• KOREAN JOURNAL OF CROP SCIENCE
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• v.53 no.2
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• pp.224-232
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• 2008

The health benefits associated with tea consumption have resulted in the wide inclusion of green tea extracts in botanical dietary supplements, which are widely consumed as adjuvants for complementary and alternative medicines. Tea contains polyphenols such as catechins or flavan-3-ols including (-)-epicatechin (EC), (-)-epigallocatechin (EGC), (-)-epicatechin gallate (ECG), and (-)-epigallocatechin gallate (EGCG), as well as the alkaloid, caffeine. The contents of catechins and caffeine in green tea are considered as a standard of quality evaluation of green tea. Therefor, the purpose of this study was to investigate the most suitable HPLC condition for simultaneous determination of catechins and caffeine in green tea extracts. The efficient HPLC analytical condition of catechins and caffeine contained green tea extracts was developed. The gradient elution employed a $250\;mm\;{\times}\;4.6\;mm$ i.d. YMC-pak ODS-AM 303 column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of 0.1% aqueous phosphoric acid, and mobile phase B, comprising 100% MeOH, and delivered at a flow rate of 1 mL/min as follows: $0{\sim}25\;min$, 80% A; $26{\sim}50\;min$, $80{\sim}70%$ A; 51 min, 80% A. $51{\sim}55\;min$, 80% A. The UV detection wavelength was set at 280 nm. The limit of detection (LOD) for catechins and caffeine standards were under 50 ng/mL.

• Journal of Pharmaceutical Investigation
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• v.36 no.5
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• pp.331-338
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• 2006

A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.34 no.1
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• pp.57-62
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• 2008

No matter how small amount of heavy metals it may be cause skin allergies through percutaneous adsorption when existing in cosmetic products as impurities. In order to develop a highly sensitive method for simultaneous determination of $Pb^{2+},\;Fe^{2+},\;Cu^{2+},\;Ni^{2+},\;Zn^{2+},\;Co^{2+},\;Cd^{2+},\;and\;Mn^{2+}$ in coloring agents and cosmetic products with rapidity and accuracy, we carried out the determination on ion chromatography. All of these metals are well separated through a bifunctional ion-exchange column(IonPac CS5A) and detected by post-column reaction and spectrophotometric detection. The calibration graphs are linear($r^2>0.999$) in the range $0.1{\sim}1000{\mu}g/mL$. Detection limits for 200 ${\mu}L$ of sample solution are at the level of ${\mu}g/L$, which is sufficient for judging whether the product is safe or not. The relative standard deviations(RSDs) of the retention time and the peak area are less than 0.21 and 1.24%, respectively. The recovery rates are $97{\sim}104%$. The new method was applied to analyze the amount of heavy metals which were contained in 22 cosmetic products and 11 coloring agents.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.3
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• pp.342-351
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• 2016

This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

• The Journal of the Convergence on Culture Technology
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• v.9 no.6
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• pp.867-873
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• 2023

In this study, for the purpose of standardized quality control of a cold medicine, we simultaneous analyzed four main chemical components of a cold medicine: acetaminophen, caffeine, methyl paraben, and propyl paraben. The sample was subjected to quantitative analysis using high performance liquid chromatography (HPLC), after pretreatment of four components. The experiment was carried out by using Isocratic elution at wavelength of 270nm. Acetonitrile and water (H₂O) were used as a mobile phase at a flow rate of 1.0mL/min in a commercial C18 reversed-phase column. A volume of 10uL cold medicine were injected into the column with column oven temperature at 35℃. As a result of the experiment, the values of Resolution were 4.983, 1.596, 5.519, and 1.678 respectively-well over Rs >1.5, which indicates that the separation of four components were efficient. In addition, value of symmetry factor of the components was 1.056, 1.069, 1.032, and 1.133 respectively, to show its symmetrical stability. The calibration curve of all four components exhibits good linearity with R² >0.9995 to 0.9999. Furthermore, the limit of detection(LOD) were between 0.0118 to 1.5973 mg/mL, while the limit of quantification (LOQ) were between 0.0353 to 4.7919 ㎍/mL with the recovery rate of 79.6% ~ 120.5%. The results of this study showed an efficient quality evaluation of a simultaneous analysis method for cold medicine components.

