• Journal of the Korean Chemical Society
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• v.58 no.6
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• pp.535-542
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• 2014

A simple and efficient preconcentration method was developed using three-phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline). The tetracycline antibiotics were separated simultaneously on a column ($C_8$, $3.0{\times}150mm$, $3{\mu}m$) with high selectivity and sensitivity using gradient elution. Under optimized conditions (extraction solvent, heptanal; pH of donor, 9.0; pH of acceptor, 1.0; stirring speed, 700 rpm; NaCl salt, 0%; and extraction time, 60 min), enrichment factors (EF) were between 5.6 and 22.3. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of $0.08{\sim}0.8{\mu}g/mL$ and $0.4{\sim}1.6{\mu}g/mL$, respectively. The calibration curves were linear within the range of $0.1{\sim}32{\mu}g/mL$ with the square of the correlation coefficient being more than 0.995. The precision (as a relative standard deviation, RSD) and accuracy (as a relative recovery) within working range were 1.3~9.1% and 84~118%, respectively.

• Journal of the Korean Society of Food Science and Nutrition
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• v.32 no.1
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• pp.115-118
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• 2003

This study was conducted to determine optimal extraction condition and free radical scavenging effect of ethanol extracts of Campell Early grape seeds and skins at different temperatures, and of organic solvent fractionated from ethanol extracts of grape seeds and skins. The free radical scavenging effect was tested using 1,1-diphenyl-2-picrylhydrazyl (DPPH) method and expressed as dose required for a 50% reduction of DPPH radical (RC$_{50}$). The extraction yields were increased with increasing the extraction temperature but it was not related with ethanol concentrations. The ethanol extract of grape seeds obtained at 5$0^{\circ}C$ showed the more stronger RC$_{50}$ (16.8 $\mu\textrm{g}$/mL) than those of both 3$0^{\circ}C$ and 78$^{\circ}C$. The ethylacetate fraction obtained from ethanol extract of grape seed showed the strongest RC$_{50}$ (15.4 $\mu\textrm{g}$/mL). Overall, both ethanol extracts and their fractions of grape seeds showed significantly stronger free radical scavenging effect than those of skin extracts.racts.

• Journal of the Korean Society of Food Science and Nutrition
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• v.36 no.7
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• pp.813-818
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• 2007

For this study, extracts of Vitex rotundifolia stems were prepared using reflux water extraction (WE), reflux ethanol extraction (EE) and hot water extract under high pressure (HWE). The extracts were investigated for the total content of phenolic compounds, antioxidant activities, and inhibitory potencies for xanthine oxidase and tyrosinase. The EE extraction method yielded the highest content of polyphenol compounds (176.34 mg/g). The electron donating abilities (EDA) were 93.46${\sim}$96.92%, when extracts were assayed at 1.0 mg/mL. The superoxide dismutase (SOD)-like activity was the highest in the WE extract (47.32% at 1.0 mg/mL). The nitrite scavenging abilities (pH 1.2) were 84.61${\sim}$88.36% and the inhibition of xanthine oxidase were over 90% at 0.5 mg/mL. Tyrosinase inhibition of HWE and WE were 57.84% and 53.47% respectively. It implies that V. rotundifolia stems have potent physiological activities and their activities were differently exhibited depending on solvent fractions.

• Korean Journal of Organic Agriculture
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• v.28 no.4
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• pp.591-604
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• 2020

The objectives of this study were to find out the best condition of extracting methods of limonene from citron and to determine effects of limonene on immune modulation activity by measuring cytokine secretion using RAW 264.7 mouse macrophage cells. When distilled water was used as a solvent instead of organic solvents to extract limonene from citron, addition of refluxing process to simultaneous steam distillation extraction method was found to be much effective in extracting limonene. However, it required longer extraction time than using other organic solvents. Limonene extracts showed increased IL-β and IL-6 but decreased the TNF-α gene expression in limonene concentration dependant manner. However oral administration of limonene extracts to mice did not influence significantly compared to control in in vivo experiment. It might be due to that the mice were kept in well controlled and complete environment. Limonene, a natural material from citron has been approved to have a immune-modulation activity in the present study and have a potential as a feed additive that is environmentally friendly and no harmful. Further study with protected limonene, for example, for the protection of limonene from oxidation or bypass the ruminal degradation in order consequently to increase immune-modulation activity might be useful as a further research.

• Journal of Life Science
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• v.34 no.6
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• pp.393-398
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• 2024

The purpose of this study was to verify the antifungal properties of various herbal medicines belonging to the Ranunculaceae family and to find an extraction method effective in inhibiting fungal growth. When antifungal activity was measured in a liquid medium with extracts obtained by either hot water extraction or organic solvent extraction of the herbal medicines Clematis apiifolia, Coptis chinensis, and Pusatilla chinensis, effective results were obtained from the chloroform extract. In addition, fungal growth inhibition experiments were performed on unicellular fungi, Candida albicans, Candida tropicalis, and Candida lusitaniae, and on filamentous fungi, such as Pythium ultimum, Aspergillus fumigatus, and Fusarium oxysporum, using disk diffusion experiments on solid media. It was confirmed that P. chinensis extract has excellent antifungal properties against Candida spp. and C. apiifolia extract against filamentous mold. Finally, GC-MS analysis was performed to explore the useful antifungal substances present in the extract. As a result of the study, thurbergenone from C. apiifolia and 16-hydroxycleroda-3, 13(14)-dien-15, 16-olide (16-HCDO) from C. chinensis were confirmed as antifungal candidates. In conclusion, it was confirmed that C. apiifolia, C. chinensis, and P. chinensis have antifungal activity against various fungi, and in GC-MS analysis, all herbal medicines were confirmed to have different antifungal candidates. These results indicate that the Ranunculaceae family has evolved in several directions for fungal resistance traits.

