• Title/Summary/Keyword: 크로마토 그래피 추출

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Isolation and HPLC-DAD validation of xanthoangelol in Lespedeza bicolor extract (싸리나무 추출물의 Xanthoangelol 분리 및 HPLC-DAD 밸리데이션)

  • Woo, Hyun Sim;Kim, Yeong-Su;Oh, Yu Jin;Cho, Hae Jin;Song, Se-Kyu;Kim, Dae Wook
    • Korean Journal of Food Science and Technology
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    • v.52 no.1
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    • pp.26-30
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    • 2020
  • This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R2>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

Structure Analysis of Water-soluble Polysaccharides Extracted from The Unripe Fruit of Cudrania tricuspidata (꾸지뽕나무 열매에서 추출한 수용성 다당류의 구조분석)

  • Kim, Seok Ju;Lee, Kyung-Tae;Youe, Won-Jae;Lee, Sung-Suk;Kim, Yong Sik
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.6
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    • pp.740-746
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    • 2014
  • The unripe fruit of cudrania tricuspidata was extracted with 50% ethanol. The crude water-soluble extracts were separated by liquid-liquid separation with n-hexane, ethyl acetate and butanol followed by precipitation with ethanol, and then the water-soluble polysaccharide (F1) was isolated by the fractionation through gel permeation chromatography using preparative PLaquagel-OH column with water. The structure was characterized by monosaccharide composition with HPAEC-PAD, methylation analysis with GC-MS, FT-IR and HPLC. According to the data, F1 was com posed of glucose (22.84 mM), galactose (13.75 mM), arabinose (45.87 mM), xylose (7.49 mM). It was revealed which uronic acid and acetyl group were not attached in F1. And it is constituted of 1-linked arabinose, 1,4-linked arabinose, 1,3-linked glucose, 1,4-linked galactose, 1,4-linked glucose, 1,3,6-linked galactose, 1,3,6-linked glucose and the ratio was showed 1.1 : 1.0 : 4.9 : 7.5 : 3.0 : 3.1 : 1.4 : 1.5.

High Performance Liquid Chromatographic Determination of Free Sugars in Ginseng and Its Products (고속액체(高速液體) 크로마토그래피에 의(依)한 인삼(人蔘) 및 인삼제품중(人蔘製品中)의 유리당(遊離糖)의 정량(定量))

  • Choi, Jin-Ho;Jang, Jin-Gyu;Park, Kil-Dong;Park, Myung-Han;Oh, Sung-Ki
    • Korean Journal of Food Science and Technology
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    • v.13 no.2
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    • pp.107-113
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    • 1981
  • Free sugars were isolated from ginseng root and its products and analyzed by using high performance liquid chromatogrphy. To isolate free sugars from aqueous sample solution fat-soluble components, crude saponin and protein were removed from the solution by extracting with benzene, water-saturated butanol and 80% ethanol, respectively. Free sugars found from both ginseng root and its products were fructose, glucose, sucrose and maltose, and the only sugar detected from red ginseng root and its products was rhamnose. Major sugar detected from fresh ginseng and white ginseng roots was sucrose, while sucrose and maltose were major sugars of red ginseng root.

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Antifungal and Insecticidal Activity of Essential Oil from Asarum sieboldii against Wood Contaminant Fungi and Lasioderma serricorne L. (세신 정유추출물의 목재부후균과 궐련벌레에 대한 항진균 및 살충활성)

  • Kang, Soyeong;Chung, Yong Jae;Lim, Jin A
    • Journal of Conservation Science
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    • v.28 no.4
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    • pp.395-401
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    • 2012
  • To investigate bioactive materials for development of natural conservative agent on organic cultural heritage, essential oil from Asarum sieboldii was screened for antifungal and insecticidal activity against 4 wood rotting fungi and adult of Lasioderma serricorne. Antifungal activity of essential oil was tested by using paper disc soaking method. Antifungal activity expressed as $IC_{50}$ value showed $1.50{\sim}2.84{\mu}l/disc$ range and the most significant antifungal activity was observed in Lentinus lepideus. The insecticidal activity of essential oil was examined by topical application method against L. serricorne adults. 50% and 100% of essential oil gave 98.3% and 100% mortality for 24 hours, respectively. The major components of the essential oil were methyl eugenol (56.32%), eucarvone (11.53%), safrole (5.79%), ${\delta}$-3-carene (2.09%), which were identified by gas chromatography-mass spectrometry. From these results, essential oil from A. sieboldii could be useful for conservation of organic cultural heritage against biological deterioration by insect and wood rotting fungi.

