• Korean Journal of Agricultural Science
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• v.48 no.2
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• pp.343-351
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• 2021

Screening was conducted using 200 kinds of plant extracts to explore herbicide-activated components of plant origin. We separated and purified active substances and elucidated chemical structures using Ligularia stenocephala M., which has strong activity and has not yet been studied. When the solvent fractions of the leaves of Ligularia stenocephala M. were tested for their herbicidal activity, ethyl acetate and chloroform layer showed an inhibition rate of 95.2% and 94.1%, respectively. In particular, the chloroform layer exerted more than 50% herbicidal activity at 10 ppm. From the chloroform layer with the highest herbicidal activity, we isolated three herbicidal active compounds using stepwise chromatography, specifically silica gel or octadecyl silica (ODS) column chromatography, Sep-pak cartridges, and high performance liquid chromatography (HPLC). Based on the analysis of the active compounds using electron ionization mass spectroscopy (EI-MS), ¹H-NMR, and ¹³C-NMR, we identified the active compounds as euparin, 5,6-dimethoxy-2-isopropenylbenzofuran, and liguhodgsonal. When the herbicidal activity of the identified compounds was tested, euparin showed selective herbicidal activity for lettuce at 10^-3 M, and both liguhogsonal and 5,6-dimethoxy-2-isoprophenylbenzofuran exerted selective activity for rice and Echinochloa crus-galli.

• Journal of Microbiology and Biotechnology
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• v.32 no.3
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• pp.302-306
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• 2022

A chemical investigation of a culture extract from Streptomyces sp. RK85-270 led to the isolation and characterization of two new oxindoles, RK-270D (1) and E (2). The structures of 1 and 2 were determined by analyzing spectroscopic and spectrometric data from 1D and 2D NMR and High-resolution electrospray ionization mass spectrometry (HRESIMS) experiments. Compound 1 exhibited anti-angiogenic activities against human umbilical vein endothelial cells (HUVECs) without cytotoxicity. Results of Western blot analysis revealed that 1 inhibits VEGF-induced angiogenesis in the HUVECs via VEGFR2/ p38 MAPK-mediated pathway.

• Analytical Science and Technology
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• v.36 no.6
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• pp.281-290
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• 2023

Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

• YAKHAK HOEJI
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• v.57 no.5
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• pp.330-336
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• 2013

"The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

• Bulletin of the Korean Chemical Society
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• v.33 no.10
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• pp.3285-3292
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• 2012

The interaction of thiazole drug with (6,0) zigzag single-walled boron nitride nanotube of finite length in gas and solvent phases was studied by means of density functional theory (DFT) calculations. In both phases, the binding energy is negative and presenting characterizes an exothermic process. Also, the binding energy in solvent phase is more than that the gas phase. Binding energy corresponding to adsorption of thiazole on the BNNT model in the gas and solvent phases was calculated to be -0.34 and -0.56 eV, and about 0.04 and 0.06 electrons is transferred from the thiazole to the nanotube in the phases. The significantly changes in binding energies and energy gap values by the thiazole adsorption, shows the high sensitivity of the electronic properties of BNNT towards the adsorption of the thiazole molecule. Frontier molecular orbital theory (FMO) and structural analyses show that the low energy level of LUMO, electron density, and length of the surrounding bonds of adsorbing atoms help to the thiazole adsorption on the nanotube. Decrease in global hardness, energy gap and ionization potential is due to the adsorption of the thiazole, and consequently, in the both phases, stability of the thiazole-attached (6,0) BNNT model is decreased and its reactivity increased. Presence of polar solvent increases the electron donor of the thiazole and the electrophilicity of the complex. This study may provide new insight to the development of functionalized boron nitride nanotubes as drug delivery systems for virtual applications.

• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2760-2764
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• 2013

Geniposide is a biologically active ingredient of gardenia fruit. A liquid chromatography-tandem mass spectrometric method was developed and validated for the determination of geniposide in rat plasma. The plasma samples were pretreated by solid-phase extraction and introduced into a BDS Hypersil $C_{18}$ column ($50{\times}2.1mm$, $5{\mu}m$) for chromatographic separation. The mobile phase consisted of 0.1% formic acid and 0.1% formic acid in acetonitrile, and gradient elution was performed at a flow rate of 0.25 mL/min. For mass spectrometric detection, multiple reaction monitoring was performed via an electrospray ionization source in positive mode. The calibration curve for geniposide was linear ($r^2=0.997$) in the concentration range of $0.005-1{\mu}g/mL$. The intra- and inter-day accuracies and precisions fulfilled the required criteria (${\pm}15%$). The developed method was subsequently used for pharmacokinetic analysis of geniposide after oral administration to rats at a dose of 50 mg/kg. The mean maximum plasma concentration of geniposide was $0.68{\pm}0.29{\mu}g/mL$ at $0.44{\pm}0.13h$, and the mean area under the plasma concentration versus time curve was $1.46{\mu}g{\cdot}h/mL$.

