The research was conducted(1) to confirm the agent(s) responsible for the antimicrobial activity contained in the fermented tomato juice with L. acidophilus(2) to extract and purify the antimicrobial agent(s)(3) to find the biological, physical and chemical properties of the agent(s). The following results were obtained and summarized as followings; 1. The agent responsible for the inhibitory activity was confirmed by both well assay method using fermented tomato juice with L. acidophilus and turbidimetric technique using the cell-free filtrate or neutralized filtrate of tomato acidohilus culture and found exerted antimicrobial agent other than lactic acid. 2. The procedures of purification : The isolation and purification of antimicrobial agent from the lyophilized acidophilus tomato culture were carried out by (1) methanol extraction (2) acetone extraction, (3) Sephadex G-50 gel filtration (4) paper chromatography and (5) thin layer chromatography. 3. The biological, physical and chemical properties of antimicrobial agent: The biological, physical, chemical properties of the purified antimicrobial agent were: (1) The antimicrobial activity was strong against test organisms; Bacillus subtilis(ATCC 6633), Escheichia coli(ATCC 25922), Staphylococcus aureus(ATCC 167), Pseudomonas fluorescens(KFCC 32394), Proteus vulgaris and Shigella dysenteriae. (2) The pH value of the agent was 2.0 and the inhibitory activity was lost when it was neutralized at 7.0 of pH and the agent was heat stable at $121^{\circ}C$ for 60 minutes. (3) The ultraviolet light absorption spectra of methanol-acetone extract and TLC fraction exhibited a maximum absorption at 260nm and 224nm respectively. (4) The most purified agent from TLC plate increased about 130-fold in activity. (5) The agent isolated from TLC plate was free from $H_2O_2$ or lactic acid. 4. Bioautographic assy: By means of bioautography of the agent on silica gel of TLC plate a strong inhibitory activity against B. subtilis was demonstrated. 5. Mass spectrometry: The agent obtained from TLC plate was analyzed by mass spectrometry which show the parent peak at m/e 264 suggesting the molecular weight of the compound and molecular group such as [$C_2H{^+}_4$], [CO], [CH=NH], [$C_3{H^}4_7$], [$\begin{array}{rcl}O\\{\parallel}\\CH_3-C\\\end{array}$], [$C_6-H{^+}_{11}$], [$C_5H{^+}_{11}$], [$\begin{array}{rcl}O\\{\parallel}\\C_5H_7-C^+\\\end{array}$] were suggested.
Background: Biogenic fabrication of silver nanoparticles from naturally occurring biomaterials provides an alternative, eco-friendly and cost-effective means of obtaining nanoparticles. It is a favourite pursuit of all scientists and has gained popularity because it prevents the environment from pollution. Our main objective to take up this project is to fabricate silver nanoparticles from lichen, Usnea longissima and explore their properties. In the present study, we report a benign method of biosynthesis of silver nanoparticles from aqueous-ethanolic extract of Usnea longissima and their characterization by ultraviolet-visible (UV-vis), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM) and scanning electron microscopy (SEM) analyses. Silver nanoparticles thus obtained were tested for antimicrobial activity against gram positive bacteria and gram negative bacteria. Results: Formation of silver nanoparticles was confirmed by the appearance of an absorption band at 400 nm in the UV-vis spectrum of the colloidal solution containing both the nanoparticles and U. longissima extract. Poly(ethylene glycol) coated silver nanoparticles showed additional absorption peaks at 424 and 450 nm. FTIR spectrum showed the involvement of amines, usnic acids, phenols, aldehydes and ketones in the reduction of silver ions to silver nanoparticles. Morphological studies showed three types of nanoparticles with an abundance of spherical shaped silver nanoparticles of 9.40-11.23 nm. Their average hydrodynamic diameter is 437.1 nm. Results of in vitro antibacterial activity of silver nanoparticles against Staphylococcus aureus, Streptococcus mutans, Streptococcus pyrogenes, Streptococcus viridans, Corynebacterium xerosis, Corynebacterium diphtheriae (gram positive bacteria) and Escherichia coli, Klebsiella pneuomoniae and Pseudomonas aeruginosa (gram negative bacteria) showed that it was effective against tested bacterial strains. However, S. mutans, C. diphtheriae and P. aeruginosa were resistant to silver nanoparticles. Conclusion: Lichens are rarely exploited for the fabrication of silver nanoparticles. In the present work the lichen acts as reducing as well as capping agent. They can therefore, be used to synthesize metal nanoparticles and their size may be controlled by monitoring the concentration of extract and metal ions. Since they are antibacterial they may be used for the treatment of bacterial infections in man and animal. They can also be used in purification of water, in soaps and medicine. Their sustained release may be achieved by coating them with a suitable polymer. Silver nanoparticles fabricated from edible U. longissima are free from toxic chemicals and therefore they can be safely used in medicine and medical devices. These silver nanoparticles were stable for weeks therefore they can be stored for longer duration of time without decomposition.
Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
The Korean Journal of Pesticide Science
/
v.18
no.4
/
pp.321-329
/
2014
This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.
Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
Korean Journal of Environmental Agriculture
/
v.37
no.1
/
pp.57-65
/
2018
BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.
A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.
Photoelectrochemical (PEC) systems are promising methods of producing H2 gas using solar energy in an aqueous solution. The photoelectrochemical properties of numerous metal oxides have been studied. Among them, the PEC systems based on TiO2 have been extensively studied. However, the drawback of a PEC system with TiO2 is that only ultraviolet (UV) light can be absorbed because of its large band gap (3.2 - 3.4 eV). Two approaches have been introduced in order to use PEC cells in the visible light region. The first method includes doping impurities, such as nitrogen, into TiO2, and this technique has been extensively studied in an attempt to narrow the band gap. In comparison, research on the second method, which includes visible light water splitting in molecular photosystems, has been slow. Mallouk et al. recently developed electrochemical water-splitting cells using the Ru(II) complex as the visible light photosensitizer. the dye-sensitized PEC cell consisted of a dye-sensitized TiO2 layer, a Pt counter electrode, and an aqueous solution between them. Under a visible light (< 3 eV) illumination, only the dye molecule absorbed the light and became excited because TiO2 had the wide band gap. The light absorption of the dye was followed by the transfer of an electron from the excited state (S*) of the dye to the conduction band (CB) of TiO2 and its subsequent transfer to the transparent conducting oxide (TCO). The electrons moved through the wire to the Pt, where the water reduction (or H2 evolution) occurred. The oxidized dye molecules caused the water oxidation because their HOMO level was below the H2O/O2 level. Organic dyes have been developed as metal-free alternatives to the Ru(II) complexes because of their tunable optical and electronic properties and low-cost manufacturing. Recently, organic dye molecules containing multi-branched, multi-anchoring groups have received a great deal of interest. In this work, tri-branched tri-anchoring organic dyes (Dye 2) were designed and applied to visible light water-splitting cells based on dye-sensitized TiO2 electrodes. Dye 2 had a molecular structure containing one donor (D) and three acceptor (A) groups, and each ended with an anchoring functionality. In comparison, mono-anchoring dyes (Dye 1) were also synthesized. The PEC response of the Dye 2-sensitized TiO2 film was much better than the Dye 1-sensitized or unsensitized TiO2 films.
$Bi_2MoO_6$ catalysts were successfully synthesized using ethylene glycol monomethyl ether (EGME), glycerol (GL), ethylene glycol (EG), and water as solvents by a conventional hydrothermal method. The synthesized catalysts were characterized by XRD, DRS, BET, SEM, and PL, and we also investigated the photocatalytic activity of these materials for the decomposition of Rhodamin B under visible light irradiation. The XRD results revealed the successful synthesis of 12-18 nm, well-crystallized ${\gamma}-Bi_2MoO_6$ crystals with an Aurivillius structure regardless of solvent. In addition, the $Bi_2MoO_6$ catalysts prepared below $140^{\circ}C$ showed an amorphous phase; however, those prepared above $160^{\circ}C$ showed well-crystallized ${\gamma}-Bi_2MoO_6$ crystals. All the catalysts have a similar absorption spectrum from the ultraviolet region up to the visible region less than 470 nm. This result suggests that all the $Bi_2MoO_6$ catalysts are potential visible-light-driven photocatalysts. The $Bi_2MoO_6$ catalysts prepared using EGME as a solvent showed the highest photocatalytic activity. In addition, the $Bi_2MoO_6$ catalysts prepared at $180^{\circ}C$ showed the highest photocatalytic activity. The PL peaks appeared at about 560 nm at all catalysts and the excitonic PL signal was proportional to the photocatalytic activity for the decomposition of Rhodamin B. This suggests that the stronger the PL intensity, the larger the amount of oxygen vacancies and defects, and the higher the photocatalytic activity.
Spinel $LiNi_xMn_{2-x}O_4$ thin films were synthesized up to x = 0.9 by a sol-gel method employing spin-coating. The Ni-substituted films were found to maintain cubic structure at low x but to exhibit tetragonal structure for $x{\geq}0.6$. Such cubic-tetragonal phase transition indicates that $Ni^{3+}(d7)$ ions with low-spin $(t_{2g}^6,e_g^1)$ state occupy the octahedral sites of the compound, thus being subject to the Jahn-Teller distortion. By x-ray photoelectron spectroscopy both $Ni^{2+}$ and $Ni^{3+}$ ions were detected. Optical properties of the $LiNi_xMn_{2-x}O_4$ films were investigated by spectroscopic ellipsometry (SE) in the visible?ultraviolet range. The measured dielectric function spectra by SE mainly consist of broad absorption structures attributed to charge-transfer (CT) transitions, $O^{2-}(2p){\rightarrow}Mn^{4+}(3d)$ for 1.9 $(t_{2g})$ and $2.8{\sim}3.0$ eV $(e_g)$ structures and $O^{2-}(2p){\rightarrow}Mn^{3+}(3d)$ for 2.3 $(t_{2g})$ and $3.4{\sim}3.6$ eV $(e_g)$ structures. Also, sharp absorption structures were observed at about 1.6, 1.7, and 1.9 eV, interpreted as due to d-d crystal-field transitions within the octahedral $Mn^{3+}$ ion. The strengths of these absorption structures are reduced by the Ni substitution. Rapid reduction of the CT transition strength involving the eg states for x = 0.6 is attributed to the reduced wavefunction overlap between the $e_g$ and the $O^{2-}(2p)$ states due to the tetragonal extension of the lattice constant by the Jahn-Teller effect.
