• Analytical Science and Technology
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• v.23 no.6
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• pp.551-559
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• 2010

This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• 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.