• Journal of Microbiology and Biotechnology
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• 제19권11호
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• pp.1328-1332
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• 2009

An activity-guided fractionation method was used to isolate anticancer components from Nuruk (Rhizopus oryzae KSD-815:KSD-815). Dried powder of KSD-815 was extracted with 80% methanol and partitioned successively using n-hexane, ethyl acetate, n-butanol, and water. The n-hexane and n-butanol fractions showed a strong antimigratory effect on human cancer cells. Both of these fractions were subjected to separation and purification procedures using silica gel, octadecyl silica gel, and Sephadex LH-20 column chromatographies to afford four purified compounds. These were identified as ergosterol peroxide (1), stigmast-5-en-$3\beta$,$7\beta$-diol (2), ergosta-7,22-dien-$3\beta$,$5\alpha$,$6\beta$,$9\alpha$-tetraol (3), and daucosterol (4), respectively, by spectroscopic methods such as nuclear magnetic resonance spectrometry, mass spectrometry, and infrared spectroscopy, and comparison with those in the literature. Compounds 1-4 were isolated from KSD-815 for the first time. Compounds 1 and 4 inhibited the migration of MDA-MB-231 cells at concentrations lower than $20\;{\mu}M$.

• Archives of Pharmacal Research
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• 제28권2호
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• pp.195-202
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• 2005

Free radicals and reactive oxygen species (ROS) caused by UV exposure or other environmental factors are critical players in cellular damage and aging. In order to develop a new antiphotoaging agent, this work focused on the antioxidant effects of the extract of tinged autumnal leaves of Acer palmatum. One compound was isolated from an ethyl acetate soluble fraction of the A. palmatum extract using silica gel column chromatography. The chemical structure was identified as apigenin-8-C-beta-D-glucopyranoside, more commonly known as vitexin, by spectral analysis including LC-MS, FT-IR, UV, $^{1}H-$, and $^{13}C-NMR$. The biological activities of vitexin were investigated for the potential application of its anti-aging effects in the cosmetic field. Vitexin inhibited superoxide radicals by about $70\%$ at a concentration of $100\;{\mu}g/mL$ and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radicals by about $60\%$ at a concentration of $100\;{\mu}g/mL$. Intracellular ROS scavenging activity was indicated by increases in dichlorofluorescein (DCF) fluorescence upon exposure to UVB $20\;mJ/cm^2$ in cultured human dermal fibroblasts (HDFs) after the treatment of vitexin. The results show that oxidation of 5-(6-)chloromethyl-2',7'-dichlo-rodihydrofluorescein diacetate ($CM-H_{2}DCFDA$) is inhibited by vitexin effectively and that vitexin has a potent free radical scavenging activity in UVB-irradiated HDFs. In ROS imaging using a confocal microscope we visualized DCF fluorescence in HDFs directly. In conclusion, our findings suggest that vitexin can be effectively used for the prevention of UV-induced adverse skin reactions such as free radical production and skin cell damage.

• Applied Biological Chemistry
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• 제37권2호
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• pp.100-104
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• 1994

상황(상황(桑黃); Phellinus linteus) 균사체 배양액의 ethyl acetate 가용성 분획으로부터 silica gel column chromatography 및 preparative thin layer chromatography를 이용하여 6개의 화합물을 분리, 정제하였다. 화합물 1은 표준품과의 비교에 의하여 succinic acid, 화합물 2는 $^1H-NMR$ 및 EI-MS로부터 p-hydroxyphenylacetic acid methyl ester로 동정되었으며, 화합물 3은 $^1H-NMR$과 EI-MS에 의하여 p-hydroxybenzaldehyde로, 화합물 4와 6은 각종 NMR data와 MS data 및 이들의 아세틸 유도체의 spectral data로부터 각각 2-hydroxymethyl-5-methoxy-methylfuran 및 2,5-dihydroxymethylfuran으로 동정되었다. 또한, 화합물 5는 $^1H-NMR$ data와 EI-MS에서의 m/z 179의 molecular ion peak로부터 N-acetyltyramine으로 추정되었으며 이 구조는 무수초산과 tyramine을 이용한 합성에 의하여 최종적으로 확인되었다.