Simultaneous determinations of anthracycline antibiotics by high performance liquid chromatography coupled with radial-flow electrochemical cell (고성능 액체 크로마토그래피/방사흐름 전기화학전지를 이용한 안트라사이클린계 항생제의 동시 정량)

  • Cho, Yonghee;Hahn, Younghee
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.308-314
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    • 2007
  • The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.

Antioxidant Activities of Stachys sieboldii MIQ. Stalks (초석잠 [Stachys sieboldii MIQ.] 줄기의 항산화 활성)

  • 백홍석;나영수;류병호;송승구
    • KSBB Journal
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    • v.18 no.4
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    • pp.266-271
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    • 2003
  • This study was worked out to investigate the compounds of antioxidant constituents extracted from Stachys Sieboldii MiQ. and their effects on antioxidant activity by DPPH method, ferric thiocyanate method, and nitrite scavenging ability. Solvents such as methanol, hexane, chloroform, ethyl acetate, butanol, and water were used for this purpose. Total concentrations of polyphenols and flavonoids were measured in the methanol fraction. The ethyl acetate fraction showed the strongest activity by DPPH method, ferric thiocyanate method, and nitrite scavenging ability. The ethyl acetate extract was fractionated on a silica gel column using elution solvent (chloroform: methanol: water = 70 : 30 : 5 lower phase) at a flow rate of 1.0 mL/min. UV-VIS spectral data of each fraction showed adsorption maxima in the range of 284~330 nm. Among fractions, the fraction 1 that has λ$\_$max/ (nm) of 284 nm showed the strongest activity by DPPH method. The UV-VIS spectral data of phenolic compounds were known to lie in the range of 210~290 nm and 300~550 nm. Therefore, the results of our study suggested that Stachys sieboldii MIQ. contains phenolic compounds showing natural antioxidant activity.

A Study on the Natural Insectifuge for Food Wrapping Corrugated Board Using Tree Extractives (수목 추출성분을 이용한 식품포장용 골판지 천연 방충처리제 개발)

  • 배영수
    • Journal of Korea Foresty Energy
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    • v.20 no.2
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    • pp.9-19
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    • 2001
  • This study was carried out to investigate natural insectifuge materials from tree extractives in order to substitute for organic synthetic insecticides for food wrapping corrugated board. Tree samples were collected, extracted, fractionated with hexane, $CH_2Cl_2$, ethylacetate(EtOAc) and $H_2O$, and then freezed dried for further study. EtOAc or $H_2O$ fractions were chromatographed on a Sephadex LH-20 column for isolation and purification, and the isolated compounds were characterized by spectroscopic tools such as NMR and MS. Crude extractives of EtOAc and $H_2O$ fractions were added to the printing ink for corrugated board with the concentration of 2% or 3% based on the weight of the ink, then the prepared ink was printed on the corrugated board to be used for evasion test using larva of indian meal moth(Plodia interpunctella(Hubner)). Robtin, dihydrorobinetin and leucorobinetinidin were isolated from the wood extractives of black locust(Robinia pseudoacacia) and the bark of poplar(Populus alba $\times$ glandulosa) contained many kinds of compounds such as (+)-catechin, naringenin, aromadendrin, eriodictyol, sakuranetin and its glycoside, taxifolin, neosaturanin, salireposide, p-coumaric acid and aesculin. Much of (+)-catechin was isolated from the bark extractives of willow(Salix koreensis) in addition to (+)-gallocatechin and p-coumaric acid and the bark of weeping willow(Salix babylonica) also contained (+)-catechin, (+)-gallocatechin, dihydromyricetin and myricetin.

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Application as a Cosmeceutical Ingredient of Euryale ferox Seed Extract (가시연꽃 종자 추출물의 화장품 원료로서의 특성)

