• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.338-351
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• 2019

BACKGROUND: To investigate distribution and seasonal variation of concentration and flux of pesticides in Han river basin, water samples were examined at 24 sites in 2012 and 2014. METHODS AND RESULTS: Water samples were collected four times per year and subjected to liquid-liquid partition extraction followed by GC-ECD/NPD analysis. Of fifteen pesticides detected, iprobenfos, diazinon, isoprothiolane, endosulfan sulfate and oxadiazon were detected in a higher frequency, while fenoxanil, carbofuran, fenitrothion, butachlor and metolachlor were only detected in a sample. Pesticides with high occurrences, iprobenfos, diazinon, isoprothiolane, endosulfan sulfate and oxadiazon were detected in residue level of 0.01-0.46, 0.01-0.24, 0.03-0.85, 0.02-0.06 and 0.05-0.24 ㎍/L, respectively. Carbofuran and acetanilide herbicides were found at lower frequencies, but their concentrations were one order of magnitude higher than those of the others. CONCLUSION: Discharge of pesticides in downstream area were mainly contributed from rice farming and suburban horticulture, while pesticide occurrences in upstream area, such as Donggang river basin were caused by highland agriculture for cabbage and potato production. Despite the influx of pesticides from tributaries through intensive agriculture areas, pesticide concentration in the main stream water was low due to the dilution effect from the upstream. Therefore, the water quality was considered to be good at the most downstream, the effluent of Paldang dam.

• Korean Journal of Environmental Agriculture
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• v.35 no.3
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• pp.166-174
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• 2016

BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C₁₈ column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R²≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

• Applied Chemistry for Engineering
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• v.8 no.5
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• pp.763-770
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• 1997

The separation of benzene-cyclohexane mixture using (O/W)/O emulsion liquid membrane was studied. The operating parameters which can affect the selectivity, benzene yield, and emulsion size distribution were examined and determined by the batch type operation. The unsteady state and steady state extraction behavior in continuous pulse stirred reactor(CPSR) were verified. The optimum conditions for benzene selectivity and yield in batch operation were as follows; emulsion mixing intensity 4000 rpm, Tween 80 concentration 0.4%, volume ratio of membrane phase to internal phase 0.75, volume ratio of dispersed phase to continuous phase 0.5, and permeation time 10 minutes, As impeller speed increased and the microdrop holdup decreased, the Sauter mean diameter decreased. Turbulence damping parameter of modified Calabrease correlation considering microdrop holdup was 2.28. The optimum conditions of continuous operation were as follows; agitation speed 300 rpm, pulse frequence 2 times/sec, flow rate of continuous phase 30ml/min, and flow rate of emulsion phase 12.0ml/min.

• Applied Biological Chemistry
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• v.50 no.4
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• pp.262-267
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• 2007

To access the natural product antibiotics produced by uncultured microorganisms, six cosmid libraries of DNA extracted directly from soil samples (environmental DNA, eDNA) were constructed and screened for the production of antibacterial active molecules. Of the approximately 60,000 clones screened, one antibacterial clone (YS92B) was detected. Ethyl acetate extracts of clone YS92B showed antibacterial activity against various pathogenic bacteria (Listeria monocytogenes, Bacillus subtilis, Pseudomonas syringae, Xanthomonas campestris pv. oryzae, Staphylococcus epidemis). Active constituents from cultures of YS92B were isolated and purified using a bioassay-guided fractionation against B. subtilis through a series of procedures (ethyl acetate extraction, Sephadex LH20 column chromatography, High Performance Liquid Chromatography). NMR (Nuclear Magnetic Resonance) spectral analysis of a major antibacterial active YS92B-VII indicated that it is a lauric acid linked to tyrosine. This report describes the characterization of antibacterially active long chain N-acyl derivatives of tyrosine that are produced by eDNA clones hosted in Escherichia coli from Korean soils.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.319-326
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• 2016

Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

• Korean Journal of Food Science and Technology
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• v.39 no.2
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• pp.200-208
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• 2007

