• Title/Summary/Keyword: $MS^n$

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Examination and Isolation of Natural Antioxidants from Korean Medicinal Plants (국내산 약용식물의 항산화물질 탐색 및 분리)

  • Song, Jung-Choon;Park, Nam-Kyu;Hur, Han-Sun;Bang, Myun-Ho;Baek, Nam-In
    • Korean Journal of Medicinal Crop Science
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    • v.8 no.2
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    • pp.94-101
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    • 2000
  • On the purpose of development of antioxidative compounds from natural sources, 38 plants known to have antioxidant activity have been examined concerning DPPH radical scavenging activity. Among 13 plants exhibiting the activity, the seed of Carthamus tinctorius L, was selected as resources to search for active compounds due to rareness of study. The seed of the plant has been used as edible oil or preventive and remedial drugs for osteoporosis, arthritis. To reveal the principal component manifesting the antioxidant activity, the MeOH extracts was successively solvent-fractionated with EtOAc, n-BuOH and water. In order to isolate active component from the EtOAc fractions, application of silica gel column chromatographies and activity tests were repeated for a active component to be isolated. Its chmical structure was determined to be N-feruloylserotonin, a conjugated serotonin compound, by the interpretation of spectral data, NMR. MS and the adaptation of chemical reactions.

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PHOTOCATALYTIC SYNTHESIS OF L-PIPECOLINIC ACID FROM $N_{varepsilon}$-CARBAMYL-L-LYSINE BY AQUEOUS SUSPENSION OF PLATINIZED TITANIUM(IV) OXIDE

  • Ohtani, Bunsho;Aoki, Eishiro;Iwai, Kunihiro;Nishimoto, Sei-Ichi
    • Journal of Photoscience
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    • v.1 no.1
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    • pp.31-37
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    • 1994
  • Photoirradiation at > 300 nm onto a suspension of platinized TiO$_2$ (TiO$_2$-Pt) particles in an aqueous solution. of N$_{\varepsilon}$-carbamyI-L-lysine (Lys(CONH)$_2$) induced the selective N-cyclization of Lys(CONH$_2$) into almost optically pure L-pipecolinic acid (PCA) under argon atmosphere at ambient temperature. Among various TiO$_2$-Pt catalysts, a P-25 (Degussa) powder platinized via impregnation from chloroplatinic acid followed by hydrogen reduction at 753 K exhibited the highest photocatalytic activity for Lys(CONH$_2$) consumption and L-PCA production. GC-MS analyses of L-PCA obtained photocatalytically from $^{15}$N$\alpha$-Lys(CONH$_2$) revealed the selective formation $^{15}$N-substituted L-PCA. This implies that the mechanism for L-PCA production contains selective cleavage of C$_{\varepsilon}$-N bond and intramolecular alkylation at $\alpha$-amino group. Effect of pH on the rate of this photocatalytic reaction was investigated in detail and compared with the pH-dependent charge distribution in Lys(CONH$_2$) molecule. It is clarified that protonation-deprotonation of $\alpha$-amino group gives marked influence on the rate and selectivity of the photocatalytic reaction. On the basis of these results, it is concluded that the selective production of optically pure L-PCA, especially in an acidic suspension of TiO$_2$-Pt, was attributed to the enhanced protonation of $\alpha$-amino group to prevent undesirable oxidation by photogenerated positive holes and blocking of $\varepsilon$-amino group to yield racemic Schiff base intermediate.

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A Novel Al-Bridged Trinuclear Iron(II) Bis(imino)pyridyl Complex with Catalytic Ethylene Polymerization Behavior

