• Title/Summary/Keyword: preparative TLC

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Analysis of Essential Oil from Chrysanthemum sibiricum and the Comparision with Essential Oils from Some Chrysanthemum spp. (구절초의 정유분석 및 동속생약 정유와의 비교연구)

  • Shin, Soon-Hee;Choi, Young-Im
    • Korean Journal of Pharmacognosy
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    • v.13 no.4
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    • pp.153-156
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    • 1982
  • The essential oil fraction of Chrysanthemum sibiricum Turcz. (Compositae) was analysed by means of TLC and GLC. Utilizing silicagel column chromatography, a blue-color compound was isolated, and purified by preparative TLC. The obtain compound had the same Rf-value on TLC and exactly same UV-visible and IR spectra with that of chamazulene isolated from Matricaria chamomilla L. The composition of the essential oil was also compared with those from flowers of Chrysanthemum indicum L. and Chrysanthemum morifolim Ramatuelia.

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Studies on the Carotenoid Pigment in the Abdominal Skin of Bombina Orientalis(II). Occurrence of ${\alpha}$-Cryptoxanthin(3-hydroxy-${\alpha}$-carotene) in the Abdominal Skin of Bombina Orientalis (무당개구리의 복피 Carotenoid 색소에 관한 연구 (제2보). ${\alpha}$-Cryptoxanthin(3-hydroxy-${\alpha}$-carotene)의 분리 및 확인)

  • Chang Sae Hee;Chong Ui Chun
    • Journal of the Korean Chemical Society
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    • v.18 no.5
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    • pp.368-372
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    • 1974
  • Dark red extract of abdominal skin of Bombina Orientalis was separated and purified with TLC, PLC(preparative thin layer chromatography) and column chromatography. Through the physical and chemical properties, visible and infrared spectral characteristics the third major pigment was identified as ${\alpha}$-cryptoxanthin(3-hydoroxy-${\alpha}$-carotene)

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Identification of triacylglycerols in coix seed extract by preparative thin layer chromatography and liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry

  • Sim, Hee-Jung;Lee, Seul gi;Park, Na-Hyun;Kim, Youna;Cho, Hyun-Woo;Hong, Jongki
    • Analytical Science and Technology
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    • v.30 no.2
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    • pp.102-111
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    • 2017
  • Here we reported a methodology for identification of triacylglycerols (TAGs) and diacylglycerols (DAGs) in coix seed by preparative thin layer chromatography (prep-TLC) and non-aqueous reversed-phase liquid chromatography (NARP LC)-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS/MS). Lipid components were extracted from coix seed by reflux extraction using n-hexane for 3 hr. TAGs and DAGs in coix seed extract were effectively purified and isolated from matrix interferences by prep-TLC and then analyzed by LC-APCI-MS and MS/MS for identification. TAGs were effectively identified taking into consideration of their LC retention behavior, APCI-MS spectra patterns, and MS/MS spectra of $[DAG]^+$ ions. In MS/MS spectra of TAGs, diacylglycerol-like fragment $[DAG]^+$ ions were useful to identify TAGs with isobaric fragment ions. Based on an established method, 27 TAGs and 8 DAGs were identified in coix seed extract. Among them, 15 TAGs and 8 DAGs were for the first time observed in coix seed. Interestingly, some of TAGs isolated by prep-TLC were partly converted into DAGs through probably photolysis process during storing in room temperature. Thus, degradation phenomenon of TAGs should be considered in the quality evaluation and nutritional property of coix seed. LC-APCI-MS/MS combined with prep-TLC will be practical method for precise TAG and DAG analysis of other herbal plants.