• Journal of the Korean Chemical Society
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• v.37 no.5
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• pp.513-522
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• 1993

The purpose of this study is to optimize the selectivity of mobile phase solvents for separation of 25 phenols in reversed phase liquid chromatography and to accomplish the simultaneous preconcentration and separation of trace phenols from water samples. Phenols used in this study were classified into three groups, chloro-, methyl-, and nitrophenols. Quaternary solvent mobile phases were employed to improve the selectivity. Overlapping resolution maps(ORM) as a statistical simplex techniques was used to predict the optimum solvent system. Additional criterion such as pH and temperature were also investigated. In order to improve the resolution and decrease the analysis time, isoselective multisolvent gradient elution system was employed with ORM-Prism method. The simultaneous preconcentration and separation of trace phenols from water samples were performed by using XAD-2/Dowex 1-X8 tandem column. When the extraction efficiency was evaluated by sampling up to 1 L of distilled water, recovery of the phenols, except phenol, was above 90% and the limit of detection of the phenols was 5 ppb. The XAD-2/Dowex 1-X8 method was superior to C18 cartridge in terms of recovery and selectivity.

• Analytical Science and Technology
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• v.15 no.5
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• pp.466-474
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• 2002

The analytical method of 14 kinds of coplanar - PCBs was established and applied the soil sample. The three kinds of extraction solvents (toluene, acetone: n-hexane, dichloromethane) were selected to apply the soil sample. The silica gel, florisil and alumina column cleanup also performed to compare the elution recovery. The average recovery of selected solvents in soil A, B and C was surveyed the 84.25%, 56.09% and 44.69% for toluene, 52.56%, 81.42% and 58.53% for acetone : n - hexane and 55.94%, 71.33% and 61.05% for dichloromethane. The average recovery is represented 49.99% for silica gel (n - hexane 100 mL), 69.65% for florisil (6% ether/n - hexane 100 mL), and 65.23% for alumina (2% DCM : n - hexane 100 mL, 50% DCM: n-hexane 150 mL). In silica gel (n - hexane) and florisil (6% ether : n - hexane) cleanup, the 14 kinds of coplanar PCBs eluted until 40 mL. In the silica gel and florisil columns cleanup, the amounts of elution solvent can be reduced from these results, but the researcher has to confirm the elution amounts before performing the experiments. In alumina cleanup process, the result was obtained to the 100 mL of elution solvents (2% DCM: n-hexane 100 mL and 50% DCM: n-hexane 40 mL), therefore the change of elution solvent is necessary to develop the simple procedure.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.9 no.1
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• pp.23-40
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• 1999

The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

• Journal of Conservation Science
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• v.31 no.2
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• pp.95-104
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• 2015

Excavated archaeological cast iron objects in improper storage are quickly corroded and disintegrated into block and powder finally. Hence desalination treatment which is a way of removing internal corrosive factors, especially chloride ion, is an important process. But desalination is often omitted or objects are dehydrated by alcohol because the destruction of objects could occur during desalting. Although current desalting methods mostly use an aqueous alkali solution, $OH^-$ ions of water could accelerate corrosion and broaden internal cracks cause of high surface tension. Therefore this study experimented desalting using ethyl alcohol, which is low surface tension, to investigate an effect of desalination. As a result, desalting using ethyl alcohol showed the similar or more effective results of desalting using water. In addition, as aspects of desalting safety, ethyl alcohol desalting method was smaller destruction of objects and extraction of Fe from the objects than the aqueous alkali solution. However, this study explored the possibility of desalting methods using organic solvent in fieldwork, so the results would provide basic date for making the safe and effective desalting method for archaeological cast iron objects through further experiments.

• Analytical Science and Technology
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• v.16 no.1
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• pp.48-58
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• 2003

The effects of physico-chemical properties of soils on PCBs analysis in Korea was studied Three kinds of extraction solvents(toluene, acetone:hexane, dichloromethane) was selected to apply three different soils. The silicagel, florisil and alumina column cleanup also performed to compare the elution patterns, and three different methods (EPA, Japan, Proposed method in this study) of 62 PCBs also compared the individual peaks recoveries. The solvent average recovery was surveyed the order of toluene, acetone:hexane, dichloromethane as 77.94%, 58.59%, 54.20% for soil A, 53.65%, 80.32%, 68.27% for soil B and 44.52%, 60.35%, 56.36% for soil C, respectively. The average recovery was depended on the soil characters. The highest recoveries of each soil were obtained the toluene for soil A, acetone:hexane for soil B and C. However, the coplanar PCBs was obtained the highest recovery with dichloromethane. Thus, to select the solvent for the analysis of PCBs in solid, the selected compounds have to consider to get good result. The silicagel, florisil, alumina I and alumina II column cleanup process were surveyed the range of 38.73%~98.26%, and the higher chlorinated compounds was obtained the lower recovery compared to the low chlorinated compounds, generally. This results are also consistent with the coplanar PCBs isomers. The compared results of three different countries were obtained the 37.15% for USA, 45.92% for Japan and 44.46% for proposed method in this study.