• Title/Summary/Keyword: 용출법

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Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • 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.

Development of an Analytical Method for the Determination of Pyriofenone residue in Agricultural Products using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살균제 pyriofenone 분석법 확립)

  • Park, Hyejin;Kim, HeeJung;Do, Jung-Ah;Kwon, Ji-Eun;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.18 no.2
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    • pp.79-87
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    • 2014
  • Pyriofenone is an aryl phenyl ketone fungicide that is newly registered in Korea in 2013 to control powdery mildew on food. The objective of this study was to develop reliable and sensitive analytical method for determination of pyriofenone residue in agricultural products for ensuring the food safety. The pyriofenone residues in all samples(Korean melon, pepper, potato, mandarin, soybean, and hulled rice) were extracted with acetonitrile, partitioned with dichloromethane, and then purified with a silica cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of pyriofenone was 0.05~5 mg/kg with the correlation coefficient ($r^2$) > 0.999. Average recoveries of pyriofenone ranged from 72.8% to 99.5% at the spiked level of 0.05 and 0.5 mg/kg, while the relative standard deviation was 2.3%~6.4%. In addition, the limit of detection and limit of quantification were 0.01 and 0.05 mg/kg, respectively. The results revealed that the developed and validated analytical method was suitable for pyriofenone determination in agricultural products.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

The Distribution Characteristics of Heavy Metals at Field and Upland Soils (경작지 및 산지토양의 층위별 중금속농도의 분포 특성)

  • Choi, I-Song;Park, Jea-Young;Oh, Jong-Min
    • Journal of the Korean earth science society
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    • v.23 no.5
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    • pp.406-415
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    • 2002
  • Heavy metal concentrations (Cu(II), Zn(II), Pb(II) and Cd(II)) at field and upland soils were investigated with two extraction methods, 0.1mole L$^{-1}$ HCI extraction and HNO$_3$-HCIO$_4$ digestion, in order to estimate soil pollution and to understand their distribution and accumulation characteristics. Through an application of 0.1mole L$^{-1}$ HCI extraction method, the surface horizons of field soils were found to have higher concentrations of heavy metals (except Pb(II)) than those of upland soil. It was also seen that Cu(II), Zn(II) and Cd(II) were enriched in surface horizon of field soils, whereas upland soils did not show much difference across depth. When the method of HNO$_3$-HCIO$_4$ digestion was used, upland soils showed higher concentrations than those of other soils, and the distribution of heavy metals did not show much difference between horizons of all soils. From these results, it was recognized that, although total natural contents of heavy metals were the largest in upland soil, surface horizons of field soils became gradually polluted with heavy metals. Especially, Cd(II) is considered as a potential metallic pollutant in field soils because of its weak adsorption strength. Concentrations of heavy metals also seemed to be influenced by their adsorption characteristics. When we computed 0.1HCl$_{ext}$HNCL$_{dig}$ ratios to estimate the adsorption strengths of soil heavy metals, their adsorption strengths decreased on the order of Cu(II) > Zn(II)> Pb(II) > Cd(II). The distribution characteristics of heavy metals in field soil, especially Cd(II),are required more detail study because of its importance of land use and complicated mobilization characteristic.

Development of Pharmaceutical Dosage Forms with Biphasic Drug Release using Double-Melt Extrusion Technology (이중 고온용융 압출 성형된 이중 방출능을 가지는 제형의 개발)

