• Title/Summary/Keyword: 잔류용매

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Facile [11C]PIB Synthesis Using an On-cartridge Methylation and Purification Showed Higher Specific Activity than Conventional Method Using Loop and High Performance Liquid Chromatography Purification (Loop와 HPLC Purification 방법보다 더 높은 비방사능을 보여주는 카트리지 Methylation과 Purification을 이용한 손쉬운 [ 11C]PIB 합성)

  • Lee, Yong-Seok;Cho, Yong-Hyun;Lee, Hong-Jae;Lee, Yun-Sang;Jeong, Jae Min
    • The Korean Journal of Nuclear Medicine Technology
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    • v.22 no.2
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    • pp.67-73
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    • 2018
  • $[^{11}C]PIB$ synthesis has been performed by a loop-methylation and HPLC purification in our lab. However, this method is time-consuming and requires complicated systems. Thus, we developed an on-cartridge method which simplified the synthetic procedure and reduced time greatly by removing HPLC purification step. We compared 6 different cartridges and evaluated the $[^{11}C]PIB$ production yields and specific activities. $[^{11}C]MeOTf$ was synthesized by using TRACERlab FXC Pro and was transferred into the cartridge by blowing with helium gas for 3 min. To remove byproducts and impurities, cartridges were washed out by 20 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ solution (pH 5.1) and 10 mL of distilled water. And then, $[^{11}C]PIB$ was eluted by 5 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ into the collecting vial containing 10 mL saline. Among the 6 cartridges, only tC18 environmental cartridge could remove impurities and byproducts from $[^{11}C]PIB$ completely and showed higher specific activity than traditional HPLC purification method. This method took only 8 ~ 9 min from methylation to formulation. For the tC18 environmental cartridge and conventional HPLC loop methods, the radiochemical yields were $12.3{\pm}2.2%$ and $13.9{\pm}4.4%$, respectively, and the molar activities were $420.6{\pm}20.4GBq/{\mu}mol$ (n=3) and $78.7{\pm}39.7GBq/{\mu}mol$ (n=41), respectively. We successfully developed a facile on-cartridge methylation method for $[^{11}C]PIB$ synthesis which enabled the procedure more simple and rapid, and showed higher molar radio-activity than HPLC purification method.

Studies on the Organo-mercury Residues in Rice Grain -I. Mercury residues in rice seeds treated with organo-mercury fungicide- (수도(水稻)에 처리(處理)된 유기수은제(有機水銀劑)의 잔류성(殘留性)에 관(關)한 연구(硏究) -제1보(第1報) 침지용유기수은제(浸漬用有機水銀劑)로 처리(處理)된 수도종자중(水稻種子中)의 수은잔류량(水銀殘留量)에 관(關)하여-)

  • Lee, Dong-Suk
    • Applied Biological Chemistry
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    • v.8
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    • pp.87-93
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    • 1967
  • 1) For the micro-analysis of mercury in plant materials, the method of Furutani was shown to be the simplest and most efficient way and the recovery of the assay was about 98%. 2) When the rice grain was soaked in 1/1000 diluted solution of organo-mercury fungicide for 8 hours at the end of March, the amounts of mercury residues in the brown rice and unhulled rice were 8.8 to $9.5\;{\mu}g/g$ seeds and 10.1 to $10.7\;{\mu}g/g$ seeds, respectively. 3) By washing the treated rice seeds with running water for three days, tile residual mercury concentration was reduced to 1/4 to 1/5; thus the mercury residues were 1.86 to $1.92\;{\mu}g/g$ for brown rice and 1.96 to $2.93\;{\mu}g/g$ for unhulled rice. 4) The residual mercury was present more in the unhulled rice than in the brown rice, either before or after washing of the treated seeds. 5) Among the different rice varieties, no difference was observed in mercury residues by seed treatment and washing.

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Anti-coagulation and Anti-platelet Aggregation Activities of Black Ginger (Kaempferia parviflora) (흑생강(Kaempferia parviflora)의 항응고 및 혈소판 응집저해 활성)

