• 제목/요약/키워드: 용매 분해

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A Convenient Radiolabeling of [$^{11}$C](R)-PK11195 Using Loop Method in Automatic Synthesis Module ($^{11}$C 표지 자동합성장치에서 루프법을 이용한 ($^{11}$C)(R)-PK11195의 간편한 합성법)

  • Lee, Hak-Jeong;Jeong, Jae-Min;Lee, Yun-Sang;Kim, Hyung-Woo;Choi, Jae-Yeon;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul
    • Nuclear Medicine and Molecular Imaging
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    • v.43 no.4
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    • pp.337-343
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    • 2009
  • Purpose: ((R)-1-(2-chlorophenyl)-N-1-[$^{11}$C]methyl-N(1-propyl)-3-isoquinoline carboxamide ((R)-PK11195) is a specific ligand for the peripheral type benzodiazepine receptor and a marker of activated microglia, used to measure inflammation in neurologic disorders. We report here that a direct and simple radiosynthesis of [$^{11}$C](R)-PK11195 in mild condition using NaH suspension in DMF and one-step loop method. Materials and Methods: (R)-N-Desmethyl-PK11195 (1 mg) in DMSO (0.1 mL) and NaH suspension in DMF (0.1 mL) were injected into a semi-prep HPLC loop. [$^{11}$C]methyl iodide was passed through HPLC loop at room temperature. Purification was performed using semi-preparative HPLC. Aliquots eluted at 11.3 min were collected and analyzed by analytical HPLC and mass spectrometer. Results: The labeling efficiency of [$^{11}$C](R)-PK11195 was 71.8$\pm$8.5%. The specific activity was 11.8:$\pm$6.4 GBq/$\mu$mol and radiochemical purity was higher than 99.2%. The mass spectrum of the product eluted at 11.3 min showed m/z peaks at 353.1 (M+1), indicating the mass and structure of (R)-PK11195. Conclusion: By the one-step loop method with the [$^{11}$C]CH3l automated synthesis module, [$^{11}C$](R)-PK11195 could be easily prepared in high radiochemical yield using NaH suspension in DMF.

Monitoring of Forbidden Medicines as Adulterants in Dietary Supplements Marketed Online by HPLC and ESI-tandom Mass Spectrometry (HPLC 및 ESI-tandom Mass Spectrometry를 이용한 인터넷에서 판매되는 기능성표방식품 중 부정유해물질 모니터링)

  • Lee, Yong-Cheol;Kim, Bog-Soon;Yun, Eun-Sun;Kim, Sung-Dan;Chang, Min-Su;Park, Young-Ae;Shin, Young;Jung, Sun-Ok;Lee, Jae-In;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.2
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    • pp.148-154
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    • 2012
  • It was carried out to detect anti-impotence drug-like compounds, sibutramine and their analogues in dietary supplements, which are doubtful whether they include illegal compounds. A total of 51 food products were bought online and have been investigated. The separation was achieved on a C18 column, with the mobile phase made up of water (5 mM sodium hexanesulfonate and 0.1% phosphoric acid) and 95% acetonitrile, at a flow rate of 1.2 mL/min with gradient elution using by HPLC-DAD. The UV signals were monitored at 220 nm and 291 nm. LC-ESI-tandom MS was utilized to confirm that detected compounds in samples are the same as the reference materials. Two nutrient supplement foods and ginseng products were found to contain 1.3-82.1 mg of sildenafil, dimethylthiolsildenafil and pseudovardenafil per serving size. In addition, two other processed products were detected to contain 1.7 and 2.2 mg of didesmethylsibutramine, derived from sibutramine per serving size.

