scholarly journals Optimization of a Digestion Method to Determine Total Mercury in Fish Tissue by Cold Vapor Atomic Fluorescence Spectrophotometry

2020 ◽  
Vol 3 (2) ◽  
pp. 45
Author(s):  
Gabriela S. Yánez-Jácome ◽  
David Romero-Estévez ◽  
Hugo Navarrete ◽  
Karina Simbaña-Farinango ◽  
Pamela Y Vélez-Terreros

Several microwave-assisted digestion methods were tested at the Centro de Estudios Aplicados en Química laboratory in Quito, Ecuador, to determine the accuracy and performance efficiency of the mineralization process for the determination of total mercury in fish tissue by cold vapor atomic fluorescence spectrophotometry. The use of MARSEasyPrep high-pressure vessels, low amounts of reagents (1 cm3 HNO3, 1 cm3 H2O2, and 1 cm3 HClO4), an irradiation temperature of 210 °C, and 35 min of mineralization time resulted in accurate performance, with recoveries of certified reference material DORM-4 between 90.1% and 105.8%. This is better than the Association of Official Analytical Chemists 2015.01 method, which has a reported accuracy of 81%. The repeatability precision and intermediate precision were established at three concentration levels (0.167, 0.500, and 0.833 mg·kg−1) and expressed as the percentage of the relative standard deviation ranging from 1.5% to 3.0% and 1.7% to 4.2%, respectively. Further, the method was satisfactorily applied to analyze fortified samples of tilapia (Oreochromis niloticus), with recoveries ranging from 98.3% to 104.3%. The instrumental limits of detection and quantification were 0.118 µg·dm−3 and 0.394 µg·dm−3, respectively.

1992 ◽  
Vol 49 (5) ◽  
pp. 1010-1017 ◽  
Author(s):  
Nicolas S. Bloom

Total mercury, monomethylmercury (CH3Hg), and dimethylmercury ((CH3)2Hg) in edible muscle were examined in 229 samples, representing seven freshwater and eight saltwater fish species and several species of marine invertebrates using ultraclean techniques. Total mercury was determined by hot HNO3/H2SO4/BrClldigestion, SnCl2 reduction, purging onto gold, and analysis by cold vapor atomic fluorescence spectrometry (CVAFS). Methylmercury was determined by KOH/methanol digestion using aqueous phase ethylation, cryogenic gas chromatography, and CVAFS detection. Total mercury and CH3Hg concentrations varied from 0.011 to 2.78 μg∙g−1 (wet weight basis, as Hg) for all samples, while no sample contained detectable (CH3)2Hg (<0.001 μg∙g−1 as Hg). The observed proportion of total mercury (as CH3Hg) ranged from 69 to 132%, with a relative standard deviation for quintuplicate analysis of about 10%; nearly all of this variability can be explained by the analytical variability of total mercury and CH3Hg. Poorly homogenized samples showed greater variability, primarily because total mercury and CH3Hg were measured on separate aliquots, which vary in mercury concentration, not speciation. I conclude that for all species studied, virtually ail (>95%) of the mercury present is as CH3Hg and that past reports of substantially lower CH3Hg fractions may have been biased by analytical and homogeneity variability.


1972 ◽  
Vol 55 (3) ◽  
pp. 583-589 ◽  
Author(s):  
J F Uthe ◽  
J Solomon ◽  
B Grift

Abstract A fast semimicro method for the determination of methyl mercury in fish tissue is described. The procedure involves extracting the methyl mercury into toluene as methyl mercuric bromide, partitioning the bromide into aqueous ethanol as a thiosulfate complex, and re-extracting into benzene as methyl mercuric iodide. Methyl mercury is quantitated with gas chromatography. The method is sensitive to 0.01 ppm. Recoveries of added methyl mercury were 99% and the presence of methyl mercury in the final extract was shown by thin layer chromatography and gas chromatography of the thin layer spot. A variety of mercurial compounds do not interfere in the analyses. The amounts of both methyl and total mercury found in a variety of tissues of aquatic animals are compared. The presence of a demethylase in seal is suggested by the findings of high levels of nonmethyl mercury. Additional cleanup by column chromatography on Florisil was necessary with certain samples. The gas chromatographic columns were kept operational by the intermittent injection of 3M potassium iodide. Due to column bleed and resulting detector contamination, the use of the easily cleaned concentric tube electron capture detector is recommended.


