• Title/Summary/Keyword: EI/MS

Search Result 118, Processing Time 0.032 seconds

Synthesis of DMDBTDMA and determination of radiolysis products by GC/MS (DMDBTDMA의 합성 및 방사선 분해산물의 GC/MS 분석)

  • Yang, Han-Beom;Lee, Eil-Hee;Park, Gyo-Beom
    • Analytical Science and Technology
    • /
    • v.21 no.5
    • /
    • pp.403-411
    • /
    • 2008
  • Dimethyldibutyltetradecylmalonamide (DMDBTDMA) extractant was used in a solvent extraction process for a radioactive liquid waste treatment. For the study of radiolysis phenomena, DMDBTDMA was synthesized and the degradation compounds (n-methylbutylamine, tetradecane, 1-tetradecanol) in the DMDBTDMA extractant, irradiated with $^{60}Co$ gamma ray, were identified and determined as radiolysis products by a Fourier transform infrared (FT-IR), gas chromatograph/mass spectrometer (GC/MS) analysis and GC/MS with selected ion monitoring (SIM) mode. Retention behavior of n-methylbutylamine, n-dodecane, tetradecane and 1-tetradecanol in the total ion chromatogram with the standard materials and n-dodecane as the internal standard (ISTD) were 2.35 min., 8.83 min., 10.68 min. and 12.75 min., respectively. In the case of tetradecane, there was a linear relationship between the concentration of the tetradecane and the absorbed dose of the ${\gamma}$-ray irradiated DMDBTDMA.

A Study on the Chemical Constituents from Marine Sponge Luffariella sp. (해면 Luffariella sp.의 화학적 성분 연구)

  • Park, Sun Ku;Kim, Sung Soo;Park, Jun Dae;Hong, Jung Sun;Kim, In Kyu
    • Journal of the Korean Chemical Society
    • /
    • v.39 no.7
    • /
    • pp.559-563
    • /
    • 1995
  • The three metabolites, Germacrene alcohol(1), Aaptamine(2) and Hexacyclic terpene(3) were isolated from Marine Sponge Luffariella sp., collected in October 1992, Manado Bay, Sulawesi in Indonesia showed in vitro activity against KB cancer cell line, and structure assignment for 1 was corrected by comparison of their spectral data with the literature $values^1$. Their structure were elucidated by $^1H$, $^13C$ NMR, $^1H$ $^13C$(1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy$(HMQC)^2$, $^1H$ $^13C$(2 and 3 bond) Heteronuclear Multiple Bond Correlation Spectroscopy$(HMBC)^3$, Electron Impact Mass Spectroscopy(EI ms), Ultra-violet Spectroscopy(UV) and Infrared Spectroscopy(IR).

  • PDF

Study on Cadalene Compounds Purified from Zelkova serrata Wood I - Purification of 7-hydroxy-3-methoxycadalene and Its Distribution in Xylem - (느티나무에서 단리한 카달렌 화합물에 관한 연구 I -7-hydroxy-3-methoxycadalene 단리 및 목부 내 분포 -)

  • Choi, Joon-Weon;Mun, Sung-Hee;Choi, Don-Ha
    • Journal of the Korean Wood Science and Technology
    • /
    • v.36 no.6
    • /
    • pp.130-137
    • /
    • 2008
  • In this study cadalene, which is classified into sesquiterpenes constructed with 15 carbons of naphthalene skeleton, was isolated from ethanol extracts of Zelkova wood (Zelkova serrata) using successive silica gel column chromatography. The purified cadalene compound was subjected to structural analysis using HPLC, EI-MS and $^1H$, $^{13}C-NMR$. Its molecular weight was measured to 244 (m/z) and methyl and isopropyl group were attached at C1 and C4 position, as well as hydroxyl group at C7 and methoxyl group at C3 in the naphthalene skeleton, respectively. Yield of 7-hydroxy-3-methoxycadalene amounts to 0.03% based on air dried Zelkova wood powder. It was distributed only in xylem tissues(only in heartwood) of Zelkova wood, not in leaves and bark.

