• Title/Summary/Keyword: Two-phase extraction

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Chiral separation of amino acids in urine specimens from patients with inherited metabolic disorders by achiral gas chromatography

  • Paik, Man-Jeoneg;Choi, Young-Mie;Nguyen, Duc-Toan;Kim, Ji-Yung;Kim, Jung-Han;Kim, Kyoung-Rae
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.218.2-218.2
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    • 2003
  • An efficient method is described for the enantioseparation of urinary amino acids to determine their absolute configurations. It involves two-phase extractive ethoxycarbonylation in alkaline aqueous solution with subsequent extraction after acidification. The resulting derivatives of amino acids are converted to volatile diastereomeric esters or amides for the direct analysis by gas chromatography (GC) on achiral dual-columns with different polarities. The present method was applied to urine specimens from patients with inherited metabolic disorders. In this study, the usefulness for the chiral separation of diagnostic amino acids will be discussed.

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Analysis of alkaloids in Polygala tenuifolia by HPLC (HPLC에 의한 원지 중 알칼로이드 성분의 정량)

  • Park, Man Ki;Park, Jeong Hill;Kim, Bao-Yuan;Kim, Jong Moon;Liem, Kyung-Jin;Han, Byung Hoon
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.255-259
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    • 1993
  • ${\beta}$-Carboline alkaloids of Polygala tenuifolia (Polygalaceae), an expectorant, tonic and sedative drude drug, were determined by HPLC. The alkaloids were separated by RP-18 column with gradient elution of 0.01M potassium phosphate buffer(pH=3.5) and acetonitrile and detected at UV 254nm. Two methods for the preparation of alkaloid fraction were compared. One was solvent extraction method using acid and base, and the other was solid phase extraction with ion exchange resin (Amberlyst 15). A more refined HPLC chromatogram was obtained using the solid phase extraction method. The alkaloidal contents in P. tenuifolia determined by this method were : harman $2.8{\times}10^{-3}%$, norharman $1.7{\times}10^{-3}%$, 1-carbomethoxy-${\beta}$-carboline $1.3{\times}10^{-3}%$, 1-carboethoxy-${\beta}$-carboline $1.4{\times}10^{-3}%$ and perlolyrine $3.3{\times}10^{-3}%$, respectively.

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Recovery of Co and Ni from Strong Acidic Solution by Cyanex 301 (강산성용액에서 Cyanex 301에 의한 Co 및 Ni 회수 연구)

  • Cho, Yeon-Chul;Kim, Ki-Hun;Ahn, Jae-Woo
    • Resources Recycling
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    • v.30 no.6
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    • pp.28-35
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    • 2021
  • An experiment was conducted to separate or recover Co and Ni using Cyanex 301 from process by-products and waste resources containing Co and Ni. To separate and recover Co and Ni from simulated leaching solutions, 10 v/v% Cyanex 301 was used as an extractant in this study; Li was not extracted. At equilibrium pH 1.5 and a phase ratio (A/O) of 1.0, 0.44% of Mg and 11.57% of Mn were extracted, and more than 99% of Co and Ni were extracted. McCabe-Thiele diagram analysis confirmed that more than 99.9% of Co and Ni could be extracted simultaneously through two-stage extraction with an extraction phase ratio (A/O) of 2. It was possible to extract Mg and Mn simultaneously through the scrubbing process. In the scrubbing process, more than 99% of Mg and 87% of Mn were scrubbed using 0.05 M of H2SO4, and 99.9% of Mg and more than 80% of Mn were scrubbed using 0.05 M of HCl. In the stripping process, 93% of Co and 5% of Ni were stripped selectively by 3.0 M of H2SO4. However, when 8.0 M of HCl was used as a stripping solution, more than 99.9% of Co and more than 90% of Ni were stripped simultaneously.

