• Environmental Analysis Health and Toxicology
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• v.29
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• pp.18.1-18.9
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• 2014

Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.

• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.420-426
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• 2019

Selenoproteins,in Korean blood serum, GPx, SelP, and SeAlb were separated and determined with the use of HPLC-ICP/MS. Deuterium was used as a collision gas and affinity column with ammonium formate was used as an eluting solvent for the accurate quantitation of selenoproteins in human blood serum. Certified reference material BCR 639 (133±12 ng g^-1) was tested for the accuracy and the result was satisfactory 130±6 ng g^-1. Blood serum for the rectal cancer and controlled groups were collected and analyzed to give 84±27 ng g^-1, and 119±28 ng g^-1, respectively. The difference was statistically obvious when t-test was performed (t_cal 4.93 > t_95% 2.04). The decrease for cancer group was more obvious for female and aged group. The distributions of three selenoproteins were similar with each other, which means rectal cancer group did not show any specificity for any selenoproteins. As cancer developed, GPx showed a slight decrease but not obvious while the total concentration was increasing particularly at the second stage of cancer.

• Korean Journal of Environmental Agriculture
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• v.36 no.2
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• pp.119-128
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• 2017

BACKGROUND: Miscellaneous cereal have been largely consumed in Korea as due to their physiological functions beneficial to human health. The cereals are currently a social concern because they have been found to contain heavy metals. Thus, monitoring heavy metals in the cereals is an important requirement for food safety analysis. In this study, we determined arsenic concentration in the cereals randomly harvested from different markets. METHODS AND RESULTS: Inorganic arsenic was determined by ICP-MS coupled with HPLC system. The HPLC-ICP-MS analysis was optimized based on the limit of detection and recover test to reach $0.13-1.24{\mu}g/kg$ and 94.3-102.1%, respectively. The concentrations of inorganic arsenic equivalent to daily exposure were levels of $19.91{\mu}g/day$ in mixed grain, $1.07{\mu}g/day$ in glutinous rice, $0.77{\mu}g/day$ in black brown rice, $0.13{\mu}g/day$ in barley and $0.11{\mu}g/day$ in soybeans. CONCLUSION: The levels of arsenic in miscellaneous cereals were found lower than the recommended The Joint FAO/WHO Expert Committee on Food Additives (JECFA) levels, suggesting that the cereals marketed in Korea are not potential concern in risk assessment.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.291-301
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• 2018

BACKGROUND: Rice is one of the main sources for inorganic arsenic among the consumed crops in the world population's diet. Arsenic is classified into Group 1 as it is carcinogenic for humans, according to the IARC. This study was carried out to assess dietary exposure risk of inorganic arsenic in husked rice and polished rice to the Korean population health. METHODS AND RESULTS: Total arsenic was determined using microwave device and ICP-MS. Inorganic arsenic was determined by ICP-MS coupled with HPLC system. The HPLC-ICP-MS analysis was optimized based on the limit of detection, limit of quantitation, and recovery ratio to be $0.73-1.24{\mu}g/kg$, $2.41-4.09{\mu}g/kg$, and 96.5-98.9%, respectively. The inorganic arsenic concentrations of daily exposure (included in body weight) were $4.97{\times}10^{-3}$ (${\geq}20$ years old) $-1.36{\times}10^{-2}$ (${\leq}2$ years old) ${\mu}g/kg\;b.w./day$ (PTWI 0.23-0.63%) by the husked rice, and $1.39{\times}10^{-1}$ (${\geq}20$ years old) $-3.21{\times}10^{-1}$ (${\leq}2$ years old) ${\mu}g/kg\;b.w./day$ (PTWI 6.47-15.00%) by the polished rice. CONCLUSION: The levels of overall exposure to total and inorganic arsenic by the husked and polished rice were far lower than the recommended levels of The Joint FAO/WHO Expert Committee on Food Additives (JECFA), indicating of little possibility of risk.

