• 제목/요약/키워드: extraction chromatography

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지리바꽃 괴경의 알카로이드 (Alkaloids from the Tuber of Aconitum chiisanense)

  • 이무택;성환길;황완균;김일혁
    • 약학회지
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    • 제41권2호
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    • pp.161-173
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    • 1997
  • Tuber of Aconitum chiisanense(Ranunculaceae) a specific medicinal plant in Korea, which is known to have the activity to recover reduced metabolism of feeble patients and has been used to symptoms such as pain, paralysis, atonia and coldness of extremities, etc. were studied. The powdered tubers of the plant were extracted with 10% EtOH 3 times and the combined extract was dissolved in 1N HCl solution and washed with ethyl acetate. The aqueous layer was basified with solid $Na_2CO_3$ and extracted with $CHCl_3$ to obtain an alkaloidal fraction. The alkaloidal fraction was subjected to column chromatography using silica gel, alumina and Sephdex LH 20, etc. From the alkaloidal fraction, five diterpene alkaloids, mesaconitine, aconitine, hypaconitine, 8-O-ethyl 14-benzoylmesaconine and talatizamine, were isolated and identified on the basis of their physico-chemical properties and spectroscopic evidences($^1H$-, $^{13}C$-NMR, EI-MS, IR, 2D-NMR) respectively. Especially the Compound IV, 8-O-ethyl 14-benzoylmesaconine, was assumed to be an artifact resulting from mesaconitine during extraction procedures. The contents of mesaconitine, aconitine and hypaconitine in the mother tuber of this plant were 0.300%, 0.024%, and 0.068%. And that of the attached tuber(new one) of this plant were 0.336%, 0.034% and 0.240% respectively.

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Volatile Flavor Compounds in the Leaves of Fifteen Taxa of Korean Native Chrysanthemum Species

  • Kim, Su Jeong;Ha, Tae Joung;Kim, Jongyun;Nam, Jung Hwan;Yoo, Dong Lim;Suh, Jong Taek;Kim, Ki Sun
    • 원예과학기술지
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    • 제32권4호
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    • pp.558-570
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    • 2014
  • This study was conducted to compare the volatile flavor compounds found in the leaves of 15 taxa of Korean native Chrysanthemum species. The volatile flavor compounds from the taxa were collected using a simultaneous steam distillation and extraction technique and were analyzed using gas chromatography/mass selective detector (GC/MSD). A total of 45 volatile flavor compounds were identified with six functional groups: 14 alcohols, 4 ketones, 19 hydrocarbons, 5 esters, 2 acids, and 1 aldehyde. The main functional group in 15 taxa of Chrysanthemum species was alcohols, accounting for 28.7% of volatile flavor compounds, followed by ketones (21.2%) and hydrocarbons (13.2%). Camphor, which is known for its antimicrobial properties, was the most abundant volatile compound (30%) in C. zawadskii ssp. latilobum and var. leiophyllum. In particular, C. indicum subspecies and C. boreale contained ${\alpha}$-thujone, which has outstanding anti-bacterial, anti-cancer, anti-inflammatory, anti-ulcer, and anti-diabetic efficacies. C. indicum var. albescens could be used in perfumes, since it showed 21 times more camphene than C. indicum. In addition, C. indicum var. acuta contained a fairly high content of 1,8-cineole, which has an inhibitory effect on mutagenesis. C. lineare contained only pentadecanoic acid compounds, whereas other taxa hexadecanoic acids. Overall, the Korean native Chrysanthemum species had considerable variation in volatile flavor compounds in their leaves. This study provides a good indication of specific potential use for various applications.

토양 및 토양수 중 살충제 Clothianidin 및 대사산물 잔류분석법 확립 (Determination of Analytical Method for the Insecticide Clothianidin and its Metabolites in Soil and Surface Water)