• Korean Journal of Medicinal Crop Science
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• v.27 no.6
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• pp.419-426
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• 2019

Background: This study aimed to identify antioxidant compounds from the seeds of Dolichos lablab L. by bioassay-guided isolation and recrystallization. Methods and Results: The water layer of D. lablab L. seed extract inhibits intracellular reactive oxygen species (ROS) expressing the 2',7'-dichlorofluorescein diacetate (DCF-DA), Cu/Zn superoxide dismutase (SOD) and catalase genes, as determined by quantitative real-time PCR (qRT-PCR). Two compounds were purified from the water layer of the seeds of D. lablab L. using column chromatography and prep-high performance liquid chromatography (HPLC). Using nuclear magnetic resonance (NMR) and electrospray Ionization mass spectrometry (ESI-MS), their chemical structures were identified as 5-[(2-acetyl-2,3-dihydro-1H-indazol-1-yl)carbonyl]-4,5-dihydro-3H-furan-2-one (C₁₄H₁₄N₂O₄) and stachyose. Conclusions: Two active antioxidant compounds were purified from the seed extract of D. lablab L. seed extract and the structures of these compounds were identified as C₁₄H₁₄O₄N₂ and stachyose.

• International Journal of Highway Engineering
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• v.17 no.4
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• pp.53-61
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• 2015

PURPOSES : The objective of this study is to evaluate the SDAR (solvent deasphaltene residue), which is obtained from the solvent deasphalting (SDA) process, as a pavement material. METHODS : The physical properties of the SDAR were evaluated based on its chemical composition, and asphalt mixtures with the SDAR were fabricated and used for the evaluation of mechanical properties. Firstly, the chemical composition of SARA (saturate, aromatic, resin and asphaltene) was analyzed using the TLC-FID (thin-layer chromatography-flame ionization detector). Moreover, the basic material properties of the asphalt binder with the SDAR were evaluated by the penetration test, softening point test, ductility test, and PG (performance grade) grade test. The rheological properties of the asphalt binder with the SDAR were evaluated by the dynamic shear modulus ($G^*$) obtained using the time-temperature superposition (TTS) principle. Secondly, the mechanical properties of the asphalt mixtures with the SDAR were evaluated. The compactibility was evaluated using the gyratory compacter. Moreover, the tensile strength ratio (TSR) was used for evaluating the moisture susceptibility of the asphalt mixtures (i.e., susceptibility to pothole damage). The dynamic modulus $E^*$, which is a fundamental property of the asphalt mixture, obtained at different temperatures and loading cycles, was used to evaluate the mechanical properties of the asphalt mixtures. RESULTS AND CONCLUSION : The SDAR shows stiffer and more brittle behavior than the conventional asphalt binder. As the application of the SDAR directly in the field may cause early failures, such as cracks on pavements, it should be applied with modifiers that can favorably modify the brittleness property of the SDAR. Therefore, if appropriate additives are applied on the SDAR, it can be used as a pavement material because of its low cost and strong resistance to rutting.

• Journal of Korean Society for Atmospheric Environment
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• v.19 no.4
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• pp.387-396
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• 2003

A field study was conducted during the summer time of 2002 to determine compositions of volatile organic compounds (VOCs) emitted from vehicles and to develop source emission profiles that is applied to CMB model to estimate the source contribution of certain area. Source emission profile is widely used for the estimation of source contribution by the chemical mass balance model and have to be developed applicable for the target area of estimation. This study was aimed to develop source emission profile and estimation of source contribution of VOCs after application of the chemical mass balance (CMB) receptor model. After considering the emission inventory and other research results for the VOCs in Seoul, Korea, the sources like vehicle emission (tunnel), gas station (gasoline, diesel), solvent usage (painting operation, dry cleaning, graphic art), and gas fuels were selected for the major VOCs sources. Furthermore, ambient air samples were simultaneously collected from 09:00 to 11:00 for four days at eight different official air quality monitoring sites as receptors in Seoul during summer of 2001. Source samples were collected by canisters, and then about seventy volatile organic compounds were analyzed by gas chromatography with flame ionization detector (GC/FID). Based on both the developed source profiles and the database of the receptors, CMB model was intensively applied to estimate mass contribution of VOCs sources. Examining the source profile from the vehicle, the portion of alkanes of VOCs was highest, and then the portion of aromatics such toluene, m/p-xylene were followed. In case of gas fuel. they have their own components; the content of butane, propane, ethane was higher than any other component according to the fuel usage. The average of the source apportionment on VOCs for 8 sites showed that the major sources were vehicle emission and gas fuels. The vehicle emission source was revealed as having the highest contribution with an average of 49.6%, and followed by solvent with 21.3%, gas fuel with 16.1%, gasoline with 13.1%.

• Korean Journal of Food Science and Technology
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• v.43 no.1
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• pp.12-16
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• 2011

This study was conducted to identify the differences in proteomic characteristics between Ca-enriched king oyster mushrooms and general king oyster mushrooms. A combined high-throughput proteomic approach was employed to determine the expression profiles and identity of proteins using 2-dimensional gel electrophoresis and matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF) mass spectrometry. The overall distribution patterns of the proteins were quite similar, but many of the protein spot intensities varied. A total of 10 proteins, representing a significant difference in the quantities of protein betweenthe two types of mushrooms, were successfully identified. Among these proteins, eight kinds were increased in the Ca-enriched king oyster mushrooms and two kinds were decreased. This study showed that proteomic analysis can help define specific changes in protein level and composition, which can occur in mushrooms where Ca content may or may not be enriched.