• Title/Summary/Keyword: P-ACN buffer

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Chiral Separation on Sulfonated Cellulose Tris(3,5-dimethylphenylcarbamate)-coated Zirconia Monolith by Capillary Electrochromatography

  • Lee, Jeong-Mi;Jang, Myung-Duk;Park, Jung-Hag
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2651-2656
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    • 2012
  • Sulfonated cellulose tris(3,5-dimethylphenylcarbamate) (SCDMPC)-coated zirconia monolith (ZM) was used as the chiral stationary phase in capillary electrochromatography for separation of enantiomers of ten chiral compounds in acetonitrile (ACN)-phosphate buffer mixtures as the eluent. Influences of the ACN content, buffer concentration and pH on chiral separation have been investigated. Separation data on SCDMPC-ZM have been compared with those on CDMPC-ZM. Resolution factors were better on SCDMPC-ZM than CDMPC-ZM while retention factors were in general shorter on the former than the latter. Best chiral resolutions on SCDMPC-ZM were obtained with the eluent of 50% ACN containing 50 mM phosphate at pH around 4.

Determination of Aldehydes in Tap Water by Reverse Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 수도수 중 알데하이드류의 정량)

  • Choi, Yong Wook;Choi, Yun Jung
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.438-446
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    • 1999
  • The optimum analytical method of aldehydes, ozone by-products, was established by reverse phase liquid chromatography. Six aldehydes including formaldehyde, acetaldehyde, acrolein, propionaldehyde, butylaldehyde and benzaldehyde, and one ketone including acetone were selected as aldehyde test samples through preliminary experiments. Such analytical conditions as the pH of citrate buffer solution, reaction temperature, reaction time, and concentration of DNPH, the component and composition of desorption solvent were optimized. As the result, pH 3.0 of citrate buffer solution, 40$^{\circ}C$ of reaction temperature, 15 minutes of reaction time, and 0.012% of DNPH concentration were chosen as optimum conditions. Aldehydes-DNPH derivatives in water were concentrated on $C_18$ Sep-Pak cartridge and followed by elution of their derivatives fraction with THF/ACN(70/30) mixture, and showed recoveries of the range from 87 to 107%. Separation condition on Nova-Pak $C_18$ column with low pressure gradient elution from ACN/MeOH/water(30/10/60) of an initial condition to 80% ACN of a final condition was found to give a good resolution within 20 minutes of run time. 86% to 103% of recovery for aldehydes using this method was similar to that for aldehyde using EPA Method 554 which is ranged from 84% to 103%.

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Discrimination of Domestic Rice Cultivars by Capillary Electrophoresis (Capillary Electrophoresis를 이용한 국내산 쌀의 품종 판별)

  • Rhyu, Mee-Ra;Kim, Eun-Young;Ahn, Mee-Ok;Kim, Sang-Sook
    • Korean Journal of Food Science and Technology
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    • v.30 no.6
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    • pp.1252-1258
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    • 1998
  • Capillary electrophoresis (CE) with rice proteins was used to discriminate 10 domestic rice cultivars in less than 25 min. Most cultivars were differentiated quickly and easily using P-ACN buffer system. CE of rice prolamins allowed classifying ten varieties of Korean rice into three groups. Peak h was characteristic peak for Dongjinbyeo, Gaehwabyeo and Yongnambyeo which were classified into the group of Dongjinbyeo. Chuchungbyeo, Odaebyeo, Mangeumbyeo and Bonggwangbyeo easily differentiated from the group of Dongjinbyeo by the absence of peak h which were classified into the group of Chuchungbyeo. Peak g typical for Illpumbyeo, Hwaseungbyeo and Hwayoungbyeo accounted for 70% of total peak area. They belong to the group of Illpumbyeo. Some cultivars showed specific peak patterns among ten cultivars, Illpumbyeo was differentiated from others by several peaks between peak c and peak f, and the peak d was apparently detected in Odaebyeo not in others. Other minor differences were also found within each group. The result of the study showed that CE has potential for discrimination of rice cultivars. It also possesses the inherent advantages such as low mass requirements, fast seperations, and quantitative analysis through on-capillary UV detection.

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Simultaneous Determination of Isocyanates by High Performance Liquid Chromatography (고속액체크로마토그래피를 이용한 이소시아네이트의 동시 정량)

  • Lee, Seon Joo;Lee, Kwang Mook;Roh, Young Man
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.4 no.2
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    • pp.137-147
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    • 1994
  • This study was designed to identify and quantitate airborne isocyanate simultaneously by HPLC. These samples were collected using 1-(2-pyridyl)piperazine(1-2PP) coated glass fiber filter from polyurethane painting works at 8 wood furniture factories in Kimpo and Inchun. The results obtained were as follows : 1. The most suitable mobile phase condition of simultaneously analyzing isocyanates was 0.01 M ammonium acetate buffer ACN(70/30) adjusted to pH 6.2 from the beginning of the analysis to 20 min and 0.01 M ammonium acetate buffer/ACN(50/50) adjusted to pH 6.2 from 21 min to 40 min using the gradient mode. The peaks of isocyanates were able to obtain within 30 min. 2. The recovery efficiencies for 2,6-TDI, 2,4-TDI, HDI and MDI urea derivates spiked at the target concentration on coated glass fiber tillers were 91.00, 93.42, 91.31 and 94.21 %, respectively. 3. The qualitative analysis of the isocyanates samples from polyurethane spray painting works in wood furnture factories identified Ihree isocyanates, 2,6-TDI, 2,4-TDI and MOI. And their concentration ranges were 0-312.6, 0-56.3 and $0-62.1{\mu}g/m^3$, respectively. A disadvantage of using the colorimetric method for isocyanate analysis is its inability of separating isocyanates. This study identified such three isocyanates as 2,6-TDI, 2,4-TDI and MDI from polyurethane spray painting works in wood furniture factories. These isocyanates were successfully quantitated by HPLC by modifying the mobile phase condition and switching to gradient mode.