  • Long, Zerong;Li, Zhongquan;Ma, Ning;Wu, Biao
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2537-2543
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    • 2011
  • A self-assembled Al-bridged diiminopyridine-based ligand (3) was synthesized and characterized by FT-IR, ESI-MS and NMR spectroscopy. Electron spectral titrations were performed to confirm the formation of a novel trinuclear bis(imino)pyridyl iron(II) complex (4) upon addition of $FeCl_2$ into Al-bridged ligand 3 in methanol solution. Simultaneously, a typical bis(imino)pyridine-iron(II) complex (2) was synthesized and fully characterized. The X-ray crystal study of the iron(II) complex 2 disclosed a five-coordinate, distorted square-pyramidal structure with the tridentate N^N^N ligand and chlorides. The optimal molecular structure of 4 was obtained by means of molecular mechanics, which showed that each iron atom in the complex 4 is surrounded by two chlorides, a tridentate N^N^N ligand and one oxygen atom, supporting considerations about the possibility of six-coordinate geometry from MMAO or the ethylene access. A comparison of 4 with the reference 2 revealed a remarkable decrease of the catalytic activity and MMAO consumption (activity up to $0.41{\times}10^3\;kg\;{mol_{Fe}}^{-1}h^{-1}bar^{-1}$, Al/Fe = 650 for 4 and $7.02{\times}10^3\;kg\;{mol_{Fe}}^{-1}h^{-1}bar^{-1}$, Al/Fe = 1600 for 2).

Growth Inhibition and Apoptosis Induction of Essential Oils and Extracts of Nepeta cataria L. on Human Prostatic and Breast Cancer Cell Lines

  • Emami, Seyed Ahmad;Asili, Javad;HosseinNia, Shima;Yazdian-Robati, Rezvan;Sahranavard, Mehrdad;Tayarani-Najaran, Zahra
    • Asian Pacific Journal of Cancer Prevention
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    • v.17 no.sup3
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    • pp.125-130
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    • 2016
  • Nepeta cataria L. has been used in traditional medicine of some countries. Here the cytotoxic and apoptogenic activity of methanol extracts, n-hexane, dichloromethane, ethyl acetate, n-butanol, and acqueous extracts and the essential oil obtained from the aerial parts of the plant were evaluated with PC3, DU-145 and MCF-7 cell lines. Cell viability, histograms of PI stained fragmented DNA in apoptotic cells and Western blot analysis of proteins involved in the cascade of apoptosis were compared in all samples. Thirty components were identified as volatile, representing 99.7% of essential oil composition after GC-MS analysis of the oil obtained from aerial parts of the N. cataria by hydro-distillation. The major oil components of the essential oil were nepetalactone stereoisomers. Comparing IC50 values showed estrogen receptor positive PC3 cells were more sensitive to the cytotoxic effects of N. cataria in comparison with low hormone-receptor presenting DU-145 cells. Among multiple extracts and essential oils of the plant, only the ethyl acetate extract could significantly decrease cell viability in PC3 cells, in a concentration dependent manner. Ethyl acetate extract of N. cataria treated cells showed a sub-G1 peak in PC3 cells in a concentration dependent manner that indicates the involvement of an apoptotic process in ethyl acetate extract-induced cell death. Western blotting analysis showed that in PC3 cells treated with ethyl acetate (48 h) caspase 3 and PARP were cleaved to active forms. Overall, the results suggest that further analytical elucidation of N. cataria in respect to finding new cytotoxic chemicals with anti-tumor activity is warranted.

East Asian Monsoon History as Indicated by C/N Ratios and ${\delta}^{13}C$ Evidence from the Estuarine Tidal Flat Sediments in the West Coast of Korea (서해안 염하구 습지 퇴적물의 지화학적 분석 (C/N 및 ${\delta}^{13}C$)에 기반한 동아시아 몬순 변동 연구)

  • Park, Jung-Jae;Shin, Young-Ho
    • Journal of the Korean Geographical Society
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    • v.45 no.5
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    • pp.541-552
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    • 2010
  • Geochemical and physical investigations such as ${\delta}^{13}C$ isotope ratio, carbon/nitrogen (C/N) ratio, magnetic susceptibility (MS), and particle size analyses were carried out on the estuarine tidal flat sediments from the west coast of Korea in order to reconstruct the East Asian summer monsoon variability during the late Pleistocene and Holocene Our results indicated that the summer monsoon probably peaked around 7,700-7,800 yr BP and then started to decline about 7,400 yr BP in the Korean peninsular, and that the monsoon was relatively weak between 24,000-24,500 yr BP but relatively strong between 18,500-19,500 yr BP during the Last Glacial Maximum. Our estuarine geochemical data have proven to be valuable as a new proxy for detecting the shifts in monsoon strength. This new evidence will be helpful, especially for Korean paleoenvironmental studies with few proxy data archives.