  • Lee, Man-Hyo;Sung, Hwa-Jung;Kwon, Chong Suk;Sohn, Ho-Yong
    • Journal of Life Science
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    • v.28 no.9
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    • pp.1068-1075
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    • 2018
  • Kaempferia parviflora, an herbaceous plant in the family Zingiberaceae, is popular in many tropical regions. It is called as black ginger or krachaidum in Thailand and Laos, and its raw or dried root have been used as spices and teas. The rhizomes also have been traditionally used to treat gastrointestinal disorders, ulcers, gout, dysentery, allergies and to improve physical work capacity. Recently, its anti-obesity, anti-oxidant, anti-inflammatory and blood clot-lysis activities were reported. In this study, the anti-thrombosis activity of black ginger was investigated, since improvement in blood fluidity leads to the prevention of various lifestyle-related diseases. The hot water and ethanol extract and their subsequent solvent fractions (hexane, ethylacetate, butanol fractions and water residue) were prepared, and their anti-coagulation and platelet aggregation inhibitory activities were determined, respectively. Among the black ginger extracts and their fractions, the ethylacetate fraction (EAF) of ethanol extract only showed significant extensions of blood coagulation time determined by thrombin time (TT), prothrombin time (PT), and activated partial thromboplastin time (aPTT). At 5 mg/ml concentration, TT, PT and aPTT were extended to 1.22, 1.49 and >15-folds compared to non-treatment. The EAFs of ethanol and hot water extract showed strong inhibitions against collagen-induced platelet aggregations, which are comparable to inhibitions of aspirin. Also the EAFs from black ginger did not show any hemolysis activity against human RBC up to 0.5 mg/ml. Our results suggest that the EAF of black ginger has a potential as novel anti-coagulation and ant-platelet aggregation agent. This report provides the first evidence of anti-coagulation activity of black ginger.

Antifungal Activity of Zanthoxylium schinifolium Against Fusarium graminearum, a Barley Powdery Mildew Fungus. (보리 흰가루병 곰팡이 Fusarium graminearum에 대한 산초 추출물의 항진균 활성)

  • Kim, Byum-Soo;Jang, Han-Su;Choi, Chung-Sig;Kim, Jong-Sik;Kwon, Gi-Seok;Kwun, In-Sook;Son, Kun-Ho;Sohn, Ho-Yong
    • Journal of Life Science
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    • v.18 no.7
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    • pp.974-979
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    • 2008
  • The powdery mildew, a fungal plant disease found in varieties of plant cultures, is occurred by attack with Fusarium sp., Sphaerotheca sp., Leveilluna sp., and Eryshipe sp.. In this study we investigated the control of Fusarium graminearum, a barley powdery mildew fungus, by natural plant extracts. Among the 900 plant extracts tested, Zanthoxylum schinifolium, Ligusticum acutilobum, Bidens frondosa L., Dictamnus dasycarpus, Evodia officinalis, Disporum sessile, Scopolia japonica Max., Styrax japonica S. et Z., Dictamnus dasycarpus Turcz., Sinomenium acutum Rehder et Wils., Eugenia aromaticum, Rubus parvifolius L., Reynoutria elliptica, Coptis chinensis, Paeonia lactiflora Pall., Rheum undalatum, Paeonia suffruticosa, Oenothera odorata Jacq., Euphorbia pekinensis Rupr., and Nepeta cataria were selected based on spore germination inhibition assay. Further mycelial growth inhibition assay with economical and safety considerations led us to finally select Z. schinifolium (sancho) for control of F. graminearum. To produce antifungal sancho extract, methanol was suitable for extraction and subsequent fractionations of the extract showed that the water residue mainly had antifungal activity. The sancho extract and its fractions showed minor antibacterial activity against different pathogenic or food spoilage bacteria, but they did not show any harmful effects against young tomato plant by treatment of $1,000\;{\mu}g/ml$ in green chamber test. These results suggested that the extract of sancho has high potentials on control of a powdery mildew fungus, F. graminearum.

Kinetics and Mechanism of Hydrolysis of Insecticidal Imidacloprid (살충성 Imidacloprid의 가수분해 반응 메카니즘)

  • Yu, Sung-Jae;Kang, Moon-Sung;Sung, Nack-Doo
    • Applied Biological Chemistry
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    • v.40 no.1
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    • pp.53-57
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    • 1997
  • The rate of hydrolysis of insecticidal 1-(6-chloro-3-pyridylmethyl) -2-nitro-iminoimidazolidine (common name; imidacloprid) have been investigated in 15%(v/v) aqueous dioxane at $45^{\circ}C$. From the kinetics and non-kinetics data such as pH-effect, solvent effect(m=0.04, n=0.30 IT m<${\Delta}H^{\neq}=16.14kcal{\cdot}mol^{-1}\;&\;{\Delta}S^{\neq}=-0.03e.u.$), rate equation ($k_{obs.}=4.56{\times}10^{-3}[OH^-]$) and analysis of hydrolysis product, 1-(6-chloro-3-pyridylmethyl-2)-imidazolidinon, the hydrolysis mechanism of imidacloprid is proposed that the specific base catalyzed hydrolysis($K_{OH^-}$) through nucleophilic addition-elimination ($Ad_N-E$) mechanism proceed via intermediate, 1-(6-chloro-3- pyridylmethyl)-2-hydroxy-2-imidazolidinylisonitraminate (I) and ${\beta}$-3-(6-chloro-3-pyridylmethyl)aminoethyl-1-nitrourea(III). And the half-life(t1/2) of hydrolytic degradation at pH 8.0 and $45^{\circ}C$ was about 4.5 months.