Production, isolation and characterization of the antibiotic from Pseudomonas aeruginosa 3120 (Pseudomonas aeruginosa 3120으로부터 항생물질의 생산,분리 및 특성)

  • Ko, Hack-Ryong;Chun, Hyo-Kon;Kho, Yung-Hee;Sung, Nack-Kie
    • Applied Biological Chemistry
    • /
    • v.36 no.6
    • /
    • pp.428-433
    • /
    • 1993
  • A strain that inhibited the growth of Pellicularia sasakii was isolated from the soil and identified as Pseudomonas aeruginosa 3120. A dark brownish antibiotic, MRL3120 isolated and purified from the culture broth of P. aeruginosa 3120 was soluble in ethylacetate, chloroform and methanol, and it was active against gram-positive and negative bacteria as well as fungi. The structure of MRL3120 was identified as a chelate compound consisting of two N-methyl-N-thioformyl-hydroxylamine and a copper ion by the analysis of UV, IR, and EI-MS spectra and other physico-chemical properties and supposed to have a structure of fluopsin C related compound. Addition of $CuSO_4$ into the fermentation medium containing soybean meal increased antifungal activity but no activity was found in the presence of EDTA (0.1%, v/v). However antibiotic MRL3120 was not produced in the fermentation medium containing soytone instead of soybean meal but it was rapidly produced by the addition of $CuSO_4$.

  • PDF

Biological Activity of Phenol Compound from a Cactus Cheonnyuncho (Opuntia humifusa) in Korea (천년초선인장으로부터 분리한 페놀성 화합물의 생리활성 효과)

  • Lee, Kyung-Seok;Lee, Ki-Young
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.39 no.8
    • /
    • pp.1132-1136
    • /
    • 2010
  • After Cheonnyuncho (Opuntia humifusa) was extracted by 70% ethanol and partitioned with hexane, chloroform, ethyl acetate, butanol, and water in order, ethyl acetate fraction with excellent antioxidant activities was acquired. Ethyl acetate fraction was conducted by TLC, and the third spot of 10 spots was selected due to its best antioxidant activities. When the third fraction further isolated on silica gel chromatography, the fourth fraction of 10 fractions had the best antioxidant activities and purified by HPLC. The molecular weight on EI-MS, and $^1H$- and $^{13}C$-NMR spectrum showed that the purified compound was taxifolin. In addition, antioxidant activities were analyzed, and the purified compound from Cheonnyuncho was found to be effective as much as $\alpha$-tocopherol, BHA. According to the analysis on antibacterial activities, the purified compound also showed more activity than benzoic acid against all pathogenic bacteria.

Isolation and Identification of Antifungal Compounds from Eugenia caryophyllata Extracts (정향 추출물로부터 항진균성 물질의 분리 및 동정)

  • Lee, Jin-Man;Hur, Sang-Sun
    • Journal of the Korean Applied Science and Technology
    • /
    • v.31 no.4
    • /
    • pp.740-747
    • /
    • 2014
  • Antifungal properties of clove(Eugenia caryophyllata) against food spoilage microorganism, Penicillium rugullosum IFO 4683 was investigated. Antifungal activity of the essential oil was as equivalent as potassium metabisulfite and myconazole. The clove extracts was fractionated to hexane, chloroform, ethyl acetate, butanol and water fraction. Hexane fraction showed the highest inhibitory effect on the Penicillium rugullosum IFO 4683. Hexane fraction was further fractionated by silica gel column chromatography and thin layer chromatography(TLC). The antifungal compound was isolated from their fractions and their chemical structures were identified as eugenol, eugenol acetate and chavicol by EI-MS, $^1H$-NMR and $^{13}C$-NMR.

Isolation and Identification of Quercetin with Antioxidative Activity from the Fruits of Rubus coreanum Miquel (복분자 열매에서 항산화활성을 지닌 quercetin의 분리 및 동정)

  • Yoon, In;Wee, Ji-Hyang;Moon, Jae-Hak;Ahn, Tae-Hoe;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
    • /
    • v.35 no.3
    • /
    • pp.499-502
    • /
    • 2003
  • The methanol (MeOH) extracts from the fruits of Rubus coreanum showed antioxidative activity. The antioxidative substance in MeOH extracts was successively purified with solvent fractionation, adsorption chromatography, and gel filtration. The purified active substance was isolated by HPLC and identified as quercetin by EI-MS, and $^1H-NMR$ analyses. The amount of quercetin was 0.25 mg per 100 g in fresh fruits of Rubus coreanum Miquel.

