• Title/Summary/Keyword: reversed phase

Search Result 605, Processing Time 0.03 seconds

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
    • /
    • v.33 no.2
    • /
    • pp.153-157
    • /
    • 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 $1.4 {\mu}M$.

  • PDF

Formation of TiO(OH)$_2$ Ultrafine Particles by Reverse Micelle (역마이셀에 의한 TiO(OH)$_2$ 미세분말 제조)

  • 장화익;강석원;이광래
    • Journal of the Korean Ceramic Society
    • /
    • v.35 no.6
    • /
    • pp.594-602
    • /
    • 1998
  • Titanium hydroxide (TiO({{{{ {OH }_{2 } }})) fine particles were produced by the reverse micelle technique. For the formation of titanium hydroxide (TiO({{{{ {OH }_{2 } }})) particles with the technique reversed micellar solution was prepared by solubilizing water into organic solvent (isooctane) with a surfactant and titanium alkoxide (tetraisopropyl orthotitanate) diluted with isopropyl alcohol was added to the reversed micellar solution. The hdrolyzed species (TiO({{{{ {OH }_{2 } }})) was formed by the hydrolysis of titanium alkoxide and titanium dioxide is then formed by the condensation of the hydrolyzed species. There are several process variables such as surfactants concentration of surface cosurfactant hydrolysis temperature and pH. In this work the ef-fects of process variables on paticle shapes particle size distribution and paticle agglomeration were bi-nodal for an anionic surfactant(AOT) in the whole range of temperature pH and surfactant concentration of this experiment. The addition of ethanol as a cosurfactant resulted in narrow particle size distribution of the experiment. The additiono of ethanol as a cosurfactant resulted in narrow particle size distribution and 0.12${\mu}{\textrm}{m}$ of smaller average particle diameter. FT-IR spectrum of particles shows the absorption peak of Ti-OH bonding and Ti-O bonding. An exothermic peak around 41$0^{\circ}C$ in TGA-DTA curve shows that crys- tallized anatase phase appears and completely transits to anatase around 45$0^{\circ}C$.

  • PDF

Quantitative determination of inosine 5'-monophosphate dehydrogenase activity in human peripheral blood mononuclear cells by ion-pair reversed-phase high-performance liquid chromatography (이온쌍 역상 HPLC를 이용한 인체 말초혈액단핵구에서 이노신 5'-일인산 탈수소효소 활성의 정량적 측정)

  • Shin, Hye-Jin;Kwon, Soon-Ho;Park, Ji-Myeong;Kwon, Soon-Hyo;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
    • /
    • v.23 no.6
    • /
    • pp.531-536
    • /
    • 2010
  • A quantitative analytical method has been established for the measurement of inosine 5'-monophosphate dehydrogenase (IMPDH) activity in human peripheral blood mononuclear cells (PBMCs) by ion-pair reversed-phase high performance liquid chromatography equipped with ultraviolet detection (HPLC/UV). IMPDH is a ${\beta}$-nicotinamide adenine dinucleotide hydrate (NAD+)-dependent dehydrogenase in which the enzyme converts inosine 5'-monophosphate (IMP) into xanthosine 5'-monophosphate (XMP). Its activity was measured by quantifying a HPLC chromatogram corresponding to XMP produced during the incubation of lysed PBMCs with IMP as a substrate and $NAD^+$ as a coenzyme. XMP produced was detected at a wavelength of 260 nm. The mobile phase was composed of a mixture of 37 mM potassium dihydrogen phosphate containing 7 mM tetra-n-butylammonium hydrogen sulfate adjusted to pH 5.5 and methanol (85:15, v/v) with a flow rate of 1 mL/min. The calibration curve was linear ($r^2$=0.999999) in the range of $0.2-50.0\;{\mu}M$ and the limit of quantification (LOQ) was $0.2\;{\mu}M$. The intra- and inter-day precisions were between 0.88-1.47% and 0.85-5.24%, respectively. The intra- and inter-day accuracies were between 98.74-99.99% and 99.95-101.65%, respectively. IMPDH activity in 11 Korean healthy volunteers ranged from 18.29 to 36.60 nmol/h/mg protein (mean = $27.70{\pm}6.28\;nmol/h/mg$ protein).

