• Title/Summary/Keyword: IC-MS/MS

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Determination of Trace-Level Perchlorate by IC-MS/MS and Distribution in the Han River (IC-MS/MS를 이용한 수중의 과염소산이온 분석방법 최적화 및 한강수계내 분포조사)

  • Kim, Hyun-Hee;Han, Ihn-Sup;Jeong, Gwan-Jo;Park, Hyeon;Han, Sun-Hee;Cho, Wan-Seon
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.4
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    • pp.349-356
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    • 2010
  • Ion chromatography (IC) coupled with conductivity detector (CD) is a common system for the determination of perchlorate in water samples. Although the IC method with CD has been widely used for the determination of trace level perchlorate ion in water, sensitivity decreases dramatically as the complexity of the matrices increases. Here we proposed the application of ion chromatography coupled with mass spectrometry (IC-MS/MS) to significantly improve selectivity of perchlorate. The mean recovery of the method was 104.4 ${\pm}$ 5.7% and the relative standard deviation (RSD%) was 1.9 ${\pm}$ 1.3%. The alculated method detection limit (MDL) was 0.0207 ${\pm}$ 0.0099 ${\mu}g/L$. The concentrations of perchlorate were minimum <0.1 ${\mu}g/L$ and maximum 18.3 ${\mu}g/L$ in source water (Namhan, Bukhan and Han River). Hongreung showed higher concentrations ($1^{st}$-14.3 ${\mu}g/L$, $2^{st}$-18.3 ${\mu}g/L$) than the other places. And the concentrations of perchlorate were 0.18~0.34 ${\mu}g/L$ in the samples taken from the six water treatment plants and six intake stations in Seoul.

Monitoring and Evaluation of Analytical Methods of Perchlorate with IC and LC/MS (IC와 LC-MS를 이용한 퍼클로레이트 분석 방법 비교 및 모니터링)

  • Kim, Hwa-Bin;Sim, Won-Jin;Kim, Min-Young;Oh, Jeong-Eun
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.1
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    • pp.37-44
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    • 2008
  • In this study, we tried to establish analysis methods of perchlorate with ion chromatography(IC) and liquid chromatography/mass spectrometry(LC/MS) and monitored perchlorate levels in various kinds of water and soil samples. The obtained method detection limit(MDL) of IC was 1 ppb and that of LC/MS was 0.005 ppb in water sample. We monitored the ground and spring water in Busan and the average perchlorate level in ground water was 0.031 $\pm$ 0.011 ppb and that of spring water was 0.013 $\pm$ 0.014 ppb. Wastewater samples were also examined and the levels of perchlorate ranged from 0.007 to 0.380 ppb. The perchlorate levels in all water samples investigated in this study were below the EPA guideline.

Simultaneous determination of low molecular weight amines and quaternary ammonium ions by IC/ESI-MS

  • Jung, Joo-Young;Park, Han-Seok;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.255-260
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    • 2007
  • A new method for the simultaneous determination of low molecular weight amines and quaternary ammonium ions based on the separation by IC with a suppressor and the detection by MS with ESI has been developed. The method has been applied to the analysis of a mixture containing tetramethylammonium ion, tetraethylammonium ion, tetrapropylammonium ion, triethanolamine, trimethylamine and triethylamine. The constituents were separated by isocratic elution using an IonPac CS17 column, a cation-exchange column, and detected by conductivity and mass spectrometry. The newly developed method for the six components demonstrated that the repeatability in terms of relative standard deviation for three measurements was in the range of 0.1-0.5 %. The detection limits were between 0.2 and $0.9{\mu}g/mL$ by the IC/ESI-MS.

Development of Enhanced Analytical Method for Perchlorate in Food by IC-MS/MS with an Internal Standard (IC-MS/MS와 내부표준물질을 이용한 식품 중 perchlorate 분석법 개선)

  • Yang, Min-June;Kim, Jong-Sung;Han, Jong-Hun;Her, Nam-Guk
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.532-536
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    • 2011
  • The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.

Direct Determination of Total Arsenic and Arsenic Species by Ion Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry

  • Nam, Sang-Ho;Kim, Jae-Jin;Han, Soung-Sim
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1805-1808
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    • 2003
  • The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS.

