• Applied Biological Chemistry
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• 제47권1호
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• pp.49-54
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• 2004

소톨론은 호로파(fenugreek)라는 콩과식물을 원료 물질로 하여 여러 가지 전환반응에 의해 생산될 수 있는 천연향미소재로서 본 연구에서는 생물 전환율을 높이기 위한 미생물이나 효소원을 탐색하였다. 원료로부터 소톨론을 추출하기 위한 유기용매로서 dichloromethane이 선별되었다. 효소원으로 사용될 수 있는 유산균, 효모, 사상균 등의 여러가지 미생물에 대한 스크리닝 결과 신령버섯(Agaricus blazei)이 높은 전환율을 보였다. 다양한 첨가물 및 전처리 조건에 따른 전환율을 조사한 결과 호로파 현탁액에 isoleucine, ${\alpha}-ketoglutaric$ acid, ascorbate, $FeSO_4$ 등의 첨가물을 첨가한 후 신령버섯의 균사체 배양액을 혼합하여 반응시키는 공정을 통하여 원료의 초기 소톨론 함량을 대략 77배 수준으로 높일 수 있었다.

• KSBB Journal
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• 제29권2호
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• pp.124-130
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• 2014

Acer tegmentosum was a traditional Korean herbal medicine showing various pharmacological activities. In this work, A. tegmentosum were extracted with boiling water and then successively partitioned with dichloromethane, ethyl acetate, n-butyl alcohol (n-BuOH), and water. Salidoside, the target compound, was purified in n-BuOH phase using a chromatography method. For the analysis of salidoside, TLC and LC-MS were used as well as on-line screening $HPLC-ABTS^+$ assay with three different wavelength of 254, 280, and 320 nm. An amount of 1.34 g of salidoside were obtained in n-BuOH phase fromAcer tegmentosum was a traditional Korean herbal medicine showing various pharmacological activities. In this work, A. tegmentosum were extracted with boiling water and then successively partitioned with dichloromethane, ethyl acetate, n-butyl alcohol (n-BuOH), and water. Salidoside, the target compound, was purified in n-BuOH phase using a chromatography method. For the analysis of salidoside, TLC and LC-MS were used as well as online screening $HPLC-ABTS^+$ assay with three different wavelength of 254, 280, and 320 nm. An amount of 1.34 g of salidoside were obtained in n-BuOH phase from 3 kg of dry biomass. The on-line screening $HPLC-ABTS^+$ assay is rapid and efficient tool to search bioactivity from A. tegmentosum. 3 kg of dry biomass. The on-line screening $HPLC-ABTS^+$ assay is rapid and efficient tool to search bioactivity from A. tegmentosum.

• 생명과학회지
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• 제22권6호
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• pp.852-856
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• 2012

한약재의 원료 및 전세계적 외래종으로 알려져 있는 녹조류 청각(Codium fragile)의 디클로로메탄, 에탄올, 열수 추출물을 대상으로 하여 생쥐에서의 항 염증, 해열, 및 진통 활성을 조사하였다. 청각의 디클로로메탄과 에탄올 추출물은 phorbol 12-myristate 13-acetate로 유도된 생쥐 귀의 부종과 충혈에 대한 염증 증상을 74% 이상의 높은 저해 작용을 보였으며, 이들 추출물은 acetyl salicylic acid와 유사하게 발열증상을 억제하였다. 청각으로부터 주된 항 염증 활성물질은 eicosapentaenoic acid인 것으로 분리되었다. 이러한 결과는 청각이 여러 염증 관련 증상에 대처할 약제로서도 사용되어 질 수 있다는 사실을 뒷받침해 준다.

• 한국환경농학회지
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• 제28권4호
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• pp.427-434
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• 2009

Analytical method for prochloraz in cabbage, apple, pepper, mandarin, and hulled rice was established by conversion it to 2,4,6-trichlorophenol (TCP). Crop samples were extracted with acetonitrile, and partitioned with dichloromethane. The sample extracts were hydrolyzed with pyridine hydrochloride in a vial by heating for 1 hour, and analyzed with GC-ECD after partitioning with dichloromethane. Method quantification limit (MQL) of prochloraz was 0.01 mg/kg. Recoveries at 0.1 mg/kg level was 105-113% while at 0.5 mg/kg level was 82-87%. In both of the cases CV was less than 10%. Through this procedure soxhlet extraction and refluxing apparatus of conventional method were discarded and simple solvent extraction and small vial were successfully employed, resulting in simple, rapid, economic and more precise method.

