• Title/Summary/Keyword: 크로마토 그래피 추출

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Analysis and management of new hazard chemicals in foods (식품 중 신종유해물질의 관리 및 분석)

  • Choi, Dongmi;Hu, Soojung;Suh, Junghyuck;Yoon, Taehyung;Kim, Eunju;Choi, Jangduck;Park, Sung-Kug;Lee, Kwangho
    • Analytical Science and Technology
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    • v.22 no.2
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    • pp.172-185
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    • 2009
  • To help understanding about hazard chemicals occurring newly in food, it has been reviewed characteristics, mechanism, food standards and analytical trend of the hazard chemicals occurring avoidably in food manufacturing process. The new hazard chemicals in food are classified by 4 regarding mechanism such as heat, fermentation, additives and unknowns. The new hazard chemicals by heat process are acrylamide, furan, HCAs and PAHs. By the fermentation, ethylcarbamate and biogenic amines are occurred. According to food additives, 3-MCPD, benzene and nitrosamines can be produced. And the last group is the illegal compounds including anti-impotence drug analogues and anti-obesity drug analogues. To analyze the new hazard chemicals in food, GC or LC with UVD, FLD or MSD are used mainly after sample pretreatment by LLE, SPE or headspace method.

Purification of Complement System-Activating Polysaccharide from Hot Water Extract of Young Stems of Cinnamomum cassia Blume (계지(桂枝) 열수추출물로부터 보체계 활성화 다당의 정제)

  • Kweon, Mee-Hyang;An, Hyun-Jung;Shin, Kwang-Soon;Na, Gyeong-Su;Sung, Ha-Chin;Yang, Han-Chul
    • Korean Journal of Food Science and Technology
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    • v.29 no.1
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    • pp.1-8
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    • 1997
  • A complement system-activating (anti-complementary) polysaccharide was purified from the hot water extract of young stems of Cinnamomum cassia Blume. Crude polysaccharide fraction (CC-1) was prepared from the hot water extract of the young stems followed by methanol-reflux, precipitation with ethanol, dialysis, and lyophilization. The anti-complementary activity of CC-1 was decreased greatly by periodate oxidation, but was not changed by pronase digestion. These suggest that carbohydrate moiety may be related to the activation of complement system. According to its ionic strength CC-1 was fractionated first using cetavlon to give 4 fractions, CC-2, 3, 4 and 5. Among them CC-2 fraction was found to retain the highest activity and yield. CC-2 was separated to an unabsorbed neutral sugar portion (CC-2-I) and seven absorbed acidic sugar fractions $(CC-2-II{\rightarrow}CC-2-VIII)$ on DEAE-Toyopearl 650C (Cl-). CC-2-III showing higher anti-complementary activity and yield than those of other fractions, was further purified on the gel permeation of Sephadex G-100 and Sepharose CL-6B to CC-2-IIIa-3. CC-2-IIIa-3 was determined to have a homogeneity hy GPC (Sepharose CL-6B) and HPLC. Gel chromatography using standard dextrans gave a value of $2.4{\times}10^5$ for the molecular weight. The purified polysaccharide, CC-2-IIIa-3 consisted of arabinose, xylose, glucose, galactose, galacturonic acid and glucuronic acid in a molar ratio of 5.56 : 3.77 : 1.87 : 1.00 : 5.12 : 3.13 and contained no nitrogen.

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Biological Control of Fusarium Head Blight on Wheat by Polyacetylenes Derived from Cirsium japonicum Roots (대계근에서 분리한 Polyacetylene계 화합물을 이용한 밀 이삭마름병 방제)