  • 최영준;권찬혁;한병수;이영득
    • 한국환경농학회지
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    • 제33권2호
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    • pp.69-77
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    • 2014
  • BACKGROUND: The purpose of this study was to investigate the effects of clothianidin on the soil in terms of clothianidin dissipation and degradation to evaluate its safety in order to provide an analytical foundation for clothianidin and the 5 metabolites related to it. METHODS AND RESULTS: High-performance liquid chromatography(HPLC) was used to separate clothianidin and its metabolites in this study. In soil, after suppressing dissociation-proned ions with weak alkalic $NH_4OH$ and extracting the metabolites with methanol, clothianidin, Methylaminoimidazole(MAI), Methylnitroguanidine(MNG), Thiazolylmethylurea(TZMU) and Thiazolylnitroguanidine(TZNG). Thiazolylmethylguanidine(TMG) were extracted with the addition of neutral $NH_4OAC$ to increasing the intensity of ions. Compounding elements were separated by using Hydrometrix ($ChemElut^{TM}$) and ion-exchanging Solid-phase extraction(SPE) Strong cation-exchanger(SCX) and C18 were used. The recovery rates of clothianidin and 5 metabolites in soil and water ranged from 87.4% to 104.3%. A standard deviation of our analysis for the soil and water samples were less than 5%. CONCLUSION: Well accepted detection limits for clothianidin and 5 metabolites in soil samples based on a dissipation analysis is 0.005 mg/kg and 0.001 mg/L in water samples. The dissipation concentration of this study was decided to be enough to evaluate the dissipation levels of clothianidin and its metabolites.

나이트로사민류의 국내 정수장 분포 특성 및 위해성 평가 (Risk assessment and distribution characteristics of N-nitrosamines in drinking water treatment plants)

  • 손보영;이이내;양미희;박상민;표희수;이원석;박주현
    • 상하수도학회지
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    • 제32권5호
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    • pp.389-398
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    • 2018
  • A nationwide survey of 8 N-nitrosamines in finished water samples from drinking water treatment plants (DWTPs) in Korea was conducted. The samples were pre-treated by solid-phase extraction (SPE) and analyzed using a gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). According to the study results, four N-nitrosamines (NDMA, NDEA, NMOR, NDBA) were detected for three consecutive years, NMEA and NPYR were only found in samples collected in 2013. Two of these N-nitrosamines, N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA), have received attention and were the most commonly detected. The concentration of NDMA and NDEA in this study ranged from $0.002{\mu}g/L$ to $0.013{\mu}g/L$ and in $0.001{\mu}g/L$ to $0.008{\mu}g/L$, respectively. In comparison to studies performed in EPA(UCMR2), the concentrations of NDMA (from $0.002{\mu}g/L$ to $0.630{\mu}g/L$) and NDEA (from $0.005{\mu}g/L$ to $0.100{\mu}g/L$) observed in the this study were low.

THE ORIGIN AND DISTRIBUTION OF ANIONIC GROUPS IN TMP

  • Anna Sundberg;ndrey Pranovich;Bjarne Holmobom
    • 한국펄프종이공학회:학술대회논문집
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    • 한국펄프종이공학회 1999년도 Pre-symposium of the 10th ISWPC Recent Advances in Paper Science and Technology
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    • pp.254-258
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    • 1999
  • The distribution of anionic groups in the fibers, the fines, the colloidal fraction and the dissolved fraction, respectively, of thermomechanical pulp (TMP) suspensions was determined and peroxide bleaching of spruce TMP were also studied. Spruce TMP was extracted with hexane, treated with alkali, or bleached with peroxide. Suspensions made at pH 5.5 were fractionated into long fibres, large fines, small fines, a colloidal fraction and a dissolved fraction. The charge of the fractions was determined using polyelectrolyte titration. To determined the origin of the charges, the contents of fatty acids, resin acids and acidic units in hemicelluloses in the different fractions were determined by has chromatography. Extraction of TMP with hexane prior to fractionation increased the measured charge of the fibres. The removal of the wood resin probably uncovered some carboxyl groups on the fibre surfaces, or improved th e penetration of polybrene into the pores of the fibres. The charge of the fines and the colloidal fraction was lower when the wood resin had been removed. Alkaline treatment of the TMP increased the charge of the fibres and fines, mainly because of demethylation of pectins. Alkaline treatment increased the charge also of the dissolved fraction, because of the release the charge also of the dissolved fraction, because of the release of pectic acids into the water phase. Alkaline peroxide bleaching further increased the charge of fibres and the dissolved fraction, most likely because of lignin oxidation. The charge of the colloidal fraction, consisting mainly of wood resin, was only slightly affected by alkaline treatment and peroxide bleaching. The anionic groups in TMP suspensions were mainly free uronic acids in the hemicelluloses. The contribution from the fatty and resin acids was substantial only for the colloidal fraction.

