• Title/Summary/Keyword: 80% acetone

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Isolation of Alliin in Garlic and Its Quantitative Determination by High Performance Liquid Chromatography and Studies on the Antimicrobial Efforts of Alliin and Ethanol Extracts from Korean Garlic(Alliium sativum L.) (마늘 중 고속 액체 크로마토그래피에 의한 알린의 분리 및 정량과 Alliin과 에탄올 추출물의 항균효과에 관한 연구)

  • 위성언
    • The Korean Journal of Food And Nutrition
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    • v.16 no.4
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    • pp.296-302
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    • 2003
  • First. the purification and analysis of alliin in garlic from different origins by alliin-HPLC determination method were studied. Allinase in garlic was inactivated by heating in boiling water followed by extraction of alliin in garlic with 80% methanol. To remove free amino acids and alliin homologs in garlic, garlic extract was separated by cation exchange column which was packed with amberlite CG-120 resin using 40L d-water as eluent. Alliin in garlic extract was crystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=70:29:1 and then recrystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=75:24:1. Obtained alliin was identified by melting point. TLC, microscope observation and mass spectrometry. High performance liquid chromatography (HPLC) following pre-column derivatization of cystein derivatives with o-phthaldialdehyde/2-mercaptoethanol has succeessfully been applied to the analysis of various garlics. Each alliic of standard solution and garlic extract was derivatized to isoindole derivative by o-phthaldialdehyde /2-mercaptoethanol and then analyzed by HPLC. Six point calibration was done by using alliin peak area. Lineality was observed at 0 ∼ 1.0mg/ml of alliin concentration. Weighted regression line function was Y=6254X - 256077. By this function, alliin contents in various garlics were 0.34 ∼ 0.73% fresh weight. Second study was designed to evaluate the effects of garlic extracts of various concentrations on the growth of various pathogenes (Eubacterium limonsum, Bacteroides fragilis, Salmonella typhimurium, Salmonella typhi, Shigella sonnei, Kiebsiella pneumoniae, Enterobacter cloacae, Pserdomonas aeruginosa, Escherichia coli). For antimicrobial effects against microorganism, totally minimal inhibition concentrations (MIC) of alliin were from 5,000 to 20,000ppm. MIC of ethanol extract were 1,250 to 10,000ppm.

Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

Analysis and Decrease of Cyanogenic Glucosides in Flaxseed (아마인에 함유된 시안배당체의 분석과 저감화)

  • Park, Eun-Ryong;Hong, Jin-Hwan;Lee, Dong-Ha;Han, Sang-Bae;Lee, Kang-Bong;Park, Jae-Seok;Chung, Hyung-Wook;Hong, Kyung-Hyun;Kim, Myung-Chul
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.6
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    • pp.875-879
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    • 2005
  • Linustatin and neolinustatin in flaxseed are called cyanogenic glucosides which produce acetone, hydrogen cyanide (HCN) and sugar when hydrolyzed. The HCN is the chemical whose toxin is being issued in food safety. Linustatin and neolinustatin were found in flaxseed by 206.5 and 174.2 mg/100 g, respectively using a RI-HPLC and LC/MSn analysis of $80\%$ methanol extraction. Also, HCN (137.38 mg/kg) was found in flaxseed distillate by autohydrolysis and IC analysis. More than 85$\%$ of linustatin, neolinustatin and HCN were removed when flaxseed was heated for more than 2 hours in $200^{\circ}C$. Especially, HCN was decreased to $98\%$ by heating only 30 min in $200^{\circ}C$.

Study on Anti-oxidant Effect of Extracts from Pyrus ussuriensis Leaves (산돌배나무(Pyrus ussuriensis) 잎 추출물의 항산화활성에 관한 연구)

  • Lee, Chang-Eon;Kim, Young-Hun;Lee, Byung-Guen;Lee, Do-Hyung
    • Journal of Korean Society of Forest Science
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    • v.99 no.4
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    • pp.546-552
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    • 2010
  • The aim of the study was to assess the cosmeceutical activity of Pyrus ussuriensis leaves and it is possible that can be used as a cosmetic ingredient for application of cosmetic industries. P. ussurensis leaf was extracted with various solvents including water, 70% ethanol and 60% acetone. In the result of DPPH (1,1-diphenyl-2-picryl-hydrazyl) scavenging radical activity, water, ethanol and acetone extract of P. ussuriensis leaf were higher than 70%, 80% and 85% at 50 ppm concentration, respectively. Xanthine oxidase inhibition activity and superoxide dismutase (SOD)-like activity by P. ussuriensis extract were higher than 30%. In addition, SODlike activity of all extracts showed tendency of the significant increase with the increase of concentration. In the anti-inflammatory test, P. ussuriensis leaf extract inhibited generation of nitric oxide (NO) stimulated by LPS in the macrophage cell line (raw 264.7) after 12 to 24 hours. As above results, P. ussuriensis has a great potential as a cosmeceutical raw material as well as anti-oxidant and anti-inflammatory ability.

