• Title/Summary/Keyword: C4 column

Search Result 1,796, Processing Time 0.035 seconds

HPLC Analysis and Pharmacokinetics of KAL-1120, a Novel Anti-inflammation Agent, in Rats (흰쥐에서 항염증제 후보물질 KAL-1120의 HPLC 분석 및 약물동태)

  • Shin, Dae-Hwan;Lee, Jung-Yeol;Park, Seong-Hyeok;Lee, Gyeong-Bok;Han, Kun;Chung, Youn-Bok
    • Journal of Pharmaceutical Investigation
    • /
    • v.40 no.2
    • /
    • pp.101-107
    • /
    • 2010
  • A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of N-(-4-Chlorophenyl)-6-hydroxy-7-methoxy-2-chromanecarboxamide (KAL-1120), a novel anti-inflammation agent, in the rat plasma. The method was applied to analyze the compound in the biological fluids such as bile, urine and tissue homogenates. After liquid-liquid extraction, the compound was analyzed on an HPLC system with ultraviolet detection at 275 nm. HPLC was carried out using reversed-phase isocratic elution with a $C_{18}$ column, a mobile phase of a mixture of acetonitril (40 v/v%) at a flow rate of 1.0 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma was linear over the concentration range of 0.05-50 ${\mu}g$/mL. The intra- and inter-day assay accuracies of this method ranged from 0.06% to 9.33% of normal values and the precision did not exceed 6.28% of relative standard deviation. The plasma concentration of KAL-1120 decreased to below the quantifiable limit at 1.5 hr after the i.v. bolus administration of 2-10 mg/kg to rats ($t_{1/2,({\alpha})}$ and $t_{1/2,({\beta})$ of 2.15 and 26.7 min at a dose of 2 mg/kg, 3.91 and 33.0 min at a dose of 10 mg/kg, respectively). The steady-state volume of distribution ($V_{dss}$) and the total body clearance ($CL_t$) were not significantly altered in rats given doses from 2 to 10 mg/kg. Of the various tissues tested, KAL-1120 was mainly distributed in the lung and heart after i.v. bolus administration. KAL-1120 was detected in the bile by 30 min after its i.v. bolus administration. However, the concentration in the urine after i.v. bolus administration became too low to measure, suggesting that KAL-1120 is mostly excreted in the bile. In conclusion, this analytical method was suitable for the preclinical pharmacokinetic studies of KAL-1120 in rats.

Chemical Structure of the Major Color Component from a Korean Pigmented Rice Variety (한국산 유색미에서 분리한 안토시아닌의 화학구조)

  • Cho, Man-Ho;Paik, Young-Sook;Yoon, Hye-Hyun;Hahn, Tae-Ryong
    • Applied Biological Chemistry
    • /
    • v.39 no.4
    • /
    • pp.304-308
    • /
    • 1996
  • The major color component of a Korean pigmented rice (Oeyza sativa var. Suwon 415) was purified with Amberlite XAD-7 column and preparative paper chromatography. The purified pigment was determined as anthocyanin by paper chromatography, UV/Vis and NMR spectroscopy. The $\lambda_{max}$ of the Purified anthocyanin on UV/Vis spectrum were 529 nm and 281 nm. The $A_{440}/A_{529}$ value of the purified anthocyanin was 23% suggesting the presence of 3-glycosidic structure. The aglycone from acid hydrolysis showed bathochromic shift (18 nm) in the presence of $AlCl_3$ indicating that the anthocyanidin contained free adjacent hydroxyl groups such as cyanidin, delphinidin, petunidin or luteolinidin. The sugar moiety obtained from acid hydrolysis was determined as glucose by paper chromatography. The NMR spectra showed that the aglycone was cyanidin and the sugar was ${\beta}-D-glucopyranose$. Thus, the chemical structure of the purified anthocyanin was identified as cyanidin $3-O-{\beta}-D-glucopyranoside$.

