• Title/Summary/Keyword: determination of molecular weight

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Complex Formation of Uranium(VI) with Organic Phosphate Ligands in the Solvent Extraction System (용매 추출계에서의 우라늄(VI)-유기인산에스테르 착물의 형성에 관한 연구)

  • Do Young Kyu;Sohn Youn Soo
    • Journal of the Korean Chemical Society
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    • v.22 no.5
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    • pp.320-325
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    • 1978
  • In order to elucidate the mechanism associated with the solvent extraction of uranium(VI) using DEPA and DPPA as extractant the uranium(VI) complexes formed during the solvent extraction were isolated and characterized by means of IR, NMR, chemical analysis and molecular weight determination. It has been found that uranium(VI) replaces the acidic hydrogen ions of the extractants DEPA and DPPA to form chelated polynuclear complexes, the molecular weight of U(VI)-DEPA complex being $2.1{\times}10^4$. The isolated U(VI)-DEPA complex has been found to be the same chemical species as is formed during the solvent extraction process. In case of DEPA the distribution coefficient of uranium is the largest of the pure aqueous uranium solution and is increasing for the acidic solutions in the order of $H_3PO_4.

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Isolation, Structure Determination and Biological Activity of 25-Epi, $3{\alpha}-Carboxyacetylquercinic$ Acid in Daedalea dickinsii (띠미로버섯 중 25-Epi, $3{\alpha}-Carboxyacetylquercinic$ Acid의 분리정제, 구조결정 및 생리활성)

  • Bae, Kang-Gyu;Min, Tae-Jin
    • Journal of the Korean Chemical Society
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    • v.44 no.1
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    • pp.37-44
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    • 2000
  • In order to develope bioactive substances, dried fmit body of Daedalea dickinsii collected from Taeback mountain was extracted with ethanol, The compounds 1 and 2 were purified by solvent extraction, silica gel column chromatography and recrystallization from the ethanol extracts. Melting point, molecular weight and molar extinction coefficient of the compound 1 were estimated to be $167{\sim}168^{\circ}C$, 572 and 5,040 at 208 nm. The structure of this compound 1 has been elucidated to be 24S, 25S, $3{\alpha}-carboxyacetylquercinic$ acid using spectroscopic properties. This compound showed antibiotic activities against fungi, yeasts and bacteria and it also showed anticancer activity $IC_{50}=64.5\;{\mu}M$) against Korean stomach cancer cell. Melting point, molecular weight and molar extinction coefficient of the compound 2 were estimated to be $233{\sim}235^<\circ}$, 572 and 5,080 at 208 nm. The structure of this compound was elucidated to be 24S, 25R, $3{\alpha}-carboxyacetylquercinic$ acid. The compound 2 showed different antibiotic activities with the compound 1.

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Structure Determination of Antifungal KRF-001 Produced by Bacillus subtilis subsp. krictiensis (Bacillus subtilis subsp. krictiensis가 생산하는 항진균 물질 KRF-001의 구조 결정)

  • 김성기;이남경;정태숙;김영국;최진자;복성해
    • Microbiology and Biotechnology Letters
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    • v.19 no.6
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    • pp.598-603
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    • 1991
  • An antifungal mixture of six members (component A to F), KRF-001 produced by Bacillzts subtilis subsp. krictiensis was isolated from the fermentation broth. Molecular weight of component A to F was determined by FAB-MS to be 1042, 1056, 1056, 1070, 1070 and 1084 respectively. Various instrumental analyses (amino acid analysis, GC-MS, $^1H-NMR, ^1HH$ COSY NMR) revealed that the mixture was a homologous cyclic peptide composed of each one mole of glutamine, proline, tyrosine, serine, unusual $\beta$-amino acid and three moles of asparagine. The structural differences of component A to F were found in carbon number and terminal structure of the unusual $\beta$-amino acid. After determination of the sequence and stereochemistry of those amino acids, the tentative structure of KRF-001 was determined.

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Quality Properties of Enteric-Coated Soft Capsule Using PEG as a Plasticizer (PEG를 가소제로 사용한 장용성 연질캡슐의 코팅 품질 특성)