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Separatipon of Oryzanol from the Refining By-Product of Rice Bran Oil (미강유 정제 부산물로부터 오리자놀 분리)

  • Kim, In-Hwan;Kim, Chul-Jin
    • Korean Journal of Food Science and Technology
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    • v.23 no.1
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    • pp.76-80
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    • 1991
  • To isolate oryzanol from the by-product of rice bran oil refinning, experiment of solvent fractional crystallization was carried out at various conditions with the dark oil obtained by acidifying the soap stock of micella refinning process and the pitch obtained from vacuum distillation of the dark oil. The impurity interfering the crystallization process such as waxes can be removed as precipitates by cooling the 1:1 mixtrue of acetone and dark oil to $0^{\circ}C$, From the dewaxed dark oil, oryzanol concentrate with 51.3% purity was obtained by fractional crystallization at$0^{\circ}C$ with the mixture of 8 part volume of hexane and 1 part of the dewaxed dark oil. The concentrate was recrystallized at room temperature with 20 part volume of methanol to yield oryzanol crystal of 98.3% purity. The optimum condition of vacuum distillation was temperature of $180^{\circ}C\;at\;0.2{\sim}0.4\;torr$ with 2% steam sparging. At this condition, the free fatty acid in the dark oil was removed as distillate without thermal deomposition to yield 82.3% of oryzanol as the pitch of 27.3% purity. After concentration from the pitch with 20 part volume of hexane to yield yellow powder of 75.4% purity, the yellow powder was recrystallized in methanol at room temperature to obtain the crystal containing 99.0% oryzanol. The overall oryzanol yield from the dark oil and the pitch was 9.5 and 28.5%, respectively. The change of the composition of sterols and triterpenoid alcohols in the compounds isolated during fractionation was analyzed by GC-MS.

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Evaluation of the Antimicrobial Activities of 35 Seaweed Extracts against Pathogenic Bacteria and Candida sp. (35종 해조류 추출물의 병원성 세균 및 Candida sp. 진균에 대한 항균 활성 평가)

  • Kim, Mi-Sun;Kwon, Kyung-Jin;Lee, Min-Jin;Ahn, Seon-Mi;Sohn, Ho-Yong
    • Microbiology and Biotechnology Letters
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    • v.40 no.2
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    • pp.144-151
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    • 2012
  • In the course of this study aimed at the development of functional food ingredients from seaweeds, the in vitro antimicrobial activities of methanol extracts prepared from 35 different seaweeds (17 phaeophyta, 11 rhodophyta and 7 chlorophyta) were determined against food-borne diseases and pathogenic microorganisms including multi-drug resistant (MDR) Pseudomonas sp. and Candida sp. Based on disc-diffusion assays at 500 g/disc concentration of the methanol extracts, Ishige okamurai, I. foliacea, Sargassum confusum, and S. yamade exhibited strong antibacterial activities in a broad-spectrum, except against Pseudomonas aeruginosa. In addition to the latter four seaweeds, Ecklonia stolonifera, E. cava and Eisenia bicyclis also demonstrated antifungal activity against C. albicans. Among these 8 selected seaweeds, I. okamurai, I. foliacea, and S. yamade exhibited strong hemolytic activity (55-93%) at 500 g/ml against human RBC. Organic solvent sequential fractions using hexane, ethylacetate and butanol, and water residues were prepared from the 8 selected seaweeds and their anti-Candida sp. activities were further determined. The ethylacetate and butanol fraction of I. okamurai, and the hexane fraction of I. foliacea demonstrated antifungal activity against MDR-pathogenic Candida sp. Although the solvent fractions had no activity against MDR-Pseudomonas sp., our results suggest that seaweeds, especially Ishige okamurai, I. foliacea, S. confusum, and S. yamade could be developed as broad-spectrum antimicrobial ingredients.