The Composition of the Root of Ixeris dentata var. albiflora Nakai. and Cell Viability and DPPH Radical Scavenging Activities of its Extract (흰씀바귀 (고채(苦菜), Ixeris dentata var. albiflora Nakai)뿌리의 성분 분석과 추출물의 세포 생존율 및 DPPH 라디칼 소거 활성)

  • Hong, Seul-Gi;Jeong, Dong-Myong;Kim, Ki-Young;Hwang, Eun-Hee
    • Journal of Nutrition and Health
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    • v.43 no.2
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    • pp.105-113
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    • 2010
  • Ixeris dentata var. albiflora Nakai, a herbal plant, is often used to make a strong stomach as an antiphlogistic used when dyspepsia and to improve appetite in Korea and China. And also it is used for adult diseases such as diabetes and liver diseases as Korean traditional medicine. In this study, the composition and DPPH radical scavenging activities of the root of Ixeris dentata var. albiflora Nakai and its effects on cell viability on vero and chang cells were investigated. Moisture, crude ash, crude protein and crude lipid were 79.14, 2.49, 8.28 and 2.56 g/100 g respectively. The highest mineral content was K. The major free sugars were glucose, fructose and sucrose. Major fatty acid are linoleic acid, palmic acid and linolenic acid. Major amino acids were glutamic acid, arginine and aspartic acid and the total contents of amino acids were 28.12 mg/g. The methanol extracts were further fractionated with n-hexane, chloroform, ethylacetate, butanol and water to get an active fraction. In addition, cell viabilities in each fraction were determined. Methanol extract, butanol, and aqueous fraction showed strong survival rates in vero cell and chang cell viability test, and hexane, chloroform, and ethylacetate fraction were examined for toxin in a cell. The root of Ixeris dentata var. albiflora Nakai had scavenging activities against DPPH radicals in a dose-dependent assay. Ethylacetate fraction's SC50 was $6.8\{\mu}g/mL$, very strong DPPH radical scavenging activities, but water fraction did not show any activity.

Amount and Chemical Characteristics of the Epicuticular Waxes on Leaves at Active Tillering and Heading Stages of Rice Varieties (벼 품종들의 분얼성기 및 출수기의 엽표면Wax의 양 및 화학적 조성)

  • Yong Woong, Kwon;Bong Jin, Chung
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.37 no.2
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    • pp.185-197
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    • 1992
  • Differences in the amount and chemical characteristics of the epicuticular waxes on rice leaves were studied for the active tillering and heading stages of rice varieties differing widely in gross leaf-surface property and genetics. The amount of waxes on surfaces of rice leaf-blades was determined by extraction with chloroform and chemical composition of the waxes was characterized by thin layer chromatography, gas liquid chromatography and infrared spectrophotometry. The amount of waxes varied by variety and significantly with growth stage. The amount at the heading stage was 1.7 to 3.6 mg/g fresh weight of leaves, which was two to three times as much as that at the tillering stage of 0.8 to 1.8 mg/g fresh weight. The waxes consisted of seven chemical classes, namely diols, fatty acids, fatty alcohols, fatty aldehydes, fatty esters, saturated and unsaturated hydrocarbons. Diols and unsaturated hydrocarbons were identified as new chemical classes of the rice epicuticular waxes. The polar constituents such as dials, fatty acids and fatty alcohols and the non-polars such as fatty aldehydes, fatty esters, and saturated and unsaturated hydrocarbons were identified at the heading stage, but at the tillering stage only the non-polar compounds were identified. In the carbon numbers (C) of the chemical classes, diols were composed entirely of C30 and acids were mainly of C30 and C31. In alcohols, primary alcohols were composed of C13 and C32, and the secondary alcohols were of C14, C16 and / or C30 regardless of the rice varieties. The acid portion of fatty esters, mainly composed of C22 and C23, showed low cabon numbers compared with the aldehydes. The alcohol portion of them showed a wide distribution in carbon numbers from C13 to C26 depending on the rice varieties. Hydrocarbons had odd carbon numbers, consisting mainly of C29 and C31.

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Characterization of Bacteriocin Produced from Isolated Strain of Bacillus sp. (Bacillus 속 분리주가 생산하는 박테리오신의 특성 조사)

