• Title/Summary/Keyword: Isotope ratio

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Optimization of Enzyme Digestion Conditions for Quantification of Glycated Hemoglobin Using Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

  • Jeong, Ji-Seon
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.52-56
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    • 2014
  • Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

A Technique to Minimize Impurity Signal from Blank Rhenium Filaments for Highly Accurate TIMS Measurements of Uranium in Ultra-Trace Levels

  • Park, Jong-Ho;Choi, In-Hee;Song, Kyu-Seok
    • Mass Spectrometry Letters
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    • v.1 no.1
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    • pp.17-20
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    • 2010
  • As background significantly affects measurement accuracy and a detection limit in determination of the trace amounts of uranium, it is necessary to minimize the impurities in the filaments used for thermal ionization mass spectrometry (TIMS). We have varied the degassing condition such as the heating currents and duration times to reduce the backgrounds from the filaments prepared with zone-refined rhenium tape. The most efficient degassing condition of the heating current and the duration time was determined as 3.5 A and 60 min, respectively. The TIMS measurement combined with the isotope dilution mass spectrometry (IDMS) technique showed that the uranium backgrounds were determined to be in a few fg level from blank rhenium filaments. The background minimized filaments were utilized to measure the uranium isotope ratios of a U030 (NIST) standard sample. The excellent agreement of the measurement with the certified isotope ratios showed that the degassing procedure optimized in this study efficiently reduced the impurity signals of uranium from blank rhenium filaments to a negligible level.

First GC-IRMS in Korea and Its Application Fields (국내 최초로 도입된 GC-IRMS와 응용분야 소개)

  • Shin, Woo-Jin;Lee, Kwang-Sik;Ko, Kyung-Seok
    • Economic and Environmental Geology
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    • v.40 no.5
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    • pp.699-703
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    • 2007
  • Compound-specific isotope analysis (CSIA) by isotope ratio mass spectrometer (IRMS) interfaced with gas chromatography (GC) is a state of the art analytical technique for stable isotopes in earth sciences, environmental sciences and forensics. Since early 1990s, GC-IRMS has been widely used to investigate the authenticity of food in forensic science and to trace the sources of organic contaminants in environmental science. In Korea, a GC-IRMS was firstly installed at the Korea Basic Science Institute (KBSI) in early 2005. In this study, we introduce the GC-IRMS of the KBSI shortly to stimulate various isotope-related researches of Korea, and report preliminary CSIA results for BTEX of different manufacturers.

Provenance Study on Ancient Lead Glass Relics Using a Lead Isotope Ratio (납동위원소비를 이용한 고대 납유리 유물의 산지추정)

  • Han, Min Su;Kim, So Jin
    • Journal of the Mineralogical Society of Korea
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    • v.28 no.2
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    • pp.187-193
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    • 2015
  • The purpose of the present study is to trace the provenance of lead raw materials using the lead isotope ratio of 9 lead glasses excavated from the Sarira hole of Mireuksaji stone pagoda and to determine correlation between them and other lead glasses excavated from the Wanggungri site. The results of chemical analysis of the 9 lead glasses show that they are common lead glass system($PbO-SiO_2$) with respect to the contents of PbO (70 wt.%) and $SiO_2$ (30 wt.%). The lead isotope ratios of them plot to northern Korean peninsula when applied to the distribution map of lead isotopes of East Asia. On the other hand, southern Korean peninsula is verified as the main deposits of the lead ore in the distribution map of lead isotopes of South Korea. With respect to the results, it is notable that the provenance of the 9 lead glasses can be very different depending on the distribution map. In addition, a comparative study between them and the lead glasses excavated from the Wanggungri which was built in the same region and period shows that their lead isotopes are highly correlated.

