• Title/Summary/Keyword: 크로마토 그래피 추출

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Studies on the Elution Behavior and the Simultaneous Analysis of Some Metal-Dithiocarbamate Chelates by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속-Dithiocarbamate 킬레이트의 용리거동 및 동시분석에 관한 연구)

  • Dai Woon Lee;Yun Je Kim;Hyun Chul Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.32 no.3
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    • pp.211-226
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    • 1988
  • Liquid chromatographic behavior of several metal ions in dithiocarbamate(DTC) chelates were investigated by reversed phase high performance liquid chromatography on Novapak $C_{18}$ and ${\mu}$-Bondapak $C_{18}$ columns. The optimum conditions for the separation of DTC-metal chelate were examined with respect to the pH, shaking time, flow rate, extraction solvent, and mobile phase strength. The metal ions in mixtures at trace level, chelated with some dithiocarbamate derivatives were separated successfully on Novapak $C_{18}$ column using acetonitrile/methanol/water or acetonitril/water mixtures as mobile phases. It was found that all DTC metal chelates studied were eluted in an acceptable range of capacity factor values ($0{\leqq}log\;k'{\leqq}1$). Although several foreign metal ions were coexisted, high recovery and good precision were attained ; 97.0-106.7 % for the recovery and 0.98-3.41% for the coefficient of variation. Under the optimum analytical conditions, trace metal ions in the composite water samples were determined sucessfully with in relative error of about {\pm}$6.7 %.

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Analysis of Half-life Time and Residual Concentration of Fungicide Iminoctadine Triacetate in Soils (토양에서 살균제 Iminoctadine Triacetate의 반감기와 잔류농도의 분석)

  • Oh, Hae-Bum;Kim, Il-Kwang;Jeong, Seung-ll;Lim, Bang-Hyun;Han, Sung-Soo;Choi, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.34-40
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    • 2000
  • The optimum conditions for the half-life time and residual analysis of the iminoactadine triacetate fungicide on soils were investigated by using the gas chromatography. Iminoctadine triacetate(IOTA) was extracted from soils with 2.0 M-NaOH/methanol and chloroform. The extracted IOTA was derivatized to pyrimidine hexafluroacetylacetone by the acetylation and analyzed with GC/ECD after elimination of moisture and impurities on the Sep-Pak column. From the standard addition experiments with 0.1 and 1.0 ppm, the average recoveries were ranged from 83.8 to 93.2 % and the detection limit was 0.005 ppm. The half-life time of iminoctadine triacetate in the silty clay was 30 days in the laboratory and 19.5 days in the field test whereas it was 27 days and 17.5 days for each in case of silty loam.

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Analytical method of the polychlorinated biphenyls in soil using GC/ECD and GC/MS (GC/ECD 및 GC/MS을 이용한 토양 중 PCBs 분석방법 고찰)

  • Kim, Tae-Seung;Shin, Sun-Kyoung;Yoon, Jeong-Ki;Kim, Jong-Ha;Kim, Hyoung Seop;Lee, Jeong Ah
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.91-108
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    • 2007
  • This study was investigated both the Korean official soil test method and the international various methods for PCBs in soil sample. The analytical guideline of PCBs in contaminated soil were proposed based on the official soil test methods by discussing the extraction, column cleanup, instrumental conditions, quantification methods of peak matching and individual isomers. The total 28 soil samples were selected by consideration of PCBs-contamination, land use etc., and then analyzed using gas chromatography/electron capture detection (GC/ECD) and gas chromatography/mass spectrometry(GC/MS). In this study, the PCBs were not detected as peak matching method using GC/ECD, but PCBs detected $0.002{\sim}0.487{\mu}g/kg$ using GC/MS in background concentrations.