• 한국수산과학회지
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• 제34권5호
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• pp.556-562
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• 2001

본 연구에서는 비교적 성장이 빠르고 배양이 용이한 황갈편조 식물문 중 규조강에 속하는 P. tricornutum으로부터 선정하여 항 산화성 물질을 분리$\cdot$정제하여 물질의 구조를 밝혔다. P. tricornutum의 각 유기용매 추출물의 항산화성은 chloroform획분이 가장 좋았으며, 이 획분을 시료로 하여 silica gel column chromatography, PTLC 및 HPLC를 사용하여 항산화성 물질을 분리$\cdot$정제하였다. Silica gel column을 사용하여 분리된 획분의 항산화성은 dichloromethane: methanol (5: 1)로 용출시킨 획분에서 가장 높았으며, 이 획분의 PTLC 획분은 항산화성이 $20\%$ 증가하였다. 최종 정제된 물질의 $IC_50$값은 $8.3{\mu}g/mL$으로 화학적으로 합성된 항산화제인 BHT 및 BHA보다는 낮았지만 천연 항산화제인 $\alpha-tocopherol$보다는 다소 높게 나타났으며, 이 물질의 화학적 구조는 carotenoid류인 zeaxanthin으로 동정되었다.

• 농약과학회지
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• 제8권2호
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• pp.129-136
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• 2004

생장조절제 Atonic 원제 중 부성분의 함량과 화학구조를 구명하기 위하여 diethyl ether와 dichloromethane 분배액을 각각 GC-FID와 GC-MSD로 분석하여 5종 부성분의 화학구조를 구명하였다. 주성분인 Atonic의 함량은 약 84%이었으며, 부성분의 함량은 $0.24\sim10.74%$이었다. 확인된 부성분은 2-methoxy-phenol (guaiacol, m/z 124), 2-chloro-6-methoxyphenol 또는 4-chloro-6-methoxyphenol (m/z 158), 1,2-dimethoxy-4-nitrobenzene (m/z 183), 그리고 2,6-bis(1,1-dimethylethyl)-4-methylphenol (m/z 220)이었으며, 국내에서 규제중인 6종의 유해성분은 포함되지 않은 것으로 판단되었다.

• 분석과학
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• 제9권2호
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• pp.123-133
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• 1996

기체 크로마토그래피법을 이용하여 과수 재배용 살균제인 difenoconazole의 분석을 위한 최적 조건을 구하고, 사과와 토양 중에서의 잔류성을 조사하였다. 사과사료는 5% NaCl과 n-hexane액으로 분리, 농축하여 florisil column상에서 acetone과 n-hexane 혼합액으로 정제하여 GLC(ECD)로 분석하였다. 0.20과 1.0ppm의 표준물 첨가실험결과 평균회수율은 86.0~92.0% 였고, 검출한계는 0.01ppm 이었다. 사과에 대한 안정 사용기간은 수확 15일 전 3회 사용이 적당한 것으로 나타났으며, 이 경우 difenoconazole의 잔류량은 0.037ppm에서 0.044ppm 이었다. 토양시료를 methanol과 ammonium hydroxide 의 혼합액으로 추출하여 여과한 후 포화 NaCl 용액과 dichloromethane층으로 분배하였다. 유기층을 농축하여 toluene 용매로 재용해하였고, Sep-Pak column으로 정제한 후 GLC(FID)로 분석하였다. 0.10, 0.50과 1.0ppm 표준물 첨가실험 결과 평균 회수율은 101.2~103.7% 였고, 검출한계는 0.025ppm 이었다.

• 한국응용과학기술학회지
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• 제11권1호
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• pp.7-16
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• 1994

