HPLC-ICP-MS Determination of 7 Element Species in Fresh Water
摘 要
建立了高效液相色谱-电感耦合等离子体质谱法同时测定淡水中亚砷酸盐[As(Ⅲ)]、砷酸盐[As(Ⅴ)]、一甲基胂酸(MMA)、二甲基胂酸(DMA)、亚硒酸盐[Se(Ⅳ)]、硒酸盐[Se(Ⅵ)]和六价铬[Cr(Ⅵ)]的方法。采用以不同体积比的pH 8.7的20 mmol·L-1硝酸铵溶液和pH 8.7的60 mmol·L-1硝酸铵溶液为流动相进行梯度洗脱,通过优化的色谱条件实现了7种元素形态在14 min完成色谱分离,氯化物对75As、77Se、53Cr无干扰。7种元素形态在一定范围内呈线性,As(Ⅲ)、As(Ⅴ)、MMA、DMA、Se(Ⅳ)、Se(Ⅵ)和Cr(Ⅵ)的检出限(3S/N)分别为0.06,0.02,0.04,0.05,1.00,1.00,0.20 μg·L-1。按标准加入法进行回收试验,回收率为80.1%~101%,相对标准偏差(n=6)为0.59%~5.2%。
Abstract
A method was proposed for simultaneous determination of arsenite[As(Ⅲ)], arsenate[As(Ⅴ)], monomethylarsenic acid (MMA), dimethylarsenic acid (DMA), selenite[Se(Ⅳ)], selenate[Se(Ⅵ)] and Cr(Ⅵ) in fresh water by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). A mixture of 20 mmol·L-1 NH4NO3 solution (pH 8.7) and 60 mmol·L-1 NH4NO3 solution (pH 8.7) in different volume ratios was used as the mobile phase for gradient elution. Seven element species were separated under the optimized chromatographic conditions within 14 min, and the chloride had no interference to 75As, 77Se and 53Cr. Linear relationships of 7 element species were found in definite ranges, and the detection limits were 0.06 μg·L-1 for As (Ⅲ), 0.02 μg·L-1 for As(Ⅴ), 0.04 μg·L-1 for MMA, 0.05 μg·L-1 for DMA, 1.00 μg·L-1 for Se(Ⅳ), 1.00 μg·L-1 for Se(Ⅵ) and 0.20 μg·L-1 for Cr(Ⅵ), respectively. Test for recovery was made by standard addition method, giving results in the range of 80.1%-101%, with RSDs (n=6) ranged from 0.59% to 5.2%.
中图分类号 O65 DOI 10.11973/lhjy-hx201807020
所属栏目 专题报道(环境分析)
基金项目
收稿日期 2017/7/9
修改稿日期
网络出版日期
作者单位点击查看
备注祝银,学士,主要从事海洋生态与渔业环境监测工作,zhuyin2697@163.com
引用该论文: ZHU Yin,LIU Qin,YANG Chenghu,WANG Fansheng,LI Zimeng,SONG Kai. HPLC-ICP-MS Determination of 7 Element Species in Fresh Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(7): 836~840
祝银,刘琴,杨承虎,王范盛,李子孟,宋凯. 高效液相色谱-电感耦合等离子体质谱法测定淡水中7种元素形态的含量[J]. 理化检验-化学分册, 2018, 54(7): 836~840
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】CARUSO J A, MONTES-BAYON M. Elemental speciation studies-new directions for trace metal analysis[J]. Ecotoxicology and Environmental Safety, 2003,56(1):148-163.
【2】陈静,周黎明,曲刚莲.HPLC联用技术在环境砷形态分析上的应用[J].环境科学与技术, 2003,26(2):60-62.
【3】KRULL I S. Trace metal analysis and speciation[M]. [S.l.]: Distributors for the United States and Canada, Elsevier Science Pub. Co., 1991.
【4】World Health Organization. Guidelines for drinking water quality[M]. Geneva: Printed in Malta by Gutenberg, 2017.
【5】孙梅,吴强华.环境中铬形态分析研究进展[J].理化检验-化学分册, 2008,44(10):1012-1016.
【6】方军,舒永红,滕久委,等.HPLC-ICP-MS测定中药中砷的形态[J].分析试验室, 2006,25(12):95-98.
【7】周赛春,江海亮,周先波,等.浊点萃取-石墨炉原子吸收光谱法对不锈钢餐具溶出铬的形态分析[J].分析测试学报, 2008,27(4):405-407.
【8】李妍,刘书娟,江冬青,等.气相色谱-电感耦合等离子体质谱联用技术应用于水产品中汞形态分析[J].分析化学, 2008,36(6):793-798.
【9】黄志勇,吴熙鸿,胡广林,等.高效液相色谱/电感耦合等离子体质谱联用技术用于元素形态分析的研究进展[J].分析化学, 2002,30(11):1387-1393.
【10】BEAUCHEMIN D, SIU K W M, MCLAREN J W, et al. Determination of arsenic species by high-performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1989,4(3):285-289.