A study on the heat transfer characteristics during outward melting process of ice in a vertical cylinder (수직원통형 빙축열조내 외향용융과정시 열전달특성에 관한 연구 -작동유체의 유동방향 및 축열조 형상비에 따른 열성능 비교-)

  • Kim, D.H.;Kim, D.C.;Kim, I.G.;Kim, Y.K.;Yim, C.S.
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
    • /
    • v.9 no.2
    • /
    • pp.171-179
    • /
    • 1997
  • During the day time in summer, peak of air conditing load, and electric power management system lies under overloaded condition. The reason is the enlarged peak load value of electric power caused by increased air-cooling load in summer. To prevent load concentration during day time and overloaded condition of power management system, some energy storage methods are suggested. One of these methods is ice storage system. Water has some good properties as P.C.M.(Phase Chang Material) : Its melting point is the range of required operation temperature. It has large specific latent heat and is chemically stable compared to other organic or inorganic substances. It is cheap and easy to treat. This study represents experimental results of heat transfer characteristics of P.C.M. under the outward melting process in a vertical cylinder. We experimented with twelve combinations of conditions, i.e., three different inlet temperatures($7^{\circ}C,\;4^{\circ}C\;and\;1^{\circ}C$), two working fluid directions(upward and downward), and two aspect ratios, H/R(4 and 2). At the inlet temperature of $7^{\circ}C$ and $4^{\circ}C$, there was temperature stagnation region where the temperature of P.C.M. remains constant at $4^{\circ}C$ regardless of aspect ratio and direction of working fluid. This temperature stagnation occurs as the water, at its maximum density, flows down to the lower region. The phase change interface formed bell-shaped curve as the melting process continued. With a new set of conditions(4H/R, inlet temperature $4^{\circ}C$ and $1^{\circ}C$, downward/upwerd inlet direction), the movement of phase change interface was faster when the working flued inlet direction was downward. With the same set of conditions, melting rate and total melting energy were larger when the working fluid inlet direction was downward. The results were reversed when the other sets of conditions were applied.

  • PDF

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
    • /
    • v.53 no.1
    • /
    • pp.25-30
    • /
    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

The Stereospecific Analysis of the Triacylglycerols of Ginkgo Nut Oils by High-Performace Liquid Chromatography(HPLC) in the Silver Ion and Reversed Phase Modes (銀Ion 및 역상(逆相) HPLC를 이용(利用)한 입체이성체적(立體異性體的) 분석(分析)에 의한 은행종실유(銀杏種實油)의 트리글리세리드의 분자종(分子種)에 관한 연구(硏究))

  • Joh, Yong-Goe;Woo, Hyo-Kyeng;Kim, Hoon-Sook
    • Journal of the Korean Applied Science and Technology
    • /
    • v.14 no.1
    • /
    • pp.61-76
    • /
    • 1997
  • Triacylglycerols of the seeds of Ginkgo biloba have been resolved by high-performace liquid chromatography(HPLC} in the silver-ion and reverse-phase modes. The fatty acids were identified by a combination of capillary gas chromatography and gas-chromatography /mass spectrometry as the methyl and /or picolinyl ester. The main components are $C_{18:2{\omega}6}$(39.0mol%), $C_{18:1{\omega}7}$(asclepic acid 21.5mol%), and $C_{18:1{\omega}9}$(oleic acid, 13.8mol%). Considerable amounts of unusual acid such as $C_{20:3{\Delta}^{5,11,14}$ (5.7mol%), $C_{18:2{\Delta}^{5,9}$(2.8mol%), and $C_{18:3}{\Delta}^{5,9,12}$(1.6mol%), were checked. In addition, an anteiso-branched fatty acid, 14-methylhexadecanoic acid, was also present as a minor component(0.9 mol%). The triacylglycerols were separated into 17 fractions by reverse-phase HPLC, and the fractionation was achieved according to the partition numnber(PN) in which a ${\Delta}^5$-non methylene interrupted double bond($^5$-NMDB) showed different behaviour from a methylene interrupted double bond in a molecule with a given cahinlength. Silver-ion HPLC exhibited excellent resolution in which fractions(23 fractions) were resolved on the basis of the number and configuration of double bonds. In this instance, the strength of interaction of a ${\Delta}^5$-NMDB system with silver ions seemed to be weaker than a methylene interrupted double bond system. The principal triacylglycerol species are as follows ; $(C_{18:2{\omega}6)2}/C_{18:1{\omega}7}$, $C_{18:1{\omega}9}/C_{18:1{\omega}7}/C_{18:2{\omega}6}$, $(C_{18:1{\omega}7)2}/C_{18:2{\omega}6}$, $C_{16:1{\omega}7}/C_{18:1{\omega}9}/C_{20:3}{\Delta}^{5,11,14}$, $C_{16:1{\omega}7}/C_{18:1{\omega}7}/C_{20:3}{\Delta}^{5,11,14}$, $C_{18:1{\omega}9}/C_{18:1{\omega}7}/C_{18:2{\omega}6}$, $C_{18:1{\omega}9}/C_{18:2}{\Delta}^{5,5}/C_{20:3}{\Delta}^{5,11,14}$, $(C_{18:1{\omega}7)2}/C_{18:2{\omega}6}$ and $(C_{18:1{\omega}9)2}/C_{18:2{\omega}6}$, while simple triacylglycerols without $C_{18:2{\omega}6})_3$ were not present. Stereospecific analysis showed that fatty acids with ${\Delta}^5$-NMDB system and saturated chains were predominantly located at the site of sn-3 carbon of glycerol backbones. It is evident that there is asymmetry in the distribution of fatty acids in the TG molecules of Ginkgo nut oils.

