The
Malaysian Journal of Analytical Sciences Vol 16 No 2 (2012): 134 – 141
DETERMINATION OF ORGANIC AND INORGANIC MERCURY
SPECIES IN SUNGAI KINTA, PERAK BY REVERSED-PHASE HIGH PERFORMANCE LIQUID
CHROMATOGRAPHY (HPLC) ON-LINE COUPLED WITH ICP-MS
(Penentuan
Kandungan Spesis Raksa Organik dan Bukan Organik di Sungai Kinta, Perak Melalui
Kaedah HPLC-ICP-MS)
Norshidah
Baharuddin 1*, Norashikin Saim 2, Rozita Osman 2,
Sharifuddin Md. Zain 3,
Hafizan Juahir 4,
Siti Rafzah Saari 1
1Sirim
Berhad, 40911 Shah Alam, Selangor, Malaysia
2Faculty
of Applied Sciences,
Universiti Teknologi MARA, 40450 Shah Alam,
Selangor, Malaysia
3Department
of Chemistry, Faculty of Science,
Universiti Malaya, 56000 Kuala Lumpur, Malaysia
4Department
of Environmental Sciences, Faculty of Environmental Study,
Universiti Putra Malaysia, 43400 Serdang, Selangor,
Malaysia
*Corresponding author: shidah@sirim.my
Abstract
This paper describes a simple
method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and
measurement were done by high-performance liquid chromatography on-line with
inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Separation of mercury species was accomplished within 6
minutes on an AQ C18 4.6mm i.d x 150mm, 5µm reversed phase column with 0.1%
(w/v) L-cysteine as mobile phase. Under the
optimum instrumental conditions, recoveries of 101-104% for MeHg+ and
96 – 104% for Hg2+ were obtained with experimental
detection limits of 1ngL-1 for inorganic mercury and 1.5µgL-1
for organic mercury.
Keywords:
HPLC/ICP-MS, reversed phase,
L-cysteine, mobile phase
References
1.
Lan-Fang C., Shiuh-Jen J., and
Sahayam A.C. (2007). “Speciation analysis of mercury and lead in fish samples
using liquid chromatography–inductively coupled plasma mass spectrometry.” Journal of Chromatography A. 1176. 143–148.
2.
Jianguo, C., Hengwu C., Xianzhong
J., and Haiting C. (2009). “Determination of ultra-trace amount methyl-,
phenyl- and inorganic mercury in environmental and biological samples by liquid
chromatography with inductively coupled plasma mass spectrometry after cloud
point extraction preconcentration.” Talanta.
77. 1381–1387.
3.
Castillo, A., Roig-Navarro A.F.,
and Pozo O.J. (2006). “Method optimization for the determination of four
mercury species by micro-liquid chromatography–inductively coupled plasma mass
spectrometry coupling in environmental water samples.” Analytica Chimica Acta. 577.
18–25.
4.
Cairns, W.R.L., Ranaldo M., Hennebelle R., Turetta
C., Capodaglio G., Ferrari C.F., Aur´elien D., Cescon P., and Barbante C. (2008 ). “Speciation
analysis of mercury in seawater from the lagoon of Venice by on-line
pre-concentration HPLC–ICP-MS.” Analytica Chimica Acta. 622. 62–69.
5.
Susan, C. Hight, and
John C. (2006). “Determination of
methylmercury and estimation of total mercury in seafood using high performance
liquid chromatography (HPLC) and inductively coupled plasma-mass spectrometry
(ICP-MS): Method development and validation.” Analytica Chimica Acta. 567.
160–172.
6.
Roberto, M.B., Margarita T.V., Jose
E.S.U, and Alfredo S.M. (2000). “Field sampling, preconcentration and
determination of mercury species in river waters.” Analytica Chimica Acta. 419.
137–144.
7.
José, S.D.S., Miguel de
la G., Augustin, P., Maria, L. PD.S. (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.
8.
Wang, M.F., Weiyue, S.
J, Zhang, F., Wang B., Zhu M., Li B. Z. Y., Chai, Z. (2007). “Development of a
mild mercaptoethanol extraction method for determination of mercury species in
biological samples by HPLC–ICP-MS.” Talanta.
