• Bulletin of the Korean Chemical Society
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• v.27 no.6
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• pp.903-908
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• 2006

Various extraction procedures were investigated using reference materials and samples to evaluate extraction efficiency and effectiveness. Inductively coupled plasma mass spectrometry (ICP-MS) was used to measure total arsenic and to quantitate arsenic species when coupled to an HPLC (high pressure liquid chromatography). Arsenic species were extracted from rice flour (NIST SRM 1568a) with water/methanol mixtures using accelerated solvent extraction (ASE). Total arsenic extraction efficiency ranged from 42 to 64%, for water and various methanol concentrations. From spinach (NIST SRM 1570), freeze-dried apple, and rice flour (NIST SRM 1568a), arsenic species were extracted with trifluoroacetic acid (TFA) at 100 ${^{\circ}C}$. Total arsenic extraction efficiency was 90% for spinach, 75% for freeze-dried apple, and 83% for rice flour. Enzymatic extraction with alpha-amylase and sonication resulted in extraction efficiency of 104% for rice flour, 98% for freeze-dried apple, and 7% for spinach. Chromatograms of arsenic species extracted by the optimum extraction methods were obtained, and the species were quantified. Arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were found in the apple sample, and DMA and As(V) in the rice flour sample. As(V) and MMA were found in three herbal dietary supplement samples.

• Journal of Biosystems Engineering
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• v.34 no.5
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• pp.377-381
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• 2009

Excessive presence of heavy metals in environment may contaminate plants and fruits grown in that area. Rapid on-site monitoring of heavy metals can provide useful information to efficiently characterize heavy metal-contaminated sites and minimize the exposure of the contaminated food crops to humans. This study reports on the evaluation of a bismuth-coated glassy carbon electrode for simultaneous determination of cadmium (Cd) and lead (Pb) in a NIST-SRM 1568a rice flour by anodic stripping voltammetry (ASV). The use of a supporting electrolyte 0.1 M $HNO_3$ at a dilution ratio (sample pretreated with acid digestion in a microwave oven: supporting electrolyte) of 1:1 provided well-defined, sharp and separate peaks for Cd and Pb ions, thereby resulting in strongly linear relationships between Cd and Pb concentrations and peak currents measured with the electrode ($R^2\;=\;0.97$, 0.99 for Cd and Pb, respectively). The validation test results for spiked standard solutions with different concentrations of Cd and Pb gave acceptable predictability for both spiked Cd and Pb ions with mean prediction errors of 6 to 30%. However, the applicability of the electrode to the real rice flour sample was limited by the fact that Cd concentrations spiked in the rice flour sample were overly estimated with relatively high variations even though Pb ion could be quantitatively measured with the electrode.

• Analytical Science and Technology
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• v.29 no.4
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• pp.170-178
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• 2016

Accuracy and precision of ID methods for different spike isotopes of ⁷⁶Se, ⁷⁷Se, and ⁷⁸Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and ⁷⁸Se showed was a bit better than ⁷⁶Se and ⁷⁷Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for ⁷⁸Se, ⁷⁶Se and ⁷⁷Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of ⁷⁸Se isotope spike (over 100 % RSD). ⁷⁶Se and ⁷⁷Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, ⁷⁸Se should be avoided when large amount of Br exists in matrix. Either ⁷⁶Se or ⁷⁷Se would provide accurate results.