Development and Interlaboratory Validation of an Analytical Method for the Determination of Saflufenacil in Agricultural Products by HPLC-UVD and LC-MS

  • Do, Jung-Ah;Park, Hyejin;Kwon, Ji-Eun;Oh, Jae-Ho;Cho, Yoon-Jae;Chang, Moon-Ik;Choi, Won-Jo;Lee, Hyun-Sook;Hong, Jin-Hwan
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.285-291
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    • 2014
  • Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

Effects of Extraction Condition on Extraction Efficiency of Rubiadin in Adventitious Roots of Noni (Morinda citrifolia) (추출조건이 노니 부정근에 함유된 rubiadin의 추출 효율에 미치는 영향)

  • Kim, Myong-Ki;Jeong, Cheol-Seung;Shin, Yong-Kook;Park, Kyong-Hee;Lee, Woon-Jang;Lee, Eun-Jung;Paek, Kee-Yoeup
    • Horticultural Science & Technology
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    • v.28 no.4
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    • pp.685-690
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    • 2010
  • Rubiadin, a major compound of noni ($Morinda$ $citrifolia$) adventitious root, is highly valued in pharmaceutical industry due to hepatoprotective activity. To dissect rubiadin's effective extraction condition, extraction process of noni adventitious roots was performed with different solvent types, ratio of water to methanol (water, 20, 40, 60, 80, and 100% of methanol), extraction time, and extraction method. In contrast, we also developed a reverse- phase HPLC assay method to determine rubiadin from noni adventitious roots. The HPLC assay of rubiadin was performed by C-18 column using a gradient solvent system of methanol and water with UV detector at 280 nm. The extraction efficiency of different types of solvents were increased in order of methanol (0.08%) > ethanol (0.05%) > acetonitrile (0.03%) > acetone (0.02%) and methylene chloride (0.02%). The results of rubiadin extraction using different solvents showed that 1 hour of ultrasonic extraction was effective in order of 60% methanol (0.21%) > 80% methanol (0.13%) > 100% methanol (0.07%), 40% methanol (0.07%) and 2 hours of reflux extraction was effective in order of 60% methanol (0.21%) > 40% methanol (0.17%) > 80% methanol (0.14%). To compare the extraction efficiency of rubiadin according to the extraction methods and time for high rubiadin content, the extracts of rubiadin in noni adventitious roots were isolated with the methods of ultrasonic extraction, shaking extraction and reflux extraction. Rubiadin extracted from the methods of ultrasonic waves and shaking displayed the highest contents at 8 and 24 hours, respectively.

Behaviour of the Soil Residues of the Acaricide-Insecticide, [$^{14}C$]Acrinathrin;I. Behaviour during Crop(Maize) Cultivation (살비살충제 [$^{14}C$Acrinathrin 토양 잔류물의 행적 규명;I. 농작물(옥수수) 재배시의 행적)

  • Lee, Jae-Koo;Kyung, Kee-Sung;Kwon, Jeong-Wook;Ahn, Ki-Chang;Jung, In-Sang
    • Korean Journal of Environmental Agriculture
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    • v.14 no.2
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    • pp.186-201
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    • 1995
  • In order to elucidate the fate of the residues of the pyrethroid acaricide-insecticide, acrinathrin in soil, maize plants were grown for one month on the specially-made pots filled with two different types of soils containing fresh and one-month-aged residues of [$^{14}C$]acrinathrin, respectively. The mineralization of [$^{14}C$]acrinathrin to $^{14}CO_2$ during the one-month period of aging and of maize cultivation amounted to $23{\sim}24%$ and $24{\sim}33%$, respectively, of the original $^{14}C$ activities. At harvest after one-month growing, the shoots and roots contained less than 0.1% and 1% of the originally applied $^{14}C$ activity, respectively, whereas the $^{14}C$ activity remaining in soil was $65{\sim}80%$ in both soils. Three degradation products with m/z 198(3-phenoxybenzaldehyde), m/z 214(3-phenoxybenzoic acid), and m/z 228(methyl 3-phenoxybenzoate) besides an unknown were identified from acetone extracts of both soils without and with maize plants after treatment of [$^{14}C$]acrinathrin, by autoradiography and GC-MS, and those with m/z 225(3-phenoxybenzaldehyde cyanohydrin) and m/z 198 (3-phenoxybenzaldehyde) from acetone extract of the Soil A treated with 50 ppm acrinathrin and grown with maize plants for 30 days were identified by mass spectrometry. These results suggested that the hydrolytic cleavage of the ester linkage adjacent to the $^{14}C$ with a cyano group, forming 3-phenoxybenzaldehyde cyanohydrin. The removal of hydrogen cyanide therefrom leads to the formation of 3-phenoxybenzaldehyde as one of the major products. The subsequent oxidation of the aldehyde to 3-phenoxybenzoic acid, followed by decarboxylation would evolve $^{14}CO_2$. Solvent extractability of the soils where maize plants were grown for 1 month and/or [$^{14}C$]acrinathrin was aged for 1 month was less than 31% of the original $^{14}C$ activity and over 95% of the total $^{14}C$ activity in soil extracts was distributed in the organic phase. Accordingly, acrinathrin turned out to be degraded rapidly in both soils and be bound to soil constituents as well, not being available to crops.