  • Yang, Joo Hwan;Han, Joon Taek;Oh, In Ho;Park, Geum Duck
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.2
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    • pp.260-267
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    • 2015
  • We investigated the applicability of polyethylene glycol (PEG) as a plasticizer in enteric-coated soft capsules based on determination of quality characteristics according to molecular weight and concentration of enteric-coating PEG solution. There was no difference according to molecular weight of PEG, whereas a low PEG concentration in the enteric-coating solution was associated with higher whiteness index and slower disintegration time in pH 6.8 media. Brittleness was observed in the coating film at seam areas in 5% PEG enteric-coating solution after 2 weeks of storage at room temperature. The enteric-coating properties of PEG were compared with those of acetylated monoglyceride (AMG) and triacetin, which are enteric-coating plasticizers. Enteric-coated soft capsule containing PEG as a plasticizer showed a lower whiteness index and faster dissolution profile than AMG and triacetin. Moreover, enteric-coated soft capsule containing AMG and triacetin as plasticizers showed coating film brittleness at seam areas after 2 months of accelerated storage [$40^{\circ}C$, relative humidity (RH) 75%] but no difference at room temperature storage ($25^{\circ}C$, RH 60%). The present study suggests that concentration of PEG is important to determine enteric-coating quality, regardless of the molecular weight of PEG. In conclusion, PEG has potential as a plasticizer due to its transparency and storage stability in enteric-coated soft capsules.

Chemical Structures and Physiological Activities of Plant Growth Substance, Malformin A's (식물생장조절물질 말포민 A동족체의 화학구조 및 생리활성)

  • Kim, K.W.
    • Korean Journal of Weed Science
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    • v.15 no.1
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    • pp.73-84
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    • 1995
  • Four malformin A's produced by Aspergillus niger van Tiegh. were separated by HPLC equipped with $C_{18}$ reversed-phase column and subjected to structural determination. Amino acid analyses and mass spectra data of the compounds indicate that they structurally resemble the cyclic pentapeptide malformin $A_1$. Their structures were deduced by two dimensional NMR and MS/MS experiments as cyclo-D-Cys-D-Cys-L-Val-D-Leu-L-Ile for $A_1$, cyclo-D-Cys-D-Cys-L-Val-D-Leu-L-Val for $A_2$, cyclo-D-Cys-D-Cys-L-Val-D-Leu-L-Leu for $A_3$, and cyclo-D-Cys-D-Cys-L-Val-D-Ile-L-Val for $A_4$. Among the mal-formin A's, the structure of $A_3$ was identical to that of malformin C, which was produced by A. niger strain AN-1. All the malformin A's caused severe curvatures of corn(Zea mays L.) roots and the activities of the malformin A's with molecular weight 529 were greater than those with molecular weight 515. Malformin $A_1$ caused the corn root curvature by 83% at a concentration of $0.25{\mu}M$. In the mung bean(Phaseolus aureus Roxb.) hypercotyl segment test, however, the molecular weight of malformin A's was not a factor influencing the physiological activities. Malformin $A_1$ stimulated the growth of mung bean hypercotyles by 165% at a $0.1{\mu}M$ concentration.

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Structural determination of triterpenic acids in Prunellae Spica by fast atom bombardment tandem mass spectrometry (하고초의 생리활성 성분 Triterpenic Acids의 FAB-MS를 이용한 구조 규명)

  • Ahn, Young Min;Lee, Kang Ro;Hong, Jongki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.245-258
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    • 2008
  • Five triterpenic acids as marker compounds were extracted and isolated from Prunellae Spica by column chromatography and reversed-phase high-performance liquid chromatography (HPLC), and their purity was determinated by HPLC (purity ${\geq}90%$). Molecular weight and elemental compositions of the five marker compounds were determined by fast atom bombardment high-resolution mass spectrometry (FAB-HRMS). The structural determination of the five marker compounds was carried out fast atom bombardment collision-induced dissociation tandem mass spectrometry (FAB-CID-MS/MS). The collision-induced dissociation (CID) of protonated molecules $[M+H]^+$ and deprotonated molecules $[M-H]^-$ produced diverse product ions due mainly to retro Diels-Alder reaction (RDA), dehydration and decarboxylation. Moreover, the CID-MS/MS spectra of the $[M-H]^-$ ions were observed charge-remote fragmentation (CRF) patterns. On the basis of interpretation of CID-MS/MS spectra, structural elucidation of triterpenic acids isolated from Prunellae Spica was clearly performed.

A New Analytical Method for Fluoroquinolones in Fisheries Products by High Performance Liquid Chromatography (HPLC를 이용한 어패류 중의 fluoroquinolone계 항균제의 분석법)