• Carbon letters
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• 제5권4호
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• pp.159-163
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• 2004

The polymer-ceramic hybrid, known as 'ceramer', was synthesized by a sol-gel process by incorporating different amount of alkoxide as source of silicon in resorcinol-formaldehyde in presence of basic catalyst to get different percentage of silicon in ultimate carbonized composites. FTIR of the ceramer confirms that it is a network of Si-O-Si, Si-O-$CH_2$ and Si-OH type groups linked with benzene ring. Different amount of silicon in the ceramer exhibits varying temperature of thermal stability and lower coefficient of thermal expansion as compared to pure resorcinol-formaldehyde resin. The lower value of CTE in ceramer is due to existence of silica and resorcinol -formaldehyde in co-continuous phase. Unidirectional composites prepared with ceramer matrix and high-strength carbon fibers show lower value of flexural strength at polymer stage as compared to those prepared with resorcinol-formaldehyde resin. However, after heat treatment to $1450^{\circ}C$, the ceramer matrix composites show large improvement in the mechanical properties, i.e. with 7% silicon in the ceramer, the flexural strength is enhanced by 100% and flexural modulus value by 40% as compared to that of pure resorcinol-formaldehyde resin matrix composites.

• Applied Biological Chemistry
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• 제46권2호
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• pp.144-149
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• 2003

산철쭉 끝을 MeOH로 추출하고, 이를 EtOAc, n-BuOH과 $H_2O$로 분배 추출하였다. EtOAc추출물과 n-BuOH 추출물에 대하여 silica gel과 ODS column을 이용하여 chromatography하거나, 아세틸화 한 후 sillica gel column chromatography를 수행하여 2종의 triterfenoid와 3종의 diterpenoio를 분리하였다. 각 화합물은 $^1H-^lH\;COSY$, HMQC, HMBC와 같은 2D-NMR기법을 포함한 스펙트럼 데이터를 해석하여 $2{\alpha}\;3\{beta}-dihydroxylolean-12-ene (1), ursolic acid (2), grayanotoxin IV (3), grayanotoxin I (4) 및 grayanotoxin III (5) 등으로 동정하였다.

• 한국재료학회지
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• 제12권7호
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• pp.573-579
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• 2002

Stoichiometric mullite ($3Al_2$$O_3$. $2SiO_2$) precursor sol has been prepared by sol-gel method. The effects of the precursor pH and sintering temperature on the synthesizing behavior and morphology of mullite have been studied. Mullite precursor sol was prepared by dissolution of aluminum nitrate enneahydrate (Al($NO_3$)$_3$.9H$_2O) into the mixture of silica sol. Precursor pH of the sols was controlled to acidic condition ($PH\leq$ 1~1.5) and to basic condition ($pH\geq$8.5~9). The synthesized aluminosilicate sols were formed under 20 MPa pressure after drying at $150^{\circ}C$ for 24 hours, and then sintered for 3hours in the temperature range of $1100~1600^{\circ}C$. From TGA/DTA analysis, total weight loss in the aluminosilicate gel of the acidic sample was (equation omitted) 56% and that of the basic sample was (equation omitted) 85%, indicating that the synthesizing temperature of mullite phase for acidic and basic samples was above $1200^{\circ}C$ and $1300^{\circ}C$, respectively. The morphologies of the synthesized mullite were fine and needle-like (or rod-like) for acidic sample, and granular for basic sample that has been sintered above $1300^{\circ}C$. It was found that the morphology of mullite particle was predominantly governed by precursor pH and sintering temperature.

• 한국응용과학기술학회지
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• 제24권2호
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• pp.174-181
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• 2007