  • PDF

Optimal HPLC Condition for Simultaneous Determination of Catechins and Caffeine in Green Tea Extracts (녹차 함유 카테친 및 카페인 동시분석을 위한 최적 HPLC 분석 조건)

  • Choung, Myoung-Gun;Lee, Min-Seuk
    • KOREAN JOURNAL OF CROP SCIENCE
    • /
    • v.53 no.2
    • /
    • pp.224-232
    • /
    • 2008
  • The health benefits associated with tea consumption have resulted in the wide inclusion of green tea extracts in botanical dietary supplements, which are widely consumed as adjuvants for complementary and alternative medicines. Tea contains polyphenols such as catechins or flavan-3-ols including (-)-epicatechin (EC), (-)-epigallocatechin (EGC), (-)-epicatechin gallate (ECG), and (-)-epigallocatechin gallate (EGCG), as well as the alkaloid, caffeine. The contents of catechins and caffeine in green tea are considered as a standard of quality evaluation of green tea. Therefor, the purpose of this study was to investigate the most suitable HPLC condition for simultaneous determination of catechins and caffeine in green tea extracts. The efficient HPLC analytical condition of catechins and caffeine contained green tea extracts was developed. The gradient elution employed a $250\;mm\;{\times}\;4.6\;mm$ i.d. YMC-pak ODS-AM 303 column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of 0.1% aqueous phosphoric acid, and mobile phase B, comprising 100% MeOH, and delivered at a flow rate of 1 mL/min as follows: $0{\sim}25\;min$, 80% A; $26{\sim}50\;min$, $80{\sim}70%$ A; 51 min, 80% A. $51{\sim}55\;min$, 80% A. The UV detection wavelength was set at 280 nm. The limit of detection (LOD) for catechins and caffeine standards were under 50 ng/mL.

Studies on Soybean Protein [Part ll]-Isolation and Subunit Composition of Multiple 7S Globulins- (대두(大豆) 단백질(蛋白質)에 관(關)한 연구(硏究) 제2보[第二報]-7S Globulin중의 복합단백질(複合蛋白質)의 분리(分離) 및 그 구성(構成) Subunit에 대하여)

  • Lee, C.Y.;Kim, I.S.;Kim, S.U.
    • Applied Biological Chemistry
    • /
    • v.20 no.1
    • /
    • pp.26-32
    • /
    • 1977
  • The multiple 7S globulins composed of two fractions (A and B) in the electrophoresis with Davis' method were isolated at different stages of the soybean seed development. Electrophoresis of their subunits liberated in PAWU solvent [phenol-acetic acid-water (2 : 1 : 1) solution plus 5M urea] yielded 4 major bands. Observation of both the electrophoretic bands of the multiple 7S fractions(7S-A and 7S-B) and those of their subunits was suggestive of a similarity of the subunit pattern between two 7S fractions. The two fractions in multiple 7S globulins were isolated with DEAE-Sephadex A-50 column$(2.0{\sim}100cm)$ chromatography. They were separated into 2 fractions in a linear gradient concentration of 0.28 to 0.40M NaCl with phosphate buffer (pH 7.8) containing 10mM ${\beta}-mercaptoethanol$(ME). The isolated protein was dissociated into subunits with two different solvent systems; in PAWU solvent and in Tris-HCl buffer(pH 8.0) containing 1% sodium dodecyl sulfate (SDS) and 40mM ME. The dissociated subunits were subjected to electrophoresis in PAWU-treated 7.5% acrylamide gel and in 1% SDS-treated 5.6% acrylamide gel. In PAWU gel electrophoresis, total 7S globulin was separated into 5 major bands, two of which were occupied in common by two 7S fractions(7S-A and 7S-B). In SDS gel electrophoresis, total 7S globulin was separated into 7 major bands, three of which were overlapped with the subunit of the two 7S fractions. The above results alluded us to the presence of a common and/or similar subunit between the multiple 7S globulins.

  • PDF

Formation and Removal of Trihalomethanes based on Characterization of Hydrophobic and Hydrophilic Precursors (전구물질의 소수성 및 친수성 특성에 따른 트리할로메탄의 생성과 제거에 관한 연구)