Cytotoxic Constituents of Diadema setosum

  • Minh, Chau-Van;Kiem, Phan-Van;Huong, Le-Mai;Kim, Young-Ho
    • Archives of Pharmacal Research
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    • v.27 no.7
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    • pp.734-737
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    • 2004
  • 5,8-Epidioxycholest-6-en-3-ol (1), cholesterol (2), glycerol 1-palmitate (3) and glycerol 1,3-dioleate-2-stearate (4) were isolated from the methanol extract of the sea urchin Diadema setosum, which was collected from the Halong sea, Vietnam. Chemical structures were established based on extensive 1D, 2D-NMR, FAB-MS, EI-MS spectroscopic data and GC-MS analysis. The NMR spectral data of compound 1 were reassigned by using HMQC and HMBC. Compound 1 was found to have strong cytotoxic effect against various cancer cell lines, such as KB ($IC_{50}$, 2.0 $\mu\textrm{g}$/mL), FL($IC_{50}$, 3.93 $\mu\textrm{g}$/mL), and Hep-2 ($IC_{50}$, 2.4 $\mu\textrm{g}$/mL) by in vitro assay.

Characteristic Effects of Dangnyo-hwan for Diabetes Control Studied Using LC-MS/MS and ICP (LC-MS/MS 및 ICP를 이용한 당뇨환의 화학적 특성 분석)

  • In, Jeong-do;Im, Dai-sig;Moon, Seung-ho;Ki, Won-ill
    • The Journal of Internal Korean Medicine
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    • v.36 no.3
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    • pp.217-227
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    • 2015
  • Objectives: The primary aim of this study was to identify bioactive compounds in Dangnyo-hwan, a Korean herbal medicine, through instrumental analysis using LC-MS/MS and ICP, and investigate its potential use in diabetes treatment. Methods: The extract of Dangnyo-hwan has 12 medicinal herbs; these were compared with 18 marker substances selected from literature survey. Results: LC-MS/MS analysis could detect 9 of the 18 bioactive compounds: citruline, catalpol, berberine, ginsenoside Rb1, ginsenoside Rg1, oleanolic acid, β-sitosterol, mangiferin, and schizandrin. While harmful heavy metals such as As, Pb, Cd, Hg, Ni, and Cu were not present in high concentrations, Zn concentration was 4.2 mg in 100 g Dangnyo-hwan. Conclusions: Instrumental analysis such as LC-MS/MS and ICP was successfully used to identify bioactive compounds in Dangnyo-hwan. Detection of 9 bioactive substances and Zn from the herb medicine is a valuable finding, and suggests that Dangnyo-hwan is a candidate medicine for diabetes. Further investigations like in vitro assay, percent GPR 119 activity, and percent human DGAT-1 inhibition are underway.

Quality Characteristics of Sulgidduk Added with Makgeolli (막걸리 첨가 설기떡의 품질 특성)

  • Shim, Eun Kyoung;Kim, Hyun Jeong;Lee, Su Jin;Kim, Mee Ree
    • Journal of the Korean Society of Food Culture
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    • v.29 no.6
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    • pp.605-614
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    • 2014
  • The objective of this study was to investigate the quality characteristics of Baeksulgi (BS) and Sulgidduk added with Makgeolli (MS, BS+ Makgeolli) during storage at $20{\pm}2$ for 3 days. Moisture contents of MS were significantly higher than those of BS during storage. Reducing sugar contents (%) were higher in MS. The pH values were 6.23 and 5.93, for BS and MS, respectively. The pH of MS was lower and thus indicated higher in acidity. The Hunter color L (lightness) and a (redness) values were higher for BS, whereas b (yellowness) value of MS was lower. In the texture analysis, hardness and chewiness of MS were found to be lower, whereas springiness, gumminess, and resilience were higher than those of MS. According to DSC (Differential scanning calorimeter) analysis, enthalpy of MS appeared to be lower than that of BS during storage, which suggests retrogradation of MS was delayed. The total phenol content was higher in MS. The $IC_{50}$ value of DPPH and hydroxyl radical scavenging activity was lower in MS, which means antioxidant activity increased in MS. Results of the preference test showed that appearance, flavor, taste, and overall acceptability of MS scored higher than those of BS. From these results, high quality of MS was derived from Makgeolli addition.

