• 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 Environmental Health Sciences
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• v.41 no.5
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

• Journal of the Korean Chemical Society
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• v.64 no.4
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• pp.203-209
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• 2020

Selenium species in hair and nails were extracted, separated and analyzed with HPLC-ICP/MS. The result showed that Se species was mostly SeCys and the information related to the change of selenium concentration in a body could be obtained. The Se fortification study was performed for 5 participants during 12 months. The average of Se concentration was 858.6 ± 201.2 ng g^-1, which did not change much during the research period nor the difference between the individuals was striking. In the case of hair, the average concentration was 205.3 ng g^-1 which was lower than nails. Se supplement of 22 ㎍ day^-1 was taken for 3 months by the volunteers and the difference between before and after (3 months period for each) the taking of supplement was not striking. However, when the dose was increased to 300 ㎍ day^-1 for 2 months, the concentration was increased noticeably to 1,230 ng g^-1. It can be thought that the analysis of finger nail for Se can provide valuable information for the long period (several months) of exposure or intake of Se for a human body.

• Journal of the Korean Chemical Society
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• v.63 no.5
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• pp.387-391
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• 2019

• Korean Journal of Environmental Agriculture
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• v.29 no.3
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• pp.266-272
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• 2010

The present study was carried out to assess exposure & risk for Korean by total and inorganic As intake through agricultural products. Total arsenic analysis was performed using microwave device and ICP-MS. 50% MeOH extraction and anion-exchange HPLC-ICP-MS method has been used to determine arsenic species. 329 samples covering 20 kinds of agricultural products were collected from various retail outlets and markets across Korea. The concentration of total As was in the range of 0.001~0.718 mg/kg, while inorganic and organic arsenic species in all samples was not determined. For risk assessment, probable daily intake was calculated and compared with provisional tolerable weekly intake (PTWI, 15 ${\mu}g$/kg b.w./week for inorganic arsenic) established by JECFA. The median daily exposure to total and inorganic As by intake of agricultural products except rice was ranged 0.0002~0.012, 0.0001~0.001 ${\mu}g$/kg b.w./day, corresponding to 0.01~0.5%, 0.002~0.1% of PTWI, respectively. The median level of total and inorganic As intake through rice was 0.603 and 0.041 ${\mu}g$/kg b.w./day, and 28.1% and 1.9% of PTWI, respectively. Therefore, the level of overall exposure to arsenic for Korean through agricultural products was below the recommended JECFA levels, indicating of least possibility of risk.

• Journal of Food Hygiene and Safety
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• v.37 no.6
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• pp.385-393
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• 2022

The contamination level of inorganic arsenic, a human carcinogen, was investigated in 87 grains and 66 processed grain foods. Two inorganic arsenic species arsenite (As(III)) and arsenate (As(V)) and four organic arsenic monomethylarsonic acid, dimethylarsinic acid, arsenobetaine, arsenocholine were analyzed using HPLC-ICP/MS with high separation and sensitivity and ICP/MS was used to quantify total arsenic. Inorganic arsenic was detected in all grains. And the total arsenic in grains consists of about 70-85% inorganic arsenic and about 10-20% DMA. The concentration of inorganic arsenic was high in rice and black rice cultivated in paddy soil with irrigated water, while the miscellaneous grain in field was low. Mean concentration of inorganic arsenic in rice germ, brown rice and polished rice was 0.160 mg/kg, 0.135 mg/kg, 0.083 mg/kg, respectively, indicating that rice bran contains more arsenic. In processed grain foods, inorganic arsenic concentration varied according to the kind of ingredients and content, and the detection amount was high in processed food with brown rice and germ. The arsenic content of all samples did not exceed each standard, but the intake frequency is high and it is considered that continuous monitoring is necessary for food safety.

