• The Korean Journal of Food And Nutrition
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• v.31 no.1
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• pp.104-108
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• 2018

The purpose of this study was to establish valerenic acid as a marker compound for the standardization of ethanol extract of Valerinan officinalis (valerian) root as a functional health food. We established valerenic acid as a marker compound using HPLC. HPLC was used to quantify the marker compound in the valerian extract after validation of methods with linearity, accuracy, and precision. The specificity for retention time was met by comparative analysis of the valerian extract and standard compound using HPLC. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The limit of quantification (LOQ) was $10{\mu}g/mL$. The accuracy of measurement was 99.88~00.68% and the relative standard deviation (RSD) value was 0.59%. In addition, our analytical method yielded a 29% mean content of valerenic acid in the valerian ethanol extract. These results indicate that the established HPLC method facilitated the determination of marker compounds in the valerian extract for the standardization of health functional foods.

• Food Science of Animal Resources
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• v.23 no.4
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• pp.356-360
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• 2003

The purpose of this paper was to determine the quantity of selenium in milk by inductively coupled plasma optical emission spectrometry. The sample was digested in teflon vessel containing nitric-hydrogen peroxide acid mixture. After digestion, the sample is treated with additional hydrochloric acid. Total selenium was reduced with sodium borohydride and concentrated hydrochloric acid in a simplified hydride generation(HG) manifold. The optimum conditions of HG are 2 M for HCl, 1.5％ for NaBH$_4$, 1.2 mL/mim for sample flow. Recovery rates by the standard addition method were 88.0％ at 10 ppb and 92.2％ at 10 ppm. The relative standard deviations were 4.8 and 3.2％, respectively. This method showed a good accuracy and precision. And so it was highly suitable for determination of small quantity of selenium in milk.

• Journal of Korean Medicine Rehabilitation
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• v.19 no.2
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• pp.157-185
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• 2009

Objectives : The aim of this study is to suggest approach of oriental medical management and necessity by research of eastern and western medical literatures for Complex Regional Pain Syndrome(CRPS). Methods : We reviewed the clinical and experimental literatures of eastern and western concerned with CRPS which is related causation, signs and symptoms, diagnosis, etiology and management. Results : 1. CRPS is divided into type I and II by nerve injury. Two types of CRPS have been recognized: type I, corresponds to RSD and occurs without a definable nerve lesion, and type II, formerly called causalgia refers to cases where a definable nerve lesion is present. These conditions can be charaterized clinically by the sensory abnormalities, vascular abnormalities, oedema, sweating abnormalities, motor or trophic changes. 2. CRPS are well known to patients and physicians relatively, but the pathophysiology, causation and treatments are still unclear. 3. CRPS is needed to take the early diagnosis and multidisciplinary approach for significant effect. 4. CRPS can be regarded for obstruction syndrome of Ki and blood(痺證), blood stasis(瘀血), Wei symptom(痿證), numbness(痲木) in the oriental medical management of CRPS. Conclusions : Above the results, it is suggested that further studies and active approach of management of CRPS will be conducted precisely in oriental medicine.

• Bulletin of the Korean Chemical Society
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• v.33 no.1
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• pp.105-110
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• 2012

A europium (III)-sensitized, spectrofluorimetric (FL) method is presented for the determination of sparfloxacin (SPAR) using an anionic surfactant, sodium dodecyl benzene sulphonate (SDBS). The method is based on the strong fluorescence (FL) enhancement of SPAR after the addition of $Eu^{3+}$ ions as fluorescence probes. The experimental results indicated that the FL intensity of the SPAR-$Eu^{3+}$ system was enhanced markedly by SDBS. The maximum FL emission signal was obtained at about 615 nm when excited at 372 nm. The experimental conditions that affected the FL intensity of the SPAR-$Eu^{3+}$-SDBS system were optimized systematically. The enhanced FL intensity of the system exhibited a good linear relationship with the SPAR concentration over the range of $1.5{\times}10^{-9}-1.2{\times}10^{-7}mol\;L^{-1}$ with a correlation coefficient (r) of 0.9987. The limit of detection ($3{\delta}$) was $4.15{\times}10^{-10}mol\;L^{-1}$ with a relative standard deviation (RSD) of 1.65%. This method was successfully applied for the determination of SPAR in pharmaceuticals, and human serum and urine samples with higher sensitivity, wide dynamic range and better stability. The possible interaction mechanism of the system is also discussed in detail by ultraviolet absorption spectra and FL spectra.

• Bulletin of the Korean Chemical Society
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• v.33 no.1
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• pp.177-182
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• 2012

A new composition of standardized Scutellariae Radix extract (HPO12) was developed for treatment of Alzheimer's disease. For the preclinical pharmacokinetic study of HPO12, a rapid, sensitive, and selective LCMS/MS method was developed and validated for the simultaneous determination of 4 bioactive compounds, baicalein, baicalin, wogonin, and wogonoside. After extraction with ethylacetate, chromatographic analysis was performed on a Thermo $C_{18}$ column ($150mm{\times}2.1mm$, $3{\mu}m$) with a mobile phase consisting of 0.1% formic acid (A) and 0.1% formic acid in 95% acetonitrile (B) by using gradient elution at a flow rate of $250{\mu}L/min$. Analytes introduced to a mass spectrometer were monitored by multiple reaction monitoring (MRM) in positive ion mode. Using $25{\mu}L$ of plasma sample, the method was validated over the following concentration ranges: 25-5000 ng/mL for baicalein, 20-40000 ng/mL for baicalin, 1-1000 ng/mL for wogonin, and 5-10000 ng/mL for wogonoside. The intra- and inter-day precision and accuracy of the quality control samples at the 4 concentrations showed $\leq$ 13.7% relative standard deviation (RSD) and 86.6-105.5% accuracy. The method was successfully applied to determine the concentrations of baicalein, baicalin, wogonin, and wogonoside in rat plasma after intraperitoneal and oral administrations of HPO12.