A Study of the Potential Interference of ArC+ on the Direct Determination of Trivalent Chromium and Hexavalent Chromium Using Ion Chromatography Coupled with ICP-MS

  • Nam, Sang-Ho;Park, Young-Il;Kim, Jae-Jin;Han, Sun-Ho;Kim, Won-Ho
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.447-451
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    • 2004
  • Low and high resolution inductively coupled plasma mass spectrometry (ICP-MS) coupled with ion chromatography (IC) has been investigated for speciation of Cr(III) and Cr(VI). In particular, the interference of ArC^+formed by the carbon in a sample on the simultaneous determination of Cr(III) and Cr(VI) has been studied. In chemical speciation, this study shows that quadrupole type ICP-MS with low resolution has a limitation of simultaneous determination fo chromium species if the sample contains the carbon elements. The interference problems can be solved by high resolution ICP-MS.

IC카드 동향 및 향후 과제

  • Kim, Yeong-Gap;Lee, Yong-Ho;Choe, Myeong-Hyeon;Kim, Gwang-Hyeon
    • Review of Korean Society for Internet Information
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    • v.9 no.2
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    • pp.27-36
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    • 2008
  • 2008년 상반기 국내 민간최종소비지출 중 카드 사용비중은 54%로, 이제 카드는 결제수단의 최대 강자로 자리잡았다. 경제활동인구 1인당 신용카드 소지수도 2002년 4.6매에서 2005년 3.5매로 떨어졌다가 2008년도까지 3.8매 선으로 안정되고 있다. 신용카드 이외의 은행, 증권, 저축은행 등의 현금인출용 카드와 교통카드, 모바일 칩카드, 백화점카드, 학생증카드, 직원ID카드, 마일리지카드, 기타 멤버십카드 등을 합하면 국민들의 지갑은 현금보다도 플라스틱카드로 두툼해져 있다. 이동통신서비스 사업자들은 이동통신단말기를 이용하여 다양한 서비스를 개발 제공함으로써 시장의 주도권을 노리고 있고, 교통카드 사업자들은 자사의 전자화폐인 교통카드로 주도권을 지키려 하고 있으며, 기존의 강자였던 은행과 카드사들은 고객을 빼앗기지 않기 위해 고객이 필요로 하는 다양한 서비스는 제공하면서도 주도권은 지키려고 하는 경쟁과 협력이 활발하게 전개되고 있다. 한편, MS카드는 읽기/쓰기가 쉬워 정보유출, 위변조, 복제 등을 통한 사고의 위험이 커서, 선진국뿐 아니라 중동, 중남미, 아시아 국가들까지도 IC카드로의 전환이 진행되고 있다. 국제브랜드 카드사들은 2006년 1월부터 IC카드가 MS 단말기에서 부정 사용될 경우 그 책임을 매입사에 전가시키는 제도(Transitional Chip Liability Shift Program)를 시행하고 있어 국내 카드사들의 피해도 예상된다. 금융감독 당국은 2003년 2월 “IT및 전자금융 안전성 제고대책”에 의거 2008년 말까지 100% IC카드로 전환을 목표로 연도별 전환목표를 통보하고 지도감독하고 있다. 이에 따라 은행의 현금카드는 2008년 6월까지, 신용카드는 2008년 12월까지 전환을 수행하고 있으나, 기타 금융권이나 카드사용자들은 비용부담, 재고소진 등의 문제로 잘 지켜지지 않고 있다. 특히 가맹점 단말기를 교체하여야 할 VAN사 들은 교체비용이 자기 자본을 상회하는 어려움으로 POS나 CAT단말은 거의 전환이 진행되지 않고 있어 IC카드를 가지고 있어도 MS를 이용하는 형편이다. 카드의 종류는 주도권 경쟁으로 늘어만 가고 있어 애초 취지처럼 하나의 카드로 다양한 사업자의 서비스가 통합되기 어려운데다, 단말기의 표준화도 어려워 막상 카드를 안전하고 편리하게 사용하여야 할 소비자들의 지갑만 무거워지고 있다. 본고는 이렇게 우리의 생활 깊숙이 들어온 카드를 편리하고 안전하게 사용할 수 있도록 하는 인프라는 과연 어느 수준이고 시장의 주자들은 어느 방향으로가고 있는지 살펴보고 그 문제점과 과제를 제시하고자 한다.

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