• Title/Summary/Keyword: Liquid Liquid Extraction

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Matrix solid phase dispersion(MSPD) extraction and HPLC determination of enrofloxacin and ciprofloxacin in pork muscle tissue (시료고체상분산(matrix solid phase dispersion)전처리법과 액체크로마토그라피를 이용한 돈육중 enrofloxacin 및 ciprofloxacin 분석)

  • Kang, Hwan-goo;Son, Seong-wan;Lee, Hye-sook;Kim, Jae-hak;Cho, Myung-haing
    • Korean Journal of Veterinary Research
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    • v.37 no.1
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    • pp.195-202
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    • 1997
  • A method for the isolation by matrix solid phase dispersion method and liquid chromatographic determination of enrofloxacin and ciprofloxacin in pork muscle tissue is presented. Blank or enrofloxacin and ciprofloxacin spiked samples(0.5g) containing 0.05g oxalic acid were blended with $C_{18}$(octadecylsilyl derivatized silica) packing material. After homogenization, $C_{18}$/muscle tissue matrix was transferred to glass column made from 10ml glass syringe and filter paper, and compressed to 4~4.5ml volume. A column was washed with 8ml of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8ml and dried, following which enrofloxacin and ciprofloxacin were eluted with 8ml of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278nm. Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of $0.05{\sim}1.0{\mu}g/ml$ and eluted within 5ml elution volume of methanol from the matrix. Fortified sample containing 0.05g oxalic acid represented more good recoveries than that of control sample. Average percentages of enrofloxacin and ciprofloxacin were $93.30{\pm}4.56%$ and $91.84{\pm}4.17%$, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and $0.75{\mu}g/g$). The interassay variability of enrofloxacin was $6.02{\pm}5.33%$ with an intra-assay variability of 4.89% and $6.75{\pm}2.68%$ with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was $0.030{\mu}g/g$ in the spiked sample.

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Simultaneous Determination of Vitamin $D_3\;and\;K_1$ in Infant Formula by Column-switching High Performance Liquid Chromatography with UV Detection (Column-switching HPLC를 이용한 성장기용 조제식 중 비타민 $D_3,\;K_1$의 동시분석)

  • Kwak, Byung-Man;Ahn, Jang-Hyuk;Chang, Chi-Hoon
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.1024-1027
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    • 2005
  • Rapid and simple method was developed for simultaneous determination of vitamins $D_3\;and\;K_1$ contents in infant formula. Contents of vitamins $D_3\;and\;K_1$, extracted by column-switching HPLC with reversed phase column using enzymatic hydrolysis and organic solvent, in CRM determined by developed method were within certified ranges of standard values.

Anticancer Activity of Sulfated Polysaccharides Isolated from the Antarctic Red Seaweed Iridaea cordata

  • Kim, Hak Jun;Kim, Woo Jung;Koo, Bon-Won;Kim, Dong-Woo;Lee, Jun Hyuck;Nugroho, Wahyu Sri Kunto
    • Ocean and Polar Research
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    • v.38 no.2
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    • pp.129-137
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    • 2016
  • This study aimed to isolate and characterize sulfated polysaccharides (SPs) from Iridaea cordata and evaluate their anticancer activity. SPs of the Antarctic red seaweed were obtained by $CaCl_2$ (SP1) and ethanol precipitations (SP2) following diluted acid extraction at room temperature. Yields of SP1 and SP2 were approximately 14% and 23%, respectively, of the dry weight of red seaweed. The average molecular mass of the SP1 and SP2 was estimated about $1.84{\times}10^3$ and $1.42{\times}10^3kDa$, respectively, by size-fractionation High-Performance Liquid Chromatography (HPLC). From the High-Performance Anion-Exchange Chromatography-Pulsed Amperometric Detection (HPAEC-PAD) analysis, the main monosaccharide was galactose with glucose and fucose as minor components. The sulfate content of SP2 (40.4%) was slightly higher than that of SP1 (33.8%). The FT-IR spectra also showed characteristic band of carrageenan-like sulfated polysaccharides. Taken together the SPs are thought to be carrageenan-like sulfated galactan. The polysaccharides (SPs) from I. cordata exhibited weak antitumor activity against PC-3 (prostate cancer), HeLa (cervical cancer), and HT-29 (human colon adenocarcinoma). To our knowledge, this is the first data on biological activity of the Antarctic red seaweed I. cordata.