Emulsion Liquid Membrane Transport of Heavy Metal Sons by Macrocyclic Carriers (거대고리 운반체에 의한 중금속이온의 에멀죤 액체막 수송)

  • 정오진
    • Journal of Environmental Science International
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    • v.4 no.2
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    • pp.223-232
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    • 1995
  • New two macrocyclic compounds using as carriers of liquid emulsion menbrame, have been synthesized. These reuslts provide evidance for the usefulness of the theory in designing the systems. The efficiency of selective transport for heavy metal ions have been discussed from the membrane systems that make use of $SCN^-$,<>,$I^-$,CN- and $Cl^-$ ion as co-anions in source phase and make use of $S_2O_3^{2-}$ and $P_2O_7^{4-}$ ion as receiving phase, respectively. The transport rate of M(II) was highest when a maximum amount of the M(II) in the source phase was present as$Cd(SCN)_2$$(P[SCN^-]= 0.40M)$, $Hg(SCN)_2([SCN^-]=0.40M)$ and Pd(CN)$([CN^-]= 0.40M)$. The Cd(II) and Pb(II) over each competitive cations were well transprted with 0.3M-S2032- and 0.3M-P2O74-, respectively in the receiving phase. Results of this study indicate that two criteria must be met in order to have effective macrocycle-mediated transport in these emulsion system. First one must effective extraction of the $M^{n+}$ into the toluene systems. The effectiveness of this extraction is the greatest if locK for $M^{n+}$macrocycle interaction is large and if the macrocycle is very insoluble in the aqueous phase. Second, the ratio of the locK values (or Mn+-receiving phase ($S_2O_3^{2-}$- or $P_2O_7^{4-}$) to $M^{n+}$-macrocycle (($L_1$이나 $L_2$) interaction must be large enough to ensure quantitative stripping of Mn+(($Cd^{2+}$,$Pb^{2+}$)at the toluene receiving Phase interface. $L_1$(3.5-benzo-10,13,18,21-tetraoxa-1,7,diazabicyclo(8,5,5) eicosan) forms a stable ($Cd^{2+}$ and >,$Pb^{2+}$ complexes and $L_1$ is very insoluble in water and its $Cd^{2+}$ and >,$Pb^{2+}$ complex is considerably less stable than $Cd^{2+}$-(S2O3)22- and $Pd^{2+}-P_2O_7^{4-}$ complexes. On the other hand, the stability of the $Hg^{2+}$)+-$L_1$( complex exceed that of the $Hg^{2+}$- (S2O3)22- and Hg2+-P2O74-, and the distribution coefficient of $L_2$(5,8,15,18,23,26-hexaoxa-1,12- diazabicyclo-(10,8,8) octacosane) is much smaller than that of $L_1$. Therefore, the partitioning of Lr is favored by the aqueous receiving Phase, and little heavy metal ions transport is seen despite the large logK for $Hg^{2+}$+-$L_1$ and $Mn^+$($Cd^{2+}$+, $Pb^{2+}$+ and $Hg^{2+}$)-$L_2$ interactions. Key Words : macrocycles, transport, heavy metal, co-anion, source phase, receiveing, complex separation, interaction, destribution coefficient.

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Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1791-1795
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    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

Studies on Solvent Extraction and Analytical Applications of Metal-Dithiocarbamate Complexes(Ⅰ). Extraction and Determination of Trace Bismuth, Cadmium and Indium in Sea Water (Dithiocarbamate 금속착물의 용매추출 및 분석적 응용(제 1 보). 해수중 흔적량 비스무트, 카드뮴, 인듐의 용매추출 및 정량)

  • Jeon, Moon Kyo;Choi, Jong Moon;Choi, Hee Seon;Kim, Young Sang
    • Journal of the Korean Chemical Society
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    • v.40 no.7
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    • pp.492-500
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    • 1996
  • The solvent extraction of trace Bi, Cd and In in seawater samples using ammonium pyrrolidine dithiocarbamate(APDC) as a complexing agent was studied. The pH of sample solution, the amount of APDC, the type of solvent and the shaking time were investigated together with back-extraction conditions. After the pH of 200 mL seawater was adjusted to 4.0 and 5.0 mL of 1% APDC was added, analytes were extracted with 10.0 mL of MIBK by shaking for 35 minutes. The organic phase seperated was washed with a 0.05 M NaOH 10.0 mL to remove HPDC. The analytes were stripped by the back-extraction of 5 minute shaking with 5 mL of 4 M HNO3 containing 150 ㎍/mL Pd(Ⅱ). Detection limits of Bi, Cd and In were 0.038, 0.0057 and 0.023 ng/mL, respectively. Both of Bi(Ⅲ) and In(Ⅲ) were not detected in two kinds of water samples of the East Sea and the contents of Cd(Ⅱ) were 0.018 and 0.016 ng/mL. The recoveries of over 90% showed that this procedure was applicable to the determination of such trace elements in seawater samples.