  • Choo, Soo-Jin;Kim, Young-Hee;Ryoo, In-Ja;Xu, Guang-Hua;Yoo, Ick-Dong
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.35 no.4
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    • pp.309-315
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    • 2009
  • In our search for the natural cosmetic ingredients, we found that Euryale ferox seed extract exhibited the strong antioxidative activity. Five active compounds were isolated from the ethyl acetate extract through various chromatographic methods and their structures were determined by NMR and MS spectral analysis. These compounds were identified as fucosterol (1), 3-(4-hydroxy-3-methoxybenzyl)-4-[(7'R),5'-dihydroxy-3'-methoxybenzyl]tetrahydrofuran (2), resorcinol (3), pyrogallol (4) and 4-O-methylgallic acid (5).We evaluated the antioxidative, antielastase activities and melanogenesis inhibitory effects of these compounds. The $SC_{50}$ values of compounds 2 ~ 5 for free radical scavenging activity were $17.0\;{\sim}\;100.2\;{\mu}M$ and especially compounds 4 and 5 were 6-fold more effective than ferulic acid as a positive control. And compounds 2 ~ 4 inhibited human neutrophil elastase with $IC_{50}$ values of $18.8\;{\sim}\;78.2\;{\mu}M$ and compound 3 also inhibited melanin synthesis in B16F10 melanoma cells with an $IC_{50}$ value of $492.8\;{\mu}M$. These results suggest that Euryale ferox extract having a lot of various active ingredients may be useful as a natural multi-functioning agent.

Isolation, Identification and Characterization of Paraquat Activity-Inhibiting Substances in Squash (Cucurbita moschata Duchesne ex Poiret) Leaves (호박잎에서 Paraquat 활성 억제 물질의 분리, 동정 및 특성 구명)

  • Hyun, Kyu-Hwan;Yun, Young-Beom;Jang, Se-Ji;Shin, Dong-Young;Kwon, Oh-Do;Choi, Hyun-Sug;Jung, Ha-Il;Kuk, Yong-In
    • Korean Journal of Weed Science
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    • v.32 no.3
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    • pp.211-221
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    • 2012
  • The fourth leaves (younger leaves) amongst extended 4-upper leaves in 18 squash cultivar were the highest tolerance to the paraquat application, followed by third, the second, and the first leaves (older leaves). The forth leaves in Joongangaehobak showed more than three times higher tolerance to the paraquat application than did the first leaves. When the combining of water extract from the fourth leaves with paraquat were applied to the leaves and stems of maize, the paraquat phytotoxicity in maize was reduced compared to the paraquat application alone. Therefore, this study continued to investigate if the phytotoxicity inhibitor exist in the fourth leaves. The water extract in the fourth leaves were isolated by silica gel column chromatography, Sephadex LH-20 column chromatography, TLC, and HPLC, and the substance in the extract was speculated as a malic acid by identifying through NMR. The mixture malic acid and paraquat were applied to the maize to verify the application effect of malic acid on paraquat toxicity. The 100 ${\mu}M$ of paraquat application alone showed 62% of paraquat toxicity to the corn leaves, while the combined application of 100 ${\mu}M$ paraquat with malic acid at 0.1, 0.3, 0.5, and 1.0% did not show the symptom.

Screening and Purification of an Anti-Prostate Cancer Compound, Deoxypodophyllotoxin, from Anthriscus sylvestris Hoffm (전호(Anthriscus sylvestris Hoffm)로부터 전립선 암세포 저해물질인 deoxypodophyllotoxin 의 탐색 및 분리)

  • Cho, Hyo-Jin;Yu, Sun-Nyoung;Kim, Kwang-Youn;Sohn, Jae-Hak;Oh, Hyun-Cheol;Ahn, Soon-Cheol
    • Journal of Life Science
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    • v.19 no.1
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    • pp.9-14
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    • 2009
  • The prostate cancer is the critical health problem, increasing of its related death in worldwide. Unfortunately present surgery and chemotherapeutic choices seem to be impossible in curing or controlling prostate cancer, because metastasis occasionally advances even after these potentially curative therapies. Therefore, there is immediate need to alternative chemoprevention and chemotherapeutic agents. Over one hundred species of dried medicinal herbs were tested for proliferation inhibitory effects on prostate cancer cell line, PC-3. One of them, Anthriscus sylvestris was selected because of potent anti-proliferation effect. The dried root of A. sylvestris was extracted with 100% methanol for 2-3 days and its extract was fractionated by using ethyl acetate. And ethyl acetate layer was subjected to column chromatographies on silica gel, reverse phase-18 (RP-18) and Sephadex LH-20, in turn. Finally, the pure compound was obtained by crystallization in methanol at $4^{\circ}C$ for overnight and identified as deoxypodophyllotoxin by NMR spedorscopic and physico-chemical analyses. In addition, it was confirmed that deoxypodophyllotoxin clearly inhibits the proliferation of PC-3 cells in a dose and time-dependent manner.