• Title/Summary/Keyword: 이온크로마토그래피

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Separation of Inorganic Anions by Reversed-phase Ion Chromatography (역상 이온 크로마토그래피에서 무기음이온의 분리)

  • Kih Soo Joe;Tae Yoon Eom;Seung Soo Kim;Youn Doo Kim
    • Journal of the Korean Chemical Society
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    • v.32 no.5
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    • pp.452-457
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    • 1988
  • Capacity factors (k') of some inorganic anions including $BF_4^{-1}$ were measured on cetylpyridinium coated column, and with dynamic system using tetrabutylammonium salicylate on PRP-1 reversed-phase column, respectively. After optimum separation condition was obtained this method was applied to the determination of boron in some different type samples.

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A study on the derivatization technique for tamoxifen metabolites in human urine by gas chromatography/mass spectrometry (기체크로마토그래피/질량분석기를 이용한 인체 내 뇨시료에서의 Tamoxifen 대사체 검출을 위한 유도체화 연구)

  • Kim, Yunje;Lee, Yoonjung
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.322-336
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    • 2004
  • The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

Purification and Characterization of the β-Galactosidase from Edible Snail (식용달팽이 β-Galactosidase의 정제와 생화학적 특성)

  • 윤경영;김광수
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.1
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    • pp.50-56
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    • 2002
  • The $\beta$-galactosidase was purified from the internal organs of edible snail by fractionation with ammonium sulfate, ion exchange chromatography on DEAE-Sephadex, Mono Q HR 5/5 and gel filtration on Sephacryl S-200. Superose 12 HR 10/30 chromatography. The specific activity of the purified $\beta$-galactosidase was 18.8 units/mg protein with 31.3 purification fold from crude extract. The $\beta$-galactosidase had native molecular weight of 144,000 dalton and was composed of two subunits of 72,000 dalton. The isoelectric point of the enzyme was determined 4.1. This enzyme was the most active at pH 3.0 and 6$0^{\circ}C$, and was stable in the pH range 2.0~8.0 and below 5$0^{\circ}C$. The enzyme was inhibited by metal ions and sugars such as fructose, glucose, galactose, maltose and xylose.

Determination of Iodide in spent PWR fuels (경수로 사용 후 핵연료 내 요오드 정량)

  • Choi, Ke Chon;Lee, Chang Heon;Kim, Won Ho
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.110-116
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    • 2003
  • A study has been done on the separation of iodide from spent pressurized water reactor (PWR) fuels and its quantitative determination using ion chromatography. Spent PWR fuels were dissolved with mixed acid of nitric and hydrochloric acids (80 : 20 molL%) which can oxidize iodide to iodate to prevent it from be vaporized. After reducing ${IO_3}^-$ ­to $I_2$ in 2.5 M $HNO_3$ with $NH_2OH{\cdot}HCl$, Iodine was selectively separated from actinides and all other fission products with carbontetrachloride and back-extracted with 0.1 M $NaHSO_3$. Recovered iodide was determined using the ion chromatograph of which the column was installed in a glove box for the analysis of radioactive materials. In practice, spent PWR fuel with 42,000~44,000 MWd/MtU was analyzed and its quantity was compared to that calculated by burnup code, ORIGEN2. The agreement was achieved with a deviation of -8.3~-0.5% from the ORIGEN 2 data, $324.5{\sim}343.6{\mu}g/g$.

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.

Conversion of D-$\alpha$-Amino-$\varepsilon$-Caprolactam into L-Lysine Using Cell-free Extracts of Alcaligenes eutrophus A52 (Alcaligenes eutrophus A52의 무세포 추출액에 의한 D-$\alpha$-Amino-$\varepsilon$-Caprolactam으로부터 L-Lysine으로의 전환)

  • 박희동;최선택;이인구
    • Microbiology and Biotechnology Letters
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    • v.15 no.6
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    • pp.375-380
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    • 1987
  • D-$\alpha$-Amino-$\varepsilon$-carpolactam racemase (EC 5.1.1) and L-$\alpha$-amino-$\varepsilon$-caprolactam hydrolase (EC 3.5.2) were fractionated from cell-free extracts of Alcaligenes eutrophus A52 using ammonium sulfate precipitation and DEAE-cellulose ion exchange chromatography. It was made sure that D-$\alpha$-amino-$\varepsilon$-caprolactam was converted to L-$\alpha$-amino-$\varepsilon$-caprolactam by racemase, and then hydrolyzed into L-lysine by hydrolase in Alcaligenes eutrophus A52. For the conversion of D-$\alpha$-amino-$\varepsilon$-caprolactam into L-lysine by cell-free extracts of Alcaligenes eutrophus A52, the optimum temperature and pH were 6$0^{\circ}C$ and 8.5 respectively. The results showed that 0.5% D-$\alpha$-amino-$\varepsilon$-caprolactam was converted to L-lysine at 55$^{\circ}C$ for 10 hr with a conversion rate of 98% by cell-free extracts containing 3.1mg of protein.