  • Kim, Ji-In;Kim, Kihyun;Park, Ae Ran;Choi, Gyung Ja;Park, Hae Woong;Kim, In Seon;Kim, Jin-Cheol
    • Research in Plant Disease
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    • v.22 no.3
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    • pp.145-151
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    • 2016
  • Chemical fungicides have reduced Fusarium head blight (FHB) severity. However, by the effects of fungicide residues, they can only be used up to 30 days before time of harvest. Therefore, the development of new biofungicides that are applicable until harvest is required. In order to select plant extracts having antifungal activity against Fusarium graminearum for the control of FHB, we investigated the inhibitory effects of 225 medicinal plant extracts on spore germination of F. graminearum. Of these plant extracts, the methanol extract of Cirsium japonicum (CJ) roots showed the strongest antifungal activity. Through solvent partitioning, repeated column chromatography, and spore germination bioassay, two chemicals were purified and then their chemical structures were identified as ciryneol C (CC) and 1-heptadecene-11,13-diyne-8,9,10-triol (HD-ol) which are polyacetylene substances. Two active compounds effectively inhibited the germination of F. graminearum macroconidia; HD-ol ($IC_{50}$ of $3.17{\mu}g/ml$) showed stronger spore germination inhibitory activity than that of CC ($IC_{50}$ of $28.14{\mu}g/ml$). In addition, the wettable powder type formulation of ethyl acetate extract of CJ roots suppressed the development of FHB in dose-dependent manner, with control values of 78.92% and 31.56% at 250- and 500-fold dilutions, respectively. Combining these findings suggest that the crude extract of CJ roots containing polyacetylene compounds could be used as botanical fungicide for the control of FHB.

Identification of Antioxidant Compound Derived from Methanolic Extract of Houttuynia Cordata (어성초 메탄올 추출물로부터 항산화 효능을 가진 활성물질의 확인)

  • Kim, Hyeji;Hwang, Heesung;Park, Sumin;Kang, Sungwook;Kim, Hyejeong;Hong, Sugyeong;Kim, Moon-Moo;Oh, Yunghee
    • Journal of Life Science
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    • v.27 no.7
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    • pp.796-804
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    • 2017
  • This study was carried out to evaluate the antioxidant effect of methanolic extract of Houttuynia cordata (HCME) and to identify a compound having antioxidant effect. The ethyl acetate fraction of HCME showed the highest antioxidant effect in organic solvent fractions. The fraction was then separated into 12 fractions by open column chromatography. Among these fractions, the fraction 10 (Fr. 10) with the highest antioxidant activity was isolated, and its antioxidant effect was evaluated by DPPH radical scavenging activity, reducing power, TBARS, cell viability, DNA oxidation and DCF fluorescence. The Fr. 10 at a $64{\mu}g/ml$ showed 60% of inhibitory effect similar to that of vitamin C at $10{\mu}g/ml$, compared with blank group. The Fr. 10 at $64{\mu}g/ml$ showed 264% of reducing power, compared with blank group. TBARS assay showed that the Fr. 10 at $64{\mu}g/ml$ had 35.5% of inhibitory effect similar to that of vitamin E at $1,000{\mu}g/ml$, compared with blank group. The Fr. 10 above $32{\mu}g/ml$ displayed cytotoxicity. However, it was observed that the Fr. 10, above $1{\mu}g/ml$ reduced DNA damage. DCF fluorescence assay showed that the Fr. 10 inhibited oxidative stress by $H_2O_2$ in a dose dependent manner. The compound of Fr. 10 was identified to be rutin whose molecular weight is 610 by the IR and LC-MS analyses. Therefore, these results suggest that the rutin of Fr. 10 could use as a natural antioxidant for development of cosmetics and functional foods.

Metabolizing analysis according to the sawdust media of Pleurotus ostreatus (산겨릅나무와 옻나무 톱밥배지에서 재배한 느타리버섯의 함유성분 분석)

  • Shin, Yu-Su;Yang, Bo-Hyun;Kang, Bo-Yeon;Kim, Hyun-Soo;Lee, Ji-Hyun;Hong, Yoon-Pyo;Lee, Sang-Won;Lee, Chan-Jung;Kim, Seung-Yoo
    • Journal of Mushroom
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    • v.9 no.4
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    • pp.194-197
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    • 2011
  • The transitivity of Chemical constituents by Pleurotus ostreatus cultivated in different raw sawdusts, which are Acer tegmentosum MAX, Rhus verniciflura, was investigated. The HPLC chromatography patterns on the chemical constituents of P. ostreatus showed the similar chromatography patterns in the different raw sawdusts and control sawdust. The unknown chemical constituents of P. ostreatus cultivated in the mixed medium added 10 %, 20% raw sawdusts, respectively, were increased. But the significance results in the mixed medium added 50% raw sawdusts were not showed. The chromatography patterns of mycelia grown in media added the 80% MeOH extracts of A. tegmentosum and R. verniciflura showed the similar patterns in comparison with control mycelia. In the results, the secondary metabolites of functional media were not degrade and changed to other derivatives compounds by P. ostreatus.

