• Toxicological Research
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• v.29 no.3
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• pp.203-209
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• 2013

A simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of ${\varepsilon}$-acetamidocaproic acid (AACA), the primary metabolite of zinc acexamate (ZAC), in rat plasma by using normetanephrine as an internal standard. Sample preparation involved protein precipitation using methanol. Separation was achieved on a Gemini-NX $C_{18}$ column ($150mm{\times}2.0mm$, i.d., 3 ${\mu}m$ particle size) using a mixture of 0.1% formic acid-water : acetonitrile (80 : 20, v/v) as the mobile phase at a flow rate of 200 ${\mu}l/min$. Quantification was performed on a triple quadrupole mass spectrometer employing electrospray ionization and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.0 min, and the calibration curves of AACA were linear over the concentration range of 20~5000 ng/ml in rat plasma. The coefficient of variation and relative error at four QC levels were ranged from 1.0% to 5.8% and from -8.4% to 6.6%, respectively. The present method was successfully applied for estimating the pharmacokinetic parameters of AACA following intravenous or oral administration of ZAC to rats.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.46 no.4
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• pp.309-316
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• 2001

Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

• Archives of Pharmacal Research
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• v.25 no.5
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• pp.647-651
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• 2002

An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard. KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.

• Bulletin of the Korean Chemical Society
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• v.24 no.9
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• pp.1319-1323
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• 2003

This paper presents a successful demonstration of the on-line coupling of MEKC (micellar electrokinetic chromatography) to ESIMS (electrospray ionization mass spectrometry) for the quantitative analysis of seven s-triazine herbicides. The on-line MEKC-ESIMS was used to determine the structure of CE-separated peaks of seven triazine herbicides. The mixture of triazine herbicides was separated in a 20 mM sodium borate buffer (pH 8.5) containing 15 mM sodium dodecylsulfate (SDS) by using a bare fused-silica capillary. Electrospray ionization mass spectrometer was operated in the positive-ion mode when the mass spectra of seven triazine herbicides were observed from each peak, and the solution of water-methanol-formic acid (50/49/1 v/v/v) was used as a sheath liquid. The effects of SDS concentration, the run buffer pH, and the electric field on the separation of seven s-triazine herbicides were investigated. The MEKC-ESIMS detection showed 5 to 10 times higher sensitivity compared to the MEKC-UV detection. In addition, it did not need any pretreatment step.

• Journal of the Korean Ceramic Society
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• v.33 no.9
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• pp.1064-1072
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• 1996

The synthetic conditions and characteristics of ZSM-5 type zeolites (ZSM-5/silicalite) for the preparation of the zeolite composite membranes for gas separation were investigated. ZSM-5 zeolites could be synthesized by the hydrothermal treatment of the mixture of colloidal silica sol aluminum nitrate sodium hydroxide and TPABr at a temperature range of 150-17$0^{\circ}C$ in the autoclave. Silicalties were done from the solution of water glass water and TPABr. Their crystalline structures transformed from orthorhombic to monoclinic from and their pore structures of three-dimensional channels were opened as TPABr filling channels was burned off at the calcination temperature of 50$0^{\circ}C$. The specific surface area of the calcined zeolite was about 360 m3/g and its surface property was hydrophobic. Crystal sizes of ZSM-5 and silicalite were 0.5-1.0${\mu}{\textrm}{m}$ and 8-10${\mu}{\textrm}{m}$ respectively having no change due to the calcination. In particular the shape and the size of the ZSM-5 type zeolite were sensitively varied with silica sources and concentrations of reaction solutions/sols.

