• Title/Summary/Keyword: Mass spectroscopy

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Dioxygen Binding to Dirhodium(Ⅱ, Ⅱ), (Ⅱ, Ⅲ), and (Ⅲ, Ⅲ) Complexes. Spectroscopic Characterization of $[Rh_{2}(ap)_{4}(O_{2})]^{+},\;Rh_{2}(ap)_{4}(O_{2}),\;and\;[Rh_{2}(ap)_{4}(O_{2})]^-$, where ap=2-anilinopyridinate Ion

  • Lee, Jae-Duck;Yao, Chao-Liang;Capdevielle, Francoise J.;Han, Bao-Cheng;Bear, John L.;Kadish, Karl M.
    • Bulletin of the Korean Chemical Society
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    • v.14 no.2
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    • pp.195-200
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    • 1993
  • The neutral, reduced, and oxidized 2,2-trans isomers of $Rh_2(ap)_4$ (ap=2-anilinopyridinate) were investigated with respect to dioxygen binding in $CH_2Cl_2$ containing 0.1 M tetrabutyl-ammonium perchlorate. $Rh_2(ap)_4$ binds dioxygen in nonaqueous media and forms a $Rh^{II}Rh^{III}$ superoxide complex, $Rh_2(ap)_4(O_2)$. This neutral species was isolated and is characterized by UV-visible and IR spectroscopy, mass spectrometry and cyclic voltammetry. It can be reduced by one electron at $E_{1/2}$ = -0.45 V vs. SCE in $CH_2Cl_2$ and gives ${[Rh_2(ap)_4(O_2)]}^-$ as demonstrated by the ESR spectrum of a frozen solution taken after controlled potential reduction. The superoxide ion in ${[Rh_2(ap)_4(O_2)]}^-$ is axially bound to one of the two rhodium ions, both of which are in a +2 oxidation state. $Rh_2(ap)_4(O_2)$ can also be stepwise oxidized in two one-electron transfer steps at $E_{1/2}$ = 0.21 V and 0.85 V vs. SCE in $CH_2Cl_2$ and gives ${[Rh_2(ap)_4(O_2)]}^+$ followed by ${[Rh_2(ap)_4(O_2)]}^{2+}$. ESR spectra demonstrate that the singly oxidized complex is best described as ${[Rh^{II}Rh^{III}(ap)_4(O_2)]}^+$ where the odd electron is delocalized on both of the two rhodium ions and the axial ligand is molecular oxygen.

Molecular and Enzymatic Features of Homoserine Dehydrogenase from Bacillus subtilis

  • Kim, Do Hyeon;Nguyen, Quyet Thang;Ko, Gyeong Soo;Yang, Jin Kuk
    • Journal of Microbiology and Biotechnology
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    • v.30 no.12
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    • pp.1905-1911
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    • 2020
  • Homoserine dehydrogenase (HSD) catalyzes the reversible conversion of ʟ-aspartate-4-semialdehyde to ʟ-homoserine in the aspartate pathway for the biosynthesis of lysine, methionine, threonine, and isoleucine. HSD has attracted great attention for medical and industrial purposes due to its recognized application in the development of pesticides and is being utilized in the large scale production of ʟ-lysine. In this study, HSD from Bacillus subtilis (BsHSD) was overexpressed in Escherichia coli and purified to homogeneity for biochemical characterization. We examined the enzymatic activity of BsHSD for ʟ-homoserine oxidation and found that BsHSD exclusively prefers NADP+ to NAD+ and that its activity was maximal at pH 9.0 and in the presence of 0.4 M NaCl. By kinetic analysis, Km values for ʟ-homoserine and NADP+ were found to be 35.08 ± 2.91 mM and 0.39 ± 0.05 mM, respectively, and the Vmax values were 2.72 ± 0.06 μmol/min-1 mg-1 and 2.79 ± 0.11 μmol/min-1 mg-1, respectively. The apparent molecular mass determined with size-exclusion chromatography indicated that BsHSD forms a tetramer, in contrast to the previously reported dimeric HSDs from other organisms. This novel oligomeric assembly can be attributed to the additional C-terminal ACT domain of BsHSD. Thermal denaturation monitoring by circular dichroism spectroscopy was used to determine its melting temperature, which was 54.8℃. The molecular and biochemical features of BsHSD revealed in this study may lay the foundation for future studies on amino acid metabolism and its application for industrial and medical purposes.

