• Title/Summary/Keyword: ODS

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Isolation and Identification of Terpenoids from the Flower of Rhododendron yedoense var. poukhanense (산철쭉(Rhododendron yedoense var. poukhanense) 꽃으로부터 Terpenoid의 분리.동정)

  • Hong, Yoon-Hee;Song, Myoung-Chong;Han, Jae-Taek;Jang, Tae-O;Lee, Youn-Hyung;Kim, Sung-Hoon;Kim, Seung-Ae;Park, Mi-Hyun;Baek, Nam-Ln
    • Applied Biological Chemistry
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    • v.46 no.2
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    • pp.144-149
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    • 2003
  • Extracts were obtained from the flower of Rhododendro yedoense var. poukhanense. (7 kg) in 80% aqueous MeOH and successively fractionated with solvent of EtOAc, n-BuOH and $H_2O$, successively. Silica gel and ODS column chromatographies of the EtOAc and n-BuOH fractions were repeatedly carried out by using the various solvent systems to give five terpenoids. Chemical structures of the isolated terpenoids were determined as $2{\alpha},3{\beta}-dihydroxylolean-12-ene$ (1), ursolic acid (2), grayanotoxin IV (3), grayanotoxin I (4) and grayanotoxin III (5) based on the interpretation of several spectral data including 2D-NMR such as $^1H-^1H\;COSY$, HMQC and HMBC.

Purification and Characteristics of Tyrosinase Inhibitor Produced by Actinomycetes F-97 (방선균 F-97이 생산하는 Tyrosinase 저해제의 정제 및 특징)

  • Bang, Byung-Ho;Rhee, Moon-Soo;Kim, Jin-O;Yi, Dong-Heui
    • Applied Biological Chemistry
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    • v.51 no.3
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    • pp.153-158
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    • 2008
  • An actinomycetes F-97 producing tyrosinase inhibitor was isolated from soil samples. Isolation and purification of tyrosinase inhibitor produced by F-97 was performed as follows: IRC-120 ($NH_4^+$ type) column chromatography, silica gel column chromatography, $C_{18}$ column chromatography and Sephadex LH-20 column chromatography were used successively after the centrifuged supernatant was adjusted to pH 4.0. To identify the purity of the inhibitor, octadecylsilyl(ODS) HPLC was carried out with 5% methanol as a mobile phase. Finally, the purification yield of a tyrosinase inhibitor was 5.24%. The inhibitor was very soluble in water, methanol and ethanol but insoluble in acetone, butanol, ethylacetate and chloroform. The ${\lambda}_{max}$ value of this inhibitor in water was 194nm under UV light. The biochemical test of the inhibitor was positive in Molish, Benedict, cone. $H_2SO_4$, and $KMnO_4$ tests but negative in iodine, ninhydrin, Million, Sakaguchi, xanthoproteic and Emerson tests. The tyrosinase inhibitor was stable against heat treatment of $100^{\circ}C$ for 50 minutes and pH $4{\sim}9$. The $IC_{50}$ value of this inhibitor was $19.2{\mu}g/ml$ for mushroom tyrosinase. In $1,000{\mu}g/ml$ inhibitor concentration, inhibition zone was 27 mm for Streptomyces bikiniensis NRRL B-1049. The inhibition of F-97 against mushroom tyrosinase was competitive with tyrosine.

Separation and Purification of Angiotensin I-converting Enzyme Inhibitory peptide from Mackerel (고등어 유래 항고혈압 peptide의 분리 정제)

  • DO Jeong-Ryong
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.33 no.2
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    • pp.153-157
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    • 2000
  • Hydrolysate which inhibit the Angiotensin I-converting enzyme (ACE) was prepared from mackerel muscle by pretense. The ACE inhibitory activity of mackerel muscle hvdrolysate (MMH) was $967 {\mu}g of IC_(50)$. ACE inhibitory peptides were isolated by ultrafiltration, gel permeation column chromatography (GPC), reversed phase column chromatography(RPC), reversed phasehigh performance liquid chromatography (RP-HPLC), and gel permeation high performance liquid chromatography (GP-HPLC) from the MMH. The amino acid sequence of the ACE inhibitory peptides was Tyr-Val-Ala. The $IC_(50)$ of this peptide for ACE from rabbit lung was $1.4 {\mu}M$.

