• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Korean Journal of Weed Science
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• v.30 no.4
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• pp.361-370
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• 2010

This study was carried out to establish the analytical method of MCPA residue in brown rice and rice straw by HPLC/UVD. When MCPA was extracted from sample under the pH 3.6 by adding acetone 200 mL and 1N-HCl 100 mL, the extraction efficiency was high by 87%. And purification efficiency was high by 83% when 5 mL of 1% methanol/acetonitrile was eluated by the florisil Sep-pak cartridge column. From spiking of $0.1{\mu}g\;mL^{-1}$ and $0.25{\mu}g\;mL^{-1}$ of MCPA to control sample, respectively, average recovery rate of MCPA in brown rice was 96.0% and 94.9% and that in rice straw was 92.5% and 88.2%, respectively. Precision of experiment was very high by relative standard deviation of 1.5% to 5.7%. In brown rice and rice straw treated with bentazone+MCPA (11+1.2%) of 30 kg and 60 kg per ha at 30 days after rice transplanting, respectively, maximum residue limit was under $0.05{\mu}g\;mL^{-1}$ of the recommended rate of Korean Food and Drug Administration. From the above results, the analytical procedure of MCPA in plants such as hydrolysis, saponification and derivatization were ommited, and retention time was faster and recovery rate was higher than the existed results of HPLC/UVD. Therefore, these results were greatly improved and seemed to be usefully applied for residue analysis of MCPA in plants.

• Korean Chemical Engineering Research
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• v.44 no.1
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• pp.65-72
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• 2006

Recent technical advances in the biorecognition engineering and the microparticle fabrication may enable us to develop the single step purification using magnetic particle, because of its simplicity, efficacy, ease of automation, and process economics. In this study, we used commercial magnetic particles from Seradyn, Inc. (Indianapolis, USA). It was ca. 2.8 micron in diameter, consisted of polystyrene core and magnetite coating, and its surface had carboxyl groups. The model, capture protein was IgG and anti-IgG was used as the ligand molecule. We studied the different surfaces ('nude', ester-activated, and anti-IgG coated) for their biorecognition of IgG. At a high pH condition, we could reduce non-specific binding. Also anti-IgG immobilized magnetic particle could capture IgG more selectively. We attempted 'oriented immobilization' of anti-IgG, in which the polysaccharides moiety near the C-terminus was selectively oxidized and linked to the hydrazine-coated MP, to improve the efficacy of biorecognitive binding. Using this method, the IgG capturing ability was improved by ca. 2 fold. From the binary mixture of the IgG-insulin, IgG could be more selectively captured. In summary, the oriented immobilization of oxidized anti-IgG proved to be as effective as the streptavidin-biotin system and yet simpler and cost-effective. This immobilization method can find its applications in protein biochips and biotargeting.

• Journal of the Mineralogical Society of Korea
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• v.16 no.2
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• pp.135-149
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• 2003

Domestic zeolite ores are mostly composed of Ca-type clinoptilolite, accompanying a little amounts of mordenite. However, other types of zeolite ores rich in ferrierite, heulandite, or mordenite are less commonly found. Based on the quantitative XRD analysis, zeolite contents are determined to be nearly 50∼90 wt%. Impurities (mostly ＞ 10 wt%) in the zeolite ores chiefly consist of quartz, feldspar, smectite, and opal-CT. The determined CEC values ($CEC_{AA}$ ) of powdery samples (grain size: < 125 $\mu\textrm{m}$) of zeolite ores by the Ammonium Acetate method are mostly higher than 100 meq/100 g. Some zeolites from the Guryongpo area, corresponding to the clinoptilolite ore, are measured to be dominantly high in CEC values ranging 170∼190 meq/100 g. Cation exchange property of the zeolite ores varies greatly depending on the types or zeolite species present in the ores. Despite of the lower grade in zeolite content, the $CEC_{AA}$ of ferrierite ore is comparatively high. Compared to this, the $CEC_{AA }$ of heulandite ore is very low, though the zeolite ore exhibits the highest grade ranging up to about 90 wt%. In addition, the CEC values calculated theoretically from the framework composition of clinoptilolite-heulandite series are not consistent with those determined by the cation exchage experiment. The measured $CEC_{AA}$ of clinoptilolite ores are generally higher than those of heulandite ores. This may be due to the higher Ca abundance in exchangeable cation composition and the presence of probable stacking faults in heulandite. The variation of $CEC_{CEC}$ is roughly proportional, though not strictly compatible, to the zeolite contents in clinoptilolite ores. It seems to be caused by the fact that the $CEC_{AA}$ of clinoptilolite locally varies depending on crystal-chemical diversity, i. e., the variation in framework composition (Si/Al) and exchangeable cation composition (especially, the contents of Ca and K). In addition, the determined CEC values ($CEC_{MB}$ ) of zeolite ores by the Methylene Blue method are much higher than those calculated from smectite contents. It suggests a probable reaction of Methylene Blue ion ($C_{16}$ $H_{18}$ $N_3$S+) with larger-pore zeolites than clinoptlolite-heulandite series, i.e., ferrierite and mordenite as well as with smectite. This can be supported by the fact that the ferrierite ore accompanying little amount of smectite has the highest value in CE $C_{MB}$ .