  • Ham, Seung-Hee;Choi, Nack-Shick;Moon, Ja-Young;Baek, Sun-Hwa;Lee, Song-Min;Kang, Dae-Ook
    • Journal of Life Science
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    • v.27 no.2
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    • pp.202-210
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    • 2017
  • As an effort to find a potential biopreservative, we isolated bacterial strains producing bacteriocin from fermented foods. A strain was finally selected and characteristics of the bacteriocin were investigated. The selected strain was identified as Bacillus subtilis E9-1 based on the 16S rRNA gene analysis. The culture supernatant of B. subtilis E9-1 showed antimicrobial activity against Gram-positive bacteria. Subtilisin A, ${\alpha}$-chymotrypsin, trypsin and proteinase K inactivated the antimicrobial activity, which means its proteinaceous nature, a bacteriocin. The bacteriocin activity was fully retained at the pH range from 2.0 to 8.0 and stable at up to $100^{\circ}C$ for 60 min. Solvents such as ethanol, isopropanol and methanol had no effect on the antimicrobial activity at the concentration of 100% but acetone and acetonitrile reduced the activity at up to 100% concentration. Cell growth of four indicator strains was dramatically decreased in dose-dependent manner. Listeria monocytogenes was the most sensitive, but Enterococcus faecium was the most resistant. Bacillus cereus and Staphylococcus aureus showed the medium sensitivity. The bacteriocin showed its antimicrobial activity against B. cereus and L. monocytogenes via bactericidal action. The number of viable cells of L. monocytogenes started to reduce after addition of bacteriocin to the minced beef. The bacteriocin was purified through acetone concentration, gel filtration chromatography and RP-HPLC. The whole purification step led to a 6.82 fold increase in the specific activity and 6% yield of bacteriocin activity. The molecular weight of the purified bacteriocin was determined to be 3.3 kDa by MALDI-TOF/TOF mass spectrometry.

Evaluation of free radical scavenging and pancreatic lipase inhibitory effects of Aquilaria agallocha extracts (침향 추출물의 라디칼 및 췌장 지방분해 효소저해 활성 평가)

  • Lee, Ha Yeong;Lee, In-Chul;Kwak, Jae Hoon;Kim, Tae Hoon
    • Food Science and Preservation
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    • v.22 no.3
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    • pp.437-442
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    • 2015
  • In a continuing screening of selected medicinal plants native to South Korea, the antioxidant and pancreatic lipase inhibitory activities of an aqueous methanolic extract from the heartwood of Aquilaria agallocha were investigated. Eighty percent of the methanolic extract of A. agallocha was further divided into $CH_2Cl_2$, EtOAc and n-BuOH in order to yield four solvent-soluble portions, namely $CH_2Cl_2$-soluble, EtOAc-soluble, n-BuOH-soluble and $H_2O$ residue. The antioxidant properties were evaluated by employing radical scavenging assays using 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulphonic acid) ($ABTS^+$) radicals, while the anti-obesity efficacy of A. agallocha extracts and solvent-soluble portions were tested by porcine pancreatic lipase assay. All tested samples showed dose-dependent radical scavenging and pancreatic lipase inhibitory activities. Among the tested extracts and solvent-soluble portions, the $CH_2Cl_2$-soluble portion showed much higher radical scavenging activity and pancreatic lipase inhibitory properties when compared with other solvent-soluble portions. This result suggested that there was a significant relationship between the total phenolic content and biological efficacies, and A. agallocha extract might be considered as a new potential source of natural antioxidants and as a pancreatic lipase inhibitory source. A more systematic investigation of this biomass will be performed for further investigation of activity against antioxidative and anti-obesity effects.

Extraction Characteristics of Saponin and Acidic Polysaccharide Based on the Red Ginseng Particle Size (홍삼의 입자크기에 따른 사포닌 및 산성다당체의 추출 특성)

  • Cho, Chang-Won;Kim, Sang-Wook;Rho, Jeong-Hae;Rhee, Young-Kyung;Kim, Kyung-Tack
    • Journal of Ginseng Research
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    • v.32 no.3
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    • pp.179-186
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    • 2008
  • Effect of pulverization on total solid, crude saponin, and acidic polysaccharide contents of dried red ginseng main root were tested. Several particle size samples, including red ginseng main root (non pulverized), $10{\sim}40$ mesh powder, $40{\sim}100$ mesh powder, and >100 mesh powder were used in the extraction. The sequential solvent extraction method (1st: 70% EtOH at $70^{\circ}C$ for 12 hr, 2nd: 70% EtOH at $70^{\circ}C$ for 12 hr, 3rd: water at $70^{\circ}C$ for 12 hr) was applied to extract the saponins and acidic polysaccharide. Extraction yield of total solid of pulverized red ginseng ($10{\sim}40$ mesh size) was increased to 20% compared with that of non-pulverized. Especially, the crude saponin content of pulverized red ginseng ($10{\sim}40$ mesh size) showed an increase of 47% over non-pulverized. No difference in the component ratio was observed by pulverization, when the individual ginsenosides were quantified by HPLC. Also, extraction yield of acidic polysaccharide of pulverized red ginseng ($10{\sim}40$ mesh size) was increased 57% compared with that of non-pulverized. The results suggested that pulverization might be useful for increasing the extraction yield of red ginseng components.