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Analysis of Cyclic Adenosine Monophosphate (cAMP) Separation via RP-HPLC (reversed-phase high-performance liquid chromatography) by the Moment Method and the van Deemter Equation (역상 크로마토그래피에서 모멘트 방법과 van Deemter 식을 이용한 고리형 아데노신 일인산의 분리특성 연구)

  • Lee, Il Song;Ko, Kwan Young;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.53 no.6
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    • pp.723-729
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    • 2015
  • The moment analysis of cyclic adenosine monophosphate (cAMP) was performed using chromatograms that were obtained with the pulse input method from an octadecyl silica (ODS) high-performance liquid chromatography (HPLC) column. The general rate (GR) model was employed to calculate the first absolute moment and the second central moment. Three important coefficients for moment analysis, which are molecular diffusivity ($D_m$), external mass transfer coefficient ($k_f$), and intra-particle diffusivity ($D_e$), were estimated by the Wilke-Chang equation, Wilson-Geankoplis equation, and comparing van Deemter equation to theoretical plate number equation, respectively. Experiments were conducted by various conditions of flow rates, methanol volume ratio of the mobile phase, and solute concentration. After the moment analysis, results were organized by van Deemter plots. Also van Deemter coefficients were compared each other to effect $H_{ax}$, $H_f$, and $H_d$ on height equivalent to a theoretical plate (HETP, $H_{total}$). The value of intraparticle diffusion ($H_d$) was the primary factor which makes for HETP whereas external mass transfer ($H_f$) was disregardable factor.

Development of Analytical Method for Rutin in Buckwheat Plant using High Performance Liquid Chromatography (메밀 식물체 함유 Rutin의 HPLC 분석방법 개발)

  • Choung Myoung-Gun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.50 no.spc1
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    • pp.181-186
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    • 2005
  • This experiment was conducted to know the appropriate methods for extraction and determination of rutin contained buckwheat plants. The efficient HPLC analytical condition of rutin contained buckwheat plants was developed. The gradient elution employed a $250mm\times4.6mm$ i.d. Tosoh ODS 120T column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of $2\%$ Acetic $acid-45\%$ Acetonitrile, and mobile phase B, comprising $2\%$ aqueous acetic acid, and delivered at a flow rate of 1mL/min as follows: 0-18 min, $50-100\%$ A; 18-20 min, $100-50\%$ A; 20-22 min, $50\%$ A. The UV detection wavelength was set at 355 nm. The limit of detection (LOD) for rutin standard compound was 20 ng/mL. And, the higher content of rutin in the extracts was obtained by $80^{\circ}C$ reflex extraction for 120 min. from plants of buckwheat using ethanol.

Development of Method for Analysis of Four Sulfonylurea Pesticides, Rimsulfuron, Ethametsulfuron-methyl, Tribenuron-methyl, Chlorimuron-ethyl Residues by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC/DAD를 이용한 림술푸론, 에타메트설푸론메틸, 트리베누론메칠, 클로리무론에칠 4종 성분의 잔류농약 분석법 개발)

  • Koo, Yun-Chang;Yang, Sung-Yong;Wang, Zeng;An, Eun-Mi;Heo, Kyoung;Kim, Hyeng-Kook;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1231-1235
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    • 2010
  • The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

Establishment of content criteria of marker compounds through the monitoring of Achyranthis Radix collected from Korea and China (한국 및 중국 지역에서 수집된 우슬의 모니터링을 통한 지표성분의 함량기준 설정)

  • Kim, Dae-Hyun;Kim, Sang-Hyuk;Jang, Yu-Seon;Shin, Min-Chul;Chu, Van Men;Lee, Young-Keun;Woo, Mi-Hee;Kang, Jong-Seong
    • Analytical Science and Technology
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    • v.25 no.4
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    • pp.250-256
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    • 2012
  • Two marker compounds of Achyranthis Radix, ecdysterone and inokosterone, were analyzed by HPLC on an ODS column ($250{\times}4.6$ mm, 5 ${\mu}m$) with a mobile phase of 15% acetonitrile containing 0.08% formic acid at a flow rate of 1.0 mL/min and a detection wavelength of UV 254 nm. The method was validated by ICH guideline and applied to the monitoring of marker compounds in 93 samples of Achyranthis Radix collected at various areas in Korea and China. The new content criteria of ecdysterone and inokosterone, established using linear regression method were 0.033% and 0.020%, respectively. When the new content criteria were applied to the quality control test of commercial Achyranthis Radix, 95.4% of total samples including 100% of Korean and 92.6% of Chinese samples were passed the test. Application of new content criteria could protect the Korean products and decrease the distribution of Chinese products with lower quality.

