• Title/Summary/Keyword: 컬럼

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Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

Hypopigmentary Effect of Milk Thistle Extract Silymarin (엉겅퀴 추출물 실리마린의 피부 미백효과)

  • Yoo, Ick-Dong;Choo, Soo-Jin;Ryoo, In-Ja;Kim, Young-Hee;Xu, Guang-Hua;Kim, Ki-Ho;Han, Chang-Sung;Kim, Su-Jin;Kim, Jin-Woong;Son, Eui-Dong
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.35 no.2
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    • pp.151-158
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    • 2009
  • We found that silymarin exhibited the inhibitory effect on melanogenesis in a spontaneously immortalized mouse melanocyte cell line, Mel-Ab. Silymarin is a standardized extract obtained from the dried seeds of milk thistle (Silybum marianum Gaertn.). Silymarin significantly prevented melanin production in a dose-dependent manner with an $IC_{50}$ value of 28.2 ${\mu}g/mL$ without effects on cell viability. Also, silymarin inhibited tyrosinase activity in melanocyte, while it did not affect the catalytic activity of cell-free tyrosinase. Furthermore, Western blot analysis indicated that silymarin decreased the expression of tyrosinase protein. Silybin A/B and isosilybin A/B were also able to inhibit melanin production and tyrosinase expression in protein level. Double blind study on the clinical efficacy of a cream containing 2 % silymarin showed that silymarin have a significant skin whitening effect. Therefore, this study suggests that silymarin may be useful as a natural skin whitening agent.

A Study on Capillary Gas-Liquid Chromatographic Determination of Diosgenin in Costus Speciosus (모세관 기체-액체 크로마토그래피에 의한 Costus Speciosus 중 Diosgenin의 정량에 관한 연구)

  • Taek Jae Kim;Cha Kee Surk;Kim Young Sang
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.369-376
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    • 1986
  • Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

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A Study of Liquid Chromatographic Detection Method for Thiocarbamates by Using Photochemical Reaction (광화학 반응을 이용한 티오카바메이트류의 액체 크로마토그래피 검출법에 관한 연구)

  • Dai Woon Lee;Young Hun Park;Yong Wook Choi
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.453-461
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    • 1993
  • Detection method was developed using a simply designed photochemical reactor made of teflon coil and low pressure mercury lamp. This method of UV photolysis of analytes followed by UV, fluorescence and electrochemical detection was found to be useful for four thiocarbamates. Analytes eluting from the column are irradiated with a high flux of 254 nm UV light, so that they change to either fluorescent active forms or highly electrochemically sensitive products. Appling this technique to the UV detection, thiocarbamates were converted into long wavelength absorbing products upon UV irradiation. In fluorescence detector four thiocarbamates are not detected at nonirradiated condition but fluorescence signals of MPTC, CPTC photolysates are appeared after irradiation with UV light. The electrochemical detection for the determination of thiocarbamates was enhanced up to 5∼20 fold signal after UV irradiation, compared to that of the nonirradiated. The detection limit of thiocarbamates on electrochemical detector was 13.3∼0.02 ng under pH 7.0, ionic strength $0.5{\times}10^{-2}$ M, phosphate buffer solution. Adducts produced by reaction of photolysates and OPA-MERC in the reaction coil were monitored at 425 nm with fluorescence detector, and one of the photolysates was primary amine.

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Production of Mycelia and Water Soluble Polysaccharides from Submerged Culture of Ganoderma applanatum Using Different Types of Bioreactor (생물반응기 유형에 따른 잔나비불로초(Ganoderma applanatum)의 균사체 및 수용성 다당체 생산 특성)