Chemical Composition of Aromas and Lipophilic Extracts from Black Morel (Morchella importuna) Grown in China

  • Tu, Xiaoman;Tang, Lan;Xie, Guangbo;Deng, Kejun;Xie, Liyuan
    • Mycobiology
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    • v.49 no.1
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    • pp.78-85
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    • 2021
  • Morels (Morchella spp.) are valuable medicinal and edible mushrooms. In this study, chemical profiles of aromas and lipophilic extracts of black morel (Morchella importuna) grown in China were analyzed by gas chromatography/mass spectroscopy, along with the evaluation of antioxidant and antimicrobial activities for the lipophilic extracts. Sixty-five compounds in total were identified from the aromas, and 1-octen-3-ol was the main component for aromas of fresh (34.40%) and freeze-dried (68.61%) black morels, while the most abundant compound for the aroma of the oven-dried sample was 2(5H)-furanone (13.95%). From the lipophilic extracts, 29 compounds were identified with linoleic acid as the main compound for fresh (77.37%) and freeze-dried (56.46%) black morels and steroids (92.41%) as the main constituent for an oven-dried sample. All three lipophilic extracts showed moderate antioxidant activities against 2,2-diphenyl-1-picrylhydrazyl and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) with the IC50 values ranging 7.56~17.52 mg/mL and 5.75~9.73 mg/mL, respectively, and no obvious antimicrobial activity was observed for lipophilic extracts. The drying methods affect the chemical profile of black morel, and freeze-drying was favorable for retaining nutrients and morel smell. This is the first report on the aroma and lipophilic extracts of M. importuna grown in China.

Rotation Speed Dependence of ZnO Coating Layer on SnSe powders by Rotary Atomic Layer Deposition Reactor (회전형 원자층 증착기의 회전 속도에 따른 SnSe 분말 상 ZnO 박막 증착)

  • Jung, Myeong Jun;Yun, Ye Jun;Byun, Jongmin;Choi, Byung Joon
    • Journal of Powder Materials
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    • v.28 no.3
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    • pp.239-245
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    • 2021
  • The SnSe single crystal shows an outstanding figure of merit (ZT) of 2.6 at 973 K; thus, it is considered to be a promising thermoelectric material. However, the mass production of SnSe single crystals is difficult, and their mechanical properties are poor. Alternatively, we can use polycrystalline SnSe powder, which has better mechanical properties. In this study, surface modification by atomic layer deposition (ALD) is chosen to increase the ZT value of SnSe polycrystalline powder. SnSe powder is ground by a ball mill. An ALD coating process using a rotary-type reactor is adopted. ZnO thin films are grown by 100 ALD cycles using diethylzinc and H2O as precursors at 100℃. ALD is performed at rotation speeds of 30, 40, 50, and 60 rpm to examine the effects of rotation speed on the thin film characteristics. The physical and chemical properties of ALD-coated SnSe powders are characterized by scanning and tunneling electron microscopy combined with energy-dispersive spectroscopy. The results reveal that a smooth oxygen-rich ZnO layer is grown on SnSe at a rotation speed of 30 rpm. This result can be applied for the uniform coating of a ZnO layer on various powder materials.

Ni Nanoparticle-Graphene Oxide Composites for Speedy and Efficient Removal of Cr(VI) from Wastewater

  • Wang, Wan-Xia;Zhao, Dong-Lin;Wu, Chang-Nian;Chen, Yan;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.31 no.6
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    • pp.345-352
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    • 2021
  • In this study, Ni nanoparticle supported by graphene oxide (GO) (Ni-GO) is successfully synthesized through hydrothermal synthesis and calcination, and Cr(VI) is extracted from aqueous solution. The morphology and structure of Ni-GO composites are characterized by scanning electron microscopy (SEM), trans mission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). High-resolution transmission electron microscopy (HRTEM) and XRD confirms the high dispersion of Ni nanoparticle after support by GO. Loading Ni on GO can obviously enhance the stability of Ni-GO composites. It can be calculated from TGA that the mass percentage of Ni is about 60.67 %. The effects of initial pH and reaction time on Cr(VI) removal ability of Ni-GO are investigated. The results indicate that the removal efficiency of Cr(VI) is greater than that of bared GO. Ni-GO shows fast removal capacity for Cr(VI) (<25 min) with high removal efficiency. Dynamic experiments show that the removal process conforms to the quasi-second order model of adsorption, which indicates that the rate control step of the removal process is chemical adsorption. The removal capacity increases with the increase of temperature, indicating that the reaction of Cr(VI) on Ni-GO composites is endothermic and spontaneous. Combined with tests and characterization, the mechanism of Cr(VI) removal by rapidly adsorption on the surface of Ni-GO and reduction by Ni nanoparticle is investigated. The above results show that Ni-GO can be used as a potential remediation agent for Cr(VI)-contaminated groundwater.