Uncertainty evaluation for the determination of creatinine in urine by LC-MS/MS (LC-MS/MS를 이용한 소변 중 크레아티닌 분석의 측정불확도 평가)

  • Kim, Jin-Young;Kwon, Woon-Yong;Suh, Sung-Ill;In, Moon-Kyo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.83-90
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    • 2012
  • The objective of the study was to estimate the measurement uncertainty associated with determination of creatinine (Cr) in urine samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Centrifuged urine samples (10 ${\mu}L$) were diluted with 390 ${\mu}L$ of distilled water. To 20 ${\mu}L$ aliquots of diluted urine samples, 30 ${\mu}L$ of internal standard solution (Cr-$d_3$, 5 ${\mu}g/mL$) and 10 ${\mu}L$ of acetonitrile were added and filtered. The samples (1 ${\mu}L$) were introduced into LC-MS/MS with no further pretreatment. Cr was separated on a multi-mode ODS column (Scherzo SM-C18, 75 ${\times}$ 2.0 mm I.D., 3 ${\mu}m$) and quantified by LC-MS/MS operating in MRM mode (Cr, m/z 114.0${\rightarrow}$ 86.0; Cr-$d_3$, m/z 117.0${\rightarrow}$ 89.1). The four factors that contribute uncertainty to the final result were extracted and evaluated. The principal factors of contribution to combined standard uncertainty were sample dilution, calibration curve and repeatability, while the preparation of standard solution was only a minor factor. Relative extended uncertainty of the measured concentration was 14.2% in a real urine sample.

Noise Prediction of Korea High Speed Train (KHST) and Specification of Sub-components (한국형 고속전철 차량소음 예측 및 부품 소음관리방안)

  • ;;;H.W. Thrane
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • 2002.05a
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    • pp.917-923
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    • 2002
  • KITECH and ODS performed a study of internal and external noise prediction of the KHST test train. The object of this study was 3 kind of cars; trailer car(TT2), motorized car(TM1) and power car(TP1) and the predicted noise was calculated for the two different driving speeds in free field and tunnel conditions. Data of carbody design and noise sources were delivered from each manufactures. Some of noise sources which were not available in project team, were chosen by experiences of ODS. Internal noise level of each car were predicted for two cases i.e, at 300 km/h and 350 km/h. In addition sound transmission path and dominant noise sources were also investigated of each section of car, which is circular shell typed part of whole carbody. In case of TT2, the dominating sound transmission path is floor in terms or structure-borne noise and air-borne noise. The main noise sources are structure-borne noise from the yaw-damper and air-borne noise from the wheel/rail contact, whereas the dominating sound transmission path of TM1 are floor and sidewall below the window in terms of structure-borne noise. The main noise sources of TM1 are structure-borne noise from motor/gear unit and the yaw-damper in the free field, and air-borne noise from the wheel/rail contact and structure-borne noise from motor/gear unit in the tunnel. Through the external noise prediction for the KHST test train formation, the noise form the wheel/rail contact is estimated as one of the major sources. In addition, the noise specification of sub-component was proposed for managing each sub-surpplier to reach the KHST noise requirement. The specification provide the sound power of machinery part and transmission loss of component of carbody structure. The predicted noise level in each case exceeded the required limit. Through this study, the noise characteristics of the test train were investigated by simulation, and then the actual test will be performed in near future. Both measured and calculated data will be compared and further work for noise reduction will be continued.

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Alkyl Glycosides from the Flowers of Magnolia obovata (황목련 꽃으로부터 Alkyl Glycoside의 분리 동정)

  • Oh, Eun-Ji;Seo, Kyeong-Hwa;Kwon, Jung-Hwa;Lee, Dae-Young;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.58 no.3
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    • pp.233-236
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    • 2015
  • The flowers of Magnolia obovata were extracted with aqueous MeOH and fractionated into EtOAc, n-BuOH, and $H_2O$ fractination. Three alkyl glycosides were isolated from the EtOAc fraction through repeated silica gel and ODS column chromatography. The structures were identified to be 2-methylbutan-1-ol-${\beta}$-$\small{D}$-galacto-pyranoside (1), 2-methylbutan-1-ol-${\beta}$-$\small{D}$-glucopyranoside (2), and 2-methylpropan-1-ol-${\beta}$-$\small{D}$-glucopyranoside (3) on the basis of spectroscopic analyses such as fast atom bombardment mass spectrometry, infrared spectroscopy, 1D nuclear magnetic resonance (NMR) ($^1H$ and $^{13}C-NMR$), and 2D NMR (gCOSY, gHSQC, and gHMBC). These compounds were isolated for the first time from the flower of M. obovata in this study.