• Title/Summary/Keyword: TLC analysis

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Simultaneous Identification/Determination System for Sildenafil, Homosildenafil, Vardenafil and Tadalafil as Adulterants in Foods (식품중 불법함유된 발기부전치료제 성분 검출을 위한 동시분석법 연구)

  • Jang, Jae-Hee;Park, Kun-Sang;Park, Hye-Kyung;Koo, Yong-Eui;Choi, Youn-Ju;Hwang, In-Kyung;Kim, Dai-Byung
    • Journal of Food Hygiene and Safety
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    • v.18 no.4
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    • pp.195-201
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    • 2003
  • An easily available, simultaneous identification/determination procedure for sildenafil, homosildenafil, tadalafil, vardenafil in adulterated health related foods was established by using a combination of three different analytical methods; thin layer chromatography(TLC), liquied chromatography-mass spectrometry (LC/MS) and high-performance liquied chromatography (HPLC)/photo-diode-array detector. The sample solution for TLC was applied to silica gel 60 $F_{254}$ plates with ethylacetate/acetonitrile/25%ammonia (90:10:5) as a developing solvent. Spots were located under UV radiation at 254 nm and dragendolfs reagent. Mass spectra of the compounds by LC/MS were investigated with electrospray ionization (ESI) interface, under positive ion mode. The HPLC analysis was performed on a column of capcell pack $C_{18}$ (UG120, 4.6${\times}$250mm I.D. 5 ${\mu}$m)with 0.1% sodium 1-hexansulfonate (in 0.1% phosphoric acid)/acetnitrile (73:27) as a mobile phase, and effluent was minitored with a photo-diode-applied to commercial foods, Sildenafil content was inthe range of 0.4mg/g~360.9 mg/g from 7 out of 35 samples. Homosildenafil content was in the range of 2.2 mg/g~336.0 mg/g from 7 out of 35 samples. Tadalafil content was 429.3 mg/g, 9.6 mg/500 mg from 2 out of 35 samples. The procedure described here is available for the screening of sildenafil, homosildenafil, tadalafil, vardenafil.

Identification of NMR Data for ginsenoside Rg1 (Ginsenoside Rg1의 NMR 데이터 동정)

  • Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Park, Hee-Jeong;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.32 no.4
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    • pp.291-299
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    • 2008
  • The fresh ginseng roots were extracted in aqueous methanol (MeOH), and the obtained extracts were partitioned using ethyl acetate (EtOA), n-butanol (n-BuOH), and water, successively. The repeated silica gel column chromatography for n-BuOH fraction afforded a purified ginsenoside $Rg_1$. The physico-chemical, spectroscopic and chromatographic data of ginsenoside $Rg_1$, such as crystallization characteristics, melting point, specific rotation, infrared spectrometry (IR) data, fast atom bombardment/mass spectrometry (FAB/MS) data, nuclear magnetic resonance (NMR) data, retention factor (Rf) in thin layer chromatography (TLC) experiment, and retention time (r.t.) in HPLC analysis, were measured and compared with those reported in literatures. Especially, the previous literatures reported different data for ginsenoside $Rg_1$ in the $^{1}H-$ and $^{13}C$-NMR experiments. This paper gives the exactly assigned NMR data through 2D-NMR experiments, such as $^{1}H-^{1}H$ correlation spectroscopy (COSY), hetero nuclear single quantum correlation (HSQC), and hetero nuclear multiple bond connectivity (HMBC).

Preparation of $Gal^3Man_4(6^3-mono-{\alpha}-D-galacto-pyranosyl-{\beta}-mannotetraose)$ by Bacillus sp. ${\beta}-mannanase$ and Growth Activity to Intestinal Bacteria (Bacillus sp.유래 ${\beta}-mannanase$에 의한 $Gal^3Man_4(6^3-mono-{\alpha}-D-galacto-pyranosyl-{\beta}-mannotetraose)$ 조제 및 장내세균에 대한 생육활성)