Some seeds of the Rutaceae family, Zanthoxylum piperitum, Z. schinifolium officinalis, Poncirus trifoliata, Citrus unshin, were investigated to clarify their antioxidative components. Finely powdered samples were extracted by hexane, followed by dichioromethane and then 70% methanol in a hot bath. Its unsaponifiables containing X-and Y-tocopherol with trace amount of ${\beta}-and$\;{\delta}-tocopherol$. also showed comparatively weak activity, although the hexane fraction itself had no significant antioxidative effect on lard. Levels of total tocopherols in the samples averages 42. 24-154. 11 mg/lOOg total extractives. The dichloromethane-and 70% methanol extractives showed strong antioxidative activity, from which antioxidative substances were purified with benzene-acetone(6:5, V/V) on a silica gel column, and with a solvent mixture of acetonitrile-methanol-$H_2O$(40:40:20, V/V/V) on a Sep-Pak $C_{18}$ hydrolyzed by 5% KOH-ethanol. The recovered unsaponifiables were, then, separated on a column of high performance liquid chromatography. The unsaponifiables produced by hydrolysis of the isolates from dichloromethane extractives has epi-catechin(40.0-57.1%) and (+)-catechin<$l9.1{\sim}24.4%$ to total phenolic substances, on area base) as major component, accompanied by chlorogenic acid, gallic acid(?), trans-p-coumaric acid and tralls-p-ferulic acid including some unknown components, and those derived from 70% methanol extractives also comprise (+)-catechin($31.3{\sim}39.6%$ to total components, on area base), epi-catechin($2O.2{\sim}36.4%$), trans-p-cournaric acid(8.4-15.3%) and trans-p-ferulic acid($7.7{\sim}14.1%$) as predominant component with some minor coponents, but the fraction supposed to be gallic acid(?) is not present. The antioxidative activities of the phenolic components isolated in this work were in order of epi-catechin>catechin>chlorogenic acid>trans-p-ferluic acid>trans-p-coumaric acid.

• 대한본초학회지
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• 제27권4호
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• pp.99-107
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• 2012

Objectives : The aim of this study was to authenticate whether fractionated extract of Rumex japonicus HOUTT. (RJ) has anti-inflammatory effects in mouse macrophage, RAW264.7 cells. Methods : Roots of RJ were extracted by methanol for 48hours. The methanol that gained was filtered and freeze dried. The methanol extract was dissolved in water and dichloromethane (DCM). After that, two layers were separated. Ethyl acetate (EA) added to the water layer and separated again. All the layers were filtered and freeze dried and the extracts were tested. Cytotoxic activity of extracts on RAW 264.7 cells was measured using MTS assay. The nitric oxide (NO) production was measured and proinflammatory cytokines and $PGE_2$ were measured by ELISA kit. The levels of inducible nitric oxide synthase (iNOS), cyclooxygenase-2 (COX-2), I ${\kappa}$-B-${\alpha}$ and nuclear NF-${\kappa}B$ p65 expression were detected by western blot. Results : Our results indicated that DCM and EA extracts of RJ inhibited the LPS-induced NO, $PGE_2$ production and iNOS, COX-2 expression accompanied by an attenuation of TNF-${\alpha}$, IL-$1{\beta}$ and IL-6 production in RAW 264.7 cells most effectively. DCM and EA extracts also had suppression effects of LPS-induced NF-${\kappa}B$ and MAPKs activation. Conclusions : This results demonstrate that fractionated extract of RJ has anti-inflammatory effects and among the fractioned extract, dichloromethane and ethyl acetate extract have best anti-inflammatory effects.

• Bulletin of the Korean Chemical Society
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• 제35권11호
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• pp.3199-3204
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• 2014

Two novel phosphorescent heteroleptic cationic Ir(III) complexes, Ir(bt)2(dmpe) (Ir1) and Ir (bt)2(dppe) (Ir2), where bt is 2-phenylbenzothiazole, dmpe is 1,2-bis(dimethylphosphino)ethane, and dppe is 1,2-bis(diphenyl-phosphino) ethane, were designed and synthesized. Their photophysical and electrochemical properties and the X-ray structure of the Ir1 complex were investigated. The prepared Ir(III) complexes exhibited blue-green emissions at 503-538 nm with vibronic fine structures in dichloromethane solution and PMMA film, implying that the lowest excited states are dominated by ligand-based $^3{\pi}-{\pi}^*$ transitions. The ${\pi}$-acceptor ability of the diphosphine ancillary ligand leads to blue-shift emission. The room temperature photoluminescent quantum yields (PLQYs) of Ir1 and Ir2 were 52% and 45%, respectively, in dichloromethane solution. These high PLQYs resulted from steric hindrances by the bulky cationic iridium complexes. The crystal structure of Ir1 was determined by X-ray crystallography, which revealed that central iridium adopted a distorted octahedral structure coordinated with two bt ligands (N^C) and one dmpe ligand (P^P) showing cis C-C and trans N-N dispositions. The bent nature of the dmpe ligand resulted in a relatively wide bite angle of $83.83^{\circ}$ of P-Ir-P.