• Title/Summary/Keyword: open column chromatography

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Study on the Development of Analytical Method (Multi-Pesticide Residue Method) for Organophosphate Pesticides (유기인제 농약 분석 방법 (Multi-Pesticide Residue Method) 개발에 관한 연구)

  • 이봉헌;김우성
    • Journal of Environmental Science International
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    • v.6 no.2
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    • pp.183-187
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    • 1997
  • Organophosphate pesticides were extracted with 70% acetone and then transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil. The florial extract was analyzed by gas chromatography with nitrogen-phosphorus detector(GC/NPD). Recoveries of the 18 organophosphate pesticides were ranged from 88.7% to 100. 0% for the narrow-bore capillary GC(Ultra-21. The minimum detectable level of this analytical method was 0.019 - 0.035 mg/kg. Sample throughput(extraction, open-column chro- matography, and GC analysts) was decreased considerably (8h per sample).

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Development of Open Tubular Capillary Columns for Ion Chromatography (이온 크로마토그래피용 Open Tubular Capillary 컬럼의 개발)

  • Pyo, Dong Jin;Kim, Ho Hyun
    • Journal of the Korean Chemical Society
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    • v.45 no.2
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    • pp.143-148
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    • 2001
  • In this study, open tubular capillary columns for ion charomatography were developed to analyze trace amount of ions in samples. When small I,D. capillary column length is 1.0~5.0 m. The capillary columns were made using fused silica capillary(I.D:50㎛) and DMEOHA latex particles. The new conductivity cell and suppressor were also developed and made for capillary column ion chromatography. When several anions(fluoride, nitrite, nitale,chlorate,phosphte, sulfate) were analyzed using these capillary columns. reproducible and good chromatograms were obtained.

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Extraction and Bioassay of Allelochemicals in Jerusalem Artichoke

  • Sungwook Chae;Lee, Ho-Jin
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.309-316
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    • 2001
  • Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

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Rational and efficient approach to the preparation of the active fractions of Scutellaria baicalensis (황금(Scutellaria baicalensis) 유효분획물 제조의 합리적이고 효율적인 접근방법)

  • Kim, Doo-Young;Kim, Won Jun;Kim, Jung-Hee;Oh, Sei-Ryang;Ryu, Hyung Won
    • Journal of Applied Biological Chemistry
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    • v.62 no.1
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    • pp.31-38
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    • 2019
  • Scutellaria baicalensis Georgi (Scutellariae Radix) has been widely used as a dietary ingredient and traditional herbal medicine such as diuretic, hyperlipidemia, antibacterial, anti-allergy, anti-inflammatory and anticancer properties. In this study, the isolation of biomarkers or bioactive compounds from complex S. baicalensis extracts represents an essential step for de novo identification and bioactivity assessment. The bioactive fraction consisted of eight compounds which was chromatographed on an analytical high performance liquid chromatography column using two different gradient runs. A simulative replacement of the analytical column with a medium pressure liquid chromatography and open column allowed the determination of gradient profile to allow sufficient separation in the preparative scale. From the optimized method, eight standard compounds have been identified in the fractions. In addition, MS, UV, HRMS detection was provided by ultraperformance liquid chromatographyequadrupole time-of-flight mass spectrometry (UPLC-QTof-MS) of all fractions. Therefore, this scale up procedure was successfully applied to a S. baicalensis extract.

Multi-Pesticide Residue Method for Organopesticide Analysis (유기농약 분석을 위한 Multi-Pesticide Residue Method)

  • 김우성;이봉헌
    • Journal of Environmental Science International
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    • v.6 no.4
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    • pp.385-389
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC /ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pegticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azlnphos-methyls. The minimum detectable levels of this analytical method were low(0.021-0.058mg/kg).

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Novel Purification Method of Kv 4.2 Potassium Channel from Rat Brain Membrane

  • Park, Sung-Soo
    • Biomedical Science Letters
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    • v.18 no.2
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    • pp.96-103
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    • 2012
  • Kv 4.2 ion channel protein has an ability to open at subthreshold membrane potentials and to recover quickly from inactivation. That is very important for neuronal signal transmission in vertebrate brain. In order to purify Kv 4.2 protein, the novel purification methods were experimented. The purification procedure utilized chromatography on DE-52 ion exchange column and affinity chromatography on a WGA-Sepharose 4B, and Kv 4.2 affinity column chromatography. It was found that 0.5% (wt./vol.) Triton X-100 detergent in lysis buffer worked well for Kv 4.2 protein solubilization from rat brain membrane. Protein quantitative determination was conducted by BCA method at 562 nm for each purification step to avoid determination interference of protein at 280 nm by detergent. The confirmation of Kv 4.2 existence and amount is performed using by SDS-PAGE/immunoblotting or 96-well dot blotting. The Kv 4.2 without interacting protein that contains carbohydrate, was purified from novel biochemical 3-steps purification method for further research.

