2】傅雄伟,李海普,杨远,孔倩,杨兆光, "高效液相色谱与电感耦合等离子体质谱联用测定水中的二价汞、甲基汞与乙基汞",理化检验－化学分册 52, 1277-1281(2016)
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参考文献
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【3】GB 2762-2005食品中污染物限量［S］.
【4】NY 5073-2006无公害食品水产品中有毒有害物质限量［S］.
【5】史建波,廖春阳,王亚伟,等.气相色谱和原子荧光联用测定生物和沉积物样品中甲基汞［J］.光谱学与光谱分析, 2006,26(2):336-339.
【6】CARRASCO L, DIEZ S, BAYONA J M. Simultaneous determination of methyl-mercury and ethyl-mercury by solid-phase microextraction followed by gas chromatography atomic fluorescence detection［J］. Journal of Chromatography A, 2009,1216(51):8828-8834.
【7】CHUNG S W C, CHAN B T P. A reliable method to determine methylmercury and ethylmercury simultaneously in foods by gas chromatography with inductively coupled plasma mass spectrometry after enzymatic and acid digestion［J］. Journal of Chromatography A, 2011,1218(9):1260-1265.
【8】徐进勇,王彤,陈杜军,等.光诱导蒸气发生-高效液相色谱-电感耦合等离子体质谱联用测定汞形态［J］.分析化学, 2012,40(1):169-172.
【9】LIANG Li-na, JIANG Gui-bin, LIU Jing-fu, et al. Speciation analysis of mercury in seafood by using high-performance liquid chromatography on-line coupled with cold-vapor atomic fluorescence spectrometry via a post column microwave digestion［J］. Anal Chem Acta, 2003,477(1):131-137.
【10】MORTON J, CAROLAN V A, GARDINER P H E. The speciation of inorganic and methylmercury in human hair by high-performance liquid chromatography coupled with inductively coupled plasma mass spectrometry［J］. Journal of Analytical Atomic Spectrometry, 2002,17(4):377-381.
【11】陈玉红,米健秋,张兰.高效液相色谱-电感耦合等离子体质谱联用测定环境水样中的二价汞、甲基汞、乙基汞与苯基汞［J］.环境化学, 2011,30(4):893-896.
【12】边静,余晓刚,谢维杰,等.在线预还原-氢化物发生-原子荧光光谱法测定尿液中总无机砷［J］.理化检验-化学分册, 2012,48(3):290-292.
【13】曾晓丹,王建刚,张慧颖,等.湿法消解-原子荧光光谱法测定人参皂苷中的重金属元素［J］.光谱实验室, 2011,28(3):1085-1088.
【14】冷庚,王俊伟,万旭,等.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［J］.分析化学, 2012,40(2):191-195.
【15】夏炳训,宋晓丽,姜军成,等.微波消解-原子荧光光谱法测定海洋生物体中汞［J］.理化检验-化学分册, 2012,48(3):318-320.
【16】刘明钟,汤志勇,刘霁欣.原子荧光光谱分析［M］.北京:化学工业出版社, 2008.
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