【11】周瑛,叶丽,竹鑫平.HPLC-ICP-MS在食品中硒和砷形态分析及其生物有效性研究中的应用[J].化学进展, 2007,19(6):982-995.
【12】LARSEN E H, PRITZL G, CORNETT C. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1992,7(4):629-634.
【13】郭志英,于水.HPLC/ICP-MS在环境样品的痕量元素形态分析中的应用[J].质谱学报, 2006,27(1):56-64.
【14】刘二保,梁建功,韩素琴,等.铬的形态分析研究与进展[J].理化检验-化学分册, 2003,39(6):368-371.
【15】WOLF R E, MORMAN S A, HAGEMAN P L, et al. Simultaneous speciation of arsenic, selenium, and chromium: Species stability, sample preservation, and analysis of ash and soil leachates[J]. Analytical and Bioanalytical Chemistry, 2011,401(9):2733-2745.
【16】JABŁOHSKA-CZAPLA M, SZOPA S, GRYGOYC K, et al. Development and validation of HPLC-ICP-MS method for the determination inorganic Cr, As and Sb speciation forms and its application for Pławniowice reservoir (Poland) water and bottom sediments variability study[J]. Talanta, 2014,120:475-483.
【17】ROIG-NAVARRO A F, MARTINEZ-BRAVO Y, LÓPEZ F J, et al. Simultaneous determination of arsenic species and chromium(Ⅵ) by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry[J]. Journal of Chromatography A, 2001,912(2):319-327.
【18】NAM S H, OH H J, MIN H S, et al. A study on the extraction and quantitation of total arsenic and arsenic species in seafood by HPLC-ICP-MS[J]. Microchemical Journal, 2010,95(1):20-24.
【2】陈静,周黎明,曲刚莲.HPLC联用技术在环境砷形态分析上的应用[J].环境科学与技术, 2003,26(2):60-62.
【3】KRULL I S. Trace metal analysis and speciation[M]. [S.l.]: Distributors for the United States and Canada, Elsevier Science Pub. Co., 1991.
【4】World Health Organization. Guidelines for drinking water quality[M]. Geneva: Printed in Malta by Gutenberg, 2017.
【5】孙梅,吴强华.环境中铬形态分析研究进展[J].理化检验-化学分册, 2008,44(10):1012-1016.
【6】方军,舒永红,滕久委,等.HPLC-ICP-MS测定中药中砷的形态[J].分析试验室, 2006,25(12):95-98.
【7】周赛春,江海亮,周先波,等.浊点萃取-石墨炉原子吸收光谱法对不锈钢餐具溶出铬的形态分析[J].分析测试学报, 2008,27(4):405-407.
【8】李妍,刘书娟,江冬青,等.气相色谱-电感耦合等离子体质谱联用技术应用于水产品中汞形态分析[J].分析化学, 2008,36(6):793-798.
【9】黄志勇,吴熙鸿,胡广林,等.高效液相色谱/电感耦合等离子体质谱联用技术用于元素形态分析的研究进展[J].分析化学, 2002,30(11):1387-1393.
【10】BEAUCHEMIN D, SIU K W M, MCLAREN J W, et al. Determination of arsenic species by high-performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1989,4(3):285-289.
【11】周瑛,叶丽,竹鑫平.HPLC-ICP-MS在食品中硒和砷形态分析及其生物有效性研究中的应用[J].化学进展, 2007,19(6):982-995.
【12】LARSEN E H, PRITZL G, CORNETT C. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1992,7(4):629-634.
【13】郭志英,于水.HPLC/ICP-MS在环境样品的痕量元素形态分析中的应用[J].质谱学报, 2006,27(1):56-64.
【14】刘二保,梁建功,韩素琴,等.铬的形态分析研究与进展[J].理化检验-化学分册, 2003,39(6):368-371.
【15】WOLF R E, MORMAN S A, HAGEMAN P L, et al. Simultaneous speciation of arsenic, selenium, and chromium: Species stability, sample preservation, and analysis of ash and soil leachates[J]. Analytical and Bioanalytical Chemistry, 2011,401(9):2733-2745.
【16】JABŁOHSKA-CZAPLA M, SZOPA S, GRYGOYC K, et al. Development and validation of HPLC-ICP-MS method for the determination inorganic Cr, As and Sb speciation forms and its application for Pławniowice reservoir (Poland) water and bottom sediments variability study[J]. Talanta, 2014,120:475-483.
【17】ROIG-NAVARRO A F, MARTINEZ-BRAVO Y, LÓPEZ F J, et al. Simultaneous determination of arsenic species and chromium(Ⅵ) by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry[J]. Journal of Chromatography A, 2001,912(2):319-327.
【18】NAM S H, OH H J, MIN H S, et al. A study on the extraction and quantitation of total arsenic and arsenic species in seafood by HPLC-ICP-MS[J]. Microchemical Journal, 2010,95(1):20-24.
相关信息