Studies of separation and quantitation for selenium species in food (식품중의 셀레늄 화학종의 분리 및 정량연구)

  • Jang, Hee-Young;Min, Hyungsik;Lee, Jonghae;Pak, Yong-Nam
    • Analytical Science and Technology
    • /
    • v.26 no.3
    • /
    • pp.182-189
    • /
    • 2013
  • The purpose of this research is to separate and quantitate selenium species in some food samples with HPLC-ICP-MS. Cation exchange chromatography showed efficient separation only for inorganic Se species while reversed phase ion pair chromatography showed good separation for both inorganic and organic Se species. $C_8$ column ($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm) was used with optimum condition of 5% methanol mobile phase, 0.05% of nonafluorovaleric acid ion pairing reagent. Five standard Se species of Se(IV), Se(VI), SeCys(selenocystein), SeMet(selenomethionine) and Se-M-C(seleno methyl cystein) were separated successfully under the optimum condition (mobile phase; 5% methanol, ion-pairing reagent; 0.05% nonafluorovaleric acid, flow rate; 0.9 mL $min^{-1}$). To extract Se species, microwave assisted and enzyme-assisted extraction methods were studied. In enzyme-assisted extraction method, protease I for garlic, protease I plus trypsin for pork and mackerel, and protease XIV for tuna showed the best extraction efficiency. With the optimum condition for each sample, it was found that mostly inorganic Se, SeCys and SeMet are present in the sample studied ranging from few ${\mu}g$ $g^{-1}$ to few tens of ${\mu}g$ $g^{-1}$.

Determination of itraconazole in human plasma by high performance liquid chromatography (HPLC/UV를 이용한 혈장 중 이트라코나졸의 분석)

  • Jang, Hae Jong;Lee, Ye Rie;Lee, Kyung Ryul;Han, Sang-Beom;Kang, Seung Woo;Lee, Hee Joo
    • Analytical Science and Technology
    • /
    • v.19 no.3
    • /
    • pp.239-243
    • /
    • 2006
  • This method is used for the determination of itraconazole in human plasma by liquid-liquid extraction and high performance liquid chromatography. Felodipine was used as an internal standard. After extraction of the plasma with diethyl ether, the centrifuged upper layer was then transferred. The supernantant was evaporated and then reconsituted with mobile phase. The mobile phase was composed of 10 mM ammonium acetate adjusted to pH 7 by phosphoric acid with a flow rate of 0.2 mL/min. A C18 reversed-phase column with a pre-column was used as the analytial column. Linear detection responses were obtained for itraconzole concentration range for 2~1,000 ng/mL. The correlation coefficient of linear regression($R^2$) was 0.9991, limit of quantification (LOQ) was 2 ng/mL, reproducibility was less than 10.8 %, and accuracy was 97.2~108.2%. This method has been successfully applied to the pharmacokinetic study of itraconazole in human plasma.

Characteristics of Extraction of Daidzein and Genistein in Soybean Using Sub/Supercritical Fluids (아임계/초임계 유체를 이용한 콩에 포함된 Daidzein과 Genistein의 추출특성)

  • Choi, Du Young;Zheng, Jinzhu;Row, Kyung Ho
    • Applied Chemistry for Engineering
    • /
    • v.16 no.5
    • /
    • pp.609-613
    • /
    • 2005
  • Daidzein and genistein were extracted from Korean soybean by supercritical $CO_2$ and sub/supercritical water. The extracted sample was analyzed by reversed-phase high performance liquid chromatography (RP-HPLC). The retention time, retention factor, column efficiency, column selectivity and resolution of aglycons were compared with the change in the temperature and pressure of supercritical fluid and ethanol concentration. The characteristics of extraction of daidzein and genistein were more affected by ethanol concentration using supercritical $CO_2$. The most desirable extraction yield was obtained by supercritical $H_2O$ with $400^{\circ}C$ and 250 bar. Generally, the extraction yield of aglycons increased over 10 times using supercritical $CO_2$ than sub/supercritical $H_2O$.

Establishment of Analytical Method for Carpropamid in Agricultural Commodities using HPLC-DAD/MS (HPLC-DAD/MS를 이용한 농산물 중 살균제 Carpropamid의 정밀 잔류분석법 확립)

  • Lee, Hyeri;Choi, Hoon;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
    • /
    • v.19 no.3
    • /
    • pp.185-194
    • /
    • 2015
  • This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.