• Journal of Life Science
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• v.23 no.8
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• pp.1025-1031
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• 2013

From a 95% ethanolic extract of H. diffusa, four marker compounds (HD1~HD4) were isolated, which were relatively unique and exist in comparably high contents. The structures of marker compounds were identified as digitolutein (1), 2-hydroxy-3-methylanthraquinone (2), (E/Z)-6-O-p-coumaroyl scandoside methyl ester (4:1 mixture) (3), and (E/Z)-6-O-p-methoxycinnamoyl scandoside methyl ester (4:1 mixture) (4), respectively, on the basis of $^{13}C$ and $^1H$-NMR analyses. The calibration curves of marker compounds showed high linearity, as their correlation coefficient ($R^2$) were in the range of 0.9991~0.9999. In addition, the limit of detection (LOD) and the limit of quantification (LOQ) were $0.03{\sim}0.07{\mu}g/ml$ and $0.099{\sim}0.231{\mu}g/ml$, respectively. The intra-day/inter-day precision and accuracy were 0.23~2.00%/0.25~1.16% and 94.60~108.44%/94.73-110.23%, respectively. The optimal HPLC conditions for the simultaneous quantification of HD1~HD4 were as follows: stationary phase; Merck Chromolith RP-18e ($100{\times}4.6mm$, $5{\mu}m$), column temp.; room temperature, UV detection at 280 nm, flow rate; 2.0 ml/min, injection volume; $10{\mu}l$, mobile phase; start with the mixture of 80% solvent A ($H_2O$ containing 0.5% acetic acid) and 20% solvent B (methanol containing 0.5% acetic acid) and gradually decrease solvent A to 40% in 9 min., then retain this condition to 18 min. Under the HPLC condition, the four marker compounds 1~4 were successfully separated without any interference of other constituents. The results obtained in this study are expected to be helpful for the development of nutraceutics and natural medicines and for the quality control of this plant.

• Journal of Food Hygiene and Safety
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• v.29 no.3
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• pp.234-240
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• 2014

Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

• Korean Journal of Food Science and Technology
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• v.39 no.2
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• pp.114-121
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• 2007

The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

• Korean Journal of Food Science and Technology
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• v.43 no.2
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• pp.125-133
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• 2011

The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.6
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• pp.639-648
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• 2010

The optimal conditions for the analysis of BPA by HPLC-MS/MS was investigated and the ultrasound degradation capacity of the BPA, with the goal to establish the proper directions for analyzing infinitesimal quantities of BPA by HPLC-MS/MS was examined. The MDL and LOQ of BPA analyzed by HPLC-MS/MS were measured 0.13 nM and 1.3 nM respectively, its sensitivity about 620 and 32 times greater than HPLC-UV (MDL: 81.1 nM, LOQ: 811 nM) and FLD (MDL: 4.6 nM, LOQ: 46 nM). In other words, the new method enables the analysis of BPA with the accuracy up to one 1,180th of the amount specified in U.S. EPA guideline for drinking water. Degradation rate of BPA by ultrasound measured over 95% under 580 kHz and 1000 kHz frequency within 30 minutes of treatment, whereas the rate showed some decrease at 28 kHz frequency. At 580 kHz of ultrasound has proven to be the most effective among others at degradation rate and $k_1$ value, so we concluded that this frequency of ultrasound creates hospitable condition for the combined process of degradation by pyrolysis and oxidization. With the addition of 0.01 mM of $CCl_4$, BPA with the initial concentration of 1 ${\mu}M$ was degraded by more than 98% within 30 minutes, the $k_1$ value measured 5 minutes and 30 minutes into the experiment both showed increases by 1.4 and 1.1 times, respectively, compared with BPA without $CCl_4$. It is also found that the main degradation mechanism of BPA by ultrasound is oxidization process by OH radical, based on the fact that the addition of 10 mM of t-BuOH decreased the rate of BPA degradation by around 60%. However, 33% of BPA degradation rate obtained with the addition of t-BuOH implies further degradation done by pyrolysis or other sorts of radical beside OH radical.