• Bulletin of the Korean Chemical Society
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• v.35 no.10
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• pp.2995-3000
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• 2014

A sensitive concentration method utilising modified gas-purge microsyringe extraction (GP-MSE) was developed. Concentration (reduction in volume) to a microlitre volume was achieved. PAHs were utilised as semivolatile analytes to optimise the various parameters that affect the concentration efficiency. The injection rate and temperature were the key factors that affected the concentration efficiency. An efficient concentration (75.0-96.1%) of PAHs was obtained under the optimised conditions. The method exhibited good reproducibility (RSD values that ranged from 1.5 to 9.0%). The GP-MSE concentration method enhances the volume reduction (concentration factor), leading to a low method detection limit ($0.5-15ngL^{-1}$). Furthermore, this method offers the advantage of small-volume sampling, enabling even the detection of diurnal hourly changes in the concentration of PAHs in ambient air. Utilising this method in combination with GC-MS, the diurnal hourly flux of PAHs from the gas phase of ambient air was measured. Indeed, the proposed technique is a simple, fast, low-cost and environmentally friendly.

• Bulletin of the Korean Chemical Society
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• v.34 no.11
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• pp.3444-3450
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• 2013

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

• Bulletin of the Korean Chemical Society
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• v.35 no.2
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• pp.371-376
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• 2014

A novel three-phase hollow fiber liquid phase microextraction was developed for the determination of malachite green (MG) in environmental waters, which selected [BMIM][$PF_6$] mixed with 1% trioctylphosphine oxide (TOPO) as supported phase. Several parameters (accepter phase pH, sample pH, supported phase membrane, volume of accepter phase, salinity, extraction time) that could affect extraction performance were investigated. Under the optimal extraction conditions, the established approach showed excellent characters as: high enrichment factor (212), wide linear range ($0.20-100{\mu}gL^{-1}$), low detection limit ($0.01{\mu}gL^{-1}$), good reproducibility (RSD, 8.9%, n=5) and satisfactory recovery (84.0-106.2%). The method was applied to detect MG at Yangtze River and pond waters in Zhenjiang, Jiangsu province, and 4 sites among 15 sampling sites were found MG with the concentration of $1.73-11.06{\mu}gL^{-1}$, which confirmed that the proposed environmentally friendly method was simple and effective for monitoring MG in aquatic system.

• Bulletin of the Korean Chemical Society
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• v.24 no.12
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• pp.1775-1780
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• 2003

A continuous flow system has been developed to determine trace Cu(II), Mn(II), Ni(II) and Zn(II) in a large volume of water samples by a solvent sublation technique. The mixed solution of 1,10-phenanthroline(phen) and thiocyanate ion was used as ligands for the formation of their ternary complexes. The continuous system was constructed in this laboratory with a peristaltic pump, a mini shaker, three mixing bottles and a flotation cell by connecting each part with a polyethylene tube. The flotation conditions such as the flow rate of sample solution and the injection rates of ligand, buffer and surfactant solutions have been investigated to obtain the best sublation efficiencies. Each solution flowed into the flotation cell through each polyethylene tube by the peristaltic pumps. The ternary complexes were floated and extracted into MIBK in a flotation cell of 2 L by bubbling a nitrogen gas. The absorbances of extracted analytes in MIBK were directly measured by graphite furnace-AAS. The concentrations of 1,10-phenanthroline and thiocyanate ion were $2.6\;{\times}\;10^{-3}$ M and $2.3\;{\times}\;10^{-2}$ M in the mixed solution, respectively. The pH of sample solution was adjusted to 5.0 with a buffer solution and 1%(m/v) sodium lauryl sulphate solution was added as a surfactant to support the effective flotation of the complexes. The $N_2$ gas was bubbled at 30 mL/min for 90 minutes for 20 L of sample. Reproducible results of less than 10% RSD and recoveries of 80-120% could be obtained in real samples.

• Bulletin of the Korean Chemical Society
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• v.32 no.3
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• pp.829-835
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• 2011

A dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) has been developed as a new approach for the extraction of trace copper in water and beverage samples followed by the determination with flame atomic absorption spectrometry. In the DLLME-SFO, 8-hydroxy quinoline, 1-dodecanol, and methanol were used as chelating agent, extraction solvent and dispersive solvent, respectively. The experimental parameters related to the DLLME-SFO such as the type and volume of the extraction and dispersive solvent, extraction time, sample volume, the concentration of chelating agent and salt addition were investigated and optimized. Under the optimum conditions, the enrichment factor for copper was 122. The method was linear in the range from 0.5 to $300\;ng\;mL^{-1}$ of copper in the samples with a correlation coefficient (r) of 0.9996 and a limit of detection of $0.1\;ng\;mL^{-1}$. The method was applied to the determination of copper in water and beverage samples. The recoveries for the spiked water and beverage samples at the copper concentration levels of 5.0 and $10.0\;ng\;mL^{-1}$ were in the range between 92.0% and 108.0%. The relative standard deviations (RSD) varied from 3.0% to 5.6%.