Development of Methylmercury Analysis by Ultra-High Performance Liquid Chromatography Coupled with ICP-MS and Its Application on Sharks’ Meat Measurement

Suratno Suratno(1*), Satriyo Krido Wahono(2), Dwi Siswanta(3), Nurul Hidayat Aprilita(4)

(1) Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Sekip Utara, Yogyakarta 55281, Indonesia; Research Center for Food Technology and Processing (PRTPP), National Research and Innovation Agency (BRIN), Gunungkidul, Yogyakarta 55861, Indonesia
(2) Research Center for Food Technology and Processing (PRTPP), National Research and Innovation Agency (BRIN), Gunungkidul, Yogyakarta 55861, Indonesia
(3) Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Sekip Utara, Yogyakarta 55281, Indonesia
(4) Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Sekip Utara, Yogyakarta 55281, Indonesia
(*) Corresponding Author


This study analyzed MeHg in a fast, simple, low-waste, and accurate by using ultra-high liquid chromatography coupled with inductively coupled plasma mass spectrometry. Simple preparation by liquid extraction with sonication at room temperature was effective extract MeHg from Certified Reference Material (CRM) and shark meat samples. Effective MeHg separation was achieved in less than 300 s using a C18 Hypersil Gold analytical column with a mobile gradient phase of 0.5% (w/v) L-cysteine in 2% (v/v) HNO3 and 100% methanol. The MeHg was extracted from 100 mg of shark meat using 1 mL of 0.5% (w/v) L-cysteine in 2% (v/v) HNO3 and sonicated for 30 min. Analysis of certified reference material (DORM-4) showed values between the experimental and certified values. The observed limit of detection and quantification MeHg were 0.86 and 2.85 pg/L, respectively. This method was applied to measure MeHg in shark meat from Binuangeun areas. The MeHg concentration in Rhizoprionodon acutus was 0.22–0.63 mg/kg wet weight (w.w.), Squalus hemipinis 0.68–1.14 mg/kg w.w., and 0.29–1.22 mg/kg w.w. for Sphyrna lewini. This study provides a quick and easy method to evaluate MeHg in shark meat or other seafood products and applies to many samples in a single assay.


UHPLC-ICP-MS; methylmercury; sonication-assisted extraction; shark meat

Full Text:

Full Text PDF


[1] Nalluri, D., Baumann, Z., Abercrombie, D.L., Chapman, D.D., Hammerschmidt, C.R., and Fisher, N.S., 2014, Methylmercury in dried shark fins and shark fin soup from American restaurants, Sci. Total Environ., 496, 644–648.

[2] Brombach, C.C., Manorut, P., Kolambage-Dona, P.P.P., Ezzeldin, M.F., Chen, B., Corns, W.T., Feldmann, J., and Krupp, E.M., 2017, Methylmercury varies more than one order of magnitude in commercial European rice, Food Chem., 214, 360–365.

[3] Karimi, R., Silbernagel, S., Fisher, N.S., and Meliker, J.R., 2014, Elevated blood Hg at recommended seafood consumption rates in adult seafood consumers, Int. J. Hyg. Environ. Health, 217 (7), 758–764.

[4] Huang, X., Liu, Z., Xie, Z., Dupont, S., Huang, W., Wu, F., Kong, H., Liu, L., Sui, Y., Lin, D., Lu, W., Hu, M., and Wang, Y., 2018, Oxidative stress induced by titanium dioxide nanoparticles increases under seawater acidification in the thick shell mussel Mytilus coruscus, Mar. Environ. Res., 137, 49–59.

[5] Nogara, P.A., Madabeni, A., Bortoli, M., Teixeira Rocha, J.B., and Orian, L., 2021, Methylmercury can facilitate the formation of dehydroalanine in selenoenzymes: Insight from DFT molecular modeling, Chem. Res. Toxicol., 34 (6), 1655–1663.

[6] Man, Y.B., Wu, S.C., and Wong, M.H., 2014, Shark fin, a symbol of wealth and good fortune may pose health risks: the case of mercury, Environ. Geochem. Health, 36 (6), 1015–1027.

[7] Yu, X., Khan, S., Khan, A., Tang, Y., Nunes, L.M., Yan, J., Ye, X., and Li, G., 2020, Methyl mercury concentrations in seafood collected from Zhoushan Islands, Zhejiang, China, and their potential health risk for the fishing community: Capsule: Methyl mercury in seafood causes potential health risk, Environ. Int., 137, 105420.

[8] Kim, T.H., Cho, M.J., Lee, Y., Kim, J.H., Hwang, J.Y., Lee, H.E., Kim, S.H., Choi, J.D., and Kang, G.J., 2020, Methylmercury determination in fish by direct mercury analyzer, J. AOAC Int., 103 (1), 244–249.

[9] de Souza, S.S., Rodrigues, J.L., de Oliveira Souza, V.C., and Barbosa, F., 2010, A fast sample preparation procedure for mercury speciation in hair samples by high-performance liquid chromatography coupled to ICP-MS, J. Anal. At. Spectrom., 25 (1), 79–83.