  • Jeon, Heekyung;Kim, Junsung;Choi, Yoonchan;Choi, Haeyeon;Chung, Yong
    • Journal of Korean Society on Water Environment
    • /
    • v.24 no.1
    • /
    • pp.123-128
    • /
    • 2008
  • The Dissolved Organic Carbon (DOC) existing in a water includes both hydrophobic and hydrophilic substances however, most of the discussion focuses on hydrophobic substances. The hydrophobic fraction was easily removed by absorption or coagulation more than hydrophilic fraction. Therefore, control of the hydrophilic fraction is very important in water treatment process. This study is to determine the variation of DOC, the removal efficiency of DOC, and Trihalomethane formation potential (THMFP) after each stage of water treatment process by fractionating Natural Organic Matters (NOM) into hydrophobic and hydrophilic substance. DOC from raw water was fractionated at acidic pH (pH<2) using XAD 8 resin column, into two fraction : hydrophobic substance (i.e. humic substance) adsorbed on XAD 8 and hydrophilic substance which represent the organics contained in the final effluent. THMFP was carried out according to the following set condition: Cl2/DOC=4 mg/mg, incubation at $25^{\circ}C$ in darkness, pH 7 adjust with HCl or NaOH as necessary, and 72hour-contact time. THMs analyzed in this study were chloroform, bromodichloromethane, dibromochloromethan, and bromoform. Sewage was almost evenly split between the hydrophobic (56%) and hydrophilic fraction (44%). But, Aldrich humic substance (AHS) was found to contain less hydrophilics (14%) than hydrophobics (86%). The formation of THMs may depend on the source which is characterized by the composition of organic matters such as AHS and sewage. The THMFP yield of sewage and AHS were assessed as follows. The value of the THMFP reaction yield, AHS $172.65{\mu}g/mg$, is much higher than that of sewage $41.68{\mu}g/mg$. This illustrates possible significant difference in THMFP according to the component type and the proportion of organic matter existing in water source. Apparently AHS react with chlorine to produce more THMFP than do the smaller molecules found in sewage. Water treatment process may reduce THMFP, nevertheless residual DOC (the more hydrophilic substance) has significant THMFP. Further reduction in organic halide precursors requires application of alternative treatment techniques.

Summer-Time Behaviour and Flux of Suspended Sediments at the Entrance to Semi-Closed Hampyung Bay, Southwestern Coast of Korea (만 입구에서 부유퇴적물 거동과 플럭스: 한반도 서해 남부 함평만의 여름철 특성)

  • Lee, Hee-Jun;Park, Eun-Sun;Lee, Yeon-Gyu;Jeong, Kap-Sik;Chu, Yong-Shik
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
    • /
    • v.5 no.2
    • /
    • pp.105-118
    • /
    • 2000
  • Anchored measurements (12.5 hr) of suspended sediment concentration and other hydrodynamic parameters were carried out at two stations located at the entrance to Hampyung Bay in summer (August 1999). Tidal variations in water temperature and salinity were in the range of 26.0-27.9$^{\circ}C$ and 30.9-31.5, respectively, indicating exchange offshore and offshore water mass. Active tidal mixing processes at the entrance appear to destroy the otherwise vertical stratification in temperature and salinity in spite of strong solar heating in summer. On the contrary, suspended sediment concentrations show a marked stratification with increasing concentrations toward bottom layer. Clastic particles in suspended sediments consist mostly of very fine to fine silt (4-16 ${\mu}$m) with a poorly-sorted value of 14.7-25.9 ${\mu}$m. However, at slack time with less turbulent energy, flocs larger than 40 ${\mu}$m are formed by cohesion and inter-collision of particles, resulting in a higher settling velocity. Strong ebb-dominated and weak flood dominated tidal currents, in the southwestern and the northeastern part, respectively, result in a seaward residual flow of -10${\sim}$-20 cm $s^{-1}$ at station H1 and a bayward residual flow less than 5.0 cm $s^{-1}$ at station H2. However, mean concentration of suspended sediments at station H1 is higher at flood (95.0-144.1 mg $1^{-1}$) than in ebb (75.8-120.9 mg $1^{-1}$). On the contrary, at the station H2, the trend is reversed with higher concentration at the ebb (84.7-158.4 mg $1^{-1}$) than that at the flood (53.0-107.9 mg $1^{-1}$). As a result, seaward net suspended sediment fluxes ($f_{s}$) are calculated to be -1.7 ${\sim}$-$15.610^{3}$ kg $m^{-2}$ $s^{-1}$ through the whole water column. However, the stations H1 and H2 show definitely different values of the flux with higher ones in the former than in the latter. Alternatively, depth-integrated net suspended sediment loads ($\c{Q}_{s}$) for one tidal cycle are also toward the offshore with ranges of 0.37${\times}$$10^{3}$ kg $m^{-1}$ and 0.21${\times}$$10^{3}$ kg $m^{-1}$, at station H1 and H2, respectively. This seaward transport of suspended sediment in summer suggests that summer-time erosion in the Hampyung muddy tidal flats is a rather exceptional phenomenon compared to the general deposition reported for many other tidal flats on the west coast of Korea.

