• Title/Summary/Keyword: 추출크로마토그래피법

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토양의 특성에 따른 토양증기추출법 (Soil Vapor Extraction)의 Trichloroethylene (TCE)과 Toluene 정화 효율 실험

  • 강현민;이민희;정상용
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2002.04a
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    • pp.191-194
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    • 2002
  • 토양증기추출(Soil Vapor Extraction)법을 이용하여 대표적 휘발성 NAPL (Non-aqueous phase liquid)인 TCE (trichloroethylene)와 toluene을 토양으로부터 제거하는 칼럼 실험을 실시하였다. 토양특성 및 증기추출 조건들이 정화효율에 미치는 영향을 규명하는데, 균질한 Ottawa sand와 실제 오염지역의 토양들을 직경 2.5cm, 길이 30cm인 유리 칼럼이 충진시켰으며, 빨갛게 염색된 TCE 또는 toluene 4 g이 주입되었다 공기 유량계를 설치하여 0.03L/min의 일정한 속도로 공기가 주입되도록 하고, 퍼지장치를 설치하여 주입 공기의 습윤도를 99% 이상으로 유지하였다. 가스크로마토그래피로 유출 가스 농도를 분석하였다. Ottawa sand로 충진된 칼럼실험에서는 매질의 입자크기, 함수율, 토양 내 오염물 체류시간 등을 변화시켜 실험을 반복하였다. TCE로 오염된 세립질 Ottawa sand 칼럼실험에서 유출 공기의 최대 농도는 조립질 Ottawa sand 칼럼의 유출 농도보다 약 20% 정도 감소하였고, 오염지역의 실제토양 칼럼실험에서는 최대유출농도가 조립질 Ottawa sand 칼럼의 농도보다 약 50% 감소하였으나, 20 liter공기 주입 후부터는 모두 비슷한 농도감소 현상을 나타내었으며, 초기 주입량의 90 % 이상이 제거되었다. 함수율증가에 따른 유출공기의 농도 감소는 거의 나타나지 않았으며, TCE 주입 후 7일 동안 방치하였다가 SVE를 실시한 칼럼 실험에서도 잔류하는 TCE의 양이 약간 증가하였지만 20 liter 공기 추출 후에는 초기 주입량의 90% 가, 40 liter공기 추출 후에는 98% 이상이 제거되었다. Toluene으로 오염된 칼럼 실험에서도 TCE와 비슷한 제거 경향을 나타냈으며 200 liter 공기 추출 후에는 오염물 초기 주입량의 98% 이상이 제거되었다. 본 실험 결과로부터 증기추출법을 이용한 TCE, toluene 정화 효율성이 규명되었으며, 휘발성 NAPL로 오염된 실제 토양을 복원하기 위한 SVE법의 적용가능성을 확인할 수 있었다.

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Fractionation of Exopeptidase from Viscera of Argentina Shortfin Squid, Illex argentinus (원양산 오징어(Illex argentinus) 내장으로부터 Exopeptidase의 분획)

  • Kim, Hye-Suk;Kim, Jin-Soo;Heu, Min-Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.8
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    • pp.1009-1017
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    • 2008
  • For the effective use of exopeptidase from squid viscera as food processing aids, the viscera of Argentina shortfin squid (Illex argentinus) were fractionated by various methods such as acetone treatment, ammonium sulfate treatment, anion exchange chromatography, and gel filtration. The positive exopeptidase fractions were obtained from the fraction II treated by cold acetone ($30{\sim}40%$, w/w), the fraction V by ammonium sulfate ($60{\sim}70%$ saturation), the fraction II (0.2 M NaCl) by anion exchange chromatography, and the fraction I ($30{\sim}50\;kDa$) by gel filtration. The specific activities of positive fractions from viscera of I llex argentinus against substrates were higher to LeuPNA than to ArgPNA. Total activity and recovery against LeuPNA of positive fraction by gel filtration were 1,867 U and 30.69%, respectively, which were the highest among those of positive fraction. The results suggested that the gel filtration chromatography method was the most efficient method for the fractionation of exopeptidase from viscera of Illex argentinus.