• Clean Technology
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• v.11 no.3
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• pp.123-128
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• 2005

Among various metal oxides semiconductors, $TiO_2$ is the most studied semiconductor for environmental clean-up applications due to its unique ability in photocatalyzing various organic contaminants, its chemical inertness, and nontoxicity. $TiO_2$, however, has a few drawbacks to be solved such as reactivity mainly working under ultraviolet irradiation (${\lambda}$ < 387 nm) and electron - hole recombination on $TiO_2$. In this study, to extend the absorption range of $TiO_2$ into the visible range and enhance electron - hole separation, we synthesized platinum (Pt) deposited $C-TiO_2$. The presence of Pt as an electron sink has been known to snhance the separation of photogenerated electron-hole pairs and induce the thermal decomposition. The characterization of as-synthesized $Pt-C-TiO_2$ was performed by Transmission Electron Microscopic (TEM), the Brunuer-Emmett-Teller (BET) method, X-ray Diffractometer (XRD), UV-vis spectrometer (UV-DRS), and X-ray Photoelectron Spectroscopy (XPS). In order to estimate the photocatalytic activity of the synthesized materials, the photoelectron Spectroscopy (XPS). In order to estimate the photocatalytic activity of the synthesized materials, the photodegradation experiment of an azo dye (Acid Red 44; $C_{10}H_7N=NC_{10}H_3(SO_3Na)_2OH$)was carried out by using an Xe arc lamp (300 W, Oriel). A 420 nm cut-off filter was used for visible light irradiation. From the results, Pt-deposited $C-TiO_2$ showed a far superior phothdegradation activity to Degussa P25, the commercial product under the irradiation of visible light and enhanced photocatalytic activity of visible-working $C-TiO_2$. This is a useful result into the application for the purification system of dye wastewater using visible energy of sun light.

• Journal of Food Hygiene and Safety
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• v.33 no.3
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• pp.176-184
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• 2018

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

• Tuberculosis and Respiratory Diseases
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• v.44 no.3
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• pp.601-610
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• 1997

Background : Monocytes/macrophages play a central role in determining the host response during Gram-negative infection through secretion of a variety of mediators after stimulation of LPS. Even though cytokine production has been shown to play an important role in host defense during sepsis, cytokine release may also lead to tissue injury. Thus, regulation of macrophage response to LPS is critical for host survival during Gram-negative sepsis. In animals exposed to nonlethal doses of endotoxin, a characteristic hyporesponsiveness to subsequent administration of endotoxin has been observed. This phenomenon was known as 'LPS tolerance'. However, little information is available regarding the underlying mechanism of LPS tolerance. Method : Peripheral blood monocyte(PBMC) was isolated from peripheral blood of normal volunteers by adhesion purification method. To evaluate the conditions to obtain LPS tolerance, preculture was carried out with LPS at 10ng/ml for 24 hours. For stimulation, culture plates were washed two times and were stimulated with LPS at $1{\mu}g/ml$ for 4, 6 and 26 hours. To assess the underlying mechanisms of LPS tolerance, autologous serum, PMA, anti-CD14 Ab, Indomethacin or $PGF_2$ were added to preculture solution respectively. Cytokine concentrations in culture supernatants were measured using ELISA for TNF-$\alpha$ and IL-8 and mRNA of TNF-$\alpha$ and IL-8 were determined by Northern blot analysis. Results : The exposure of PBMC to low dose of LPS suppressed the cytokine production and mRNA expression of TNF-$\alpha$, but not IL-8. Anti-CD14 Ab partially recovered production of TNF-$\alpha$ which was suppressed by preculture with low dose LPS. The preculture with PMA induces LPS tolerance, as preculture with low dose LPS. Conclusion : LPS tolerance to TNF-$\alpha$ is regulated pretranslationally and is influenced by protein kinase C pathway and CD14.