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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Bark Extractives of Several Populus Trees (몇가지 사시나무속 수종 수피의 추출성분)

  • Ham, Yeon-Ho;Kim, Jin-Kyu;Lee, Sang-Keuk;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.30 no.1
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    • pp.63-71
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    • 2002
  • The bark of P. alba × glandulosa, P. euramericana and P. nigra × maximounczii F1, several Populus trees, were collected, extracted with acetone-H2O(7:3, v/v), fractionated with hexane, chloroform and ethylacetate, and freeze dried to give some dark brown powder. Each fraction of the powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents and then identified by thin layer chromatography using TBA and 6% acetic acid as developing solvents. The structures of the isolated compounds were characterized by 1H, 13C and 2D-NMR tools including mass spectrometry. Most of the compounds were flavonoids and salicin derivatives as follows: (+)-catechin, taxifolin, aromadendrin, eriodictyol, naringenin, sakuranetin, sakuranetin-5-O-𝛽-D-glucopyranoside, neosaturanin, salireposide, p-coumaric acid, and aesculin from P. alba × glandulosa, (+)-catechin, salireposide, populoside and salicortin from P. euramericana and (+)-catechin, quercetin, padmatin, salireposide, populoside and salicortin from P. nigra × maximounczii F1.

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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Extractives from the Needles of Torreya (벼자나무 잎의 추출성분)

  • Kim, Jin-Kyu;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.29 no.4
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    • pp.53-59
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    • 2001
  • The needles of torreya(Torreya nucifera S. et Z) were collected, extracted with acetone-$H_2O$(7:3, v/v), fractionated with hexane, chloroform and ethylacetate, and freeze dried to give some dark brown powder. The ethylacetate soluble mixture was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. Most of the needle extractives were flavan and its methyl ether compounds such as (+)-catechin, (-)-epicatechin, (+)-gallocatechin, (-)-epigallocatechin, 3'-O-methyl-(+)-catechin and 3'-O-methyl-(-)-epicatechin including protocatechuic acid, one of benzoic acids. $^1H$- and $^{13}C$-NMR, NOE and CI-MS analyses were performed to elucidate the structures of the isolated compounds.

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Determination of 4-Nitrotoluene Exposure in Water, Soil and Sediment by Gas Chromatography- Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 토양, 저질 및 수질시료 중 4-Nitrotoluene의 노출평가)

  • Jeon Hee Kyung;Choi Hae Yeon;Ryu Jae-Chun
    • Environmental Analysis Health and Toxicology
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    • v.20 no.2 s.49
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    • pp.123-131
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    • 2005
  • 본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 4-Nitrotoluene(4-NT)을 분석하는 방법을 확립하고자 하였다. 4-NT은 수질 시료(100mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료(10g)에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 4-NT의 회수율은 $99.1\%$ 이상이였으며 토양에서의 회수율(recovery)은 약 $110\%$를 보였고 재현성 (relative standard deviation)은 $11.99\%$ 이하였다. 검정곡선은 상관계수$(R^2)$값이 수질과 토양 모두에서 0.994이상의 좋은 직선성을 보여주었다. 본 연구에서 채취한 수질 43개 지역, 토양 35개 지역 및 저질 11개 지역의 모든 시료에서 4-NT은 검출한계 이하로 나타났다. 이 분석방법은 환경 중에 미량으로 존재하는 4-NT의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

Characterization of Isoflavone in Callus Culture from Glycine max (L.) Merr. Phytoplacenta (대두 태좌조직의 캘러스배양에 의한 Isoflavone 동정)

  • Kang, Hyo-Seok;Min, Ji-Aee;Jung, Hae-Soo;Lee, Jeong-Hun;Shin, Dong-Sun;Kim, Eun-Ae;Kim, Young-Jun;Moh, Sang-Hyun
    • Proceedings of the KAIS Fall Conference
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    • 2012.05a
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    • pp.235-238
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    • 2012
  • 본 연구는 Glycine max (L.) Merr.의 태좌부위를 순수 분리하여 callus 세포를 유도하고 2차 대사산물인 isoflavone류에 속하는 daidzein의 생산성을 증진시킬 수 있는 방법을 찾는데 있다. 배양된 callus를 다양한 용매를 사용하여 추출하고, 추출물을 액체 크로마토그래피로 분석해 daidzein 함량의 차이를 확인하였다. 또한 핵자기공명분광법으로 50% 에탄올 추출물 내에 daidzein이 함유되어 있음을 증명하였다.

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Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization (Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석)

  • Ahn, Yun Gyong;Lee, Jee Yeon;Kim, Jeehyeong;Hong, Jongki
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.458-465
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    • 2003
  • The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.