본 연구에서는 졸-겔 공법을 이용하여 가스 차단 특성을 갖는 $SiO_2/EVOH$(에틸렌 비닐알콜 공중합체) 하이브리드 물질을 제조하였다. 제조된 여러 조성의 하이브리드 졸을 표면 처리한 biaxially oriented polypropylene (BOPP) 기지재에 스핀 코팅 방식을 이용하여 코팅하였다. X선 회절 및 DSC 분석에 의해 하이브리드 내의 EVOH 상과 실리카 상 사이의 결합에 따른 결정화 거동의 변화를 조사하였다. 또한 $SiO_2/EVOH$ 하이브리드 겔의 모폴로지 관찰을 통하여, 100nm 이하의 실리카 입자들이 균열하게 분산된 매우 치밀한 상 미세구조를 갖는 하이브리드 물질을 제조하기 위해 필요한 Tetraethylorthosilicate (TEOS) 무기전구체의 최적 함량이 존재함을 알 수 있었다. 첨가된 TEOS 함량이 최적 함량보다 낮거나 높은 경우에는 큰 도메인의 입자 클러스터들이 형성되어 매우 불안정한 모폴로지를 나타내는 상분리 현상이 관찰되었다. 이러한 모폴로지 결과는 하이브리드 코팅 필름의 산소 투과도의 변화 결과와 일치하였는데, TEOS 함량이 0.01 - 0.02mol로 첨가되어 제조된 하이브리드로 코팅된 필름의 경우 매우 우수한 산소 차단 특성을 나타냈으며, 0.04mol 이상으로 첨가되었을 때는 상 분리 및 미세 균열 발생으로 인하여 그 차단 특성이 급격하게 감소하는 것으로 나타났다.

• 생약학회지
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• 제45권3호
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• pp.209-213
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• 2014

The anti-melanogenic substance was isolated from the root of Angelica gigas Nakai by silica gel column chromatography, preparative HPLC and TLC. As a result of the structure analysis by mass, $^1H$-NMR, and $^{13}C$-NMR spectrometry, the compound was identified as demethylsuberosin. Demethylsuberosin reduced melanin contents of B16F1 melanoma cells in a dose-dependent manner and decreased to about 74% at a concentration $5{\mu}g/ml$. Demethylsuberosin inhibited the expression in microphthalmia associated transcription factor (MITF), tyrosinase, tyrosinase related protein-1 (TRP-1), and tyrosinase related protein-2 (TRP-2) in melanocytes. These results suggest that the whitening activity of demethylsuberosin may be due to the inhibition of the melanin synthesis by down-regulation of MITF, tyrosinase, TRP-1 and TRP-2 expression. Thus, our results provide evidence that demethylsuberosin might be useful as a potential skin-whitening agent.

• Applied Biological Chemistry
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• 제48권1호
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• pp.98-102
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• 2005

꽃마리를 80% MeOH로 추출하고, 얻어진 추출물을 EtOAc, n-BuOH 및 $H_2O$로 용매 분획하였다. EtOAc와 n-BuOH 분획에 대하여 column chromatography를 반복하여 4종의 flavonol 배당체를 분리하였다. 각각에 대하여 2D-NMR을 포함한 스펙트럼 데이터의 해석과 문헌 자료를 조사하여 $kaempferol-3-O-{\beta}-{D}-glucopyranoside(astragalin),\;kaempferol-3-O-{\alpha}-{L}-rhamnopyranosyl(1{\rightarrow}6)-{\beta}-{D}-glucopyranoside(nicotiflorin),\;quercetin-3-O-{\alpha}-{L}-rhamnopyranosyl(1{\rightarrow}6)-{\beta}-{D}-glucopyranoside(rutin),\;quercetin-3-O-{\beta}-{D}-glucopyranoside(isoquercitrin)$로 구조를 결정하였다. 이 화합물들은 꽃마리에서는 이번에 처음 분리, 보고되었다. 또한 $nicotiflorin(100\;{\mu}g/ml)$은 hACAT1에 대하여 $68.3{\pm}1.2%$ 저해활성을 나타내었다.

• 분석과학
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• 제18권4호
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• pp.298-308
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• 2005

사용후핵연료시료 중에 함유된 탄소-l4와 트리튬을 회수 및 정량하였다. $CO_2$ 운반체($CaCO_3$)를 포함한 사용후핵연료시료를 $90^{\circ}C$에서 8M $HNO_3$ 용액으로 용해하면서 휘발된 $^{14}CO_2$를 1.5 M NaOH 용액을 포함한 포집관에 수집하였다. 용해 중 휘발되는 방사성 요오드는 Ag-silica gel 흡착체를 담은 포집 관으로 사전제거하였다. 핵연료 용해용액 중에 남아있는 트리튬(HTO)를 정량하기 위하여 양이온과 음이온 교환수지 혼합물 및 무기이온교환체를 이용한 뱃치 및 분리관법으로 용해용액을 탈이온화시켜 간섭이온을 제거하였다. 포집용액 중의 탄소-14와 탈이온화수 중의 트리튬을 액체섬광계수법으로 정량하였다.