  • Lee, Wi-Young;Park, Young-Ki;Ahn, Jin-Kwon;Park, So-Young
    • The Korean Journal of Mycology
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    • v.34 no.1
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    • pp.1-6
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    • 2006
  • In order to select a suitable bioreactor type for the submerged cultivation of Ganoderma applanatum, both growth characteristics and polysaccharides production were compared among four different types of bioreactor. These include an external-loop type air-lift bioreactor (ETAB), a balloon type air bubble bioreactor (BTBB), a column type air bubble bioreactor (CTBB) and a stirrer type bioreactor (STB). The mycelial biomass produced from the reactors were in decreasing order: ETAB ($7\;g/{\ell}$) > BTBB ($6.2\;g/{\ell}$) > STB ($6\;g/{\ell}$) > CTBB ($5\;g/{\ell}$). Maximal soluble exopolysaccharides ($1\;g/{\ell}$) and endopolysaccharides (2.7%) were also obtained from ETAB. Thus, the ETAB was most suitable for submerged culture of G applanatum mycelium. Based on the results, ETAB was chosen for further detailed study. The most effective aeration rate for the mycelial growth in ETAB ranged from 0.05 to 0.1 vvm. For the maximal production, the mycelium at the initial growth stage needed low aeration rate to reduce cell damages by fluid flow. However, as the mycelia grew, the culture became viscous and thus needed higher aeration. The molecular weight of exopolysaccharides obtained from the culture grown in ETAB was higher than that from the culture grown in other bioreactors.

Development of the Pre-treatment Technology for LNG-FPSO (LNG-FPSO용 천연가스 전처리 기술 개발)

  • Jee, Hyun-Woo;Lee, Sun-Keun;Jung, Je-Ho;Min, Kwang-Joon;Kim, Mi-Jin
    • Plant Journal
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    • v.9 no.3
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    • pp.38-42
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    • 2013
  • Submarine gas fields have focused because of the increasing fuel cost, the environmental regulations, and the safety & NIMBY problems. LNG-FPSO which is available for acid gas removal, recovery of the condensate & LPG and Liquefaction in topside process is one of high technology offshore structures. On the other hands, it is necessary to verify the pre-treatment efficiency by the ship motion and to apply to the design for LNG-FPSO. This study is to develop the pre-treatment technology for LNG-FPSO as taking account to the process efficiency by ship motion effects and the area optimization. Based on the simulation results, it founds that hybrid process shows the low circulate rate, the low heat duty and the small size of column dimensions compared to typical amine process. It will be verified the process efficiency in the various conditions by sea states as performing the 6-DOF motion test and CFD simulation.

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Modulatory Effect of Four Azulene Derivatives from the Fruiting Bodies of Lactarius hatsudake on Interferon-$\gamma$ Production (젖버섯아재비 자실체로부터 분리한 Azulene계 화합물이 Interferon-$\gamma$ 생성에 미치는 영향)

  • Xu, Guang Hua;Kim, Jae-Wha;Li, Gao;Yoo, Ick-Dong
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.36 no.2
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    • pp.151-156
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    • 2010
  • Investigation of secondary bioactive metabolites from the fruiting bodies of Lactarius hatsudake led to the isolation of four azulene derivatives by means of repeated column chromatography and preparative HPLC, and they were identified as 1-formyl-4-methyl-7-isopropyl azulene (1), lactaroviolin (2), 4-methyl-7-isopropyl-azulene-1-carboxylic acid (3), and 1-formyl-4-methyl-7-(1-hydroxy-1-methylethyl) azulene (4) by their physico-chemical properties and spectroscopic analysis. The isolated compounds were evaluated for the effects on modulation of cytokines in natural killer cell line (NK92 cells). Compounds 1 and 4 strongly inhibited IFN-$\gamma$ production in a dose-dependent manner, corresponding to 101.3 % and 92.7 % inhibition at 400 ${\mu}M$, and 11.9 % and 24.1 % at 100 ${\mu}M$, respectively, whereas compounds 2 and 3 showed weak inhibitory effect on INF-$\gamma$ production, corresponding to 45.9 % and 18.0 % inhibition at 400 ${\mu}M$.