Exposure Assessment of Volatile Organic Compounds for Workers Handling Rust-preventive Oils (방청유 취급 근로자의 휘발성 유기화합물 노출 평가)

  • Jeong, Yoonkeong;Choi, Sangjun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.27 no.1
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    • pp.23-37
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    • 2017
  • Objectives : This study was conducted to evaluate the level of exposure to volatile organic compounds (VOCs) among workers handling rust preventive oils. Methods : A total of 30 bulk samples and 54 personal air samples were collected using diffusive samplers at 22 workplaces handling rust preventive oils in Daegu and Gyongsangbuk-do Province from March to October 2013. We also investigated detailed information on the related work conditions, such as kinds of products, handling methods, local exhaustive ventilation systems, and the status of the wearing personal protective equipment. All bulk samples and air samples were analyzed using gas chromatography mass spectrometry (GC-MS) to identify components to which workers potentially were exposed. Quantitative airborne concentrations of VOCs were confirmed using gas chromatography with flame ionized detectors. Results : In terms of qualitative analyses for the 30 bulk samples, we found carcinogenic, mutagenic and reproductive toxic(CMR) substances such as butane(carcinogenic Group 1A, mutagenic Group 1B), butoxy ethanol(carcinogenic Group 2), cumene (carcinogenic Group 2), ethyl benzene(carcinogenic Group 2), methyl isobutyl ketone(carcinogenic Group 2) and toluene (reproductive toxic, Group 2). As a result of full-shift based personal air samples, eight substances such as n-hexane, n-heptane, octane, nonane, decane, toluene, ethyl benzene and xylene were detected. Among them, n-hexane and n-heptane were detected in all of 54 air samples with $13.13mg/m^3$ and $8.61mg/m^3$ of maximum concentration, respectively. The level of airborne concentration from all of samples were bellow the occupational exposure limit in Korea. Conclusions : Based on the results of this study, workers handling rust preventive oils could be exposed to CMR substances contained in rust preventive oils and n-hexane and n-heptane were found as the most frequent sources of VOC exposure.

Volatiles Composition from Aerial Parts of the Insect-Pollinated and the Promising Medicinal Plant Spiraea hypericifolia L. Growing Wild in Northern Kazakhstan

  • Kirillov, Vitaliy;Stikhareva, Tamara;Atazhanova, Gayane;Ercisli, Sezai;Makubayeva, Aigerim;Krekova, Yana;Rakhimzhanov, Alimzhan;Adekenov, Sergazy
    • Natural Product Sciences
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    • v.27 no.1
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    • pp.36-44
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    • 2021
  • The essential oils from the aerial parts (leaves and flowers) of Spiraea hypericifolia L. (Rosaceae), collected in Northern Kazakhstan, were obtained by distillation in two dispersion media (distilled water and 15% NaCl solution). The chemical composition of the essential oils was evaluated by GC-MS for the first time. The yield of the essential oil was 0.04% (in fresh growth conditions) and 0.02% (in dry growth conditions) respectively regardless of which dispersion media (H2O or 15% NaCl solution) was used at the isolation of essential oil. The main compounds were aliphatic hydrocarbons (alkanes) (40.6-53.2%), aldehydes (8.4-17.4%), diterpenoids (9.1-16.7%) and ketones (6.2-8.7%). Content of monoterpenoids was depended on dispersion media (2.2-3.6% where H2O was dispersion media and 8.4-8.5% where 15% NaCl solution was dispersion media). n-Heneicosane (17.4-34.1%) and n-tricosane (14.3-19.5%) were the main constituents of the essential oil of S. hypericifolia. There were many insects from different classes in S. hypericifolia at flowering. Important components such as α-methylene-γ-butyrolactone (0.8-2.8%), benzyl cyanide (0.7-1.1%), β-damascenone (1.2-2.9%), (E,E)-4,8,12-trimethyl-1,3,7,11-tridecatetraene (1.8-2.7%), β-ionone (0.5-1.8%) and others were detected in small amounts.