Inter-laboratory Comparison of Stable Carbon and Nitrogen Isotopic Composition Data Using Elemental Analyzer-isotope Ratio Mass Spectrometers

  • Kim, Jung-Hyun;Kang, Sujin;Bong, Yeon-Sik;Park, Kwangkyu;Kang, Tae-Woo;Park, Yong-Se;Kim, Dahae;Choi, Seunghyun;Joo, Young Ji;Choi, Bohyung;Nam, Seung-Il;Lee, Sang-Mo;Shin, Kyung-Hoon
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.229-236
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    • 2018
  • In this study, inter-laboratory comparison was done using elemental analyzer-isotope ratio mass spectrometers (EA-IRMSs) to determine carbon and nitrogen contents as well as stable carbon and nitrogen isotopic compositions (${\delta}^{13}C$ and ${\delta}^{15}N$) of five environmental samples containing lake and marine sediments, higher plant leaves, and fish muscle, and one organic analytical standard (Protein (Casein) Standard OAS). Five national laboratories participated in this comparison study, and each laboratory analyzed all five samples and the analytical standard. Results showed that variations in total organic carbon (TOC) and total nitrogen (TN) contents as well as ${\delta}^{13}C_{TOC}$ and ${\delta}^{15}N_{TN}$ values among the laboratories were large compared to the analytical uncertainties. The results highlighted the inhomogeneity of the test samples and thus, the need to select suitable standard reference materials for future inter-laboratory studies. Further inter-laboratory comparison exercises could promote good measurement practices in the acquisition of stable carbon and nitrogen isotopic composition data.

Characteristics of Nitrogen and Carbon Isotopes on Organic Matter and River Sediments of Toil Stream in Yeongju Dam Basin (영주댐 유역 토일천 유입 유기물 및 하천 퇴적물에 대한 질소와 탄소 동위원소 특성 연구)

  • Kang, Han;Song, Hye Won;Kim, Young Hun;Kim, Jeong Jin
    • Economic and Environmental Geology
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    • v.55 no.5
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    • pp.439-445
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    • 2022
  • Organic pollutants that contained in stream sediments have origins of mountain soil in natural and cattle manure in human activity. Nitrogen and carbon isotope analysis for mountain soil, cattle manure and stream sediment were performed for contribution evaluation of organic pollutants in Toil stream of Yeongju dam basin. Average carbon isotope ratio(δ13C) is -25.17‰, -22.34‰, and -26.39‰ for river sediments, cattle manure and mountain soil, respectively. Result of carbon isotope analysis suggests that river sediments are more affected by acid soils. Average value of the nitrogen isotope ratio (δ15N) is 9.46% for river sediment, 1.99% for mountain soil, and 19.53% for cattle manure. Result of nitrogen isotopic analysis show that contribution of cattle mature is slightly higher than that of mountain soil in Toil stream sediments.

Rapid and Precise Determination of Pb Isotope Ratios Using Mu1ti-Collector ICP/MS (다검출기 유도결합 플라즈마 질량분석기를 이용한 신속하고 정밀한 Pb 동위원소 분석)

  • 최만식;정창식;신형선;임태선
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.157-171
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    • 2001
  • This study investigated the effects of Pb/Tl ratio, Pb concentration and concomitant matrix elements on the measurement of Pb isotope ratios using multi-collector ICP/MS (AXIOM MC model). Accuracy and reproducibility of Pb isotope ratios in NBS 981 solution were estimated for 42 data measured from March to August 2001. Pb isotopes measured in rocks, bronzes and sediments were compared to data measured by TIMS. Reproducibilities for $^{206}Pb/^{204}Pb,\; ^{207}Pb/^{204}Pb,\;and\;^{208}Pb/^{204}Pb$ ratio were about 500 ppm (2sd) and for $^{207}Pb/^{206}Pb$\;and\;^{208}Pb/^{206}Pb$ were 100~200 ppm for 200 ng of Pb in NBS 981 solution. The optimum conditions for the analysis of Pb isotope ratios with AXIOM MC for best accuracy and reproducibility were defined as follows; 1) Pb/Tl ratio is about 10 2) Pb concentration is about 100 ng/ml 3) correction for mass discrimination is performed by exponential law using 2.3887 of $^{205}Tl/^{203}Tl$ and Pb mass fractionation factor empirically obtained from $ln(^{208}Pb/^{206}Pb)-ln(^{205}Tl/^{203}Tl)$ relationship. The sample data measured with MC/ICP/MS for acid-digested and chemically separated rock samples, and acid-digested bronze samples and sediment samples coincide with those of TIMS within analytical errors. Therefore, MC/ICP/MS is a rapid analytical technique for Pb isotope ratios with the similar precision compared with TIMS.