Fifty-four natural plants from Jeju Island, Korea were extracted by 70% methanol. The extracts containing the highest total phenolic contents (TPC) (>250 mg gallic acid equivalents/g dry sample) were obtained from Ostrya japonica, Geranium thunbergii, Malus sieboldii, Ardisia japonica, and Agrimonia pilosa. DPPH inhibition activity was greatest in Ardisia crenata at 94.1%. A high correlation was observed between DPPH inhibition activity and TPC ($R^2=0.87$). Tyrosinase inhibition activities of more than 85% were obtained from the extracts of Persicaria filiformis, Rhus javanica, Alnus firma, and Myrica rubra. On the other hand, the P. filiformis and M. rubra extracts each showed more than 90% XOD inhibition activity. The five natural plants with the highest biological activities were also extracted by pressurized liquid (PLE, 100% methanol, 13.6 MPa, $40^{\circ}C$). The DPPH and tyrosinase inhibition activities were almost the same in both the 70% methanol and PLE extracts. The $IC_{50}$ for tyrosinase and elastase inhibition activities in PLE were 802 and 88 ppm in A. japonica, and 959 and 66 ppm in M. rubra, respectively.

• Journal of Pharmaceutical Investigation
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• v.39 no.1
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• pp.73-78
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• 2009

A simple LC-MS/MS method of rabeprazole in human plasma was developed and validated. Rabeprazole and Internal standard (I.S), omeprazole, were extracted from human plasma by liquid liquid extraction, chromatographic separation of rabaprazole in plasma was achieved at $45^{\circ}C$ with a Shiseido UG120 $C_{18}$ column and methanol-10 mM ammonium acetate buffer (pH 9.42 with ammonium water), as mobile phase. Rabeprazole produced a protonated precursor ion [$(M+H)^+$] at m/z 360.10 and corresponding product ion at m/z 242.21. Internal standard produced a protonated precursor ion [$(M+H)^+$] at 346.09 and corresponding product ion at m/z 198.09. This method showed linear response over the concentration range of $1{\sim}500\;ng/mL$ with correalation coefficient greater than 0.99. The lower limit of quantitation (LLOQ) using 0.2 mL plasma was 1 ng/mL, which was sensitive enough for pharmacokinetics studies. The method was specific and validated with a limit of quantitation of 1 ng/mL. The intra-day and inter-day precision and accuracy were acceptable for all samples including the LLOQ. The applicability of the method was demonstrated by analysis of plasma after administration of a single 10 mg dose to 36 healthy subject. From the plasma rabeprazole concentration versus time curves, the mean $AUC_t$ (The area under the plasma concentration-time curve from time 0 to 12 hr ) was $691.36{\pm}321.88\;ng{\cdot}hr/mL$, $C_{max}$ (maximum plasma drug concentration) of $353.21{\pm}131.52\;ng/mL$ reached $3.4{\pm}1.1\;hr$ after adiministration. The mean biological half-life of rabeprazole was $1.37{\pm}0.75\;hr$. Based on the results, this simple method could readily be used in pharmacokinetics studies.

• Journal of Food Hygiene and Safety
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• v.23 no.1
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• pp.1-5
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• 2008

The inhibition of cholesterol autoxidation by commercial ${\gamma}$-Oryzanol (0, 50, 100, and 300 ppm) was studied in an aqueous model system for 20 h at pH 5.5 and $80^{\circ}C$. The inhibition effectiveness of the commercial ${\gamma}$-Oryzanol was followed by the retention of cholesterol and the formation of C-7 oxidized cholesterol derivatives (OCDs). Changes in the amount of ${\gamma}$-Oryzanol in the aqueous system were determined during cholesterol autoxidation. A method to detect the levels of 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol and $7{\beta}$-hydroxycholesterol in an aqueous model system with ${\gamma}$-Oryzanol was developed by using the hexane-ethyl acetate extraction system and high-performance liquid chromatography. Results showed that the levels of C-7 OCDs in an aqueous dispersion containing 300 ppm of ${\gamma}$-Oryzanol were not significantly (p>0.05) increased, when compared to other treatments (0, 50, and 100 ppm), during the accelerated cholesterol oxidation.

• Journal of Pharmaceutical Investigation
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• v.35 no.3
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• pp.137-142
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• v.35 no.6
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• pp.437-443
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.