[10] Liu, H., Luo, J., Ding, T., Gu, S., Yang, S., and Yang, M., 2018, Speciation analysis of trace mercury in sea cucumber species of Apostichopus japonicus using high-performance liquid chromatography conjunction with inductively coupled plasma mass spectrometry, Biol. Trace Elem. Res., 186 (2), 554–561.

[11] Anual, Z.F., Maher, W., Krikowa, F., Hakim, L., Ahmad, N.I., and Foster, S., 2018, Mercury and risk assessment from consumption of crustaceans, cephalopods and fish from West Peninsular Malaysia, Microchem. J., 140, 214–221.

[12] Rodrigues, J.L., de Souza, S.S., de Oliveira Souza, V.C., and Barbosa, F., 2010, Methylmercury and inorganic mercury determination in blood by using liquid chromatography with inductively coupled plasma mass spectrometry and a fast sample preparation procedure, Talanta, 80 (3), 1158–1163.

[13] Vallant, B., Kadnar, R., and Goessler, W., 2007, Development of a new HPLC method for the determination of inorganic and methylmercury in biological samples with ICP-MS detection, J. Anal. At. Spectrom., 22 (3), 322–325.

[14] Wenzl, T., Haedrich, J., Schaechtele, A., Robouch, P., and Stroka, J., 2016, Guidance Document on the Estimation of LOD and LOQ for Measurements in the Field of Contaminants in Feed and Food, EUR 28099, Publications Office of the European Union, Luxembourg.

[15] R Core Team, 2021, R: A Language and Environment for Statistical Computing, R Foundation for Statistical Computing, Viena, Austria.

[16] de Souza, S.S., Campiglia, A.D., and Barbosa, F., 2013, A simple method for methylmercury, inorganic mercury and ethylmercury determination in plasma samples by high performance liquid chromatography-cold-vapor-inductively coupled plasma mass spectrometry, Anal. Chim. Acta, 761, 11–17.

[17] Reyes, L.H., Mizanur Rahman, G.M., Fahrenholz, T., and Skip Kingston, H.M., 2008, Comparison of methods with respect to efficiencies, recoveries, and quantitation of mercury species interconversions in food demonstrated using tuna fish, Anal. Bioanal. Chem., 390 (8), 2123–2132.

[18] Mohammed, A., and Mohammed, T., 2017, Mercury, arsenic, cadmium and lead in two commercial shark species (Sphyrna lewini and Caraharinus porosus) in Trinidad and Tobago, Mar. Pollut. Bull., 119 (2), 214–218.

[19] Bergés-Tiznado, M.E., Márquez-Farías, F., Lara-Mendoza, R.E., Torres-Rojas, Y.E., Galván-Magaña, F., Bojórquez-Leyva, H., and Páez-Osuna, F., 2015, Mercury and selenium in muscle and target organs of scalloped hammerhead sharks Sphyrna lewini of the se gulf of California: Dietary intake, molar ratios, loads, and human health risks, Arch. Environ. Contam. Toxicol., 69 (4), 440–452.

[20] Kim, S.J., Lee, H.K., Badejo, A.C., Lee, W.C., and Moon, H.B., 2016, Species-specific accumulation of methyl and total mercury in sharks from offshore and coastal waters of Korea, Mar. Pollut. Bull., 102, 210–215.

[21] Hauser-Davis, R.A., Pereira, C.F., Pinto, F., Torres, J.P.M., Malm, O., and Vianna, M., 2020, Mercury contamination in the recently described Brazilian white-tail dogfish Squalus albicaudus (Squalidae, Chondrichthyes), Chemosphere, 250, 126228.

[22] Elsayed, H., Yigiterhan, O., Al-Ansari, E.M.A.S., Al-Ashwel, A.A., Elezz, A.A., and Al-Maslamani, I.A., 2020, Methylmercury bioaccumulation among different food chain levels in the EEZ of Qatar (Arabian Gulf), Reg. Stud. Mar. Sci., 37, 101334.

[23] Wosnick, N., Niella, Y., Hammerschlag, N., Chaves, A.P., Hauser-Davis, R.A., da Rocha, R.C.C., Jorge, M.B., de Oliveira, R.W.S., and Nunes, J.L.S., 2021, Negative metal bioaccumulation impacts on systemic shark health and homeostatic balance, Mar. Pollut. Bull., 168, 112398.

[24] Teffer, A.K., Staudinger, M.D., Taylor, D.L., and Juanes, F., 2014, Trophic influences on mercury accumulation in top pelagic predators from offshore New England waters of the northwest Atlantic Ocean, Mar. Environ. Res., 101, 124–134.

[25] Lyons, K., and Lowe, C.G., 2013, Mechanisms of maternal transfer of organochlorine contaminants and mercury in the common thresher shark (Alopias vulpinus), Can. J. Fish. Aquat. Sci., 70 (12), 1667–1672.


Article Metrics

Abstract views : 2251 | views : 928

Copyright (c) 2023 Indonesian Journal of Chemistry

Creative Commons License
This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.


Indonesian Journal of Chemistry (ISSN 1411-9420 /e-ISSN 2460-1578) - Chemistry Department, Universitas Gadjah Mada, Indonesia.

Analytics View The Statistics of Indones. J. Chem.