Takeda, K.;Fukunaga, Y.;Tsutsumi, T.;Ishikawa, K.;Kondo, H.;Sekine, M.;Hori, M.
Proceedings of the Korean Vacuum Society Conference
/
2016.02a
/
pp.93-93
/
2016
Large scale integrated circuits (LSIs) has been improved by the shrinkage of the circuit dimensions. The smaller chip sizes and increase in circuit density require the miniaturization of the line-width and space between metal interconnections. Therefore, an extreme precise control of the critical dimension and pattern profile is necessary to fabricate next generation nano-electronics devices. The pattern profile control of plasma etching with an accuracy of sub-nanometer must be achieved. To realize the etching process which achieves the problem, understanding of the etching mechanism and precise control of the process based on the real-time monitoring of internal plasma parameters such as etching species density, surface temperature of substrate, etc. are very important. For instance, it is known that the etched profiles of organic low dielectric (low-k) films are sensitive to the substrate temperature and density ratio of H and N atoms in the H2/N2 plasma [1]. In this study, we introduced a feedback control of actual substrate temperature and radical density ratio monitored in real time. And then the dependence of etch rates and profiles of organic films have been evaluated based on the substrate temperatures. In this study, organic low-k films were etched by a dual frequency capacitively coupled plasma employing the mixture of H2/N2 gases. A 100-MHz power was supplied to an upper electrode for plasma generation. The Si substrate was electrostatically chucked to a lower electrode biased by supplying a 2-MHz power. To investigate the effects of H and N radical on the etching profile of organic low-k films, absolute H and N atom densities were measured by vacuum ultraviolet absorption spectroscopy [2]. Moreover, using the optical fiber-type low-coherence interferometer [3], substrate temperature has been measured in real time during etching process. From the measurement results, the temperature raised rapidly just after plasma ignition and was gradually saturated. The temporal change of substrate temperature is a crucial issue to control of surface reactions of reactive species. Therefore, by the intervals of on-off of the plasma discharge, the substrate temperature was maintained within ${\pm}1.5^{\circ}C$ from the set value. As a result, the temperatures were kept within $3^{\circ}C$ during the etching process. Then, we etched organic films with line-and-space pattern using this system. The cross-sections of the organic films etched for 50 s with the substrate temperatures at $20^{\circ}C$ and $100^{\circ}C$ were observed by SEM. From the results, they were different in the sidewall profile. It suggests that the reactions on the sidewalls changed according to the substrate temperature. The precise substrate temperature control method with real-time temperature monitoring and intermittent plasma generation was suggested to contribute on realization of fine pattern etching.
In this paper, ZnO:Al thin films with c-axis preferred orientation were prepared on Soda lime glass substrates by RF magnetron sputtering technique. AZO thin film were prepared in order to clarify optimum conditions for growth of the thin film depending upon process, and then by changing a number of deposition conditions and substrate temperature conditions variously, structural and electrical characteristics were measured. For the manufacture of the AZO were vapor-deposited in the named order. It is well-known that post-annealing is an important method to improve crystal quality. For the annealing process, the dislocation nd other defects arise in the material and adsorption/decomposition occurs. The XRD patterns of the AZO films deposited with grey theory prediction design, annealed in a vacuum ambient($2.0{\times}10-3$Torr)at temperatures of 200, 300, 400 and $500^{\circ}C$ for a period of 30min. The diffraction patterns of all the films show the AZO films had a hexagonal wurtzite structure with a preferential orientation along the c-axis perpendicular to the substrate surface. As can be seen, the (002)peak intensities of the AZO films became more intense and sharper when the annealing temperature increased. On the other hand, When the annealing temperature was $500^{\circ}C$ the peak intensity decreased. The surface morphologies and surface toughness of films were examined by atomic force microscopy(AFM, XE-100, PSIA). Electrical resistivity, Gall mobility and carrier concentration were measured by Hall effect measuring system (HL5500PC, Accent optical Technology, USA). The optical absorption spectra of films in the ultraviolet-visibleinfrared( UV-Vis-IR) region were recorder by the UV spectrophotometer(U-3501, Hitachi, Japan). The resistivity, carrier concentration, and Hall mobility of ZnS deposited on glass substrate as a function of post-annealing.
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