Identification of Dammarane-type Triterpenoid Saponins from the Root of Panax ginseng

  • Lee, Dong Gu;Lee, Jaemin;Yang, Sanghoon;Kim, Kyung-Tack;Lee, Sanghyun
    • Natural Product Sciences
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    • v.21 no.2
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    • pp.111-121
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    • 2015
  • The root of Panax ginseng, is a Korea traditional medicine, which is used in both raw and processed forms due to their different pharmacological activities. As part of a continued chemical investigation of ginseng, the focus of this research is on the isolation and identification of compounds from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, semi-preparative-high performance liquid chromatography, Fast atom bombardment mass spectrometric, and nuclear magnetic resonance. Dammarane-type triterpenoid saponins were isolated from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, and semi-preparative-high performance liquid chromatography. Their structures were identified as protopanaxadiol ginsenosides [gypenoside-V (1), ginsenosides-Rb1 (2), -Rb2 (3), -Rb3 (4), -Rc (5), and -Rd (6)], protopanaxatriol ginsenosides [20(S)-notoginsenoside-R2 (7), notoginsenoside-Rt (8), 20(S)-O-glucoginsenoside-Rf (9), 6-O-[$\alpha$-L-rhamnopyranosyl(1$\rightarrow$2-$\beta$-D-glucopyranosyl]-20-O-$\beta$-D-glucopyranosyl-$3\beta$,$12\beta$, 20(S)-dihydroxy-dammar-25-en-24-one (10), majoroside-F6 (11), pseudoginsenoside-Rt3 (12), ginsenosides-Re (13), -Re5 (14), -Rf (15), -Rg1 (16), -Rg2 (17), and -Rh1 (18), and vinaginsenoside-R15 (19)], and oleanene ginsenosides [calenduloside-B (20) and ginsenoside-Ro (21)] through the interpretation of spectroscopic analysis. The configuration of the sugar linkages in each saponin was established on the basic of chemical and spectroscopic data. Among them, compounds 1, 8, 10, 11, 12, 19, and 20 were isolated for the first time from P. ginseng root.

Multi-Pesticide Residue Method for Analysis of Organochlorine and Organophosphorus Pesticide

  • Bonghun Lee;Woo
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 1997.10a
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    • pp.37-39
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

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백편두(Dolichos lablab)로부터 elastase 및 serine protease inhibitor의 분리, 정제 및 그 특성에 관한 연구

  • 최수경;구선향;홍승철;이복률
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1996.04a
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    • pp.165-165
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    • 1996
  • 균의 감염에 의해 유도되는 패혈성 shock는 균이 분비하는 elastase가 관여하며, 외부에서 serine pretense inhibitor의 biopolymer의 투여로 균에 의해 유도된 패혈성 shock를 억제시킬 수 있다고 보고되고 있다. 이에 본 연구진은 패혈성 치료제의 개발의 목적으로, 국내에서 민간 약으로 많이 이용되고 있는 백편두로부터 새로운 elastase inhibitor를 분리, 정제하여 부분 아미노산 서열 및 특성을 조사하였기에 발표하고자 한다. 백편두 추출액을 여러 차례에 걸쳐 column chromatography을 수행하면서 얻어지는 각 fraction에 대하여 elastase MCA-기질 및 trypsin MCA-기질을 이용하여 활성 측정 후 elastase 기질 및 trypsin 기질에 대하여 활성을 억제하는 fraction들을 모아 $C_{18}$ open column chromatography 및 $C_{18}$ HPLC 과정을 수행하여 2종류의 trypsin 활성 억제 물질과 1종류의 elastase inhibitor를 분리, 정제하여 각각을 Ti1, Ti2 및 Ti3로 명명하였다. 전기영 동 상에서 단일 hand를 확인한 후 각각의 inhibitor들의 부분 아미노산 서열을 결정하였다.

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Phytochemical Constituents from the Seeds of Lithospermum erythrorhizon

  • Park, Jun-Yeon;Lee, Sul-Lim;Han, Saem;Kim, Hye-Min;Lee, Jeong-Min;Ahn, Young-Hee;Lee, Sook-Young;Lee, Sang-Hyun
    • Natural Product Sciences
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    • v.15 no.4
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    • pp.181-184
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    • 2009
  • Phytochemical constituents were isolated from the seeds of Lithospermum erythrorhizon through open column chromatography and prep-HPLC. Their structures were identified as ${\beta}$-sitosterol (1), daucosterol (2), luteolin (3), and allantoin (4) on the basis of spectroscopic analysis. Among them, luteolin (3) was isolated for the first time from the plant.