Diffusion Characteristics of Fatty Acid using Supercritical Fluid Chromatographic Method (초임계유체 크로마토그래피를 이용한 지방산의 확산특성 해석)

  • Lee, Seung Bum;Seong, Dae Hyung;Kim, Hyung Su;Hong, In Kwon
    • Applied Chemistry for Engineering
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    • v.7 no.6
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    • pp.1043-1052
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    • 1996
  • Supercritical fluid chromatographic method was recommended as an alternative separation method of fatty acids of the conventional method such as distillation or extraction. Although diffusion characteristics are varied by the carbon numbers and the degree of unsaturation of fatty acids, the quantitative data were so rare that the commercialization of supercritical fluid chromatographic method has been hindered. In this study, diffusion coefficients of fatty acids which are differently unsaturated are measured by CPB method in the range of 308.15K to 328.15K and 13MPa to 17MPa in supercritical carbon dioxide. A decrease in the binary diffusion coefficient was observed with an increase in temperature and pressure. Also, the decrease in the binary diffusion coefficient with increasing fluid density and viscosity. Wilke-Chang equation, Funazukuri empirical equation, and Matthews-Akgerman equation are used to correlate the experimental diffusion coefficients of fatty acids in supercritical carbon dioxide. Among the various theoretical equations, Matthews-Akgerman equation based on RHS theory was suggested as a more successful correlation model with experimental data.

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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 on the Simultaneous Analysis of Fat-Soluble Vitamins in Food Stuffs and Vitamin Products by High Performance Liquid Chromatography (고성능 액체 크로마토그래피에 의한 식품 및 비타민 제제중의 지용성 비타민의 동시 분석에 관한 연구)

  • Poongzag Kim;Chong-Hyeak Kim
    • Journal of the Korean Chemical Society
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    • v.33 no.1
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    • pp.46-54
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    • 1989
  • The extraction method and quantitative analysis for the fat-soluble vitamins present in food stuffs and vitamin products have been investigated. The simultaneous separation and analysis of the vitamins by reverse phase high performance liquid chromatographic method was conducted using an isocratic elution with methanol : water (95 : 5) eluent on a Novapak $C_{18}$ column. The detection of vitamins was achieved by a variable wavelength UV detector. To improve the detection sensitivity detection wavelengths were set at the highest absorption bands such as 330, 265, 285, and 290nm for the respective vitamins. The analysis for the fat-soluble vitamins was finished within 40 minutes. Alkaline hydrolysis and enzymatic hydrolysis were investigated for the sample preparation; and liquid-liquid extraction and liquid-solid extraction were attempted for the extraction of vitamins. Both hydrolysis methods were turned out to be appropriate for the analysis for vitamins A, D, and E, while for the analysis of vitamin K the enzymatic hydrolysis method demonstrated better results. Diethyl ether, pentane, and n-hexane were found to give higher recovery for the liquid-liquid extraction and silica cartridge for the liquid-solid extraction.

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Analysis of Half-life Time and Residual Concentration of Ethalfluralin Herbicide in Soils (토양 중 제초제 Ethalfluralin의 잔류 농도와 반감기 분석)

  • Han, Seong Soo;Rim, Yo Sup;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.168-178
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    • 1997
  • The optimum conditions for the residual analysis of the ethalfluralin herbicide on soils were investigated and the residues in soils were determined by gas chromatography with electron capture detector(GC-ECD). The soil samples extracted with methanol and dichloromethane and concentrated. The concentrated phase were redissolved with toluene and analyzed with GC-ECD after separated by cyanosilica gel Sep-Pak cartridge. From the standard addition experiments with 0.1 and 1.0ppm, the average recoveries were 92.8~101.2% and the detection limit was 0.004ppm. The half-life time of ethalfluralin in the soil(A) was 35 days in the laboratory and 7.2 days in the field test whereas it was 45 days and 9.7 days for each in case of soil(B).