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Analysis of Distribution of Propylene oxide in Nonionic Surfactant and Fatty alcohol by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 비이온 계면활성제의 Propylene oxide 분포 및 Fatty alcohol의 분석)

  • Lee, Yong-Hwa;Bak, Hong-Soon;Choi, Kyu-Yeol;Lee, Jae-Duk;Ahn, Ho-Jeong
    • Applied Chemistry for Engineering
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    • v.8 no.2
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    • pp.315-319
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    • 1997
  • In this study, the optimum analytical conditions for determination of distribution of propylene oxide in a nonionic surfactant and separation of fatty alcohols were investigated by Reversed Phase High Performance Liquid Chromatography. To analyse the distribution of propylene oxide (PO) and carbon chain length of a fatty alcohol, we derivatized samples for the purpose of using a UV detector. Also, we studied the influences of columns and mobile phase composition to obtain the optimum separation conditions. In our experiment, Waters Symmetry $C_8(3.9{\times}150mm)$ column was used. And the optimum condition were obtained by gradient elution with methanol and water as the mobile phase. In the plot of log k' vs composition of water in the binary phase, the linerality was very good. We ploted the calibration curve to conform the quality of fatty alcohol, a good linerality was obtained.

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Purification and Properties of $\alpha$-Galactosidase from Aspergillus niger (Aspergillus niger $\alpha$-Galactosidase의 정제 및 성질)

  • 금종화;오만진;김찬조
    • Microbiology and Biotechnology Letters
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    • v.19 no.5
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    • pp.477-486
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    • 1991
  • To elucidate enzymatic properties of a-glactosidase (EC 3.2.1.22) from Asp. niger, a-galactosidase from wheat bran culture was purified by ammonium sulfate fractionation, ion exchange chromatography and gel filtration. And then its enzymatic propeties were investigated. The highest level of $\alpha$-galactosidase activity was obtained when Asp. niger was grown on wheat bran medium at $30^{\circ}C$ for 96 hours. The $\alpha$-galactosidase was purified by 23.7 fold by ammonium sulfate fractionation, ion exchange chromatography on DEAE-Celluose and Sephadex A-50, and gel filtration on Sephadex G-150 and its specific activity was 1,229 Unitslmg protein and the yield was 14% of the total activity of wheat bran culture. The purified $\alpha$-galactosidase was found to be homogeneous by polyacrylamide gel electrophoresis and HPLC. The $\alpha$-galactosidase was a tetrameric glycoprotein which consisted of identical subunits with molelcular weight of 28,000 each by SDS-PAGE and isoelectric point was determined analytical isoelectric focusing to be pH 4.6. The optimal temperature and pH for the $\alpha$-galactosidase activity were $40^{\circ}C$ and pH 6.5, respectively, and 54% of its activity was lost by heating at $60^{\circ}C$ for 10 mins, It was appeared to have higher affinty to raffinose than to stachyose. The K, value and activation energy of $\alpha$-galactosidase were 5.0 mM and 8.515 Kcal per mole for p-nitrophenyl- $\alpha$--D-galactopyranoside, respectively.

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Rapid Simultaneous Determination of Anions in Mineral Water by Single Column Ion Chromatography (단일 컬럼이온크로마토그래피에 의한 광천수중 음이온의 신속한 동시정량)

  • Kim, Jong Hun;Choi, Yong Wook;Chung, Taek Kyun
    • Journal of the Korean Chemical Society
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    • v.39 no.12
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    • pp.910-917
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    • 1995
  • Analytical conditions for single column ion chromatographic determination of five anions such as F-, Cl-, NO2-, NO3-, and SO42- were optimized with respect to analysis time and separation efficiency. At the optimum condition of 2.0 mM phthalic acid at pH 4.5, five anions were effectively separated in 10 minutes so that analysis time could be reduced by 40% compared to other recommended conditions. Under this condition all the calibration curves of five anions were linear with a correlation coefficient > 0.999. Analytical results for nine commercial bottled waters were presented.

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Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid (Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.288-293
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    • 1995
  • The separation and determination of boron with chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid) as a complex agent has been studied using ion pair liquid chromatography. The use of tetrabutylammonium bromide added as an ion pair reagent to mobile phase (MeOH 61%, phosphate buffer 39% pH=8.5) allowed good separation of boron-chromotrophic acid complex anion and chromotrophic acid on poly(styrene-divinylbenzene) based reversed phase column (PRP-1, 15 $cm{\times}4.6$ mm i.d.). The complex formation between boric acid and chromotrophic acid was enhanced in the presence of 0.1 M tetrabutylammonium bromide, resulting in high sensitivity. The linear calibration was achieved over the boron concentration range of 0.5∼1000 ${\mu}g/L.$ The detection limit was 0.5 ${\mu}g/L$ (S/N=2). The proposed method was applied to the determination of boron in commercially available chemicals, $Na_2SO_4$, NaOH, KCl.

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