• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.26 no.3
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• pp.307-316
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• 2016

Objectives: In general, NIOSH method 5506 is most widely used for the occupational exposure measurement of PAHs, but 2-4 ring PAHs have poor desorption efficiency, especially for a filter. The purpose of this study was to determine a method to increase the desorption efficiency of 16-PAHs using an ultrasonic extraction procedure. Methods: Test samples prepared spiked XAD-2 tubes and PTFE filters in the range of $0.01-1.0{\mu}g/mL$ for desorption efficiency study. Four different extraction solvents, acetonitrile, acetone, tetrahydrofuran and dichloromethane, were tested in order to select the most suitable solvent for the extraction of the 16 PAHs. The addition of dimethyl sulfoxide and sonication time were considered in order to determine the method with the highest extraction efficiency. All samples were made in three sets and analysis was replicated seven times by HPLC. Results: Acetonitrile and acetone were the optimized as an extraction solvent and desorption efficiency of 2-ring PAHs such as naphthalene, acenaphthylene were increased 3~19% with dimethyl sulfoxide for XAD-2. Acetone was the best extraction solvent for PTFE filter and the desorption efficiency was increased 3~13% for 2- to 4-ring PAHs. The optimum sonication time was 60 minutes and desorption efficiency increased with extraction time. Conclusions: As a result, the best extraction solvent was acetone with dimethyl sulfoxide for ultrasonic extraction procedure and the desorption efficiency of this method was better than NIOSH 5506's. This study could be applied as a method for occupational exposure measurement of PAHs.

• Korean Journal of Veterinary Service
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• v.29 no.3
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• pp.317-330
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• 2006

This study was conducted to develop the analytical method about simultaneous determination for synthetic antimicrobials in muscle by high performance liquid chromatography - mass selective detector (HPLC- MSD). Solid phase extraction (SPE), matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) have been adapted as pretreatment procedures for HPLC- MSD. Among various solvent tested, methanol was chosen for extraction of synthetic antimicrobials in muscles. For the optimized response, the values of various MS parameters including fragment voltage, drying gas flow, nebulizer pressure, drying gas temperature were verified. The average recovery rates using MSPD and SPE for muscles of bovine and pork were 78.9-127.1% and 78.3-121.7%, respectively. This method was verified the satisfactory performance for fourteen synthetic antimicrobials excepting carbadox in muscle of pork as detection limit of $0.05{\mu}g/g$ on API/ES SIM mode.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.42 no.1
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• pp.65-73
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• 2016

Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

• 한국생물공학회:학술대회논문집
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• 2005.04a
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• pp.351-354
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• 2005

A new isolation and purification method was developed aiming at increasing yield and purity for homoharringtonine. This method was a simple andefficient procedures, for the isolation and purification of homoharringtonine from Cephalotaxus koreana, consisting of solvent extraction, adsorbent treatment, low-pressure chromatography, and high performance liquid chromatography (HPLC). The crude homoharringtonine was efficiently pre-purified adequately to perform HPLC through a combination withadsorbent treatment and low-pressure chromatogaphy. The homoharringtonine can be simply obtained with high purity and yield from crude homoharringtonine by HPLC. Purified homoharringtonine was characterized.

• YAKHAK HOEJI
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• v.40 no.2
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• pp.149-154
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• 1996

A high-performance liquid chromatographic method for the determination of ${\beta}$-sitosterol in the unsaponifiable fraction of Zea mays L. and its related drug preparations using a cholesterol as an internal standard was investigated. They were saponified with 20% methanolic KOH solution. Phytosterols in the reaction mixture were extracted with diethyl ether and separated on silica gel TLC plate with n-hexane-diethyl ether(40:60) as the solvent and then were scraped off. They were separated by reversed phase high perfomance liquid chromatography on Inertsil ODS-2 column with detection at 205nm. Cholesterol and ${\beta}$-sitosterol were resolved from interferences by adjusting the acetonitrile content in the MeOH-tetrahydrofuran-$H_2O$ eluent. The detection limit of ${\beta$-sitosterol was 0.43${\mu}$g.

• Journal of the East Asian Society of Dietary Life
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• v.5 no.1
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• pp.87-93
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• 1995

The oxidized mixture of lipid(methyl linoleate) and phenolics(phloroglucinol) at 37$^{\circ}C$, 82$m\ell$ O/min., for 9 days were separated each by C cartridge and silica cartridge making use of different eluting solvent. And the oxidation products were analyzed by HPLC. In conclusion, the oxidized mixture were separated into methyl linoleate and phloroglucinol by cartridge on HPLC. and also in this experiment, separated methyl linoleate and phloroglucinol could be analyzed in the common eluant, water and acetonitrile on HPLC. SEP-PAK cartridges were used almost sample purification until now, but under the various eluting solvents and conditions, cartridge will be expected to mini columns which can separate different polarity materials.

