• Title/Summary/Keyword: 크로마토그래피

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Experimental Evaluation of an Analytical Method for Chlorofluorocarbons (CFSs) in Air and Water Using Gas Chromatography (가스 크로마토그래피를 이용한 대기와 물시료의 CFCs(chlorofluorocarbons) 분석법의 실험적 평가)

  • Koh, Dong-Chan;Choi, Beom-Kyu;Kim, Yong-Je
    • Economic and Environmental Geology
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    • v.40 no.1 s.182
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    • pp.129-140
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    • 2007
  • CFC(CFC-12, CFC-11 and CFC-113) analytical system for air and water was constructed using a customized purge and trap extraction device and a gas chromatograph with an electron capture detector. Sampling methods of air and water for CFCs were also established. The analytical system was experimentally optimized to result in reproducibilities of triplicates less than 2% for current air samples and less than 5% for groundwater samples with CFC-12 concentration of 160 to 180 pg/kg, and verified with respect to the CFC system in USGS, which showed analytical results were in agreement within 10%. CFCs in air were monitored at three sites over 19-month period in the central part of South Korea, and the result indicates no significant local sources of CFCs in those areas. For groundwater in Jeju Island, CFCs were measured over a year with a two-month interval. The time-series data showed seasonal fluctuations which could be interpreted by the effect of recharge pulse derived from large amount of rainfall during monsoon period with a few month delay, which indicates high permeability of basaltic rocks in Jeju Island.

Separation for the Determination of $^{59/63}Ni$ in Radioactive Wastes (방사성 폐기물 내 $^{59/63}Ni$ 정량을 위한 분리)

  • Lee, Chang-Heon;Jung, Kie-Chul;Choi, Kwang-Soon;Jee, Kwang-Young;Kim, Won-Ho
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.3 no.4
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    • pp.309-317
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    • 2005
  • A study on the separation of $^{99}Tc,\;^{94}Nb,\;^{55}Fe,\;^{90}Sr\;and\;^{59/63}Ni$ in various radioactive wastes discharged from nuclear power plants has been performed for a use in their quantification which is indispensible for the evaluation of the radionuclide inventory Ni was recovered along with Ca, Mg, Al, Cr, Ti, Mn, Ce, Na, K, and Cu through the sequential separation procedure of Re(as a surrogate of $^{99}Tc$), Nb, Fe and Sr by anion exchange and Sr-Spec extraction chromatography. In this research, chemical separation of Ni from the co-existing elements was investigated by cation exchange and Ni-Spec extraction chromatography. Precipitation behaviour of Ni and the co-existing elements with dimethylglyoxime(DMG) was investigated in ammonium $citrate/ethanol-H_2O$ and tartaric $acid/acetone-H_2O$ in order to purify separated Ni fractions and to prepare $^{59/63}Ni$ source for the radioactivity measurement using a gas proportional counter. Recovery of Ni separated through ion exchange chromatographic separation procedure was $92.1\%$ with relative standard deviation of $0.9\%$. In addition, recovery of Ni with DMG in the tartaric $acid/acetone-H_2O$ was $85.6\%$ with relative standard deviation of $1.9\%$.

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Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Chemical Structure of the Major Color Component from a Korean Pigmented Rice Variety (한국산 유색미에서 분리한 안토시아닌의 화학구조)

  • Cho, Man-Ho;Paik, Young-Sook;Yoon, Hye-Hyun;Hahn, Tae-Ryong
    • Applied Biological Chemistry
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    • v.39 no.4
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    • pp.304-308
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    • 1996
  • The major color component of a Korean pigmented rice (Oeyza sativa var. Suwon 415) was purified with Amberlite XAD-7 column and preparative paper chromatography. The purified pigment was determined as anthocyanin by paper chromatography, UV/Vis and NMR spectroscopy. The $\lambda_{max}$ of the Purified anthocyanin on UV/Vis spectrum were 529 nm and 281 nm. The $A_{440}/A_{529}$ value of the purified anthocyanin was 23% suggesting the presence of 3-glycosidic structure. The aglycone from acid hydrolysis showed bathochromic shift (18 nm) in the presence of $AlCl_3$ indicating that the anthocyanidin contained free adjacent hydroxyl groups such as cyanidin, delphinidin, petunidin or luteolinidin. The sugar moiety obtained from acid hydrolysis was determined as glucose by paper chromatography. The NMR spectra showed that the aglycone was cyanidin and the sugar was ${\beta}-D-glucopyranose$. Thus, the chemical structure of the purified anthocyanin was identified as cyanidin $3-O-{\beta}-D-glucopyranoside$.