  • Jo Mi-Ra;Kim Poong-Ho;Lee Hee-Jung;Lee Tae-Seek
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.2
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    • pp.59-65
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    • 2006
  • Fluoroquinolones are the most common group of antibacterial agents currently used in the Korean aquaculture industry, and use of these agents has been increasing steadily. High performance liquid chromatography (HPLC) with fluorescence detection was used for the simultaneous determination of five fluoroquinolones in fish and shellfish: ofloxacin (OFL), pefloxacin (PEF), norfloxacin (NOR), ciprofloxacin (CIP), and enrofloxacin (ENRO). Fish and shellfish muscle was homogenized, and protein, lipid, and low molecular weight pigments were then excluded from the homogenate. The final eluates were analyzed by HPLC equipped with a Shiseido UG-120 type C18 reverse-phase column ($4.6{\times}250 mm$, $5{\mu}m$) and a fluorescence detector (excitation at 280 nm, emission at 450 nm). The mobile phase was 0.1 M phosphoric acid and acetonitrile solution (91:9, v/v) and tetrahydrofuran (THF) was added to it at a rate of 5 mL per a liter of the mobile phase. Adequate chromatography separation was obtained using the above method. Average recoveries of fortified samples at levels from 0.05 to 0.5 mg/kg were $72.3{\pm}2.5-84.5{\pm}1.2%$ for OFL, $82.7{\pm}3.3- 109.3{\pm}7.5%$ for NOR, $85.3{\pm}6.6-116.0{\pm}7.9%$ for PEF, $76.0{\pm}4.3-109.3{\pm}12.4%$ for CIP, and $78.7{\pm}5.9-100.0{\pm}9.8%$ for ENRO. The limit of detection of OFL was $5{\mu}g/L$, the others were $1{\mu}g/L$. We concluded that the new analytical method was suitable for the determination of fluoroquinolones in fish and shellfish.

Prediction of Precipitated Wax Amounts Using FTIR Spectroscopy (FTIR을 이용한 왁스 침전의 정량적 예측)

  • Oh, Kyeongseok
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.376-381
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    • 2013
  • High molecular weight paraffinic waxes dissolved in oil phases can be precipitated when the surrounding temperature becomes lower than the wax appearance temperature (WAT). While the various methods of WAT determination have been developed, the determination of precipitated wax amount has not been comparably popular at temperatures below the WAT. It is important to predict how much solid wax content precipitates in temperature variance. The study develops the previous method which uses integrated areas determined at a wavenumber range of 735~715 $cm^{-1}$. This method uses two different wavenumber ranges, 735~715 $cm^{-1}$ and 1,402~1,324 $cm^{-1}$. The study shows how the method provides reliable data in the variety of applications regardless of FTIR spectral instability often occurred, such as volume reduction during cooling procedure and existence of emulsified water in oil phase.

Effects of Salt and Heparin on the Activation of Lipoprotein Lipase(LPL)

  • Kim, Tae-Woong;Lee, Jae-Bok;Son, Heung-Soo;Kim, Sung-Wan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.24 no.3
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    • pp.355-361
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    • 1995
  • Lipoprotein lipase(LPL) is an acylglycerol hydrolase and is the extrahepatic enzyme responsible for the hydrolysis of triglyceride-rich plasma lipoproteins. LPL has been isolated from bovine milk by affinity chromatography on heparin-sepharose in 2M NaCl, 5mM barbital buffer, pH 7.4. Para-nitrophenyl butyrate(PNPB) was used as a substrate for the determination of LPL activity. Molecular weight of LPL was 55KD on 10% SDS-PAGE. When the effects of heparin on LPL activation were compared, LPL activity of heparin added group increased approximately 5 times higher than that of heparin non-added groups. These results indicated that heparin involved in the stabilization of LPL structure that led to increase enzyme activity. Furthermore, LPL activity increased about 4 times compared to the absence of heparin at various pH. LPL was stabilized when heparin was added either low or high salt concentrations. With the presence of heparin, NaCl concentration did not affect LPL activity at pH range 6∼9.

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Protein Separation in Functional Rice Grains Using Two-Dimensional Gel Electrophoresis

  • Chung, Soo Im;Lee, Sang Chul;Kan, Mi Young
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.58 no.4
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    • pp.388-392
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    • 2013
  • The proteins from functional rice cultivars (Nogwonchalbyeo, Giant embryonic, Arhyangchalbyeo, and Goamibyeo) and general white rice were extracted and separated using two-dimensional (2D) gel electrophoresis. A wide variation in the molecular weight (MW) and pH range of the expressed proteins in rice samples were observed. The green-kerneled rice (Nogwonchalbyeo) exhibited proteins with MW of 9-57 kDa and appeared at a pH range of 4-7. The Giant embryonic contained proteins with MW of 31-63 kDa and a pH range of 5-6. The aromatic glutinous rice (Arhyangchalbyeo) showed proteins with MW of 24-28 and pH of 5.8-6.8. The high-amylose rice (Goamibyeo) exhibited proteins with MW of 3-63 and pH of 5.2-5.6. The identified proteins uniquely found and highly expressed in each cultivar may have a significant role on rice functionality. The results illustrate that the 2D gel electrophoresis is a valuable method in the determination of the protein expression profiles in functional rice grains and may be useful in the identification of specific marker proteins associated with the functional property of rice.