Concentrations of N,N-dimethylformamide in Polyurethane Gloves and Risk Assessment for Dermal Exposures (폴리우레탄 코팅장갑내의 DMF 함량 및 피부노출에 대한 평가)

  • Park, Hae Dong;Ro, Jiwon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.32 no.2
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    • pp.102-110
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    • 2022
  • Objectives: The purpose of this study is to analyze the content of N,N-dimethylformamide(DMF) in polyurethane coated gloves(PU-gloves) and to assess the dermal exposure generated by wearing them. Methods: We analyzed the concentrations of DMF in 12 gloves by EN16778 standard. The samples cut into pieces of about 10 by 10 mm and extracted with methanol in flask in an ultrasonic bath at 70℃. An aliquot of the extract is analyzed with GC-MS. The dose of dermal exposure was calculated by ECETOC TRA consumer 3.1 and compared with derived no effect level(DNEL) for systemic effects due to long term exposure by workers. The extracted amount of DMF by saline solution was compared with that by EN16778 standard. Results: The mean concentration of DMF in PU-gloves was 1,377 mg/kg(range 13~3,948 mg/kg). The concentration of DMF showed significantly differences by packing type, manufacturer, and price(p<0.05). The dose of dermal exposure was 0.0007~0.572 mg/kg body weight/day when the DMF content was 10~4,000 mg/kg. The DMF extracted by saline solution was around 11% for 8 hours. Conclusions: The risk of dermal exposure due to the residual DMF in the PU-gloves was not signifiant. But, the limit of 1,000 mg/kg in PU-gloves can be recommended for international standard and trading systems.

Study for Residue Analysis of Pinoxaden in Agricultural Commodities

  • Kim, Ji Young;Yoon, Eun Kyung;Kim, Jong Soo;Seong, Nu Ri;Yun, Sang Soon;Jung, Yong Hyun;Oh, Jae Ho;Kim, Hyochin
    • Korean Journal of Environmental Agriculture
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    • v.38 no.4
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    • pp.321-331
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    • 2019
  • BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C18. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r2) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Proliferation of Embryogenic Callus of Kalopanax pictus through Suspension Culture System (현탁배양을 통한 음나무(Kalopanax pictus) 배발생 캘러스의 증식)

  • Kim, Hye-Jin;Kim, Won-Bea;Yoo, Dong-Lim;Kim, Su-Jeong;Lee, Jun-Gu
    • Korean Journal of Plant Resources
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    • v.21 no.1
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    • pp.60-65
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    • 2008
  • Kalopanax pictus was cultured in vitro to find out optimal condition for embryogenic cells proliferation in liquid media rapidly. Embryogenic cells were induced from leaves and petiols of Kalopanax pictus. Optimum culture medium appeared to be a 1/2MS medium supplemented with 2.0mg/L 2,4-D and 0.1mg/L BA. To find out optimal conditions, embryogenic cells were cultured some condition as different concentrations of 2,4-D, medium and sucrose. There was cultured on 1/2MS liquid medium containing different concentration of 2,4-D. When embryogenic cells were cultured on 1/2MS liquid medium supplemented with 1.0mg/L 2,4-D, cell propagation rate was higher than other concentration of 2,4-D. When embryogenic cells were cultured on different media that MS, Gambols B5, N6, White, SH medium, observed the highest multiplication rate among Gambols B5 and White medium. To find out of effect of sucrose to embryogenic cells propagation, we tested cells under different concentrations. Optimal concentration of sucrose appeared to be a basal medium added 3% sucrose. Above results suggest that optimal conditions for proliferation of embryogenic cells were established Gambols B5 and White medium added 1.0mg/L 2,4-D and 3% sucrose. There is every possibility achieving embryogenic cells proliferation via bioreactor culture system in Kalopanax pictus.