A Review on the Application of Ionic Liquids for the Radioactive Waste Processing (방사성 폐기물 처리를 위한 이온성 액체 활용)

  • Park, Byung Heung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.12 no.1
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    • pp.45-57
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    • 2014
  • Academic interests in ionic liquid (IL) technologies have been extended to the nuclear industry and the applicability of ionic liquids for processing radioactive materials have been investigated by many researchers. A number of studies have reported interesting results with respect to the spectroscopic and electrochemical behaviors of metal elements included in spent nuclear fuels. The measured and observed properties of metal ions in TBP(tri-butyl phosphate) dissolved ILs have led the development of alternative technologies to traditional aqueous processes. On the other hand, the electrochemical deposition of metal ions in ILs have been investigated for the application of the solvents to aqueous as well as to non-aqueous processes. In this work, a review on the application of ILs in nuclear fuel cycle is presented for the purpose of categorizing and summarizing the notable researches on ILs.

Simultaneous Determination of Doxifluridine and 5-FU in Liver and Intestine Tissue Using LC/MS/MS (LC/MS/MS를 이용한 원숭이 및 비글견의 간 및 장관 조직에서의 Doxifluridine과 대사체 5-FU 동시분석법 개발)

  • Woo, Young-Ah;Kim, Ghee-Hwan;Jeong, Eun-Ju;Kim, Choong-Yong
    • YAKHAK HOEJI
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    • v.52 no.2
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    • pp.93-100
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    • 2008
  • A liquid chromatographic method with tandom spectrometric detection (LC/MS/MS) for the simultaneous determination of doxifluridine and its active metabolite, 5-fluorouracil (5-FU) was developed over the concentration range of $5{\sim}2000$ ng/ml, respectively. Doxifluridine, 5-FU and internal standard, 5-chlorouracil (5-CU), were extracted from liver and intestine tissue via protein precipitation. Acetonitrile was used as the extraction solvent and the supernatant was evaporated and reconstructed in mobile phase. Optimum chromatographic separation was achieved on a Agilent Zorbax $C_{18}$ ($100\;mm{\times}2.1\;mm$, $3.5\;{\mu}m$) column with mobile phase run in isocratic with methanol : water (20 : 80, v/v). The flow rate was 0.2 ml/min with total cycle time of 5 min. The lower limit of quantification was validated at 5.0 ng/ml of liver and intestine tissue, for both doxifluridine and 5-FU, respectively. The intra-day and inter-day precision and accuracy of quality control (QC) samples were <11% coefficient of variation and <7% relative error from theoretical concentration for both analytes. In addition, the special designed stability study was performed, because the metabolism of doxifluridine occurs spontaneously even in ice bath for monkey liver. The stability of doxifluridine in liver and intestine of monkey and beagle dog was compared. It was found that bioanalytical validation could not be performed for the monkey liver; however, beagle dog's liver has relatively low speed of metabolism compared to monkey liver and instead of monkey liver, beagle dog's liver could be used for the validation. Bioanalytical validation could be performed in monkey intestine. Eventually, this developed method for liver and intestine will be useful in support of the toxicokinetic and pharmacokinetic studies of doxifluridine and 5-FU.

Confirmation of carbamate pesticides by liquid chromatography coupled with electrospray ionization mass spectrometry (LC/MS를 이용한 카바메이트계 잔류농약 확인방법)

  • 박준조;금모래;고광춘;박병옥;이성식
    • Korean Journal of Veterinary Service
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    • v.25 no.1
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    • pp.23-29
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    • 2002
  • A method was developed to separate, detect and qualify aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur in meats and fruits. Experimental beef and fork samples were fortified with 0.05mg/kg of carbamate pesticides for analysis. Carbamate-detected pear by HPLC fluorescence detector(HPLC/FLS) are extracted with acetonitril and refined by solid phase extraction(SPE) filled with aminopropyl-bonded silca, In the following step, the injected materials into LC/MS are analyzed to result in the fact that bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur presents several sorts of fraction ions following with; [M+H]$^{+}$, [M+Na]$^{+}$,[M-CONH$CH_3$]$^{+}$, [M-OCONH$CH_3$]$^{+}$. In addition, ethiofencarb presents [M-SCH$_2$$CH_3$]$^{+}$ ion distinctive and aldicarb presents [M+Na]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ ion which is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur excluding [M+H]$^{+}$ ion. However, [M-OCONH$CH_3$]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ fraction ion charactering carbamate pesticides are detected most efficiently with fragment voltage 50ev. As a result, for rluantitative analysis, [M+Na]$^{+}$ ion is the most decisive ion for detection of aldicarb and [M+H]$^{+}$ ion is the most decisive fraction ion for Pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur. Carbaryl-detected pear by HPLC/FLS are analyzed by L/MS and the result shows that [M+H]$^{+}$ and [M-CONH$CH_3$]$^{+}$ ions charactering carbaryl are detected.ering carbaryl are detected.

