• 한국식품위생안전성학회지
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• 제18권2호
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• pp.43-50
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• 2003

A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

• 한국동물위생학회지
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• 제36권4호
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• pp.303-309
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• 2013

This study was conducted to determine the content of 7 mycotoxins (aflatoxin $B_1$, $B_2$, $G_1$, $G_2$, $M_1$, ochratoxin A and zearalenone) using LC-MS/MS in pork available on the Korean markets. The analysis was carried out using following conditions; C18 column ($2.1{\times}100mm$, $1.7{\mu}m$), mobile phase composed of $H_2O$ (0.1 mM $NH_4Ac$ 0.01% HCOOH) : Methanol (0.1 mM $NH_4Ac$ 0.01% HCOOH), binary pump at a flow rate of 0.5 mL/min and $2{\mu}L$ of injection volume, MS/MS detector with ESI positive and negative mode. The quantication of mycotoxins was based on matrix-matched calibration curves with a correlation coefficient in excess of 0.99 for the 7 mycotoxins. The dectection limits were ranged 0.74~2.13 ng/g, with mean recoveries between 73.10~97.46% except aflatoxin $B_1$ (61.31%). We also monitored mycotoxin residues in 208 pork samples. The test results, mycotoxins were not found except one sample. Ochratoxin A in one sample of the test samples was detected below the quantification limit.

• 통합자연과학논문집
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• 제7권3호
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• pp.188-192
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• 2014

Determination of cobalt(III) ion with a perfluorinated sulfonated polymer-ethylenediamine (nafion-en) modified glassy carbon electrode is studied. It is based on the chemical reactivity of an immobilized layer, nafion-en, to yield complex $[Co(en)_3]^{3+}$. The reduction peak potential by differential pulse voltammetry (DPV) is observed at $-0.437{\pm}0.047$ V (vs. Ag/AgCl). The linear calibration curve is obtained in cobalt(III) ion concentration range $1.0{\times}10^{-8}{\sim}1.0{\times}10^{-3}M$ ($5.893{\times}10^{-12}{\sim}5.893{\times}10^{-5}g/mL$).

• 대한의생명과학회지
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• 제21권4호
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• pp.241-247
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• 2015

Lactate and ketone bodies are considered biological markers for ketosis and several inherited metabolic disorders. In the current study, the specific ratios of lactate and ketone bodies as analytical tools for differential diagnosis of various lactic acidosis were devised. The study included a protein precipitation step following tert-butyldimethylsilyl derivatisation. Total run time was approximately 30 min including sample preparation and GS/MS analysis. The limits of detection were below 0.1 pg/mL over the targeted 4 analytes. The calibration curve was linear over the concentration range of $0.001{\sim}250{\mu}g/mL$ for pyruvate, beta-hydroxybutyrate, and acetoacetate ($R^2$ > 0.99). Inter-day accuracy and precision were 87.7~94.8% with RSD of 2.5~5.7% at 2 levels. Absolute recoveries (%) of target analytes were 87.0~98.4%. The method was validated for the quantification of lactate and ketone bodies for differentiation of lactic acidosis.

• Coupled systems mechanics
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• 제7권2호
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• pp.211-232
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• 2018

In this work we present an upscaling technique for multi-scale computations based on a stochastic model calibration technique. We consider a coarse-scale continuum material model described in the framework of generalized standard materials. The model parameters are considered uncertain, and are determined in a Bayesian framework for the given fine scale data in a form of stored energy and dissipation potential. The proposed stochastic upscaling approach is independent w.r.t. the choice of models on coarse and fine scales. Simple numerical examples are shown to demonstrate the ability of the proposed approach to calibrate coarse scale elastic and inelastic material parameters.

• Bulletin of the Korean Chemical Society
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• 제25권7호
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• pp.1019-1024
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• 2004

The present paper is focused on simultaneous sorption concentration of gold (III) and silver (I) from thiocyanate solutions using high-selective anion exchanger AN-25 and subsequent separation of these ions at various concentrations of thiocarbamide (eluent). As a result, silver (I) ions are completely eluted from AN-25 and gold (III) ions remain in the resin phase and can be determined directly in the solid phase by diffuse reflection spectroscopy. It is proposed to use the sorption-spectroscopic method for Au(III) determination in aqueous solutions. The calibration curve is linear in the concentration range of 1-19 mg/L (sample volume is 10.0 mL) and the detection limit is 0.05 ${\mu}g/mL$. The presence of Cu(II), Co(II), Fe(II) do not hinder this determination. Au(III) was determined in industrial solutions.