Extractives from the needles of Juniperus rigida Siebold et Zucearin and Antioxidant activity (노간주나무(Juniperus rigida Siebold et Zucearini) 잎의 추출성분 및 항산화 활성)

  • Lee, Sang-Keug;Kim, Jin-Kyu;Ham, Yeon-Ho;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
    • /
    • v.32 no.1
    • /
    • pp.59-66
    • /
    • 2004
  • The dried neeldes(1.5 kg) of Juniperus rigida were ground, extracted with acetone-H2O(7:3, v/v), concentrated, and fractionated with a series of hexane, CH2Cl2, EtOAc and water on a separatory funnel. Each fraction was freeze dried to give dark-brown powder and EtOAc and water soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluent. Spectrometric analysis such as NMR and FAB or EI-MS including TLC were performed to characterize the structures of the isolated compounds. The needles of Juniperus rigida contained a large amount of (+)-catechin, quercetin-3-O-α-L-rhamnopyranoside and isoconiferin, in addition to a small amount of umbelliferone and quercetin-3-O-β-D-rutinoside. The antioxidative activities of each fraction and isolated compounds were tested by DPPH radical scavenging method, and EtOAc soluble fraction, (+)-catechin and quercetin-3-O-α-L-rhamnopyranoside were effective.

Synthesis of Ultra High Refractive Index Monomer for Plastic Optical Lens and Its Ophthalmic Lens Preparation (플라스틱 안경렌즈용 초고굴절 모노머 합성 및 이를 이용한 안경렌즈 제조)

  • Jang, Dong Gyu;Kim, Jong Hyo;Lee, Soo Min;Roh, Soo Gyun
    • Journal of Korean Ophthalmic Optics Society
    • /
    • v.13 no.3
    • /
    • pp.1-6
    • /
    • 2008
  • Purpose: Plastic optical monomer materials having ultra high refractive index have an income of the whole quantity from advanced nations to domestic companies which are related to plastic optical lens. It is necessary to develop novel plastic optical lens materials in order to overcome a FTA provision and revitalize a stagnating optical lens industry in the interior optical lens industries. The new plastic optical lens materials against the substitution effect of income should be gradually demanded. This work will be synthesized novel super high refractive monomer resin materials of urethane lens series and studied the properties of optical lens using it. Methods: ETS-4 (2-(2-mercaptoethylthio)-3-{2-[3-mercapto-2-(2-mercaptoethylthio)propyl thio]ethylthio}propane -1-thiol), which is optical lens monomer resin having super high refractive index, was synthesized and identified its structure and property by elemental analysis, EI-MS, TGA, FT-IR spectroscopy, $^1H$ and $^{13}C$ NMR spectroscopies. After mixing evenly from mixed monomer resin and diisocyanate series, it was casting in glass mold. After thermal curing, the obtained optical lenses were measured and compared with the refractive index and Abbe number for studies of their optical properties. Results: We have synthesized the novel ultra high refractive index monomer resin, ETS-4, and have identified its structure and property by elemental analysis, EI-MS, TGA, FT-IR spectroscopy, $^1H$ and $^{13}C$ NMR spectroscopies. The existence of three isomers for EST-4 was identified by $^{13}C$ NMR spectroscopy. The refractive index ($N_d$ at $25^{\circ}C$) of monomer resin in liquid state obtained from the Abbe refractometer was 1.647. The refractive indexes of raw plastic optical lenses prepared from the mixed ETS-4 monomer and diisocyanate series were in the range of 1.656~1.680. Conclusions: Novel super high refractive index plastic optical lens monomer was synthesized and analysed, the optical lenses prepared using it were colorless transparency and excellent properties. It is of utility for the industrialization.

  • PDF

Isolation and Gas Chromatographic Analysis of Lupenone and Lupeol from Sorbus Cortex (정공피로부터 Lupenone과 Lupeol의 분리 및 정량)

  • Lee, Sang-Myoung;Lee, Cheal-Gyu
    • Analytical Science and Technology
    • /
    • v.12 no.2
    • /
    • pp.136-140
    • /
    • 1999
  • Lupenone and lupeol, the triterpenoids of Sorbus Cortex, were isolated with silica gel column chromatography and used as the standard substances for the quantitative analysis. The compounds were identified with IR, NMR, EI-MS. They were separated on VA-5MS [(5%-phenyl)methylpolysiloxane, $30m{\times}0.25mm$, $0.25{\mu}m$] column by gas-chromatograph. The contents of lupeone and lupeol in three different samples of Sorbus Cortex were in the range of 0.050~0.056% and 0.772~0.834%, respectively.

  • PDF