Physicochemical, Antibacterial Properties, and Compatibility of ZnO-NP/Chitosan/β-Glycerophosphate Composite Hydrogels

  • Huang, Pingping;Su, Wen;Han, Rui;Lin, Hao;Yang, Jing;Xu, Libin;Ma, Lei
    • Journal of Microbiology and Biotechnology
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    • v.32 no.4
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    • pp.522-530
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    • 2022
  • In this study we aimed to develop novel ZnO-NP/chitosan/β-glycerophosphate (ZnO-NP/CS/β-GP) antibacterial hydrogels for biomedical applications. According to the mass fraction ratio of ZnO-NPs to chitosan, mixtures of 1, 3, and 5% ZnO-NPs/CS/β-GP were prepared. Using the test-tube inversion method, scanning electron microscopy and Fourier-transform infrared spectroscopy, the influence of ZnO-NPs on gelation time, chemical composition, and cross-sectional microstructures were evaluated. Adding ZnO-NPs significantly improved the hydrogel's antibacterial activity as determined by bacteriostatic zone and colony counting. The hydrogel's bacteriostatic mechanism was investigated using live/dead fluorescent staining and scanning electron microscopy. In addition, crystal violet staining and MTT assay demonstrated that ZnO-NPs/CS/β-GP exhibited good antibacterial activity in inhibiting the formation of biofilms and eradicating existing biofilms. CCK-8 and live/dead cell staining methods revealed that the cell viability of gingival fibroblasts (L929) cocultured with hydrogel in each group was above 90% after 24, 48, and 72 h. These results suggest that ZnO-NPs improve the temperature sensitivity and bacteriostatic performance of chitosan/β-glycerophosphate (CS/β-GP), which could be injected into the periodontal pocket in solution form and quickly transformed into hydrogel adhesion on the gingiva, allowing for a straightforward and convenient procedure. In conclusion, ZnO-NP/CS/β-GP thermosensitive hydrogels could be expected to be utilized as adjuvant drugs for clinical prevention and treatment of peri-implant inflammation.

Novel Antibacterial, Cytotoxic and Catalytic Activities of Silver Nanoparticles Synthesized from Acidophilic Actinobacterial SL19 with Evidence for Protein as Coating Biomolecule

  • Wypij, Magdalena;Ostrowski, Maciej;Piska, Kamil;Wojcik-Pszczola, Katarzyna;Pekala, Elzbieta;Rai, Mahendra;Golinska, Patrycja
    • Journal of Microbiology and Biotechnology
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    • v.32 no.9
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    • pp.1195-1208
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    • 2022
  • Silver nanoparticles (AgNPs) have potential applications in medicine, photocatalysis, agriculture, and cosmetic fields due to their unique physicochemical properties and strong antimicrobial activity. Here, AgNPs were synthesized using actinobacterial SL19 strain, isolated from acidic forest soil in Poland, and confirmed by UV-vis and FTIR spectroscopy, TEM, and zeta potential analysis. The AgNPs were polydispersed, stable, spherical, and small, with an average size of 23 nm. The FTIR study revealed the presence of bonds characteristic of proteins that cover nanoparticles. These proteins were then studied by using liquid chromatography with tandem mass spectrometry (LC-MS/MS) and identified with the highest similarity to hypothetical protein and porin with molecular masses equal to 41 and 38 kDa, respectively. Our AgNPs exhibited remarkable antibacterial activity against Escherichia coli and Pseudomonas aeruginosa. The combined, synergistic action of these synthesized AgNPs with commercial antibiotics (ampicillin, kanamycin, streptomycin, and tetracycline) enabled dose reductions in both components and increased their antimicrobial efficacy, especially in the case of streptomycin and tetracycline. Furthermore, the in vitro activity of the AgNPs on human cancer cell lines (MCF-7, A375, A549, and HepG2) showed cancer-specific sensitivity, while the genotoxic activity was evaluated by Ames assay, which revealed a lack of mutagenicity on the part of nanoparticles in Salmonella Typhimurium TA98 strain. We also studied the impact of the AgNPs on the catalytic and photocatalytic degradation of methyl orange (MO). The decomposition of MO was observed by a decrease in intensity of absorbance within time. The results of our study proved the easy, fast, and efficient synthesis of AgNPs using acidophilic actinomycete SL19 strain and demonstrated the remarkable potential of these AgNPs as anticancer and antibacterial agents. However, the properties and activity of such particles can vary by biosynthesized batch.

