• Analytical Science and Technology
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• v.19 no.3
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• pp.203-210
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• 2006

The determination of trace selenium in milk powder has been studied by octopole reaction cell(ORC)-ICP-MS. The interferences by polyatomic ions and other concomitant molecular species could be removed remarkably by using $H_2$ as reaction gas in ORC. Compared to the normal mode (no cell gas), the $H_2$ cell gas mode improved the accuracy and precision. The quantitative result was average 102.7% and it was slightly higher than certified standard value of milk powder and the RSD was 7.6%.

• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3817-3824
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• 2013

Various separation modes in HPLC, such as anion exchange (AE), reversed-phase (RP), and affinity (AF) chromatography were examined for the separation of selenium species in human blood serum and urine. While RP- and AE-HPLC were mainly used for the separation of small molecular selenium species, double column AF-HPLC achieved the separation of selenoproteins in blood serum efficiently. Further, the effluent of AF-HPLC was enzymatically hydrolyzed and then analyzed with RP HPLC for selenoamino acid study. The versatility of the hybrid technique makes the in-depth study of selenium species possible. For quantification, post column isotope dilution (ID) with $^{78}Se$ spike was performed. ORC ICP/MS (octapole reaction cell inductively coupled plasma/mass spectrometry) was used with 4 mL $min^{-1}$ Hydrogen as reaction gas. In urine sample, inorganic selenium and SeCys were identified. In blood serum, selenoproteins GPx, SelP and SeAlb were detected and quantified. The concentration for GPx, SelP and SeAlb was $22.8{\pm}3.4\;ng\;g^{-1}$, $45.2{\pm}1.7\;ng\;g^{-1}$, and $16.1{\pm}2.2\;ng\;g^{-1}$, respectively when $^{80}Se/^{78}Se$ was used. The sum of these selenoproteins ($84.1{\pm}4.4\;ng\;g^{-1}$) agrees well with the total selenium concentration measured with the ID method of $87.0{\pm}3.0\;ng\;g^{-1}$. Enzymatic hydrolysis of each selenium proteins revealed that SeCys is the major amino acid for all three proteins and SeMet is contained in SeAlb only.

• 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.