71. 2034–2039.
9.
Cattani, I., Spalla,
S., Beone, G.M., Del Re., A.A.M., Boccelli, R., Trevisan, M. (2008). “Characterization
of mercury species in soils by HPLC–ICP-MS and measurement of fraction removed
by diffusive gradient in thin films.” Talanta.
74. 1520–1526.
10. María, M.S., Julio, A.L. (2009). “Analytical speciation of
mercury in fish tissues by reversed phase liquid chromatography–inductively
coupled plasma mass spectrometry with Bi3+ as internal standard.”
Talanta. 79. 706–711.
11. Isabel, L., Susana, C., Carmen, C., Yolanda M. (2010).
“Approach for rapid extraction and speciation of mercury using a microtip
ultrasonic probe followed by LC–ICP-MS.” Talanta,
82. 594–599.
12. Chwei-Sheng, C., Shiuh-Jen, J., Danadurai K. S.K. (2001).
“Determination of mercury compounds in fish by microwave-assisted extraction
and liquid chromatography-vapor generation-inductively coupled plasma mass
spectrometry.” Spectrochimica Acta Part
B. 56. 1133-1142.
13. Haiting, C., Jianguo, C., Xianzhong, J., Danyi,
W. (2009). “Determination of trace
mercury species by high performance liquid chromatography–inductively coupled
plasma mass spectrometry after cloud point extraction.” Journal of Hazardous Materials. 172. 1282–1287.
14. Yong-guang, Y., Ming, C., Jin-feng, P.,
Jing-fu, L., Gui-bin, J. (2010). “Dithizone-functionalized solid phase
extraction–displacement elution-high performance liquid
chromatography–inductively coupled plasma mass spectrometry for mercury
speciation in water samples.” Talanta. 81.
1788–1792.
15. Jairo, L. R., Samuel, S. de. S., Vanessa, C. de. O.S.,
Fernando, B. Jr. (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. 1158–1163.
16. Xiaoyu, J, Yi H., Xinli L., Taicheng, D.
H.Chen. (2010). “Speciation of mercury in water samples by dispersive
liquid-liquid microextraction combined with high performance liquid
chromatography-inductively coupled plasma mass spectrometry.” Spectrochimica
Acta Part B: Atomic Spectroscopy.
17. Dengyun, C., Miao, J., Xiaoru, W. (2005). “Determination of
Methyl Mercury in Water and Soil by HPLC-ICP-MS.” Agilent Technologies.
18. Martine, L., Willy, B. P. Q., Milena, H. (2005). “Mercury in environmental
samples:Speciation, artifacts and validation.” Trends in Analytical Chemistry. 24. No. 5.
19. Yao-Chin, W. and Chen-Wen, W. (1993). “High-performance liquid
chromatography of inorganic mercury and organomercury with
2-mercaptobenzothiazole.” Journal of Chromatography. 28. 133-137.
20. Kerstin, L.d, Michael, F., Paul, W. (2010). “Methods for the determination and speciation of
mercury in natural waters—A review.” Analytica
Chimica Acta. 663. 127–138.
21. L. –P. Yu., X. –P. Yan (2003). “Factors affecting the stability of inorganic and methylmercury
during sample storage.” Trends in
Analytical Chemistry. 22.
245-253.
22. Quarterly DOE Update on Environment, Development &
Sustainability, Issue 3/2006. Available from http://www.doe.gov.my.
23. Ullrich,
S., Tanton, T. and Abdrashitova, S. (2001). "Mercury in the Aquatic
Environment: A Review of Factors Affecting Methylation". Critical Reviews
in Environmental Science and Technolog.y 31. (3): 241.
24. Winch,
S., Praharaj, T., Fortin, D. and Lean, D.R.S. (2008). “Factors affecting
methylmercury distribution in surficial, acidic, base-metal mine tailings.”
Science of the Total Environment. 392.
242-251.
25. Ebinghaus,
R., Wilken, R.D. and Gisder, P. (1994). “Investigations on the formation of
monomethylmercury (II) in the Elbe.” Vom Wasser. 82. 19-25.