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A Comparative Study on the Solvent Extraction and Supercritical Fluid Extration Method of ${\beta}-Ecdysone$ in Achyranthis radix (우슬 중 ${\beta}-Ecdysone$의 초임계추출법(SFE)과 용매추출법의 비교)

  • Kim, Mi-Ra;Kim, Myong-Seok;Shim, Jae-Han
    • Applied Biological Chemistry
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    • v.44 no.3
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    • pp.197-201
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    • 2001
  • Extraction efficiency of ${\beta}-ecdysone$ in Achyranthis radix was investigated using the methods of solvent extraction and supercritical fluid extraction (SFE). The optimum SFE conditions for the analysis of ${\beta}-ecdysone$ in A. radix were 300 atm, $80^{\circ}C$, 100 ml of extraction volume, and 20% ratio of modifier(methanol). As revealed through SFE, detection limit of ${\beta}-ecdysone$ in A. radix was 5 ng and recoveries of ${\beta}-ecdysone$ in A. radix shoots and root were $90.7{\sim}93.5%$ and $77.8{\sim}81.9%$, respectively. Recoveries of ${\beta}-ecdysone$ in A. radix shoots and root through solvent extraction were $76.4{\sim}93.0%$ and $80.6{\sim}93.1%$, respectively. ${\beta}-Ecdysone$ content was determined to be highest at 654.9 ppm in the first year A. radix roots harvested in August.

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A Sequential Separation Procedure for the Determination of Uranium, Thorium and Their Isotopes in Geological Materials (지질시료 중의 U과 Th 분석 및 자연방사성동위원소 측정을 위한 화학적 분리)

  • Kim, Jung Suk;Choi, Kwang Soon
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.307-314
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    • 1997
  • Inductively coupled plasma atomic emission spectrometry(ICP/AES) was used for the determination of uranium and thorium in geological materials. Samples were predecomposed by mixed acid digestion technique. The separation of the uranium and thorium was achieved by systematic solvent extraction with TTA(thenoyltrifluoroacetone) and TOA (tri-n-octylamine) and back extraction into HCl. The results for standard rock sample, NIST SRM 278, showed a good agreement with those certified from NIST as well as found values by other non-destructive techniques. Additional purification for extracted portions was carried out by anion exchange chromatography for measurement of several natural radioisotopes of uranium and thorium by alpha spectrometry.

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Extractive of Juniper Needle (향나무 잎의 추출성분)

  • Bae, Young-Soo;Si Chuan Ling;Kim, Jin-Kyu;Karchesy Joseph J.
    • Journal of Korea Foresty Energy
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    • v.24 no.2
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    • pp.24-30
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    • 2005
  • Four compounds, (+)-catechin (1), (-)-epicatechin (2), myricitrin (3), and hinokiflavone (4), were isolated from the needles of Juniperus occidentalis Hook. The structures of the isolated compounds were established by NMR and MS spectrometer. The antioxidant activity of the isolated compounds was determined by measuring free radical scavenging activity with DPPH and the results indicated that compound 1, 2, and 3 showed better activity than the controls, while compound 4 had weak activity compared with ${\alpha}-tocopherol$, BHT, and curcumin.

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Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (II). Determination of Pesticides by GLC (기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제2보). GLC에 의한 농약의 정량)

  • Taek-Jae Kim;Song-Ja Park;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.29 no.5
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    • pp.503-509
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    • 1985
  • Sixteen organochlorine pesticides extracted out from the crops and cleaned by solvent-solvent partitioning and Florisil column chromatography were determined by gas-liquid chromatography. The majority of the pesticides were well separated by being eluted through 5% QF-1 column and some of them through 3% OV-17 column and 2.596 DC-200/2.5% QF-1 column, and the eluted pesticides were detected by $^{63}Ni$ electron capture detector. The linear calibration curves were obtained for the most of pesticides while some curves were slightly deviated from the linearity. In the determination of 16 pesticides added to thirteen kinds of crops, the recoveries were showed over 85% for the most cases and the relative standard deviations of 5 analyses were less than 12.1%. The results were within the criteria of the AOAC method.

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