• Korean Journal of Microbiology
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• v.38 no.3
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• pp.153-161
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• 2002

Sox4, a transcription factor, consists of three functional domains: an HMG-box domain as a DNA binding domain, serine rich region as a transactivation domain and glycine rich region (GRR), an unknown functional domain. Although Sox4 is known to be functionally involved in heart, B-cell and reproductive system development, its physiological function remains to be elucidated. We used pGEX expression system to develop a simple and rapid method for purifying Sox4 protein in suitable forms for biochemical studies of their functions. Unexpectedly, we observed that full-length Sox4 appears to be protease-sensitive during expression and purification in E. coli. To map the protease-sensitive site in Sox4, we generated various constructs with each of functional domains of Sox4 and purified as the GST-Sox4 fusion proteins using glutathione beads. We found that the specific cleavage site for the proteolytic enzyme, which exists in E. coli, is localized within the novel GRR of Sox4. Our study suggest that the GRR of Sox4 may a target for the cellular protease action and this cleavage in the GRR may be involved in regulating physiological function of Sox4. Additionally, our study may provide a useful method for investigating the proteolytic cleavage of the target molecule in E. coli.

• Korean Journal of Soil Science and Fertilizer
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• v.44 no.3
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• pp.425-433
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• 2011

In order to obtain optimum pre-treatment methods and improve T-N and T-P removal efficiencies, removal rates of pollutants in small-scale livestock wastewater treatment apparatus with water plant filtration bed or activated sludge tank were investigated. Based on the results from the optimum pre-treatment in small-scale livestock wastewater treatment apparatus, removal efficiencies of pollutants in livestock wastewater treatment plant with water plant filtration and activated sludge beds. The removal rates of COD, SS, T-N, and T-P in effluent were 83, 89, 63 and 87% in small-scale livestock wastewater treatment apparatus with water plant filtration bed, respectively. The removal rates of COD, SS, T-N, and T-P in effluent were 96, 95, 86 and 92% in small-scale livestock wastewater treatment apparatus with activated sludge tank, respectively. For increasing the COD, SS, T-N, and T-P removals in small-scale livestock wastewater treatment apparatus, the water plant filtration and activated sludge beds are recommended. In livestock wastewater treatment plant with water plant filtration ($1^{st}$ treatment) and activated sludge ($2^{nd}$ treatment) beds, the concentrations of COD, SS, T-N, and T-P in effluent were 39, 15, 42 and $1mg\;L^{-1}$, respectively. It was shown that the concentrations of COD, SS, T-N, and T-P met acceptable effluent quality standard for livestock wastewater. Based on the above results, the removal rates of COD, SS, T-N, and T-P in effluent were over 99.8, 99.9, 99.2, and 99.9% in livestock wastewater treatment plant, respectively.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.1
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• pp.8-15
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• 2021

TiO2 has been used in various fields such as solar cells, dental implants, and photocatalysis, because it has high physical and chemical stability and is harmless to the body. TiO2 nanofibers which have a large specific surface area also show a good reactivity in bio-friendly products and excellent photocatalysis in air and water purification. To fabricate TiO2 nanofibers, an electrospinning method was used. To observe the diameter of TiO2 nanofibers with fabrication variables, the fabrication variables was divided into precursor composition variables and process variables and microstructure was analyzed. The concentrations of PVP (Polyvinylpyrrolidone) and TTIP (Titanium(IV) isopropoxide) were selected as precursor composition variables, and inflow velocity and voltage were also selected as process variables. Microstructure and crystal structure of TiO2 nanofibers were analyzed using FE-SEM (Field emission scanning electron microscope) and XRD (X-ray diffraction), respectively. As-spun TiO2 nanofibers with an average diameter of about 0.27 ㎛ to 1.31 ㎛ were transformed to anatase TiO2 nanofibers with an average diameter of about 0.22 ㎛ to 0.78 ㎛ after heat treatment of 3 hours at 450℃. Anatase TiO2 nanofibers with an average diameter of 0.22 ㎛ can be expected to improve the photocatalytic properties by increasing the specific surface area. To change the average diameter of TiO2 nanofibers, the control of precursor composition variables such as concentrations of PVP and TTIP is more efficient than the control of electrospinning process variables such as inflow velocity and voltage.