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Characteristics of Fish Fauna in the Lower Geum River and Identification of Trophic Guilds using Stable Isotopes Analysis (금강하류의 어류상 및 안정동위원소 분석을 이용한 섭식길드 파악)

  • Yoon, Ju-Duk;Park, Sang-Hyeon;Chang, Kwang-Hyeon;Choi, Jong-Yun;Joo, Gea-Jae;Nam, Gui-Sook;Yoon, Johee;Jang, Min-Ho
    • Korean Journal of Environmental Biology
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    • v.33 no.1
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    • pp.34-44
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    • 2015
  • Fish fauna, difference of stable isotope ratio between freshwater and seawater, and trophic guilds of freshwater fishes were investigated in the lower Geum River. The study was conducted in 2011, and total study area was about 30 km of 20 km upstream and 10 km downstream from the Geum River estuary barrage. Only freshwater fishes were used for analyzing trophic guilds, and discriminant function analysis (DFA) was utilized to reclassify trophic guilds based on stable isotope ratio. Fish fauna in freshwater and seawater areas were entirely different each other, but small number of migratory species such as Coilia nasus and Chelon haematocheilus occurred both areas. Other species were not collected in the different areas because they did not have physiological ability to adapt different salinity concentrations. Stable isotope ration of two areas were different considerably due to food sources. Estuary and seawater fishes uptake food sources originated from marine, and freshwater fishes were from freshwater and terrestrial. Some migratory species showed reverse stable isotope ratio. Even though they collected in freshwater, they showed stable isotope ratio of seawater. This is because ecological characteristics of each species. Trophic guilds of freshwater fishes were reclassified by DFA, and showed slight difference with literatures. However, because this result is related with ontogenetic shift of species, more studies are needed to explain exact and correct trophic guilds. Stable isotope ratio can be changed among regions, seasons and ontogenetic stage, thus we always consider these aspects when analyzing results to get a right answer.

Scientific Analysis and Provenance Study of Bronze Artifacts Excavated from Dongchon Site in Sunchang, Jeollabuk-do, Korea (전북 순창 동촌유적 출토 청동기의 원료 산지연구)

  • Bae, Go Woon;Chung, Kwang Yong
    • Journal of Conservation Science
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    • v.32 no.2
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    • pp.101-108
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    • 2016
  • Lead isotope ratio of bronze artifacts excavated from Dongchon Site in Sunchang have determined by TIMS. As results of comparison lead isotope ratio of bronze objects with the provenance data of galenas of Korea, China, and Japan, the provenance of three material of bronze objects were turned out to originate from the southern and northern part of China. On the other hands, data were plotted either in zone 3 of the South Korean galena map. The results of these scientific analysis of bronze objects can be used as basic data in comparison researches on manufacturing technology, provenance of bronze objects to be found in the future.

Metallurgical Observation of the Buddhist Bell of Youngmoon Mountain Sangwonsa Temple (용문산 상원사 범종의 금속학적 고찰)

  • Doh, Jungmann;Park, Bangju;Lee, Jungil;Hong, Kyungtae
    • Korean Journal of Metals and Materials
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    • v.50 no.11
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    • pp.829-838
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    • 2012
  • The microstructure, chemical composition, and lead isotope ratio of the Buddhist bell of Yongmoon Mountain Sangwonsa temple, which was selected as one of the three great bells of Korea by Japanese historians, were analyzed in order to estimate the origin of the material and the time of casting. The microstructure of the temple bell was composed of a copper matrix phase with ${\alpha}$, a face centered cubit lattice structure, a ${\delta}$ phase with $Cu_{41}$ $(Sn,Ag,Sb)_{11}$ as the chemical structural formula, dispersed lead and $Cu_2S$ particles, and locally agglomerated fine particles. Through analysis of the chemical composition of the bell, a criterion (Pb: 0-3.0 wt%, Sn: 10-15 wt%) for distinguishing the bells of the Shilla dynasty from the bells of the Koryo Chosun dynasty is proposed. Examining the lead isotope ratio of $^{207}Pb/^{206}Pb$ and $^{208}Pb/^{206}Pb$ of the Buddhist bell of Sangwonsa temple proved that the bell was fabricated using raw materials in South Korea, which led to the conclusion that the bell was cast in Korea and the top board of the bell has been damaged by an unknown individual. The criteria of distinguishing the bells from the Shilla dynasty from the bells of the Koryo Chosun dynasty presented for the first time in this research is expected to aid in identifying and estimating the previously unclear production years of other bells.