Characteristic Component of Rehmanniae Radix Preparata Compared to Rehmanniae Radix and Rehmanniae Radix Crudus (숙지황, 건지황 및 생지황 중 숙지황의 특이성분 검색)

  • Hong, Sun Pyo;Kim, Young Chul;Kim, Kyeong Ho;Park, Jeong Hill;Park, Man Ki
    • Analytical Science and Technology
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    • v.6 no.4
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    • pp.401-404
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    • 1993
  • Rehmanniae Radix Preparata is manufactured with Rehmanniae Radix accoding to KP V. For quality control of Rehmanniae Radix Preparata, its standard component is required. The methanol extracts of Rehmanniae Radix crudus, Rehmanniae Radix, Rehmanniae Radix preparata were divided into the three groups of ether, butanol and aqueous fraction by liquid-liquid separation. In the comparative TLC of ether fraction, the characteristic component of Rehmanniae Radix preparata was found. The ether fraction was evaporated and separated on the silica gel column with chloroform-methanol and further separated on the preparative silica gel TLC with chloroform-methanol-water. The component was illucidated as 5-(hydroxymethyl)-2-furancarboxaldehyde(5-HMF). 5-HMF was not found in Rehmanniae Radix crudus and found in Rehmanniae radix in much less Quantities than Rehmanniae Radix Preparata.

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Investigation of brassinosteroid substances in the shoots of japonica type Korean rice (일반계 벼의 brassinosteroid활성물질 검색)

  • Hyun, Kyu-Hawn;Park, Keun-Hyung
    • Applied Biological Chemistry
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    • v.33 no.4
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    • pp.307-314
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    • 1990
  • Brassinosteroid-like substances in two japonica type Korean rices were investigated. The extracts from the shoots at the maximum tillering stage were purified by solvent fractionation, silica gel adsorption chromatography, Sephadex LH-20 chromatography, charcoal adsorption chromatography, preparative TLC, Bondesil chromatography and HPLC of normal phase and reverse phase, successively. Biological activity of each purification step were monitored by the rice lamina inclination test. Two cultivars tested in this experiment produced brassinosteroids and endogenous brassinosteroids showing similiarity between two cultivars.

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Volatile Components of Pinenut (잣의 향기성분(香氣成分)에 관한 연구(硏究))

  • Kim, Yong-Kap;Chung, Kyu-Neung;Ishi, Hirosh;Muraki, Shigeru
    • Korean Journal of Food Science and Technology
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    • v.18 no.2
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    • pp.105-109
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    • 1986
  • Volatile components of pinenut were identified. Pinenut was extracted by simultaneous distillation and extraction method after Soxhlet extraction. The odor profile of the extract was very similar to that of pinenut. This extract was then fractionated into four fractions by Preparative TLC. These all fractions were analyzed by a combination of glass capillary gas chromatography (FTD, FID capillary GC) and mass spectrometry. One hundred and nine components, including 26 hydrocarbons,17 esters,16 aldehydes,12 ketones,31 alcohols, 11 bases, 2 acids and 3 miscellaneous components were identified.

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Isolation of Angiotensin Converting Enzyme Inhibitor from Doenjang (전통된장으로부터 Angiotensin Converting Enzyme 저해물질의 분리)

  • Kim, Seung-Ho;Lee, Yun-Jin;Kwon, Dae-Young
    • Korean Journal of Food Science and Technology
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    • v.31 no.3
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    • pp.848-854
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    • 1999
  • Inhibitory compounds of angiotensin converting enzyme (ACE) were separated from Doenjang (traditional Korean fermented soybean paste). Water extracts from Doenjang which showed ACE inhibitory activity were separated with gel permeation chromatography (GPC), in which two fractions with high ACE inhibitory activities were obtained. The first fraction from GPC was further isolated by semi-preparative reverse phase preparative-HPLC (high performance liquid chromatography) and 2-dimensional electrophoresis/thin layer chromatography (TLC). The purified spot had molecular weight of 759 daltons and ninhydrin-positive non-peptide. The second fraction from GPC was also further isolated by semi-preparative reverse phase HPLC and $NH_2-column$ HPLC. One fraction with high ACE inhibitory activity was purified and characterized. Molecular weight of this fraction by LC-MS was 272.34 daltons. The active fraction was identified as Arg-Pro with ACE $IC_{50}$ of $92\;{\mu}M$.