Effect of Extracting Conditions on Chemical Compositions of Korean Mountain Ginseng Extract (추출조건이 장뇌삼추출물의 화학성분 조성에 미치는 영향)

  • Kim, Jun-Han;Kim, Jong-Kuk
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.6
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    • pp.862-868
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    • 2005
  • Korean mountain ginseng roots were freeze-dried at $-70^{\circ}C$ and extracted by different extracting solution conditions to investigate chemical compositions of extracts. The soluble solid content of the extract from $7.04\~13.45\%\;and\;50\%$ EtOH and MeOH extracts were higher than those of other extracts. $100\%\;water\;and\;90\%$ EtOH extracts gave the highest Brix with $19.98\%$\;and\;19.65\%$, respectively. pH of the extracts were ranged from $5.82\~6.60$. Browning color at 470 nm of the extract were high value in 50$\%$ EtOH extract. In case of Hunter's color value, L value of extract was higher in $100\%$ water extract (21.28) than EtOH extract $(17.18\~21.02)$, a and b values of extract were the highest in $100\%$ water (-0.12) and $90\%$ MeOH extract (1.34). The contents of free sugars in the EtOH extract were increased with the ethanol concentration. Sucrose contents of $90\%$ EtOH and MeOH extracts were 6,159 mg/100 g and 5,238 mg/100 g. Major organic acids of the extract were citric and malic acids. Major free amino acids of the extract were L-arginine, L-proline, $\gamma$ -amino-n-butyric acid, alanine and aspartic acid. The highest ginsenoside content was shown to be about $10.50\%\;in\;90\%$ MeOH extract. Major minerals of extract were P, K, Na, Mg and Ca.

Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

The Antioxidant Ability and Nitrite Scavenging Ability of Plant Extracts (식물체 추출물의 항산화성 및 아질산염 소거작용)

  • Kim, Soo-Min;Cho, Young-Suk;Sung, Sam-Kyung
    • Korean Journal of Food Science and Technology
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    • v.33 no.5
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    • pp.626-632
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    • 2001
  • The plant extracted from Nameko, Gallic, Green tea, Allspice, Polygonum multiflorum, Schizandra chinensis, Armeniacae and Pine needle were utilized to investigate the effects of extracts on free radical reaction, lipid oxidation and nitrite scavenging ability. The pH of ethanol extracts showed a higher than that of hot water extracts, among of which were showed the lowest pH 3.0 in Schizandra chinensis. The important factor of lipid oxidation were $Fe^{2+}$ ion and active oxygen, in which were bound by plant extracts in case of $Fe^{2+}$ ion existed. However, the hydroxyl radical scavenging ability of extracts were lowed, compared to extracts reacted with $Fe^{2+}$ ion. Among of them, the hydroxyl radical scavenging ability of Nameko and Pine needle extracts had a lower TBARS value than those of control. The iron content of extracts were less than 2.0 mg/100 g, but the total iron content of Schizandra chinensis extracts were 6.8 mg/100 g. The ethanol extracts of pine needle were higher than those of hot water extracts on the basis of $Fe^{2+}$ ion content. The ascorbic acid content of green tea showed 14.3 mg/100 g in hot water extracts and 16.7 mg/100 g in ethanol extracts. Electron donating ability of extracts showed more than 50%, except Nameko and allspices, which were higher in ethanol extracts than those of hot water extracts. The superoxide dismutase(SOD)-like activity of green tea showed 85.3% and 63.5% in hot water and ethanol extracts, respectively. The nitrite scavenging ability of green tea was the most effective in both extracts.

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