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Detection of Gene Interactions based on Syntactic Relations (구문관계에 기반한 유전자 상호작용 인식)

  • Kim, Mi-Young
    • The KIPS Transactions:PartB
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    • v.14B no.5
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    • pp.383-390
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    • 2007
  • Interactions between proteins and genes are often considered essential in the description of biomolecular phenomena and networks of interactions are considered as an entre for a Systems Biology approach. Recently, many works try to extract information by analyzing biomolecular text using natural language processing technology. Previous researches insist that linguistic information is useful to improve the performance in detecting gene interactions. However, previous systems do not show reasonable performance because of low recall. To improve recall without sacrificing precision, this paper proposes a new method for detection of gene interactions based on syntactic relations. Without biomolecular knowledge, our method shows reasonable performance using only small size of training data. Using the format of LLL05(ICML05 Workshop on Learning Language in Logic) data we detect the agent gene and its target gene that interact with each other. In the 1st phase, we detect encapsulation types for each agent and target candidate. In the 2nd phase, we construct verb lists that indicate the interaction information between two genes. In the last phase, to detect which of two genes is an agent or a target, we learn direction information. In the experimental results using LLL05 data, our proposed method showed F-measure of 88% for training data, and 70.4% for test data. This performance significantly outperformed previous methods. We also describe the contribution rate of each phase to the performance, and demonstrate that the first phase contributes to the improvement of recall and the second and last phases contribute to the improvement of precision.

The Effect of Distance between Two Transducers on Sonochemical Reactions in Dual Irradiation Systems (이중 초음파 조사 시스템에서 진동부 사이의 거리가 초음파 화학 반응에 미치는 영향)

  • Kim, Eunkyung;Son, Younggyu
    • Journal of Soil and Groundwater Environment
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    • v.18 no.5
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    • pp.39-45
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    • 2013
  • Many researchers have studied the effectiveness of ultrasound in chemical and environmental engineering fields including material synthesis, pollutant removal, cleaning, extraction, and disinfection. Acoustic cavitation induced by ultrasound irradiation in aqueous phase can cause various sonophysical and sonochemical reactions without any chemicals. However most of the previous studies focused only on the relationships between ultrasonic conditions and the results of sonochemical reactions in lab-scale sonoreactors. As a results of this, only a few studies have been devoted to design and optimization of industrial scale sonoreactors. In this study, the effect of the distance between two opposite transducer modules on sonochemical reactions was investigated in single and dual irradiation systems (334 kHz) for four distances including 50, 100, 150, and 200 mm using KI dosimetry. It was found that the dual irradiation systems provided higher performance in terms of the zeroth reaction coefficient and the cavitation yield compared to the single irradiation systems. The sonochemiluminescence (SCL) images for the visualization of the cavitation field showed that cavitation active zone was larger and sonochemical reaction intensity was much higher in the dual irradiation system than in the single irradiation system.

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

Analysis of Volatile Compounds in Perilla frutescens var. acuta by Solid Phase Microextraction (SPME에 의한 소엽의 향기성분 분석)

  • Chung, Mi-Sook;Lee, Mie-Soon
    • Journal of the Korean Society of Food Culture
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    • v.18 no.1
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    • pp.69-74
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    • 2003
  • This study was conducted to find the appropriate fiber for extraction of volatile compounds from Perilla frutescens var. acuta. by solid phase microextraction (SPME). Two SPME fiber, carboxen/polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane (PDMS) were used to determine the selectivity of the fibers to the different flavor compounds present in the Perilla frutescens var. acuta. Thirty-nine compounds were identified in the volatile compounds extracted by CAR/PDMS fiber, including 6 aldehyde, 1 alcohol, 10 hydrocarbons, 17 terpene hydrocarbons, 2 ketones and 3 benzenes. In PDMS fiber, 3 aldehydes, 2 alcohols, 13 terpene hydrocarbons and 2 miscellaneouses were identified. Perillaldehyde was found to be major volatile flavor component of fresh Perilla frutescens var. acuta. Perillaldehyde and terpene hydrocarbons were more identified in PDMS fiber. These results suggested that the selectivity of PDMS fiber was better than that of CAR/PDMS fiber in Perilla frutescens var. acuta..