• Bulletin of Food Technology
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• v.22 no.1
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• pp.21-28
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• 2009

• Journal of the Korean Chemical Society
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• v.48 no.2
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• pp.203-206
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• 2004

• Journal of Korean Society of Environmental Engineers
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• v.30 no.6
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• pp.621-627
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• 2008

In this study, a technique of speciation and determination of the trace inorganic arsenic(As(III) and As(V)) in water sample using HPLC-DRC-ICP-MS has been developed. Isocratic mobile phase of 10 mM ammonium nitrate and 10 mM ammonium phosphate monobasic was used and methanol(5 v/v%) was used as flushing solvent. Selection of the best flow rate of reaction gas, O$_2$, and optimization of the parameters such as pH and flow rate of mobile phase, and injection volume of sample for the separation and detection of arsenic species were carried out. The oxygen flow rate of 0.5 mL/min, pH of 9.4 and flow rate of 1.5 mL/min of mobile phase, and injection volume of sample of 100 $\mu$L were found to be the best parameters for the speciation and determination of arsenic species. The analytical features of the method were detection limit 0.10 and 0.08 $\mu$g/L, precision(RSD) 4.3% and 3.6%, and recovery 95.2% and 96.4% for As(III) and As(V), respectively. Analysis time was 4 minutes per sample. Linear calibration graphs with r$^2$ = 0.998 were obtained for both As(III) and As(V). Speciation analysis of arsenic species in the raw water samples collected from the tributary streams to Han River and main stream of Paldnag were performed by the proposed method. The concentrations of As(III) ranged from 0.10 to 0.22 $\mu$g/L and As(V) concentrations ranged from 0.44 to 1.19 $\mu$g/L, and 93.5% of total arsenic was found to be As(V).

• Analytical Science and Technology
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• v.26 no.3
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• pp.182-189
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• 2013

The purpose of this research is to separate and quantitate selenium species in some food samples with HPLC-ICP-MS. Cation exchange chromatography showed efficient separation only for inorganic Se species while reversed phase ion pair chromatography showed good separation for both inorganic and organic Se species. $C_8$ column ($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm) was used with optimum condition of 5% methanol mobile phase, 0.05% of nonafluorovaleric acid ion pairing reagent. Five standard Se species of Se(IV), Se(VI), SeCys(selenocystein), SeMet(selenomethionine) and Se-M-C(seleno methyl cystein) were separated successfully under the optimum condition (mobile phase; 5% methanol, ion-pairing reagent; 0.05% nonafluorovaleric acid, flow rate; 0.9 mL $min^{-1}$). To extract Se species, microwave assisted and enzyme-assisted extraction methods were studied. In enzyme-assisted extraction method, protease I for garlic, protease I plus trypsin for pork and mackerel, and protease XIV for tuna showed the best extraction efficiency. With the optimum condition for each sample, it was found that mostly inorganic Se, SeCys and SeMet are present in the sample studied ranging from few ${\mu}g$ $g^{-1}$ to few tens of ${\mu}g$ $g^{-1}$.

• Journal of the Korean Chemical Society
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• v.62 no.4
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• pp.319-323
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• 2018

• Journal of the Korean Chemical Society
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• v.63 no.5
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• pp.335-341
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• 2019

Spirulina was cultured in Selenium solution and the total concentration was determined with isotope dilution technique. Low-molecular-weight-Selenium species for the water extract of Spirulina were separated and quantified with HPLC ICP/MS. Water extraction was used first and then protein enzyme (protease XIV) was used to digest and extract for the Se species in both water extract and residue. The total Se was $414.9{\pm}4.0{\mu}g\;g^{-1}$ and 77% existed in water extract while 22% remained in residue. Se species in supernatant was mostly inorganic selenate ($222.7{\mu}g\;g^{-1}$). After hydrolysis of protein, SeCys ($15.20{\mu}g\;g^{-1}$) and SeMet ($12.13{\mu}g\;g^{-1}$) were found. In residue, SeCys and SeMet were found with little inorganic Se. After protein hydrolysis of residue, more of Selenoamino acids SeCys ($9.35{\mu}g\;g^{-1}$) and SeMet ($18.23{\mu}g\;g^{-1}$) in addition to MeSeCys ($1.5{\mu}g\;g^{-1}$) were found. It is thought that inorganic selenium is mostly adsorbed on the surface of spirulina and can be easily removed by a simple distilled water extraction while most of organo-seleniums are remained in residue.