• Title/Summary/Keyword: Liquid Liquid Extraction

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Spectrophotometric Determination of Palladium after Solid-liquid Extraction with 4-(2-Pyridylazo)-resorcinol at 90°C

  • Dong, Yanjie;Gai, Ke
    • Bulletin of the Korean Chemical Society
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    • v.26 no.6
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    • pp.943-946
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    • 2005
  • An effective spectrophotometric determination of palladium with 4-(2-pyridylazo)-resorcinol (PAR) using molten naphthalene as a diluent has been studied. A red complex of palladium with PAR is formed at 90 ${^{\circ}C}$. In the range of pH 9.0-11.0, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in $CHCl_3$ to be determined spectrophotometrically at 520 nm against the reagent blank. Beer’s law is obeyed over the concentration range of 0.1-2 ${\mu}g{\cdot}mL^{-1}$. The molar absorptivity and Sandell’s sensitivity are 8.0 ${\times}\;10^5\;L{\cdot}mol^{-1}{\cdot}cm^{-}1\;and\;0.49\;{\mu}g{\cdot}cm^{-2}$ respectively. From the results of tolerance limits, it was found that there was no interferences were observed for most of the ions examined and those somewhat high interferences by Co(II), Fe(II) and Bi(III) could be effectively masked by EDTA.

Uranium Analysis in Aqueous Samples by Selective Extraction and Photon-Electron Rejecting Alpha Liquid Scintillation $(PERALS^\circledR)$ Spectrometry

  • Shin, Hyun-Sang;Lee, Myung-Ho;Park, Geun-Sik;Lee, Chang-Woo
    • Nuclear Engineering and Technology
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    • v.31 no.5
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    • pp.445-454
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    • 1999
  • This work describes the adaptation of extractive scintillation by URAE $X^{TM}$ with a photon-electron rejecting alpha liquid scintillation (PERAL $S^{)}$ spectrometer to the analysis of uranium in aqueous samples. The extraction efficiency of the system was evaluated under varing chemical conditions including pH, and sample-cocktail volume ratio. Isotopic information from the (PERAL $S^{)}$ spectrum of natural uranium was obtained using a curve fitting routine. Comparisons of the result with that obtained from alpha spectrometry method using ion implanted silicon detector showed good agreement.t.

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Analysis of Entamoeba histolytica Membrane via LC-MALDI-TOF/TOF

  • Ujang, Jorim Anak;Noordin, Rahmah;Othman, Nurulhasanah
    • Mass Spectrometry Letters
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    • v.10 no.3
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    • pp.84-87
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    • 2019
  • Liquid chromatography mass spectrometry is widely employed in proteomics studies. One of such instruments is the Liquid Chromatography (LC)-Matrix-assisted laser desorption ionisation (MALDI)-Time of flight (TOF) or LC-MALDI-TOF/TOF. In this study, this instrument was used to identify the membrane proteins of a protozoan parasite namely Entamoeba histolytica. It causes amoebiasis in human. The E. histolytica trophozoites were cultured prior to the membrane protein extraction using the conventional method, $ProteoPrep^{(R)}$ and $ProteoExtract^{(R)}$ kits. Then, the membrane protein extracts were trypticdigested and analysed by LC-MALDI-TOF/TOF. Approximately, 194 proteins were identified and 27.8% (54) were predicted as membrane proteins having 1 to 15 transmembrane regions and signal peptides by combining all three extraction methods. Also, this study has discovered 3 unique proteins as compared to our previous study which merit further investigation.

Determination of lisinopril in human plasma by liquid chromatography tendem mass spectrometry and its application to human bioavailibility study

  • Shim, Hee-Ok;Kim, Dong-Chul
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.239.1-239.1
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    • 2003
  • This study was to develop a quantification method of lisinopril using liquid chromatography tendem mass spectrometry in human plasma. Quntitation of lisinopril by MRM(multiple reaction monitoring) in the electrospray positive mode was validated according to FDA guideline. Extraction of lisinopril and enalapril as internal standard from plasma was perfomed by means solide phase extraction. The calibration curve of lisinopril showed a good linerarity in the concentration range 2∼200ng/ml. The coefficients of variations for the inter-day and intra-day precision was less than 15%, and the inter-day and intra-day accuracy was 97.6∼101.0%. (omitted)

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Determination of Grayanotoxin I and Grayanotoxin III in mad honey from Nepal using liquid chromatography-tandem mass spectrometry

  • Ahn, Su Youn;Kim, Suncheun;Cho, Hwangeui
    • Analytical Science and Technology
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    • v.35 no.2
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    • pp.82-91
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    • 2022
  • Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquid-chromatography-tandem-mass-spectrometric method (LC-MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 ㎍/g. The intra- and inter-day deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 - 64.86 ㎍/g and 0.25 - 63.99 ㎍/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.