  • Kim, Dong-Wook;Kang, Chin-Yang;Kang, Changmin;Park, Jun-Bom
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.17 no.9
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    • pp.228-234
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    • 2016
  • The aim of this study was to develop pharmaceutical dosage forms with a bi-phasic drug using a double extrusion approach. Hot melt extrusion was performed using a co-rotating twin-screw extruder. The. 1st melt extrusion was performed using polymer with a relatively higher Tg, such as HPMC and the 2nd melt extrudate was obtained using the 1st extrudate and polymers with a lower Tg, such as HPMC-AS and PEO. In addition, the formulation with all the content in the same proportion as the double extudate was produced using single extrusion for comparison. Physical characterization was performed on the formulations employing differential scanning calorimetry (DSC). In vitro release tests were studied using a USP Type-I apparatus at $37{\pm}0.5^{\circ}C$ and 100 rpm. The similarity factor (f2) was also used to check the difference statistically. The DSC results indicated that the crystallinity of ibuprofen was changed to an amorphous state after extrusion in both double and single melt extrusion. Double melt extrudate with ibuprofen showed the desired release in acidic media (pH 1.2) in the first two hours and basic (pH 6.8) during six hours. Double melt extrudate with glimepiride showed faster release in 60 min of over 80%, whereas the single extrudate with glimepiride showed retarded release due to the interaction with HPMC. The similarity factor(f2) value was 28.5, which demonstrates that there were different drug release behavior between the double and single extrusion. Consequently, the double melt extrudated formulation was robust and gave the desired drug release pattern.

Chemical Speciation of Heavy Metals in Geologic Environments on the Abandoned Jangpoong Cu Mine Area (장풍 폐광산 주변 지질환경에서 중금속의 존재형태)

  • Lee In-Gyeong;Lee Pyeong-Koo;Choi Sang-Hoon;Kim Ji-Soo;So Chil-Sup
    • Economic and Environmental Geology
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    • v.38 no.6 s.175
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    • pp.699-705
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    • 2005
  • In order to identify the speciation of As and trace elements which are contained weathered waste rocks on the abandoned Jangpoong Cu mine area, five fraction sequential extraction was carried out. Concentrations of the extraction solutions which were acquaired each fraction were mesured by ICP-AES. Mineral characters of weathered waste rocks were determinated by XRD. The weathered waste rocks could divide into two types (Type I and type II). Type land type II weathered waste rocks are mainly composed of a quartz and a calcite, respectively. The most dominant speciation of As, Co and Fe is residual phase. Most of the speciation of Cd, Mn and Zn is residual phase for type I and Fe-Mn oxide phase for type II. In case of Cu, residual phase is predominant in type I and sulfide is predominet in type II. The most dominant speciation of Pb for type I and type II is associated with the residual phase and Fe-Mn oxide phase, respectively. At pH 4-7 range, the order of relative mobility considers Zn>Cu>Cd>Pb>Co>AS in type I, and Cd>Cu>Zn>Pb>As>Co in type II.

An Experimental Study on the Properties of Chloride Binding of Mg/Al-NO3 and Ca/Al-NO3 Layered Double Hydroxides in Solution (수용액내에서 Mg/Al-NO3 및 Ca/Al-NO3 층상이중수산화물(LDHs)의 염소이온 고정화 특성에 관한 실험적 연구)

  • Lee, Seung-Yeop;Yang, Hyun-Min;Lee, Han-Seung
    • Journal of the Korea Institute of Building Construction
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    • v.16 no.3
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    • pp.219-227
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    • 2016
  • Chloride ions ingress continuously in reinforced concrete through pores of it by $Cl^-$. Finally, it causes a localized corrosion of the rebar and then it generates cracks on concrete structures. Recently, new materials removing harmful anions have been developed. Layered double hydroxides(LDHs) has an excellent ability to remove harmful anions because various anions can be adsorbed in the interlayer space between divalent and trivalent cations. Thus, LDHs has been applied in various fields. Especially, LDHs is expected to be effective adsorbent binding chloride ions. In this study, $Ca/Al-NO_3$ and $Mg/Al-NO_3$ LDHs were prepared by using a co-precipitation method. $Ca/Al-NO_3$ and $Mg/Al-NO_3$ LDHs were compared and analyzed by using XRD, SEM analysis. Many nano size hexagonal crystals were observed by SEM. Experiments for binding chloride ions of LDHs were conducted by using potentiometric method. The experimental data were measured every 15 minutes. It was observed that the chloride ion content is reduced by increasing of LDHs mass fraction and the reaction rate of $Mg/Al-NO_3$ is faster than $Ca/Al-NO_3$. In future studies, binding chloride capacity in cement materials will be evaluated based on results of this study.