Inhibitory Effects of Carex humilis Extract on Elastase Activity and Matrix Metalloproteinase-1 Expression (산거울 추출물의 Elastase 활성 저해 및 Matrix Metalloproteinase-1 발현 억제 효과)

  • Park, Sun-Hee;Lee, Kang-Hyuk;Han, Chang-Sung;Kim, Ki-Ho;Kim, Young-Heui
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.36 no.2
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    • pp.129-136
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    • 2010
  • In order to evaluate anti-wrinkle activity of Carex humilis extract, free radical scavenging activity, elastase inhibitory activity and reduction of expression Matrix metalloproteinase-1 (MMP-1) mRNA and MMP-1 protein were investigated. The roots of Carex humilis were extracted with 95 % ethanol and successively partitioned with organic solvents with increasing polarity of the solvents. Each fraction of organic solvent were investigated by using free radical scavenging activity and elastase inhibitory activity test. Among them, EtOAc fraction showed antioxidant activity ($SC_{50}$=4.89 ${\mu}g/mL$) and elastase inhibitory activity ($IC_{50}$=23.5 ${\mu}g/mL$). EtOAc fraction was developed on silica gel by open-column chromatography and consecutively re-developed on C18 resin by prep-HPLC to give ${\alpha}$-viniferin as a major component, which was confirmed by spectrometric analysis. In the assay on expression of MMP-1 mRNA by RT-PCR and protein by western-blot, EtOAc layer (10 ~ 100 ${\mu}g/mL$) was reduced about 50 ~ 60 %, 50 ~ 65 % respectively and ${\alpha}$-viniferin (0.5 ~ 2 ${\mu}g/mL$) was inhibited about 60 ~ 75 %, 55 ~ 65 % respectively in human fibroblast. Therefore, our findings suggest that EtOAc layer of Carex humilis containing ${\alpha}$-viniferin can be useful as an active ingredient for cosmeceuticals of anti-wrinkle effects.

Simultaneous Determination of Heavy Metals in Cosmetic Products by Ion Chromatography (이온 크로마토그래피를 이용한 화장품 중 중금속 동시분석)

  • Lee, So-Mi;Jeong, Hye-Jin;Kim, Han-Kon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.1
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    • pp.57-62
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    • 2008
  • No matter how small amount of heavy metals it may be cause skin allergies through percutaneous adsorption when existing in cosmetic products as impurities. In order to develop a highly sensitive method for simultaneous determination of $Pb^{2+},\;Fe^{2+},\;Cu^{2+},\;Ni^{2+},\;Zn^{2+},\;Co^{2+},\;Cd^{2+},\;and\;Mn^{2+}$ in coloring agents and cosmetic products with rapidity and accuracy, we carried out the determination on ion chromatography. All of these metals are well separated through a bifunctional ion-exchange column(IonPac CS5A) and detected by post-column reaction and spectrophotometric detection. The calibration graphs are linear($r^2>0.999$) in the range $0.1{\sim}1000{\mu}g/mL$. Detection limits for 200 ${\mu}L$ of sample solution are at the level of ${\mu}g/L$, which is sufficient for judging whether the product is safe or not. The relative standard deviations(RSDs) of the retention time and the peak area are less than 0.21 and 1.24%, respectively. The recovery rates are $97{\sim}104%$. The new method was applied to analyze the amount of heavy metals which were contained in 22 cosmetic products and 11 coloring agents.

Antimicrobial, Antihypertensive and Anticancer Activities of Medicinal Herbs (생약재의 항균, 항고혈압 및 항암 활성)

  • Do, Jeong-Ryong;Kim, Ki-Ju;Jo, Jin-Ho;Kim, Young-Myoung;Kim, Byeong-Sam;Kim, Hyun-Ku;Lim, Sang-Dong;Lee, Soo-Won
    • Korean Journal of Food Science and Technology
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    • v.37 no.2
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    • pp.206-213
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    • 2005
  • Antibacterial, antifungal, anticancer and angiotensin-converting enzyme (ACE) inhibitory activities of water and 70% ethanol extracts of 32 medicinal herbs species were investigated. Terminalia chebula extracts showed strong antibacterial activities. Ethanol extract of Cinnamomum cassia showed good antifungal activity. ACE inhibitory activities or P. corylifolia water extract and Fraction I of P. corylifolia water extract were 65.2 and 81.8%, respectively. Cytotoxicity of ethanol precipitate fraction obtained from water extract of Eugenia caryophyllata was highest.