  • PDF

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
    • /
    • v.44 no.3
    • /
    • pp.263-268
    • /
    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
    • /
    • v.16 no.16
    • /
    • pp.7179-7188
    • /
    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.

Effects of Soil Bulk Density on Saturated Hydraulic Conductivity and Solute Elution Patterns (토양의 용적밀도에 따른 포화수리전도도 및 음이온의 용출양상)

  • Kim, Pil-Joo;Lee, Do-Kyoung;Chung, Doug-Young
    • Korean Journal of Soil Science and Fertilizer
    • /
    • v.30 no.3
    • /
    • pp.234-241
    • /
    • 1997
  • The effects of bulk densities(${\rho}_b$) on saturated hydraulic conductivity (Ksat) and solute elution patterns were investigated from five different bulk densities ranging from $1.1Mg/m^3$ to $1.5Mg/m^3$ with each increment of $0.1Mg/m^3$. The hydraulic conductivities observed were divided into two stages: (1) a linearly decrease with increase in bulk density up to $1.4Mg/m^3$, (2) a steady state where the bulk density is greater than $1.4Mg/m^3$. Using the saturated hydraulic conductivity at the steady state, we figured out the equation describing the correlation between bulk densities(${\rho}_b$) and saturated hydraulic conductivity(Ksat) as follows: $Ksat=-19.2({\rho}_b{^2})+6{\rho}_b+15.5$, (r=0.985). Electrical conductivity(EC) measured from the leachate of the soil column showed that EC at the same pore volume were decreased with an increase in the bulk density from $1.2g/cm^3$, $1.5g/cm^3$, as shown in the time taken to collect the same pore volume at each respective bulk density. The maximum relative concentrations (C/Co=1) from the breakthrough curves for the anions of $Cl^-$, $NO_3{^-}$ and $SO_4{^{2-}}$, which are weakly adsorbed on the soil particles, moved to the right of the graph, while a distinctive retardation occurs at the bulk density between $1.3Mg/m^3$ and $1.4Mg/m^3$. The time taken to recover about 90% of indigenous sulphate was approximately twice as those of chloride and nitrate, resulting in slightly stronger adsorption characteristics for sorption sites on the soil surface. Thus, we can conclude that the salt accumulation in green house soil might be significantly influenced by it's bulk density at the soil depth, as well as the adsorption capacity of ions for the sorption sites in soils.

  • PDF

In-situ Treatment for the Attenuation of Phosphorus Release from Sediments of Lakes (호소퇴적물로부터 인 용출 저감을 위한 In-situ 처리)

  • Kim, Seog-Ku;Lee, Mi-Kyung;Ahn, Jae-Hwan;Kang, Sung-Won;Kim, Young-Im
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.28 no.5
    • /
    • pp.563-572
    • /
    • 2006
  • In order to propose optimum in-situ treatment for reducing phosphorous release from sediment of stationary lakes, a series of column tests were performed. The sediment used in experiment was very fine clay with a mean grain site $7.7{\phi}$ and high $C_{org}$ contents(2.4%). Phosphorous releases were evaluated in two ways : in lake water(with microbial effect) and in distilled water(without microbial effect). As in-situ capping material, sand and loess were used while Fe-Gypsum and $SiO_2$-Gypsum were used for in-situ chemical treatment. In case of lake water considering the effect of microorganism, phosphorous concentration rapidly decreased in the early stage of experiment but it was gradually increased after 10 days. Flux of phosphorous release for control was $3.0mg/m^2{\cdot}d$. Whereas, those for sand layer capping(5 cm) and loess layer capping(5 cm) were $2.5mg/m^2{\cdot}d\;and\;1.8mg/m^2{\cdot}d$, respectively because the latter two were not consolidated sufficiently. For Fe-gypsum and $SiO_2$-gypsum the fluxes were $1.4mg/m^2{\cdot}d$ which meant that reduction efficiency of phosphorous release was more than 40% higher than that of control. The case capping with complex layer was $1.0mg/m^2{\cdot}d$, which showed high reduction efficiency over 60%. The addition of gypsum($CaSO_4{\cdot}2H_2O$) into the sediment reduced release of Phosphorus from the sediments. Gypsum acted as a slow-releasing source of sulphate in sediment, which enhanced the activity of SRB(sulfate reducing bacteria) and improved the overall mineralization rate of organic matter.