• 제목/요약/키워드: Phase extraction method

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分液 및 Extrelut Column에 依한 人蔘 Saponin 抽出方法의 比較硏究 -Saponin 回收率에 대하여- (A Study on Comparison of Extraction Methods of Ginseng Saponin by Phase Separation and by Extrelut Column - For Recovery Rates of Saponin -)

  • Kim, Jong Gyu;Lee, Yong Wook;Sohn, Hyun Joo;Lee, Kwang Seung
    • 한국환경보건학회지
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    • 제10권1호
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    • pp.87-92
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    • 1984
  • Extraction method of ginseng saponin by Extrelut column was studied as compared with that by phase separation. The results obtained were as follows: 1. Extraction time consumed by Extrelut column was 2 ~ 3 hours and much shorter as compared with that by phase separation. 2. Recovery rates Of ginsenoside by Extrelut column method were 97.8 ~ 106.1% and much higher as compared with those by phase separation method.

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고상미량추출장치(SPME)를 이용한 유류 오염 지하수 평가 기법 연구

  • 조현정;백기태;박지연;양지원
    • 한국지하수토양환경학회:학술대회논문집
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    • 한국지하수토양환경학회 2001년도 추계학술발표회
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    • pp.148-150
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    • 2001
  • Solid-phase microextraction (SPME) was investigated to understand the BTEX extraction behavior of SPME in groundwater. Analytical procedure was conducted In both conventional and headspace mode. And the conventional direct extraction method and the headspace analysis method were compared. Data obtained with direct and headspace SPME were very similar and showed successful results. In headspace analysis, the linearity was better and RSD (relative standard deviation, %) was smaller than direct extraction.

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Synthesis of a New α-Dioxime Derivative and Its Application for Selective Homogeneous Liquid-Liquid Extraction of Cu(II) into a Microdroplet Followed by Direct GFAAS Determination

  • Ghiasvand, A. R.;Shadabi, S.;Kakanejadifard, A.;Khajehkoolaki, A.
    • Bulletin of the Korean Chemical Society
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    • 제26권5호
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    • pp.781-785
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    • 2005
  • A fast and reliable method for the selective separation and preconcentration of $Cu^{2+}$ ions using homogeneous liquid-liquid extraction was developed. A new $\alpha$-dioxime derivative (2H-1,4-benzothioazine-2,3(4H)dionedioxime, Dioxime I) was synthesized and investigated as a suitable selective complexing ligand for $Cu^{2+}$ ions. Zonyl FSA (FSA) was applied as a phase-separator agent under the slightly acidic pH conditions. Under the optimal experimental conditions ([FSA] = 3.2% w/v, [THF] = 19.5% v/v, [Dioxime I] = 1.9 ${\times}\;10^{-3}$ M, and pH = 4.7), 10 ${\mu}g\;of\;Cu^{2+}$ in 5.2 mL aqueous phase could be extracted quantitatively into 80 $\mu$L of the sedimented phase. The maximum concentration factor was 65-fold. The limit of detection of the proposed method was 0.005 ng $mL^{-1}$. The reproducibility of the proposed method, on the 10 replicate measurements, was 1.3%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of $Cu^{2+}$ ions were investigated. The proposed method was applied to the extraction and determination of $Cu^{2+}$ ion in different synthetic and natural water samples.

Determination of Acaricides in Honey by Solid-Phase Extraction and Gas Chromatography / Mass Spectrometry

  • Hong, Joo-Yeon;Jung, Ok-Sang;Ryoo, Jae-Jeong;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제30권1호
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    • pp.61-66
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    • 2009
  • An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

Analysis of Heterocyclic Amines in Human Urine Using Multiple Solid-Phase Extraction by Liquid Chromatography/Mass Spectrometry

  • Cha, Hyun-Jeong;Kim, Nam-Hee;Jeong, Eun-Kyung;Na, Yun-Cheol
    • Bulletin of the Korean Chemical Society
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    • 제31권8호
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    • pp.2322-2328
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    • 2010
  • A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.

Feature Extraction Based on Speech Attractors in the Reconstructed Phase Space for Automatic Speech Recognition Systems

  • Shekofteh, Yasser;Almasganj, Farshad
    • ETRI Journal
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    • 제35권1호
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    • pp.100-108
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    • 2013
  • In this paper, a feature extraction (FE) method is proposed that is comparable to the traditional FE methods used in automatic speech recognition systems. Unlike the conventional spectral-based FE methods, the proposed method evaluates the similarities between an embedded speech signal and a set of predefined speech attractor models in the reconstructed phase space (RPS) domain. In the first step, a set of Gaussian mixture models is trained to represent the speech attractors in the RPS. Next, for a new input speech frame, a posterior-probability-based feature vector is evaluated, which represents the similarity between the embedded frame and the learned speech attractors. We conduct experiments for a speech recognition task utilizing a toolkit based on hidden Markov models, over FARSDAT, a well-known Persian speech corpus. Through the proposed FE method, we gain 3.11% absolute phoneme error rate improvement in comparison to the baseline system, which exploits the mel-frequency cepstral coefficient FE method.

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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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.

Speciation of Chromium in Water Samples with Homogeneous Liquid-Liquid Extraction and Determination by Flame Atomic Absorption Spectrometry

  • Abkenar, Shiva Dehghan;Hosseini, Morteza;Dahaghin, Zohreh;Salavati-Niasari, Masoud;Jamali, Mohammad Reza
    • Bulletin of the Korean Chemical Society
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    • 제31권10호
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    • pp.2813-2818
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    • 2010
  • A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

새로운 직류 옵셋 제거 필터에 의한 정확한 페이저 추출에 관한 연구 (A Study on Accurate Phasor Extraction Using a New DC Offset Elimination Filter)

  • 박철원;윤희환
    • 조명전기설비학회논문지
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    • 제27권7호
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    • pp.29-36
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    • 2013
  • In this paper, a new DC offset elimination filter is proposed for an accurate phasor extraction of fundamental frequency component. The proposed method can eliminate a DC offset component which is decayed exponentially. The proposed method uses only one cycle of data for phasor extraction computation, which does not need to preset the time constant of the DC offset component. Also, the other advantages of the proposed method is that gain compensation or phase compensation is not required after filtering. Simulations using ATP were performed to evaluate the performance of the proposed filter method, and the results were compared to the ones obtained by conventional methods.

Comparison of Extraction Procedures for the Determination of Capsaicinoids in Peppers

  • Jeon, Geonuk;Lee, Jun-Soo
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1515-1518
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    • 2009
  • The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.