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Studies on Penicillinase Produced by a Streptomyces sp. (Part 2) Enzymatic Characteristics of the Penicillinase Produced by Streptomyces sp. YS-40. (Streptonyces sp. 가 생산하는 Penicillinase에 관한 연구 (제2보) Strepteptomyces sp. YS-40이 생산하는 Penicillinase의 효소학적 성질)

  • 도재호;김상달
    • Microbiology and Biotechnology Letters
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    • v.10 no.3
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    • pp.185-190
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    • 1982
  • A strain of Streptomyces sp. (YS-40) which was able to produce penicillinase, was isolated from soil and the enzymatic characteristics of this enzyme were investigated. The crude enzyme was obtained with the fractionation by 80 % cold acetone. The optimal temperature and pH of this enzyme was 45$^{\circ}C$ and 5.0 respectively. The stable pH range of the enzyme was between pH 5.5 and 8.0 at 37$^{\circ}C$. By heat treatment at 6$0^{\circ}C$ and 8$0^{\circ}C$ for 10 min, the remained relative activities were about 50%, 30% respectively. The activity of the enzyme was inhibited by Cu$^{++}$, $_Mn^{++}$, Zn$^{++}$ but Co$^{++}$, Li$^{++}$, $Ca^{++}$, $Mg^{++}$ $Ba^{++}$ did not affect. Among 11 chemical reagents, ethylenedi aminetetra-acetic acid disodium salt (EDTA-2Na), sodium dodecyl sulfate (SDS) and sodium fluoride inhibited the enzyme activity.

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Whitening and Anti-wrinkling Effects of Fractions from Prunus persica Flos (도화(Prunus persica Flos) 분획물의 미백 및 주름개선 효과)

  • Lee, Jin-Young;An, Bong-Jeun
    • Microbiology and Biotechnology Letters
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    • v.40 no.4
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    • pp.364-370
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    • 2012
  • In this study, the compounds of Prunus persica Flos were extracted with 70.0% acetone and were purified using a sephadex-LH-20 column chromatography. As a result, eight fractions were isolated. For whitening effects, the tyrosinase inhibitory activity was determined to be 92.2% in Fr.-8 isolated from P. persica Flos at 1.000 ppm. The melanoma cell-originated tyrosinase inhibitory effect of Fr.-8 from P. persica Flos was approximately 63.4% at 100 ppm. The inhibitory activity on melanin synthesis by Fr.-8 isolated from P. persica Flos was about 71.7% at 100 ppm concentration. For anti-wrinkling effects, the elastase inhibition activities by Fr.-5, 7 isolated from P. persica Flos were around 71.4 and 74.5% respectively at 1,000 ppm. The collagenase inhibition activity and collagen synthesis by Fr.-8 isolated from P. persica Flos was about 80.0% at 100 ppm. All these findings suggested that the fractions of P. persica Flos have great potential as cosmeceutical ingredients with whitening and anti-wrinkling effects.

Characterization of Humic Acid in the Chemical Oxidation Technology(II) - Characteristics by Ozonation - (화학적 산화법에 의한 부식산의 분해처리 기술에 관한 연구(II) - 오존처리에 따른 분해특성 분석 -)

  • Rhee, Dong Seok;Jung, Young-Rim
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.241-249
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    • 2000
  • In this paper, ozonation of humic acid in water was characterized using $UV_{254}$ absorbance, TOC, Ultra Filtration and $^{13}C-NMR$. Also, carbonyl compounds in ozonated water were analyzed by GC/MS using PFBOA method. Ozonation by-products of water containing humic acid were determined as formaldehyde, acetaldehyde, acetone, glyoxal and methylglyoxal. Results of $UV_{254}$ absorbance and TOC with ozonation time at humic acid 20, 100ppm represent that decrease rate of 80% within ozonation time is 20 min and TOC removal rate of 40-50% within ozonation time is 30 min. Results for $^{13}C-NMR$ and Ultra Filtration, humic acid of high molecular weight by ozonation are oxidated and decomposed so that it was conversed low molecular weight such as aldehydes, carboxylic acid.

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