• Analytical Science and Technology
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• v.36 no.3
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• pp.135-142
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• 2023

The total arsenic and 6 arsenic species were investigated in 56 fish collagen products using ICP-MS (Inductively coupled plasma-mass spectrometer) and HPLC-ICP-MS(High performance liquid chromatography-Inductively coupled plasma-mass spectrometer). The mean concentrations of total arsenic and arsenic species were 40.103±81.133 ㎍/kg (N.D.~586.686) and 30.070±50.378 ㎍/kg (N.D.~313.871), respectively. The mean concentration of inorganic arsenic was 24.610±32.706 ㎍/kg (N.D.~129.331), and the As(V) (Arsenate) was the most dominant. The standards and specifications of arsenic have not been established for fish collagen products. Our study presents that arsenic levels are relatively safe compared with not only previous studies but also domestic and international standards. However, in one sample, the total arsenic concentration was 586.686 ㎍/kg, showing the inorganic was 8.119 ㎍/kg, and the DMA was 305.752 ㎍/kg, which was high than the Canadian standard for organic arsenic. In conclusion, it is necessary to monitor arsenic levels consistently and establish standards and specifications of arsenic in fish collagen products to assure consumer safety.

• Journal of Korean Society of Environmental Engineers
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• v.27 no.6
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• pp.590-598
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• 2005

An adequate method to identify chromium separation, Cr(III) and Cr(VI), in water samples were studied by using High Performance Liquid Chromatography(HPLC) coupled with Inductively Coupled Plasma Mass Spectometer(ICP-MS) equipped with Dynamic Reaction Cell(DRC). The characteristic distribution of Cr(III) and Cr(VI) in the raw water taken at the six water intake stations in Seoul, was analyzed by the method developed by the authors. The chromium species separated by HPLC was isocratically conducted by using tetrabutylammonium phosphate monobasic(1.0 mM TBAP), ethylenediaminetetraacetic acid(0.6 mM EDTA) and 2% v/v methanol as the mobile phase. 5% v/v methanol was used as flushing solvent. A reactive ammonia($NH_3$) gas was used to eliminate the potential interference of $ArC^+$. Several Parameters such as solvent ratio, pH, flow rate and sample injection volume were optimized for the successful separation and reproducibility. Although it has been reported thai the separation sensitivity of Cr(III) is superior to that of Cr(VI), the authors observed Cr(VI) was more sensitive than Cr(III) when ammonia($NH_3$) gas was used as the reaction gas. It took less than 3 minutes to analyze chromium species with this method and the estimated detection limits were $0.061\;{\mu}g/L$ for Cr(III) and $0.052\;{\mu}g/L$, for Cr(VI). According to the results from the analysis on chromium species in the raw water of the six intake stations, the concentrations of Cr(III) ranged from 0.048 to $0.064\;{\mu}g/L$(ave. $0.054\;{\mu}g/L$) while that of Cr(VI) ranged from 0.014 to $0.023\;{\mu}g/L$(ave. $0.019\;{\mu}g/L$). Recovery ratio was very high($90.1{\sim}94.1%$). There were two or three times more Cr(III) than Cr(VI) in the raw water.

• Analytical Science and Technology
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• v.27 no.2
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• pp.92-99
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• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

• Journal of the Korean Chemical Society
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• v.47 no.4
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• pp.363-369
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• 2003

Selenized yeast (Se yeast) containing $0.1{\%}$(w/w) of selenium was obtained when the yeast was incubated at a selenium concentration of 1$1.14{\times}10_-3 M$ in rich medium. After washing several times, the inorganic selenium on the cell wall was confirmed with MBRT. There was no indication of inorganic selenium on the cell wall when the blue color in MBRT was stayed for 15 minutes. The selenized yeast was sonicated, then the selenium contained protein was obtained after salting out by ammonium sulfate at the concentration $80{\%}$ saturation. The seven protein bands were seperated by SDS-PAGE and the selenium concentration in protein was measured by ICP-AES. Analytical data showed that the large expressed protein band contained a relatively large amount of selenium. The proteins of the 47kDa was contained the concentrations of 69.5 ${\mu}$ Se/g of most many content. The protein (47 kDa) was seperated from PVDF membrane by tank-electroblotting. The isolated protein was hydrolyzed under acid condition and reacted with PITC. The derivatives of amino acids were analyzed by HPLC and compared with the data obtained from regular yeast. The resulting selenium-yeast was analyzed with the selenomethionine concentration of $2{\%}$ comparaed with general amino acids. The goal of this study is to analyze the selenium concentration in protein bands and measure the degree of biotransformation of selenomethionine in a specific protein.