Bioactivities and Isolation of Functional Compounds from Decay-Resistant Hardwood Species (고내후성 활엽수종의 추출성분을 이용한 신기능성 물질의 분리 및 생리활성)

  • 배영수;이상용;오덕환;최돈하;김영균
    • Journal of Korea Foresty Energy
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    • v.19 no.2
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    • pp.93-101
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    • 2000
  • Wood of Robinia pseudoacacia and bark of Populus alba$\times$P. glandulosa, Fraxinus rhynchophylla and Ulmus davidiana var. japonica were collected and extracted with acetone-water(7:3, v/v) in glass jar to examine whether its bioactive compounds exist. The concentrated extracts were fractionated with hexane, chloroform, ethylacetate and water, and then freeze-dried for column chromatography and bioactive tests. The isolated compounds were sakuranetin-5-O-$\beta$-D-glucopyranoside from Populus alba $\times$Pl glandulosa, 4--ethyoxy-(+)-leucorobinetinidin frm R. pseudoacacia and fraxetion from F. rhynchophylla and were characterized by $^1H$ and$^{13}C $ NMR and positive FAB-MS. Decay-resistant activity was expressed by weight loss ratio and hyphae growth inhibition in the wood dust agar medium inoculated wood rot fungi. R. pseudoacacia showed best anti-decaying property in both test and its methanol untreated samples, indicating higher activity than methanol treated samples in hyphae grwoth test. In antioxidative test, $\alpha$-tocopherol, one of natural antioxidants, and BHT, one of synthetic antioxidants, were used as references to cmpare with the antioxidant activities of the extacted fractions. Ethylacetate fraction of F. rhynchophylla bark indicated the hightest activity in this test and all fractions of R. pseudiacacia extractives also indicated higher activities compared with the other fractions. In the isolated compounds, aesculetin isolated from F. rhynchophylla bark showed best activity and followed by robonetinidin from R. pseudoacaica.

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Isolation and Characterization of Elastase Inhibitor from Areca catechu (빈랑으로부터 Elastase 저해물질의 분리 및 특성조사)

  • 조중제;이건국;조병기;최정도
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.26 no.1
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    • pp.163-186
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    • 2000
  • We have previously screened 150 medicinal plants on the inhibition of elastase and found a significant inhibitory effects of the extracts of Areca catechu L. on the aging and inflammation against the skin tissues. To isolate and identify the compounds having biological activity, we was further purified by each of the solvent fractions, silica gel column chromatography, preparative TLC and reversed-Phase HPLC. Peak in HPLC, which coincided with the inhibitory activity against elastase, was identified as Phenolic substance using various colorimetric methods, UV, and IR. $IC_{50}$/ values of phenolic substance purified from Areca catechu were 26.9 $\mu\textrm{g}$/$m\ell$ for porcine pancreatic elastase (PPE) and 60.8 $\mu\textrm{g}$/$m\ell$ for human neutrophil elastase (HNE). This Phenolic substance showed more potent activity than those of reference compounds, oleanolic acid (76.5 $\mu\textrm{g}$/$m\ell$ for PPE, 219.2 $\mu\textrm{g}$/$m\ell$ for HNE) and ursolic acid (31.0 $\mu\textrm{g}$/$m\ell$ for PPE, 118.6 $\mu\textrm{g}$/$m\ell$ for HNE). According to the Lineweaver-Burk Plots, the inhibition against both PPE and HNE by this phenolic substance was competitive with substrate. Phenolic substance from Areca catechu exhibited high free radical scavenging effect ($SC_{50}$/ : 6 $\mu\textrm{g}$/$m\ell$) and inhibited effectively hyaluronidase activity ($IC_{50}$/: 210 $\mu\textrm{g}$/$m\ell$). These results suggest that the Phenolic substance Purified from Areca catechu showed anti-aging effect by protecting connective tissue proteins.