Quantification of Three Prohibited Anabolic-Androgenic Steroids in Equine Urine using Gas Chromatography-Tandem Mass Spectrometry

  • Young Beom Kwak;Shaheed Ur Rehman;Hye Hyun, Yoo
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.104-109
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    • 2023
  • Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

Bisphenol A and other alkylphenols in the environment - occurrence, fate, health effects and analytical techniques

  • Zhu, Zhuo;Zuo, Yuegang
    • Advances in environmental research
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    • v.2 no.3
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    • pp.179-202
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    • 2013
  • Bisphenol A and other alkylphenols are widely used in plastic and other industrial consumer products. Release of these compounds into the aquatic environment during their manufacture, use and disposal has been a great scientific and public concern due to their toxicity at high concentrations and endocrine disrupting effects at low concentration on aquatic wildlife and human beings. This paper reviews the published data and researches on the environmental occurrence, distribution, health effects and analytical techniques of bisphenol A and alkylphenols. The aim is to provide an overview of the current understanding about bisphenol A and alkylphenols in the environment and the difficulties faced today in order to establish standard and systematic environmental analysis and assessment process for these endocrine disruptor compounds.

Modified Poly(3,4-ethylenedioxythiophene) with Poly(ionic liquid)s as a new hole injecting materials in organic light emitting diodes (OLEDs)

  • Kim, Earl;Kim, Tae-Young;Suh, Kwang-Seok
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.132-132
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    • 2010
  • In a previous report, we demonstrated that poly (3,4-ethylenedioxythiophene) derived from poly (ionic liquid) (PEDOT:PIL) constitutes a polymeric hole-injecting material capable of improving device lifetime in organic light-emitting diodes (OLEDs).was attributed to aprotection characteristic of PEDOT:PIL for the indium extraction from ITO electrodes, which frequently occurrs in the OLED device with the conventional PEDOT materials. In this study, we report the OLED device lifetime as well asvice efficiencycan be further improved with the modified PEDOT:PIL in whichorganic compounds are incorporated. The deviced performance will be presented in terms of device lifetime and efficiencies.

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Isoflavonoids from the liquid media of Bacillus licheniformis (Bacillus licheniformis 배지의 Isoflavonoids)

  • 이학주;박영기;이재필;이상현;여운홍
    • Journal of Korea Foresty Energy
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    • v.20 no.2
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    • pp.28-33
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    • 2001
  • Using liquid media of Bacillus licheniformis, extraction with butanol and fractionation with n-hexane and ethyl acetate(EtOAc) were performed, From the EtOAc fraction, the isolation was also performed using chromatography. Three isoflavonoids were isolated from the liquid media of Bacillus licheniformis and identified as diadzein, genistein and genistin by Mass and NMR spectroscopic analysis.

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Development of the Continuous and Instantaneous Light liquid-Heavy liquid Centrifugal Separator using Density Difference (밀도 차를 이용한 경액과 중액의 연속 순간 원심분리기 개발)

  • 김영환;윤지섭;정재후;홍동희;박기용
    • Proceedings of the Korean Society of Precision Engineering Conference
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    • 2001.04a
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    • pp.655-659
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    • 2001
  • Resident time of the continuous and Instantaneous centrifugal separator using that separates the light and heavy liquids by use of density difference is the orptical factor that affects significantly the chemical metial extraction and the productivity in the chemical and mechanical process. In this paper, the overflow of the device is investigated under consideration of the relationships between inclination angle of liquid feeding screw and the centrifugal force. From the design of the length of a centrifugal separator, the radiuses of rotor and housing, theoretical formulation on the contact radius of separation weir is established through the experiments. From the experiments, it is identified that how much the capacity of inlet impeller and the emulsion phenomenon depend on the screw angle of inlet impeller. Also, we investigate the separation condition and the resident times that are functions of the phase ratio and density.

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