• Journal of Food Hygiene and Safety
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• v.10 no.4
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• pp.225.1-230
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• 1995

The ethanol extract from the root bark of Morus alba showed the strongest antimicrobial activity on the growth of almost all the tested microorganisms which were food-borne pathogens and food-related microorganisms. 1) In order to isolate and purify of antimicrobial substance extracted from the root bark of Morus alba, the antimicrobial substance from the ethanol extract which exhibited a strong antimicrobial activity was purified by solvent fractionation, silica gel column chromatography, TLC and HPLC. Among the fractions fractionated by 4 kind of solvents from the ethanol extract, the antimicrobial activity of ethyl acetate fraction had the strongest antimicrobial activity against B. subtilis. Unknown compound were isolated from the ethyl acetate fraction by silica gel column chromatography, TLC and HPLC and the compounds showed strong absorbance at 207, 217 and 285 nm, therefore, it was supposed to be a kinds of aromatic compound.

• Macromolecular Research
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• v.15 no.2
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• pp.134-141
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• 2007

The direct chromatographic separation of enantiomers by chiral stationary phases (CSPs) has been extensively developed over the past two decades, and has now become the most popular method for the analytical and preparative separations of enantiomers. Polysaccharide derivatives coated onto silica gel, as CSPs, playa significantly important role in the enantioseparations of a wide range of chiral compounds using high-performance liquid chromatography (HPLC). Unfortunately, the strict solvent limitation of the mobile phases is the main defect in the method developments of these types of coated CSPs. Therefore, the immobilization of polysaccharide derivatives onto silica gel, via chemical bonding, to obtain a new generation of CSPs compatible with the universal solvents used in HPLC is increasingly important. In this article, our recent studies on the immobilization of polysaccharide derivatives onto the silica gel, as CSPs, through radical copolymerization with various vinyl monomers are reported. Polysaccharide derivatives, with low vinyl content, can be efficiently fixed onto silica gel with high chiral recognition.

• Bulletin of the Korean Chemical Society
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• v.20 no.10
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• pp.1165-1171
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• 1999

The analysis of trace herbicides using the on-line SPE-HPLC system and a photochemical reaction was studied. 18 compounds of herbicides including eight triazines, six phenoxy acids and esters, and four other herbicides were examined. The on-line SPE-HPLC system developed for selection of eluting solvent improved chromatographic efficiency. The recoveries of herbicides were higher than 77%. With 100 mL tap water samples, the detection limits for all analytes were in the 0.1-2.3×10-10 M range. Detection was done by a UV or fluorescence spectrometer after photochemical reaction at the end of the column with 2W or 450W mercury lamp. Without a photochemical reaction, all compounds responded to 230 nm UV detector, but phenoxy acids and esters were weakly detected. However, with a photochemical reaction, these compounds were selectively detected at 320 nm wavelength of UV absorption and 400 nm emission of the fluorescence detectors. This method can be used for the analysis of environmental water containing herbicides at trace levels.

• Bulletin of the Korean Chemical Society
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• v.23 no.1
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• pp.65-70
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• 2002

We have evaluated the specific hydroxyl group-solvent and carbonyl group-solvent interactions by using an Alltima C18 stationary phase and by measuring the retention data of carefully selected solutes in 60/40, 70/30, and 80/20(v/v%) acetonitrile/water eluents at 25, 30, 35, 40, 45, and 50 oC. The selected solutes are phenol, acetophenone, alkylbenznes(benzene to hexylbenznene), 4 positional isomers of phenylbutanol, 5-phenyl-1-pentanol, 3 positional isomers of alkylarylketone derived from butylbenzene, and 1-phenyl-2-hexanone. The magnitudes of hydroxyl group-acetonitrile/water specific interaction enthalpies are larger than those of carbonyl group-acetonitrile/water specific interaction enthalpies in general while the magnitudes of carbonyl group-methanol/water specific interaction enthalpies are larger than those of hydroxyl group-methanol/water specific interactions. We observed clear discrepancies in functional group-solvent specific interaction among positional isomers. The variation trends of solute transfer enthalpies and entropies with mobile phase composition in the acetonitrile/water system are much different from those in the methanol/water system. The well-known pocket formation of acetonitrile in aqueous acetonitrile mixtures has proven to be useful to explain such phenomena.