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Production and Characterization of Cathepsin B Inhibitor from Streptomyces chromofuscus SMF28 (Streptomyces chromofuscus SMF28을 이용한 Cathepsin B 저해물질의 발효생산 및 특성분석)

  • Lee, Hyoun Suk;Kim, In Seop;Yoon, Sung Joon;Lee, Kye Joon
    • Microbiology and Biotechnology Letters
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    • v.23 no.5
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    • pp.602-608
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    • 1995
  • The aim of the present research program was to construct an optimum fermentation system and to characterize the properties of cathepsin B inhibitor from Streptomyces chromofuscus SMF28. Glucose and casitone were proved to be good carbon source and nitrogen source, respectively. The production of inhibitor was high at lower concentration than 10 mM of inorganic phosphate. The optimum temperature and pH for the production of inhibitor were 30$\circ$C and pH 7, respectively. The production of inhibitor was related to mycelial growth and was affected by medium composition. The inhibitor in culture filtrate of S. chromofuscus SMF28 was purified by butanol extraction, silica gel chromatography, Amberlite IRC-50 (H$^{+}$ form) chromatography, preparative TLC, and preparative HPLC. From amino acid analysis and UV, IR, $^{1}$H-NMR spectroscopic analysis, the inhibitor was identified as a peptide containing valine and phenylalanine derivative.

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Isolation and Purification of Tyrosinase Inhibitors from the Seeds of Thuja orientalis L. (백자인(Thuja orientallis L.)으로부터 tyrosinase 저해제의 분리 및 정제)

  • Lee, Jun-Young;Park, Sang-Won
    • Food Science and Preservation
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    • v.7 no.4
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    • pp.409-413
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    • 2000
  • Previously, the methanolic extracts of thirty Korean medicinal plant seeds were screened for tyrosinase inhibitors using a rapid and simple TLC method, which was superior to a conventional spectrophotometrical in vitro assay. As a result, the methanolic extracts of Thuja orientalis seeds was found to have strong tyrosinase inhibitory activity. To isolate active tyrosinase inhibitors, the seeds were defatted with n-hexane under reflux, and then extracted twice with methanol under reflux at 90$^{\circ}C$. The methanolic extract was evaporated to a small volumn in vacuo, and then successively fractionated with ether, ethyl acetate and n-butanol. The ether extract showing significant tyrosinase inhibitory activity was solubilized with 5% NaHCO$_3$and then acidified with 6N HCI. The ether souble acidic fraction was successively ohromatographed on silica gel, Sephadex LH-20 and preparative TLC. Among four compounds isolated, two of them showed stronger tyrosinase inhibitory activity, comparable to that of L-ascorbic acid (IC$\sub$50/=28$\mu\textrm{g}$/$m\ell$). These results suggest that Thuja orientalis seeds may be useful as potential sources of antibrowning agents in fruits and vegetables, and anti-melanoma agents in cosmetics and phamaceuticals.

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Detection of a Quorum-Sensing Inhibitor from the Natural Products (천연물로부터 Quorum Sensing 저해제의 탐색)

  • Kim, Tae-Woo;Cha, Ji-Young;Lee, Jun-Seung;Min, Bok-Kee;Baik, Hyung-Suk
    • Journal of Life Science
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    • v.18 no.2
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    • pp.206-212
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    • 2008
  • The quorum sensing (QS) regulatory network has been the subject of extensive studies during recent years and has also attracted a lot of attention because it both positively and negatively regulates various putative virulence factors, although initially considered to be a specialized system of Vibrio fischeri and related species. In this study, to identify the novel materials which inhibit QS system of microorganisms, extracts of eighteen natural products were tested by bioassay using N-(3-oxohexanoyl)-$_L$-homoserine lactone and N-(3-oxooctanoyl)-$_L$-homoserine lactone synthesized in this experiment and an Agrobacterium tumefaciens NT1 biosensor strain containing a traI::lacZ fusion. The result indicated that the extracts of cabbage, leek, and onion exhibited the QS inhibition activity. Thus, materials contained in the extracts were isolated via recycling preparative HPLC and were purified via a JAIGEL-LS255 column. The common fraction corresponding to a peak of the 83 min point of them quenched the quorum sensing of A. tumefaciens NT1 biosensor strain in ABMM containing X-gal and was designated quorum sensing inhibitor-83 min (QSI-83). The QSI-83 exhibited the heat stability and did not inhibit the growth of A. tumefaciens NTl. Furthermore, thin layer chromatography (TLC) results suggested that these novel materials may be antagonists of N-acyl homoserine lactone or may inhibit the QS autoinducer synthesis by Pseudomonas syringae pv. tabaci.