Organic Residues Analysis of Oil Bottle of Goryeo Dynasty Excavated from the Soejeoul Site, Geumneung-dong, Chungju (충주 금릉동 쇠저울유적 출토 고려시대 유병의 유기물 분석)

  • Yun, Eun Young;Kim, Suyeon
    • Journal of Conservation Science
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    • v.37 no.6
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    • pp.638-647
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    • 2021
  • Organic residues are substances derived from diverse natural sources. Recent scientific analysis of organic residues has yielded important information in restoring the lifestyles of ancient peoples. In this study, the organic material contained within the celadon oil bottle of the Goryeo dynasty, excavated from the Soejoul site in Geumneung-dong, Chungju, was analyzed using Fourier-transform infrared spectroscopy (FT-IR) and gas chromatograph-mass spectrometer (GC-MS). The results showed that the organic materials in the bottle were plant-derived oils. In particular, polyunsaturated fatty acids and phytosterols were detected using GC-MS analysis. Sesamin components were also identified. Sesamin, which is a characteristic component of sesame seeds, is a lignan and an antioxidant. As the organic residues in the oil bottle were derived from sesame seeds, it is presumed that sesame oil was stored in the bottle.

Synergistic effects of CNT and CB inclusion on the piezoresistive sensing behaviors of cementitious composites blended with fly ash

  • Jang, Daeik;Yoon, H.N.;Yang, Beomjoo;Seo, Joonho;Farooq, Shah Z.;Lee, H.K.
    • Smart Structures and Systems
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    • v.29 no.2
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    • pp.351-359
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    • 2022
  • The present study investigated the synergistic effects of carbon nanotube (CNT) and carbon black (CB) inclusions on the piezoresistive sensing behaviors of cementitious composites. Four different CNT and CB combinations were considered to form different conductive networks in the binder material composed of Portland cement and fly ash. The cement was substituted with fly ash at levels of 0 or 50% by the mass of binder. The specimens were cured up to 100 days to observe the variations of the electrical characteristics with hydration progress, and the piezoresistive sensing behaviors of the specimens were measured under cyclic loading tests. The fabricated specimens were additionally evaluated with flowability, resistivity and cyclic loading tests, and morphological analysis. The scanning electron microscopy and energy disperse X-ray spectroscopy test results indicated that CNT and CB inclusion induced synergistic formations of electrically conductive networks, which led to an improvement of piezoresistive sensing behaviors. Moreover, the incorporation of fly ash having Fe3+ components decreased the electrical resistivity, improving both the linearity of fractional changes in the electrical resistivity and reproducibility expressed as R2 under cyclic loading conditions.

DRY ETCHING CHARACTERISTICS OF INGAN USING INDUCTIVELY COUPLED $Cl_2/CHF_3,{\;}Cl_2/CH_4$ AND Cl_2/Ar PLASMAS.

  • Lee, D.H.;Kim, H.S.;G.Y. Yeom;Lee, J.W.;Kim, T.I.
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 1999.10a
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    • pp.59-59
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    • 1999
  • In this study, planer inductively coupled $Cl_2$ based plasmas were used to etch InGaN and the effects of plasma conditions on the InGaN etch properties have been characterized using quadrupole mass spectrometry(QMS) and optical emission spectroscopy(OES). As process conditions used to study the effects of plasma characteristics on the InGaN etch properties, $Cl_2$ was used as the main etch gas and $CHF_3,{\;}CH_4$, and Ar were used as additive gases. Operational pressure was varied from SmTorr to 3OmTorr, inductive power and bias voltage were varied from 400W to 800W and -50V to -250V, respectively while the substrate temperature was fixed at 50 centigrade. For the $Cl_2$ plasmas, selective etching of GaN to InGaN was obtained regardless of plasma conditions. The small addition of $CHF_3$ or Ar to $Cl_2$ and the decrease of pressure generally increased InGaN etch rates. The selective etching of InGaN to GaN could be obtained by the reduction of pressure to l5mTorr in $CI_2/IO%CHF_3{\;}or{\;}CI_2/IO%Ar$ plasma. The enhancement of InGaN etch rates was related to the ion bombardment for $CI_2/Ar$ plasmas and the formation of $CH_x$ radicals for $CI_2/CHF_3(CH_4)$ plasmas.

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