Antibacterial Activities of Et-OH Extract from Extruded White Ginseng on Tooth Decay Bacteria (압출성형 백삼 Et-OH 추출물의 충치유발균에 대한 항균활성)

  • Son, Hyun-Jung;Han, Min-Soo;Ryu, Gi-Hyung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.7
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    • pp.951-957
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    • 2009
  • In this study, antibacterial activity of extruded ginseng extract by 60 and 80% Et-OH were investigated by agar diffusion assay against two bacteria causing dental caries (Streptococcus mutans and Lactobacillus casei). Extrusion conditions were 20% moisture content $100^{\circ}C$ and $140^{\circ}C$ barrel temperature. The inhibition effect of 60% Et-OH ginseng extract was higher than 80% Et-OH ginseng extract. The minimum inhibitory concentration (MIC) of 80% Et-OH extruded ginseng extract at 140 and $100^{\circ}C$ barrel temperature against L.casei were 100 and 150 mg/mL respectively using broth assay method. The amount of glucosyltransferase (GTase) inhibitory content was the highest in extruded ginseng at $140^{\circ}C$ barrel temperature with 60% Et-OH. Moreover, n-hexane and n-butanol fraction ginseng extract had potential against tested bacteria. Our results demonstrated that antibacterial activities of extruded ginseng extract at $140^{\circ}C$ barrel temperature were more effective than Ex-$100^{\circ}C$, RG and WG.

Uncertainties of ionic species in snowpit samples determined with ion chromatography system (이온크로마토그래피 시스템을 이용한 눈 시료의 이온성분 측정자료의 불확도 산출)

  • Hong, Sang-Bum;Hur, Soon-Do;Kim, Sun-Mee;Hong, Sungmin;Chung, Ji-Woong;Kang, Namgoo;Kang, Chang-Hee
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.350-363
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    • 2012
  • To determine ionic species in snowpit samples using ion chromatography system, we described the performance of ion chromatography(IC) system, cleaning method of bottle, and interference by filtering procedure. The limit of detection, reproducibilities, and accuracies determined with BCR$^{(R)}$-408 were 0.01-0.26 ${\mu}g$/L, 0.4-17.4%, 4.5-12.0% for cations and 0.02-0.26 ${\mu}g/L$, 0.1-27.6%, 1.3-5.6% for anions, respectively. Lab blank test for sample bottle indicated that $CH_3CO_2{^-}$, $HCO_2{^-}$, and $NH_4{^+}$ can be easily contaminated in the lab environment. The positive interferences of $NO_3{^-}$ were partly attributed to the cleaning method of bottle. The filtering of melted snow sample should be carefully applied because it can positively affect the concentration levels of some ionic species. Finally, this method was applied to measure ionic species in snowpit samples from the upward area near NEEM camp and the uncertainties of measurement data of $F^-$ were also estimated.

Effect of the Viscosity of (Hydroxypropyl)methyl Cellulose on Dissolution Rate of Alfuzosin-HCl Granule Tablet (HPMC의 점도에 따른 염산 알푸조신 과립정제의 용출률 조절)

  • Kim, Won;Song, Byung-Joo;Kim, Dae-Sung;Kim, Su-Jin;Lee, Seon-Kyoung;Kim, Hye-Lin;Lee, Dong-Won;Khang, Gil-Son
    • Polymer(Korea)
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    • v.34 no.3
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    • pp.269-273
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    • 2010
  • The primary objective of this work is to find the optimal condition for the granule tablet formulation of alfuzosin-HCl that aims to achieve a sustained drug release. (Hydroxypropyl)methyl cellulose (HPMC) is one of the most widely used polymer as a drug formulation and therefore has been utilized in this study as an excipient. Alfuzosin-HCl granule tablet was developed using the various viscosities of HPMC and the effects of viscosity on drug release was investigated. Fourier transform-infrared (FTIR) and X-ray diffraction (XRD) were employed to investigate the chemical structure and crystallization of alfuzosin-HCl in the formulation. We prepared the granule tablet by a direct compression method and studied the release profile in the stimulated intestinal fluid (pH 6.8). As the viscosity of HPMC increased the release of alfuzosin-HCl decreased, demonstrating that controlled release of alfuzosin-HCl can be achieved by varying the viscosity of HPMC.