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β-Galactosidase-catalyzed Synthesis of 1, 2-Hexanediol Galactoside and its Purification using Ethyl Acetate Extraction followed by Silica Gel Chromatography (대장균 β-Galactosidse를 이용한 1, 2-Hexanediol galactoside의 합성과 Ethyl Acetate 추출 및 Silica Gel Chromatography를이용한 정제)

  • Kim, Yi-Ok;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.3
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    • pp.498-506
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    • 2016
  • 1, 2-Hexanediol galactoside (HD-gal) has been previously synthesized from 1, 2-hexanediol (HD), in which recombinant ${\beta}$-galactosidase (${\beta}$-gal) of Escherichia coli (E. coli) was used for transgalactosylation reaction. In this study, a method for HD-gal purification from the reaction mixture was particularly investigated. Using ${\beta}$-gal-containing E. coli, HD-gal was synthesized from 75 mM HD for 48 hr under 300 g/l lactose concentration. Then, HD-gal synthesis from HD was confirmed by TLC analysis, and the existence of E. coli ${\beta}$-gal during 48 hr-reaction was also confirmed by Western blotting, in which the conversion yield of HD to HD-gal reached about 94% during 48 hr. To establish an efficient method for HD-gal purification, we carried out the solvent extraction of the reaction mixture, followed by silica gel chromatography, particularly in order to remove the residual HD. Two water-immiscible solvents, such as methylene chloride and ethyl acetate, were investigated comparatively to find out appropriate solvent. Then, it was found that residual HD was almost removed when ethyl acetate extraction of water phase of reaction mixture was carried out four times. Subsequently, silica gel chromatography was carried out, and purified HD-gal could be finally obtained. The production yield for HD-gal from 75 mM HD was $8.9{\pm}0.6%$ (n=3) (mole basis) or $21.1{\pm}1.4%$ (n=3) (weight basis). For further study, using purified HD-gal, we will investigate the minimum inhibitory concentrations (MICs) of HD-gal against bacteria. In addition, cytotoxicity to human skin cells of HD-gal will be examined.

A Study on the Pollution of Polycyclic Aromatic Hydrocarbons (PAHs) In the Column Sediments around Gwangyang Bay (광양만 주변해역 주상퇴적물에서의 다환방향족탄화수소류(PAHs)의 오염에 관한 연구)

  • You, Young-Seck;Cho, Chon-Rae;Cho, Hyeon-Seo
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.14 no.4
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    • pp.257-266
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    • 2008
  • PAHs are of mainly anthropogenic origin from urban runoff, oil spill and combustion of fossil fuels. Some PAHs are potentially carcinogenic and mutagenic to aquatic organisms. This study was carried out to survey the contamination of PAHs in the column sediments around Gwangyang bay. Yeosu petrochemical industrial complex, POSCO(Pohang steel compony) and Gwangyang container harbor are located near the bay. The column sediments were collected at 4 stations(A, B, C and D) and fractionated at intervals of two-centimeter depth on July 29, 1999. PAHs in colmn sediment samples were extracted in soxhlet extractor and were identified and quantified by GC-MS. PAHs compounds were analyzed and found to be 13 species. Total PAHs concentrations in the column sediments ranged from 275.04 to 2,838.64${\mu}g/kg$ dry wt. Naphthalene had the highest concentration in the range of 40.60 to 2,294.06${\mu}g/kg$ dry wt. and Anthracene had the lowest concentration in the range of 2.63 to 11.30${\mu}g/kg$ dry wt. The correlation coefficients between individual PAHs and total PAHs in the column sediments were relatively higher in the low molecular compounds such as Naphthalene, Acenaphthylene and Phenanthrene. The relationship between the P/A(Phenanthrene/Anthracene)ratio and F/P(Fluoranthene/Pyrene)ratio showed that P/A ratio was generally above 10 and F/P ratio was above 1 in all sediment samples. These data indicate that PAHs in the column sediments around Gwangyang bay seem to be of both pyrolytic and petrogenic origin The values of PAHs in the column sediments were lower than the biological effect guidelines.

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Determination of cyromazine residues in agricultural commodities using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Cyromazine의 잔류분석법)

  • Song, Lee-Seul;Kim, Young-Hak;Lee, Su-Jin;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jung-Ah;Oh, Jae-Ho;Im, Moo-Hyeog;Chang, Woo-Suk;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.202-208
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    • 2012
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.