  • Kim, Sang-Woo;Park, Gwi-Gun
    • Applied Biological Chemistry
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    • v.47 no.4
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    • pp.379-383
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    • 2004
  • For the elucidation of substrate specificity to the brown copra meal by Bacillus sp. ${\beta}-mannanase.$, the enzymatic hydrolysate after 24 hr of reaction was heated in a boiling water bath for 10 min, and then centrifuged to remove the insoluble materials from hydrolysates. The major hydrolysates composed of D.P 5 and 7 galactosyl mannooligosaccharides. For the separate of galactosyl mannooligosaccharides, the supernatant solution of 150 ml was put on a first activated carbon column. The column was then washed with 5 l of water to remove mannose and salts. The oligosaccharides in the column were eluted by a liner gradient of $0{\sim}30%$ ethanol, at the flow rate of 250 ml per hour. The sugar composition in each fraction tubes was examined by TLC and FACE analysis. The combined fraction from F3 was concentrated to 30 ml by vacuum evaporator. Then put on a second activated carbon column. The oligosaccharides in the column were eluted by a liner gradient of $0{\sim}30%$ ethanol (total volume: 5 l), at the flow rate of 250 ml per hour. The eluent was collected in 8 ml fraction tubes, and the total sugar concentration was measured by method of phenol-sulfuric acid. The major component of F2 separated by 2nd activated carbon column chromatography were identified $Gal^3Man_4(6^3-mono-{\alpha}-D-galactopyranosyl-{\beta}-mannotetraose)$. To investigate the effects of brown copra meal galactomannooligosaccharides on growth of Bifidobacterium longum, B. bifidum were cultivated individually on the modified-MRS medium containing carbon source such as $Gal^3Man_4$, compared to those of standard MRS medium.

Anatomical Toxicity of Pufferfishes, Chinese Fugu obscurus and Indonesian Lagocepalus wheeleri (인도네시아산 흰 밀복 및 중국산 황복의 조직별 독성)

  • 김동수;이화정;이명자;이문조;김현대
    • The Korean Journal of Food And Nutrition
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    • v.9 no.4
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    • pp.361-365
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    • 1996
  • Indonesian Lagocephalus wheeleri ("White-milbog") and Chinese Fugu obscurus ("Hwang-bong") puffers were dissected into liver, intestine, ovary or testis, skin and muscle for assay of toxicity, Also, the toxins from the puffer liver were partially purified and analyzed. The frequency of toxic specimens for Lagocephalus wheeleri was 20, 40, 0 and 10%, in terms of liver, intestine, skin and muscle, respectively; and average toxicity was 5.5$\pm$0.9(Mean$\pm$S.E.), 11.8$\pm$4.2, 2.2$\pm$0.1 and 3.0$\pm$0.8 MU/g, respectively. All of Fugu obscurus specimens had toxicity ranging between 2 and 210 MU/g. The frequency of toxicity in intestine and ovary, both 100% was to be higher percentage tan that of other tissues. The toxinsgave two spots tetrodotoxin(TTX) and anhydro-tetrodotoxin(anh-TTX) on TLC. Also, the toxin of each puffer species showed two spots in electrophoresis. In HPLC analysis of Fugu obscurus, the toxins showed TTX, 4-epi-TTX and anh-TTX.epi-TTX and anh-TTX.

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Isolation an Identification of the Active Compounds from Green Mustard Leaves against Oxidative Stress in Bovine Brain Tissue (청겨자채 추출물의 뇌조직 내 Oxidative Stree 억제활성물질의 동정)

  • 이근종;김미리;심재석;황재관
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.30 no.5
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    • pp.943-948
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    • 2001
  • Green mustard leves were found to effectively prevent lipid peroxidation of bovine-brain tissue by ascor-bate/Fe system, The 50% methanol extracts mustard leaves were separated into four solvent faction using n-hexane,. EtOAc, n-BiOH and water. Then n-BiOH fraction exclusively exhibited the antioxidative activities at concentration above 100 $\mu\textrm{g}$/mL/ The n-BuOH fraction was further isolated to a single compound using TLC analysis and silica gel chromatography. The active antiodidative compounds were identified as sinapic acid methyl ester and ferulic acid methyl ester by $^{1}$H-NMR and $^{13}$ C-NMR, The sinapic acid methyl ester and ferulic acid methyl ester were prepared by methylating of sinapic acid and ferulic acid with diazomethane. The results strongly suggested that sinapic acid and ferulic acid could be emplyed as a potential antioxiative agents for preventing the bovine brain lipid peroxidation. lipid peroxidation.