1994 ◽  
Vol 40 (2) ◽  
pp. 206-210 ◽  
Author(s):  
S A Winfield ◽  
N D Boyd ◽  
M J Vimy ◽  
F L Lorscheider

Abstract An ultrasensitive method for determining total mercury concentrations in biological specimens is a prerequisite for monitoring exposure to chronic low-dose levels of Hg vapor such as those from dental silver amalgam fillings. The clinical consequences of such doses are currently in question. We describe an adaptation of a two-stage gold amalgamation preconcentration step combined with cold vapor atomic fluorescence spectrometric detection for Hg. At Hg concentrations of 40 and 350 nmol/L, the within-day assay CVs were 5% and 3%, respectively; between-day assay CVs were 8% and 5%, respectively. Accuracy, as demonstrated by analytical recovery, ranged from 98% to 105%. The detection limit for the assay is 50 pmol/L, which is suitable for measuring total Hg concentrations in specimens of human urine, blood, and breast milk, and in monkey kidney cortex and feces, obtained from subjects with and without amalgam fillings.


2016 ◽  
Vol 24 (3) ◽  
pp. 294-300 ◽  
Author(s):  
Nathália Santos Serrão de Castro ◽  
Camila Margalho Braga ◽  
Paulo Arthur de Abreu Trindade ◽  
Tommaso Giarrizzo ◽  
Marcelo de Oliveira Lima

Abstract Core subject To quantify the Hg content of sediment and fish collected along the Purus River (Acre State, Amazon) in order to identify if those samples could be a potential route of Hg exposure to the population of Manoel Urbano (a riverside community). Methods The total mercury (THg) was quantified using the Cold Vapor Atomic Absorption technique. Results We collected 06 samples of sediment and 264 samples of fish. The Hg in sediments ranged between 0.038 and 0.065 µg.g–1.The results indicate that sediment is in agreement with “uncontaminated” Amazonian rivers. The carnivorous species presented the highest level of Hg on muscle (mean 0.927 μg/g–1), followed by piscivorous (mean 0.873 μg.g–1), planktophagus (mean 0.566 μg.g–1), omnivorous (mean 0.533 μg.g–1) and detritivorous (mean 0.176 μg/g–1). Fourty four percent (44%) of the total species collected presented mean levels of THg on muscle, a percentage greater than the threshold recommended by WHO. Conclusion Some species may be a route for Hg exposure. The sediment is within the normality. The authors suggest that other factors, such as culture and society, should be considered for future researches in order to promote the population healths.


2005 ◽  
Vol 68 (4) ◽  
pp. 879-881 ◽  
Author(s):  
J. A. LASRADO ◽  
C. R. SANTERRE ◽  
S. M. SHIM ◽  
J. R. STAHL

Sportfish samples (n = 133) that originated from Indiana waters were analyzed for total mercury using inductively coupled plasma/mass spectrometry (ICP/MS) and thermal decomposition, amalgamation/atomic absorption spectrophotometry (TDA/AAS). Total mercury concentrations obtained by the two methods were not significantly different (P &gt; 0.05). The correlation coefficient for total mercury obtained for the two methods was 0.94. The limit of detection using TDA/AAS was 0.1 ppm. TDA/AAS is a preferred technique for the analysis of total mercury in fish tissue because it is rapid (6 min per sample) and easy to use and requires little sample preparation.


1983 ◽  
Vol 16 (15) ◽  
pp. 1187-1195 ◽  
Author(s):  
Hideyoshi Morita ◽  
Tetsuya Kimoto ◽  
Shigeru Shimomura

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