Analysis of Vitamin E in Some Commonly Consumed Foods in Korea (국내에서 소비되는 일부 상용 식품의 비타민 E함량 분석)

  • Lee, Seon-Mi;Lee, Hee-Bong;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.7
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    • pp.1064-1070
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    • 2005
  • Tocopherol and tocotrienol contents of commonly consumed foods in Korea were determined by saponification or direct solvent extraction followed by normal phase liquid chromatography. All samples were locally obtained in the year of 2002 and 2003. The study included 13 meats, 15 fishes and shellfishes, 4 seaweeds, 7 mushrooms, 19 milk and milk products, 6 legumes, 12 nuts, 17 processed foods and 17 Korean traditional foods. All of the vitamin E isomers were quantitated and the results were expressed as $\alpha-tocopherol$ equivalent $(\alpha-TE)$. The relatively higher amount of vitamin E was found in beef boiled in soy, dried squid, toasted seaweed, milk powder, soritae, sunflower seeds, ramyon (instant noodle), and kochujang from meats, fishes, seaweeds, milk products, legumes, processed foods, and traditional foods, respectively. This study provided reliable vitamin E data in commonly consumed foods in Korea for the nutritional information and food composition database.

Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

  • Won, Yong-Il;Jung, Pyong-Gil;Chung, Min-Young;Kim, Byung-Joo;Yim, Yong-Heon;So, Hun-Young;Kim, Yong-Seong
    • Bulletin of the Korean Chemical Society
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    • v.25 no.10
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    • pp.1508-1512
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    • 2004
  • A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

Effect of Catalyst Type and Reaction Medium on Fischer-Tropsch Synthesis for Production of Hydrocarbon from Syngas (합성가스로부터 탄화수소제조를 위한 피서트롭스 반응에 관한 촉매 종류 및 반응매체의 영향)

  • Kim, Chul-Ung;Jeong, Soon-Yong;Jeong, Kwang-Eun;Koh, Jae-Cheon;Chae, Ho-Jeong;Kim, Tae-Wan;Park, Hyun-Joo;Lee, Sang-Bong;Han, Jeong-Sik;Jeong, Byung-Hun
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2010.11a
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    • pp.658-663
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    • 2010
  • With petroleum reserves dwindling, interest has been increasing worldwide in Fischer-Tropsch synthesis (FT) as a method of producing synthetic liquid fuels and chemicals from coal, natural gas or biomass. In general, FT synthesis is operated through the gas phase fixed-bed reaction system. Recently, there are lots of study in supercritical fluid due to unique characteristics such as the quick diffusion of reactant gas, effective removal of reaction heat, and the in-situ extraction of high molecular weight hydrocarbon, such as wax. In this study, our major aim is to obtain a deeper insight into the effect of the type of support on the reaction performance over a supported cobalt catalyst in a fixed bed reactor.

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Development of Content Analysis for Cyperus rotundus by HPLC-UV and a Comparison between Chinese and Domestic Cyperi Rhizoma (HPLC-UV 방법을 이용한 향부자 분석법 개발과 국산 및 중국산 향부자의 패턴비교)

  • Seo, Jiyun;Kim, Jinah;Kim, Sungun;Liu, Ting;Whang, Wan Kyunn
    • YAKHAK HOEJI
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    • v.56 no.5
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    • pp.280-287
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    • 2012
  • A high-performance liquid chromatography (HPLC) combined with ultraviolet (UV) method for the simultaneous determination of ${\alpha}$-cyperone and nootkatone was developed for the quality control of Cyperus rotundus Linne. The separation was performed on a KR100-$5C_{18}$ ($4.6{\times}250mm$) column, and an elution gradient composed of methanol and water with a flow-rate of 1.0 ml/min. Detection wavelength was set at 254 nm. The optimum extraction for the detection of the ${\alpha}$-cyperone and nookatone was achieved by ultrasonic with methanol for an hour. Two marker compounds ${\alpha}$-cyperone and nootkatone in Cyperi Rhizoma showed good linearity ($R^2$ >0.999) in the concentration range of $12.5{\mu}g/ml$ to $200{\mu}g/ml$. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.04~1.23% and 0.08~0.68%, respectively, and the overall recoveries of 97.45~105.58% for the two compounds analyzed. Additionally, a difference was observed in the cluster analysis and principal component analysis between Cyperi Rhizoma in Korea and China. The result demonstrated that the principal component analysis is useful to distinguish between Cyperi Rhizoma in Korea and China.