혈당상승억제 기능성 소재인 달맞이꽃종자 추출물의 지표물질 분석법의 통계적 검증에 대한 연구 (A Study on the Statistical Method for the Target Component of a Glucose-lowering Functional Material in Extracts of Evening Primerose Seeds)

  • 박상욱;방준석;이원재
    • 한국임상약학회지
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    • 제26권1호
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    • pp.70-76
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    • 2016
  • Background: The use of the extracts from evening primrose seeds as a health functional food has been gradually increased. Therefore, the monitoring and screening process has been considerably required for its quality control. Objective: This study aimed to estimate the measurement uncertainty associated with determination of penta-o-galloyl ${\beta}$-D-glucose (PGG) in extracts from evening primrose seeds by high-performance liquid chromatography. Methods: The sources of measurement uncertainty was expressed in accordance with mathematical/statistical theories of GUM & EURACHEM Guide. The expanded uncertainty was calculated by using the relative standard uncertainty between analytical result and sources of uncertainty in measurement (sample weight, final volume, extraction volume, standard solution, matrix and instrument etc). Results: In the results of 95% confidence interval, the uncertainty in measurement was $10,253.34{\pm}1,844.50{\mu}g/kg$ (k = 2.0). Conclusion: In this study, it showed that the value of uncertainty in measurement for determination of PGG in extracts from evening primrose seeds by HPLC has about 18.0% influence on PGG contents of the analytical results. The results would be very useful for the monitoring and screening of evening primrose seeds marketed in Korea for its quality control as dietary supplement.

Estimation of polycyclic aromatic hydrocarbons emission from sewage sludge of sewerage treatment plants in Korea

  • Kim, Dong-Hwan;Hwang, Jong-Seob;Lee, Min-Hee;Ok, Gon
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2003년도 International Symposium on Clean Environment
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    • pp.85-88
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    • 2003
  • Polycyclic aromatic hydrocarbons (PARs) are an important group of organic contaminants present in sewage sludge, due to their persistence, toxic, bioaccumulative and long range transfer. These characters make themselves as Persistent Organic Pollutants(POPs) in Long Range Transboundary Air Pollutions convention(LRT AP) of Europe. A method of the gas chromatographic-mass spectrometric (GC-MS) determination of PARs present in sewage sludge was developed and applied to analyzed samples from five sewerage treatment plants (SWTPs), having different treatment types. PARs were extracted from freeze-dried samples by toluene 16 hours in a soxhlet extraction system. The sludge extracts were cleaned-up by an activated silica gel column chromatography. The sum of the 16 US Environmental Protection Agency PARs sewage sludge samples varied from 2.44 to 4.82 ${\mu}g$/g. Concentration of emission carcinogen PARs(PARcarc), such as Benzo(a)anthracene, Benzo(b)fluoranthene, Benzo(k)fluoranthene, Benzo(a)pyrene, Dibenzo(a, h)anthracene and Indeno(1, 2, 3-cd)pyrene ranged from 0.62 to 1.03 ${\mu}g$/g. The total amount of PAHs emission from sewage sludge in Korea was calculated as a top-down approach. PARs and $\sum$PAHcarc from sewage treatment plants had several pathway each by-products. In the ocean dumping, PAHs and $\sum$PAHcarc emissions were 1155.95 kg/year and 5040.32 kg/year. In recycle, PAHs and $\sum$PAHcarc emissions were 98.36 kg/year and 428.87 kg/year. In the landfill, PAHs and $\sum$PAHcarc emissions were 190.40 kg/year and 830.21 kg/year. In the incineration, PAHs and $\sum$PAHcarc emission were 33.10 kg/year and 830.21 kg/year. (In case of incineration, the whole provisions of PARs and $\sum$PAHcarc contained to flowed in sludge was supposed to be exhausted to environment through exhaust after incineration.)

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Activation of Macrophages by the Components Produced from Cordyceps militaris