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Gas Chromatographic Analysis on Residual Concentration and Half-life Time of Cyfluthrin in Potato and Soil (감자와 토양 중에서 Cyfluthrin의 잔류농도와 반감기에 대한 기체 크로마토그래피 분석)

  • Han, Seong Soo;Jeong, Seung Il;Chun, Hyun Ja;Hoang, Geun Chang;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.722-730
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    • 2000
  • The residual concentration and half-life time of synthetic pyrethroid insecticide cyfluthrin in potato and soil were investigated by gas chromatography (GC). The pesticide in potato was extracted with n-hexane, filtered and concentrated. The concentrated phase was transferred to the Sep-Pak silica gel column and purified with acetonitrile and acetone for the analysis by gas chromatography equipped with electron capture detector (GC-ECD). From the standard additional experiments with 0.01 and $0.1{\mu}g$, the recoveries were 85-87% and the detection limit was 0.005 ng. The soil sample was extracted with acetone and dichloromethane. The organic phase was concentrated and redissolved with n-hexane and analyzed with GC-ECD after cleaned with Sep-Pak column. From the standard additional experiments with 0.01 and 0.1 ng, the recoveries were 84-88% and the detection limit was 0.005ng. The half-life time of cyfluthrin in the silty clay was 25 days in the room laboratory and 0.6 days in the fieJd test whereas it was 38 days and 0.5 days for each in case of silty loam.

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Effect of Organic Acids on Suppression of Fishy Odor in Salted Clam Pickle (유기산에 의한 조개젓 비린내 억제효과에 관한 연구)

  • Lee, Young-Eun;Rhee, Hei-Soo
    • Korean Journal of Food Science and Technology
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    • v.14 no.1
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    • pp.6-10
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    • 1982
  • To investigate the effect of organic acids on suppression of fishy odor, the change of the odor and the remaining amount of trimethyamine (TMA), selected as the representative component of fishy odor in clam pickle (15.5% NaCl) were examined by sensory evaluation and gas chromatography. The fishy odor linearly decreased as the amount of vinegar increased at ${\alpha}=0.01$, but there was no significant difference of fishness score for the changes of storage period and kinds of acid. Overall acceptability score was found to be the best when 8 ml vinegar added to 100g clam pickle. The remaining amount of TMA showed the tendency to decrease as the amount of acetic acid and storage time increased and kinds of acid were changed in order of acetic, malic and citric acid. However when $4\;{\mu}l/ml$ acetic acid (=8 ml vinegar/100g clam pickle) was added, the percentage of the remaining amount of TMA showed little decrease from about 95% for 72 hours of storage time. From the results of sensory evaluation and gas chromatography, it was considered that acids have the effect on suppression of fishy odor by producing non-volatile salts by combining with TMA chemically and that the effect of acids on suppression of fishy odor is mainly due to the masking effect at the concentration commonly used.

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Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

A Study of Liquid Chromatographic Detection Method for Thiocarbamates by Using Photochemical Reaction (광화학 반응을 이용한 티오카바메이트류의 액체 크로마토그래피 검출법에 관한 연구)

  • Dai Woon Lee;Young Hun Park;Yong Wook Choi
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.453-461
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    • 1993
  • Detection method was developed using a simply designed photochemical reactor made of teflon coil and low pressure mercury lamp. This method of UV photolysis of analytes followed by UV, fluorescence and electrochemical detection was found to be useful for four thiocarbamates. Analytes eluting from the column are irradiated with a high flux of 254 nm UV light, so that they change to either fluorescent active forms or highly electrochemically sensitive products. Appling this technique to the UV detection, thiocarbamates were converted into long wavelength absorbing products upon UV irradiation. In fluorescence detector four thiocarbamates are not detected at nonirradiated condition but fluorescence signals of MPTC, CPTC photolysates are appeared after irradiation with UV light. The electrochemical detection for the determination of thiocarbamates was enhanced up to 5∼20 fold signal after UV irradiation, compared to that of the nonirradiated. The detection limit of thiocarbamates on electrochemical detector was 13.3∼0.02 ng under pH 7.0, ionic strength $0.5{\times}10^{-2}$ M, phosphate buffer solution. Adducts produced by reaction of photolysates and OPA-MERC in the reaction coil were monitored at 425 nm with fluorescence detector, and one of the photolysates was primary amine.

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