Publisher : The Korean Society of Environmental Agriculture
DOI : 10.5338/KJEA.2011.30.3.288
Title & Authors
Establishment of Analytical Method for Methylmercury in Fish by Using HPLC-ICP/MS Yoo, Kyung-Yoal; Bahn, Kyeong-Nyeo; Kim, Eun-Jung; Kim, Yang-Sun; Myung, Jyong-Eun; Yoon, Hae-Seong; Kim, Mee-Hye;
BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at in microwave for 20 min. Methylmercury in of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at . The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient() for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.
Craig, P., George, E., Jenkins, R., 2003. Organometallic compounds in the environment, pp. 32-38, John Wiley & Sons Ltd, USA.
Isabel, T., Marc, L., Erik, B., 2004. Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance, Trends in Anal. Chem. 23, 535-552.
Santos, J.S., Pastor, M.G.A., Santosa, M.L.P., 2009. Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS. Talanta, 80, 207-211.
Lee, J.S., Ryu, Y.J., Park, J.S., Hong E.J., Kang, H.K., Jeon, S.H., Kim, S.C., Ki, Y.H., 2007. A Study of Analytical Method for Methylmercury in Fish Using Purge and Trap Gas Chromatograph-Mass Spectrometer. Korean J. Environ. Anal. 10, 8-12.
Morita, M., Yoshinaga, J., Edmond, J.S., 1998. The determination of mercury species in environmental and biological samples, Pure Appl. Chem. 70, 1585-1615.
Qvarnstrőm, J., Frech, W., 2002. Mercury species transformations during sample pre-treatment of biological tissues studied by HPLC-ICP-MS. J. Anal. At. Spectrom. 17, 1486-1491.
Reyes, H., Mizanur, R.G.M., Skip, K.H.M., 2009. Robust microwave-assisted extraction protocol for determination of total mercury and methylmercury in fish tissues. Analytica Chimica Acta. 631, 121-128.
Westoo, G., 1967. Determination of methylmercury compounds in foodstuffs. Acta Chemica Scandinavica, 21, 1790-1800.