  • Kim, Hyun-Yul;Kim, Kwang-Hee;Han, Shin-Ha;Lee, Seong-Jung;Kwon, Jeung-Hak;Lee, Sung-Won;Kim, Kyung-Jae
    • IMMUNE NETWORK
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    • 제7권2호
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    • pp.57-65
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    • 2007
  • Background: Cordyceps militaris have been reported to modify the immune and inflammatory responses both in vivo and in vitro. Macrophages play important roles in the innate immunity through the phagocytosis of antigens. This study examined the effects of Cordyceps militaris on the activation of murine macrophage RAW 264.7 cells and primary macrophages. Methods: The components contained in culture broth of Cordyceps militaris were purified by propyl alcohol extraction and HP 20 column chromatography to CMDB, CMDBW, CMDB5P, and CMDB25P. The amounts of nitric oxide (NO) were determined by using ELISA, Griess reagent respectively. The amounts of some cytokines were determined by using ELISA, western blot, and RT-PCR The expression levels of cell surface molecules (ICAM-1, B7-1 and B7-2) were measured by flow cytometric analysis. Results: All the components of Cordyceps militaris produced significant amounts of NO. In particular, CMDB produced much more NO in RAW 264.7 cells and primary macrophages than other fractions of Cordyceps militaris. CMDB increased significantly the production of tumor necrosis factor (TNF)-${\alpha}$, interleukin (IL)-1${\beta}$, and IL-6 dose-dependently in RAW 264.7 cells. Examination of the gene expression level also showed that the enhanced production of cytokines was correlated with the up-regulation of i-NOS expression, cycloxygenase (COX)-2 expression, IL-1${\beta}$ and IL-6 expression, and TNF-${\alpha}$ expression on the expression of mRNAs by semi-quantitative RT-PCR Western blot analysis also confirmed that CMDB enhances the expression level of these cytokines. Conclusion: These results show that CMDB stimulates the production of NO and pro-inflammatory cytokines and can also up-regulate the gene expression levels in macrophages.

Effects of polysaccharides derived from Orostachys japonicus on induction of cell cycle arrest and apoptotic cell death in human colon cancer cells

  • Ryu, Deok-Seon;Baek, Geum-Ok;Kim, Eun-Young;Kim, Ki-Hoon;Lee, Dong-Seok
    • BMB Reports
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    • 제43권11호
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    • pp.750-755
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    • 2010
  • Crude Orostachys japonicus polysaccharide extract (OJP) was prepared by hot steam extraction. Polysaccharides (OJPI) were separated from OJP by gel filtration chromatography and phenol-sulfuric acid assay. The average molecular weight of the OJPI was 30-50 kDa. The anti-proliferative effect of OJPI on HT-29 human colon cancer cells was investigated via morphology study, cell viability assay, apoptosis assay, cell cycle analysis, and cDNA microarray. OJPI inhibited proliferation and growth of HT29 cells and also stimulated apoptosis in a dose- and time-dependent manner. In cell cycle analysis, treatment with OJPI resulted in a marked increase of cells in the G0 (sub G1) and G2/M phases. To screen for genes involved in the induction of cell cycle arrest and apoptosis, the gene expression profiles of HT-29 cells treated with OJPI were examined by cDNA microarray, revealing that a number of genes were up- or down-regulated by OJPI. Whereas several genes involved in anti-apoptosis, cell proliferation and growth, and cell cycle regulation were down-regulated, expression levels of several genes involved in apoptosis, tumor suppression, and other signal transduction events were up-regulated. These results suggest that OJPI inhibits the growth of HT-29 human colon cancer cells by various apoptosis-aiding activities as well as apoptosis itself. Therefore, OJPI deserve further development as an effective agent exhibiting anticancer activity.

여름 느타리 버섯 (Pleurotus sajor-caju) 저장중의 향기성분 변화 (Changes of Volatile Components of Pleurotus sajor-caju During Storage)

  • 정순택;홍재식
    • 한국균학회지
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    • 제19권4호
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    • pp.292-298
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    • 1991
  • Simultaneous distillation-extration method에 의해 국내에서 인공재배되고 있는 여름 느타리 버섯(Pleurotus sajor-caju)을 실온과 냉장하에서 저장하면서 휘발성 향기성분을 분리한 다음 GC-MS 및 GC에 의한 표준품과의 머무름시간 비교에 의해 향기성분의 변화를 검토하여 보았다. 총 aroma contentrates의 함량은 냉장 저장시는 큰차이를 보이지 않았으나 실온 저장시는 큰 감소의 경향을 보였다. 확인된 38종의 휘발성 화합물중 실온 저장시 ${\delta}-decalactone$만 약간증가하였으나 기타의 성분들은 현저히 감소한 반면 냉장 저장시는 2-methyl butanal, 1-octen-3-ol, cis,cis-1,5-octadien-3-ol, pentadecanoic acid등은 감소추세를 보였지만 3-octanone, 1-octen-3-one, 3-octanol, 5-undecanol등은 오히려 증가되는 경향을 보였다. 또한 중량 감소와 관능적 특성은 실온 저장시 냉장 저장보다 심한 변화를 보였다.

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