• Journal of the Korean Society of Fisheries and Ocean Technology
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• v.32 no.3
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• pp.273-285
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• 1996

Generally, the flow around the ship's hull often appear 3-dimensional separation at the bow and stem, and the vortex by this flow affects greatly the resistance propulsive efficiency and maneuverability of the ship. This study is compared the calculated result based on the streamlines calculation method with the experimental result by oil fIlm method to analyze the patterns and characteristics of the flows around the ship's hull of chine form. DTMB Series 62, 4667-1 vessel was selected as a sample ship of chine form and model ship was painted with the mixture of oil-color, paint, and poly wax at the surface of the vessel and tested in the model towing tank of Inha University. The results obtained in this study are listed briefly as follows ; 1. For the single chine form, after $4\frac{1}{2}$ station the streamlines are crossed at the chine line and the streamlines are converted to the vortex follow the chine line. 2. For the single chine form, the vortex appered increases and severely in and arround the stern. 3. The approximate streamlines for the ship's hull of chine form can be assigned by the use of the Watanabe's basic transformation formular.

• KSBB Journal
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• v.14 no.5
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• pp.633-637
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• 1999

Supercritical fluid of carbon dioxide was used to investigate the effects of its temperature and density on the distribuion coefficients of fatty-acid esters composing fish oil. The distribution coefficient of fatty acid ester was greatly different from each other according to the temperature and density of the supercritical fluid. The possibility of separation of a certain fatty acid from the mixture of fatty acids was tested. The density of the supercritical fluid showing the great differences ofthe distribution coefficients among the fatty acid esters ranged from 0.3 g/mL to 0.4 g/mL. The retrograde condensation took place at high densities of the supercritical fluid.

• Journal of Pharmaceutical Investigation
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• v.29 no.2
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• pp.99-103
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• 1999

Self-Emulsifying System(SES), an isotropic mixture of oil and surfactant which forms oil-in-water emulsion, is expected to improve in vitro drug dissolution and enhance in vivo drug absorption. A poorly water soluble drug, ibu-profen(IBP) was incorporated into the SES to improve absorption, and enhance bioavailability of drug. Medium chain triglyceride, glyceryl tricaprylate(GTC) as an oil, and Tween 85 as a surfactant were used to formulate SES. To characterize SESs with various concentrations of Tween 85, the phase separation and solubility of IBP-SEDDS containing IBP as a function of Tween 85 concentration were conducted, and the particle size was measured using photon correlation spectroscopic method. The SES with optimal concentration of Tween 85(35%(w/w)) was selected based on its high drug loading, small particle size and low surfactant concentration. After an oral administration of IBP-SEDDS and IBP suspension in methyl cellulose equivalent to 40.0 mg/kg to rats, the pharmacokinetic parameters were compared. The $C_{max}(163.17\;vs\;88.82\;{\mu}g/ml)$, $AUC(12897.01\;vs\;8751.13\;{\mu}g\;min/ml)$ and Bioavailability(86.44 vs 58.65%) significantly increased but $T_max(10\;vs\;20\;min)$ was significantly advanced. The current SEDDS containing IBP provide an alternative to improve an oral bio-availability of IBP.

• Bulletin of the Korean Chemical Society
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• v.31 no.8
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• pp.2235-2241
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• 2010

A reverse-phase HPLC method with detection by mass spectrometry is described for the simultaneous determination of doxifluridine and its two active metabolites, 5-fluorouracil (5-FU) and 5-fluorouridine (5-FUrd), in beagle dog plasma. The optimal chromatographic separation was achieved on a Waters $Xterra^{(R)}$ $C_{18}$ column ($4.6{\times}250\;mm$ i.d., $5\;{\mu}m$ particle size) with a mobile phase of 0.1% formic acid in a mixture of 99% methanol and purified water (99:1, v/v). The developed method was validated in beagle dog plasma with a lowest limit of quantification of $0.05\;{\mu}g/mL$ for both doxifluridine and 5-FU, and $0.2\;{\mu}g/mL$ for 5-FUrd. Doxifluridine and its two metabolites were stable under the analysis conditions, and intra- and inter-day accuracies exceeded 92.87%, with a precision variability ${\leq}11.34%$ for each analyte. Additionally, the method for quantifying doxifluridine and its two metabolites, 5-FU and 5-FUrd, in beagle dog plasma was applied successfully to the analysis of pharmacokinetic samples.

• YAKHAK HOEJI
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• v.37 no.1
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• pp.1-8
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• 1993

A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.