The Extraction Characteristics of Metal-contaminated Soil by Soil Washing (토양세척기법을 이용한 중금속 오염토양 처리에서 중금속 추출특성)

  • Hwang, Seon-Suk;Lee, Noh-Sup;NamKoong, Wan
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.10
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    • pp.1072-1080
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    • 2005
  • The extraction characteristics of heavy metals(HM) from a contaminated soil at existing lead smelters were investigated with ethylene diamine tetraacetic acid(EDTA), citrate and HCl as washing solutions. EDTA was more effective for Pb than for other heavy metals. As the mol ratio of EDTA/HM increased, the removal efficiency of heavy metals became higher. When the mol ratio of EDTA/HM approached to 6.5, it removed Pb most effectively. Citrate was effective especially in extracting Zn. The removal efficiency of HCl was comparatively high in almost all heavy metals, and at 0.3N concentration it was the highest. After soil washing process by the use of EDTA, the great part of exchangeable fractions and most of heavy metals of weakly adsorbed like carbonate fraction were extracted. For washing with citrate and HCl, four heavy metals showed the similar exchange of chemical partitioning and the exchangeable fractions of Pb which has weakly adsorbed to soil were more increased than before the process. As removal efficiency of citrate washing process depends upon the distribution of non-detrital fractions, so it can be contended that only the amount of non-detrital fractions could be removed from all the heavy metal content. EDTA and HCl could remove most of non-residual fractions in all heavy metals except Zn. As a result of EDTA washing, toxicity characteristic leaching procedure(TCLP) concentration of the processed soil met the USEPA Pb limit of 5.0 mg/L.

Evaluation of Antimicrobial, Antithrombin, and Antioxidant Activity of Fritillaria thunbergii Miquel (패모(Fritillaria thunbergii Miquel)의 항균,항혈전 및 항산화 활성 평가)

  • Shin, Yong-Kyu;Jang, Han-Su;Kim, Jee-In;Sohn, Ho-Yong
    • Journal of Life Science
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    • v.19 no.9
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    • pp.1245-1250
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    • 2009
  • Beimu (Fritillaria thunbergii Miquel), a bulbous plant of Liliaceae found in Korea, Japan and China, has been used as an antitussive and expectorant agent, and is also useful in alleviating stonsillitis and bronchiolitis. Most researches have been focused on micro-propagation and plant regeneration, component analysis, and dormancy relieving of beimu. Reports regarding the biological activity of beimu, such as anti-Helicobacter pyroli or platelet aggregation inhibition activity, are few and not widely available. In this study, methanol extract and its organic solvent fractions were prepared from Fritillaria thunbergii Miquel and their antimicrobial, antithrombin, and antioxidant activities were evaluated, respectively. The methanol extract contained lots of water-soluble materials (58.98%) and hexane-soluble oils (14.85%). The ethylacetate and butanol fraction at $500{\mu}g$/disc concentration showed strong antibacterial activity against tested bacteria, except Escherichia coli. Antifungal activity was not observed in methanol extract and its fractions. The hexane, ethylacetate and butanol fractions showed strong antithrombin activity at 4.8 mg/ml concentration. Especially, the ethylacetate fraction showed 95.4 sec of thrombin time at a concentration of 1.2 mg/ml, which is comparable to aspirin, a widely used antithrombosis agent. For antioxidation activity, the ethylacetate and butanol fraction showed good 1,1-diphenyl-2-picryl hydrazyl scavenging activity ($IC_{50}$ of $344{\sim}368{\mu}g$/ml). In superoxide dismutase-like activity and reducing power, the fractions showed $20{\sim}25%$ of vitamin C, and $51{\sim}54%$ of butyl hydroxytoluene, respectively.

Recovery of Paraffin Components from Pyrolysis Oil Fraction of Waste Plastic by Batch Cocurrent 4 Stages Equilibrium Extraction (회분 병류 4단 평형추출에 의한 폐플라스틱 열분해유 유분 중의 파라핀 성분의 회수)

  • Kang, Ho-Cheol;Shin, Sung Soon;Kim, Doo Han;Kim, Su Jin
    • Applied Chemistry for Engineering
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    • v.29 no.5
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    • pp.630-634
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    • 2018
  • The recovery of paraffin components contained in the fraction as a part of improving the quality for the fraction of waste plastics pyrolysis oil (WPPO) was investigated by batch cocurrent 4 stages equilibrium extraction. The fraction at a distilling temperature of $120-350^{\circ}C$ recovered from WPPO by the simple distillation and a little water-added dimethylformamide (DMF) solution were used as a raw material and solvent, respectively. As the number of equilibrium extraction (n) and the carbon number of paraffin component increased, the concentration of paraffin component contained in the raffinate increased. The concentrations of $C_{12}$, $C_{14}$, $C16$ and $C_{18}$ paraffin components present in the raffinate recovered at n = 4 were about 1.2, 1.5, 1.6 and 1.8 times higher than those of using the raw materials, respectively. Recovery rates (residue rates present in raffinate) of paraffin components rapidly decreased with increasing n, and increased sharply with increasing the carbon number. Furthermore, it was possible to predict the recovery rates at n = 1 - 4 for all paraffin components ($C_7-C_{24}$) contained in the raw material. The raffinate recovered through this study is expected to be used as a renewable energy.