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Lichen Flora around the Korean Antarctic Scientific Station, King George Island, Antarctic

  • Kim, Ji-Hee;Ahn, In-Young;Hong, Soon-Gyu;Andreev, Mikhail;Lim, Kwang-Mi;Oh, Mi-Jin;Koh, Young-Jin;Hur, Jae-Seoun
    • Journal of Microbiology
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    • v.44 no.5
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    • pp.480-491
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    • 2006
  • As part of the long-term monitoring projects on Antarctic terrestrial vegetation in relation to global climate change, a lichen floristical survey was conducted around the Korean Antarctic Station (King Sejong Station), which is located on Barton Peninsula, King George Island, in January and February of 2006. Two hundred and twenty-five lichen specimens were collected and sixty-two lichen species in 38 genera were identified by morphological characteristics, chemical constituents, TLC analysis and ITS nucleotide sequence analysis.

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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Analysis and Bioremediation for the Soil Contaminated by Lubricant (윤활유 오염토양의 분석 및 생물학적 복원)

  • Lee, Jae-Young;Jung, Woo-Sung;Cho, Young-Min;Choi, Sung-Kyou;Ko, Sung-Hwan;Kim, Hee-Man
    • Proceedings of the KSR Conference
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    • 2007.11a
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    • pp.1843-1845
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    • 2007
  • As the preservation law of soil environment has reinforced, several soil remediation projects have been performing for railroad sites. One of the main sources of soil contamination is the leakage of diesel from locomotives or underground storage tank. Also, the lubricant used to maintain turnouts causes railroad soil contamination. The purpose of this study was to develop the analysis and the remediation method for lubricant-contaminated soil. The lubricant in the contaminated soil was analyzed qualitatively and quantitatively by TLC (Thin Layer Chromatography) and GC (Gas Chromatography), respectively. The organic pollutants were removed from the soil using microorganisms degrading lubricant. Hereafter it will be necessary to apply this bioremediation method in the railroad field.

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Production of Tropane Alkaloids by Hairy Root Cultures of Scopolia parviflora (미치광이풀(Scopolia parviflora)의 모상근 배양에 의한 Tropane Alkaloid 생산)

  • 안준철
    • Journal of Plant Biology
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    • v.36 no.3
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    • pp.225-231
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    • 1993
  • Transformed hairy roots of Scopolia parviflora, producing tropane alkaloids and native to Korea, were obtained following infection of rhizome segments with Agrobacterium rhizogenes A4. Each root tip induced from inoculum sites excised and cultured in MS agar or liquid medium. About seventy of hairy root clones were established. Among them, several fast growing hairy root clones were examined for alkaliod content. Two dimensional TLC analysis showed that the tropane alkaloid pattern of hairy root was more complicated than that in the rhizome of mother plant. On the other hand, some hairy root clones did not produce scopolamine and hyoscyamine. In HPLC analysis, some hairy root clones yield higher levels of scopolamine and hyoscyamine than those of mother plant rhizome which used for infection. Scopolamine and hyoscyamine were identified by comparison of their retention times and of their spectra data with those of authentic compounds.

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Antimicrobial Activity and Characteristics of Amblytropis pauciflora Kitagawa Extract (털새동부 추출물의 항균효과 및 특성)

  • 김현수
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.27 no.5
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    • pp.993-999
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    • 1998
  • Methanol extract of roots of Amblytropis pauciflora Kitagawa showed the antimicrobial activity to three test strains. Antimicrobial spectra of various extracts of Amblytropis pauciflora Kitagawa were tested against 24 strains of bacteria and fungi. The crude methanol extract inhibited the growth of 12 strains of bacteria and Asp. fumigatus with the exception of yeasts. The properties of the antimicrobial substance were very stable under heat(at 12$0^{\circ}C$), acid(pH 3.0) and alkali(pH 11.0) treatment. Only the root harvested in spring showed the antimicrobial activity. Among the components extracted by butanol, ginseng saponin Rg1 and various saponin-like materials were detected by TLC analysis using a plate of silica gel 60F254. The antimicrobial compound was purified by methanol extraction, activated charcoal column chromatography, Sep-pak(C18) pretreatment and reverse phase HPLC. The purified compound was detected at 13.520 min as a single peak(about 98% purity) through the HPLC analysis.

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