• 분석과학
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• 제16권2호
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• pp.134-142
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• 2003

LC-ICP-MS를 이용한 어류중 비소의 종분화 분석을 위해 microwave-assisted extraction과 sonication extraction 방법을 비교하였다. Ultrasonic nebulizer와 cross flow nebulizer를 사용한 비소종들의 검출한계는 유사한 결과를 보였다. 분석된 비소 종들은 arsenobetaine (AsB), arsenite [As(III)], dimethylarsine acid (DMA), monomethylarsonic acid (MMA), arsenate [As(v)] 와 phenylarsonic acid (PAA) 이다. 두 가지 방법은 NRCC (National Research Council of Canada)의 표준물질인 DORM-2를 50% 메탄올로 추출하였다. arsenobetaine의 경우, 두 방법 모두 5% 이하의 상대표준편차와 82% 이상의 추출효율을 보였다. Arsenobetaine은 microwave assisted extraction 방법에서 $14.18{\pm}0.42mg\;kg^{-1}$을 보였고 sonication extraction 방법에서는 $13.54 {\pm}0.84mg\;kg^{-1}$을 보였다. dimethylarsine acid (DMA)의 경우 각각 $0.45{\pm}0.06mg\;kg^{-1}$과 $0.44{\pm}0.06mg\;kg^{-1}$를 보였다.

• Bulletin of the Korean Chemical Society
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• 제35권3호
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• pp.821-827
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• 2014

An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

• Toxicological Research
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• 제24권3호
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• pp.219-225
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• 2008

A screening study of the acute toxicity of organic arsenics such as arsenobetaine and arsenocholine, a product of arsenic methylation metabolite, and inorganic arsenic was carried out to examine hematological and serum biochemical parameters in cynomolgus monkeys(Macaca fascicularis). We found soft and liquid feces, and vomiting in all treated groups with inorganic and organic arsenics. The monkeys in inorganic arsenic-treated group showed a significant increase in vomiting frequency compared with those in three organic arsenics-treated groups. These results suggest that inorganic arsenic might be more toxic than three other organic arsenics tested. The monkeys in inorganic arsenic-treated group showed a decrease in platelet and an increase in monocyte on day 4 and the monkeys in arsenocholine-treated group showed an increase in reticulocyte percentage on day 8. The monkeys in inorganic-treated group also showed decreases in AST and ALT values and the monkeys in arsenobetaine-treated group showed a decrease in AST value and an increase in T-CHO value. However, these hematological and biochemical changes were within the physiological ranges, showing that the single dose of inorganic and organic arsenics did not affect at least hematological and serum biochemical parameters. The present study of toxicity with single dose of arsenics provides valuable indicators for longer term study of toxicity of repeated doses of arsenics in primates.

• 한국환경보건학회지
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• 제42권3호
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• pp.224-233
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• 2016

Objectives: The purpose of this study was to evaluate the relationship between residential surroundings, such as a power plant, steel mill and petrochemical facilities, and urinary arsenic concentrations in Chungcheongnam-do Province, Korea. Methods: Stratified by fish consumption and residential district, median and maximum block sampling was applied. A total of 346 spot urine samples were speciated for $As^{5+}$, $As^{3+}$, monomethylarsonic acid(MMA), dimethylarsonic acid (DMA) and arsenobetaine (AsB). Exposure assessment was based on questionnaires including data on sex, age, current tobacco use, fish consumption, type of water consumed, and occupational category. Results: Urinary $As^{5+}+As^{3+}+MMA+DMA$ concentrations of people living in the vicinity of a power plant ($GM=50.39{\mu}g/g$) were 61% higher than those of people living in the inland area according to median block sampling. Urinary $As^{5+}+As^{3+}+MMA+DMA+AsB$ concentrations of people living in the vicinity of industrial complex area were higher than those of people living in the inland area according to block sampling by median and maximum. Conclusion: Urinary arsenic concentrations of people living in vulnerable areas such as around industrial complexes, especially power plants, were higher than those of people living in an inland area.

• Environmental Analysis Health and Toxicology
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• 제29권
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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.

• 한국식품위생안전성학회지
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• 제37권6호
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• pp.385-393
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• 2022

본 연구는 유통 중인 곡류 87건 및 그 가공식품 66건을 대상으로 발암물질인 무기비소의 오염도를 조사하였다. 높은 분리능과 감도를 가진 HPLC-ICP/MS를 이용하여 무기비소 As(III), As(V) 및 유기비소 MMA, DMA, AsB, AsC를 분석했으며, ICP/MS로 총비소를 정량하였다. 모든 곡류에서 무기비소가 검출되었으며, 곡류의 총비소는 약 70-85%의 무기비소와 약 10-20%의 DMA로 구성되었다. 곡류 분석 결과, 담수재배 종인 쌀과 흑미에서 높았고, 밭재배 잡곡은 오염도가 낮았다. 쌀의 평균 무기비소 농도는 쌀눈 0.160 mg/kg, 현미 0.135 mg/kg, 백미 0.083 mg/kg으로 외피에 비소가 많은 것으로 조사되었다. 곡류 가공식품은 원재료의 종류와 함량에 따라 무기비소 농도가 달랐으며, 현미와 쌀눈 가공 제품에서 검출량이 많았다. 모든 시료는 기준규격을 초과하지 않았지만, 섭취 빈도가 높으므로 식품 안전을 위해 지속적인 모니터링이 필요할 것으로 판단된다.