• Natural Product Sciences
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• 제20권3호
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• pp.182-190
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• 2014

An ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was established for quantitative analysis of twelve components, allantoin (1), morroniside (2), 5-hydroxymethyl-2-furfural (5-HMF) (3), loganin (4), coumarin (5), cinnamic acid (6), mesaconitine (7), cinnamaldehyde (8), hypaconitine (9), aconitine (10), alisol B (11), and alisol B acetate (12) in a Palmijihwang-hwan decoction. The twelve constituents were separated on a UPLC BEH C18 column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as the mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. Calibration curves of all compounds were acquired with values of the correlation coefficient ${\geq}0.99$ within the test ranges. The limits of detection and quantification for all analytes were 0.01 - 4.53 ng/mL and 0.03 - 13.60 ng/mL, respectively. The concentrations of the compounds 1 - 9 and 12 were 72.83, 4389.00, 4859.00, 3155.17, 223.67, 33.50, 1.97, 518.00, 2.25, and $25.00{\mu}g/g$, respectively. However, compounds 10 and 11 were not detected.

• 디지털융복합연구
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• 제10권7호
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• pp.201-206
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• 2012

벤조피렌은 IARC에 의해 그룹 1로 분류된 다환 방향족 탄화수소 유기물로서 불완전 연소 시 부산물로 발생되며 유전독성과 발암성이 강한 것으로 알려져 있다. 벤조피렌의 오염원은 매우 다양하여 환경오염 등으로 인해 조리 또는 가공과정에서 열분해 되어 생성되는 것으로 알려져 있다. 본 연구에서는 유통 중인 45종의 한약재에 있어 벤조피렌의 함유량에 대한 모니터링을 HPLC/FLD로 측정하였다. 벤조피렌의 검량선은 0.5~40 ng/mL의 농도 범위에서 양호한 직선성을 나타내었다 ($r^2$=0.999). 벤조피렌의 검출한계 (LOD)와 정량한계 (LOQ)는 0.04와 0.10 ${\mu}g/mL$이었다. 모니터링 품목 총 45건 중 벤조피렌이 검출되지 않은 시료는 3건 (6.7%), 0.1 ~ 0.5, 0.5 ~ 1.0, 1.0 ~ 5.0 및 5.0 ${\mu}g/kg$ 이상 검출된 시료는 각각 26건 (57.7%), 8건 (17.8%), 7건 (15.6%) 및1건 (2.2%)이었다. 특히 황련의 벤조피렌의 함유량이 가장 높았다 (5.97 ${\mu}g/mL$). 결론적으로 이들 결과는 한약재 중 벤조피렌 함유량을 감소시키기 위한 건조 조건에 대한 기초연구와 가이드라인으로서 적용되어질 수 있다.

• 한국환경보건학회지
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• 제35권2호
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• pp.130-142
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• 2009

This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination ($r^2$) was 0.9998 in a calibration curve of $695\;cm^{-1}$, and the limit of detection was $4.9{\mu}g/sample$. 2. The highest recovery was $799\;cm^{-1}$ (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was $5.9{\mu}g/sample$. 6. The recovery and CV pooled were 104.3%, and 11 %, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing $\alpha$-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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• pp.280.3-281
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• 2003

A high-performance liquid chromatographic method for the simultaneous quantitative analysis of DMDM hydantoin, sorbic acid, phenoxy ethanol in cosmetics was studied by using a X-terra C18 column and 0.75mM KH2PO4 in 0.85％ sulfuric acid and methanol mixture(7:3) at 214nm. Calibration curves were found to be linear in the 20-100$\mu\textrm{g}$/mL range (DMDM hydantoin), 50-250$\mu\textrm{g}$/mL range (sorbic acid) and 10-50$\mu\textrm{g}$/mL range (phenoxy ethanol). The result of recovery test were 96.6％ - 104.2％. This HPLC method can be applied quality control of cosmetics.