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A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants(II) : Optimization for Separation of Alkylphenols by Reversed-Phase Liquid Chromatography (환경 오염물질의 정량법 개발과 거동에 관한 연구(II) : 역상 액체 크로마토그래피에서 알킬페놀류의 분리 최적화)

  • Lee, Dae Woon;Lee, Yong-Ju;Park, Young Hun;Kim, Ho Seob
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.25-31
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    • 1994
  • As for analytes which did not represent the differences of the selectivity on the stationary and mobile phase, secondary chemical equilibrium theory was applied to study pH effects on the separation of alkylphenols. Mobile phase was consisted of an aqueous sodium carbonate-bicarbonate buffer and acetonitrile. The maximum selectivity for adjacent peak pairs was predicted from those values of $k^{\prime}_{HA}/k^{\prime}_{A-}$ and ${\Delta}pK$. The optimum pH determined by this method was 11.18 pH and solvent selectivity were considered at the same time to invoke the full range of selectivity effects possible for separations. Quaternary mixture composed of methanol, acetonitrile, tetrahydrofuran and water was adjusted to optimum pH 11.18. As the statistical simplex technique of an overlapping resolution map (ORM) was used to predict the optimized solvent system. The optimum solvent, which gives complete separation of alkylphenols, was determined as follws MeOH : ACN : THF = 14.4 : 81.8 : 2.8.

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Simultaneous Determination of Quinolones in Flatfish and Egg Using liquid Chromatography with Fluorescence Detection (액체크로마토그래피를 이용한 광어 및 계란 중 퀴놀론계의 동시분석법 개발)

  • Lee, Sang-Hee;Shim, You-Shin;Kim, Hyun-Ju;Choi, Yoon-Hee;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
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    • v.23 no.4
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    • pp.324-329
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    • 2008
  • An analytical method for the simultaneous determination of nine quinolones (QNs) namely, marbofloxacin, norfloxacin(IS), ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, and flumequine in flatfish and egg was developed and validated using liquid chromatography with fluorescence detection (LC-FD). The samples were extracted using a traditional liquid-liquid extraction process; deproteinization was accomplished by the addition of trichloroacetic acid and acetonitrile (ACN), and defatting was performed with hexane. Chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and ACN. The proposed method was validated according to the CODEX guideline. Mean recoveries of QNs from flatfish and egg were 89.6-106.5% with relative standard deviations (RSDs) below 15% at three different concentrations of 50, 100 and $500{\mu}g/kg$. Linearity was obtained with a correlation coefficient ($r^2$) of 0.9989-1.0000. The LOD for the investigated QNs was $1-16{\mu}g/kg$ depending on flatfish and egg. The present method can be applied simultaneously to determine QNs in muscle of flatfish and egg.

Residue by elapsed time of non-enzymatic antioxidants in dentifrice (세치제에 함유된 비효소계 항산화제의 경시변화에 따른 잔류량)

  • Park, Jung-Eun;Park, Yong-Duk;Hong, Tae-Gi;Jang, Jong-Hwa
    • Journal of Korean society of Dental Hygiene
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    • v.16 no.5
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    • pp.783-790
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    • 2016
  • Objectives: The purpose of this study is to evaluate the non-enzymatic antioxidants stabilities in dentifrices by ascorbic acid and tocopherol according to the chemical condition. Methods: For the analysis of two antioxidants, HPLC UV detector system was used. HPLC was performed using sodium sulfate, acetonitrile(ACN), methanol(MeOH) and measuring absorbance at 240-295 nm. To confirm general pH reaction of two compounds, buffer solution was prepared for the analysis. The dentifrice was titrated by pH so as to examine the change of elapsed time in dentifrice. Linearity of calibration curve of two antioxidants was measured. Results: Each compound showed good linearity at optimized wavelength as well as showing good precision. General pH reaction of two antioxidants was examined. Ascorbic acid showed the highest residue(63.23%) at pH 10 and the lowest residue(2.77%) at pH 4. Tocopherol showed the highest residue(55.70%) at pH 7 and the lowest residue(3.31%) at pH 4. As a result of changing elapsed time of antioxidants in dentifrice by pH, components were remained stably at low temperature($39.2^{\circ}F$) and pH 7. Conclusions: It is necessary to keep dentifrice including ascorbic acid and tocopherol, and non-enzymatic antioxidants at pH 7 and low temperature for improving chemical stability.

Multiresidue Determination of Quinolones in Porcine, Chicken, and Bovine Muscle Using Liquid Chromatography with Fluorescence Detection

  • Lee, Sang-Hee;Shim, You-Sin;Kim, Hyun-Ju;Shin, Dong-Bin
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.978-984
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    • 2009
  • An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.