• Title/Summary/Keyword: Solid-phase Extraction

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Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) Analysis of Liquid Crystalline Mixtures

  • Park, Gregory Hyung-Jin;Park, Ae-Na;Rho, Kyung-Rae;Shin, Jong-Ho;Kim, Yeong-Jeon;Jo, Sung-Chan;Oh, Weon-Sik
    • Journal of the Korean Magnetic Resonance Society
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    • v.15 no.1
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    • pp.14-24
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    • 2011
  • We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.

GC/MS-SIM for the Determination of Alkylphenols, Chlorophenols and Bisphenol A in Paper Materials

  • Kim, Hyub
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.05a
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    • pp.145-145
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    • 2003
  • A method for the determination of alkylphenols, chlorophenols and bisphenol A in paper materials using GC/MS-SIM has been developed. Eleven endocrine disrupting chemicals (EDCs) of phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 82.4∼108.8 % by area ratio of pheranthrene-d$\sub$10/ vs bisphenol A d$\sub$l6/. (isoBOC derivatization and TBDMS derivatization) The SIM responses were linear with the correlation coefficient varying 0.9717∼0.9995 (isoBOC derivatization), and 0.9842∼0.9980 (TBDMS derivatization). The range of concentrations was respectively, 0.95∼l.44 ng/g in 2,4-dichlorophenol, 1.01∼1.17 ng/g in t-butylphenol, 2.17∼5.84 ng/g in pentachlorophenol, 12.68∼14.88 ng/g in nonylphenol and 30.84∼153.72 ng/g in bisphenol A.

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Simultaneous quantitation of enalapril and enalaprilat in human plasma by high-throughput solid phase extraction and liquid chromatography/tandem mass spectrometry

  • Son, Jung-Hyun;Lee, Jae-Ick;Kim, Dong-Hyun
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.401.3-402
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    • 2002
  • Enalapril (ENP) maleate is effective drug for the treatment of renivascular hypertension and heart failure. ENP acts as inhibitor of the enzyme angiotensin-convertase (ACE-inhibitor) and metabolized to enalaprilat (ENPT), which is the active metabolite that is really responsible for the therapeutic action. In the present study, a sensitive and rapid liquid chromatography/ electrospray ion trap tandem mass spectrometry (LC/MS/MS) method combined with high-throughput solid phase extraction (SPE) has been developed and validated for the simultaneous quantitative determination of ENP and ENPT in human plasma. (omitted)

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The Evaluation of Solid-Phase Microextraction(SPME) Techniques for Analyzing Mixed Fuel Oxygenates and Products

  • 이재선;이시진;장순웅
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.09a
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    • pp.458-461
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    • 2003
  • Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

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Part-Per-Trillion level determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water

  • Kim, Hyub
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.10a
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    • pp.149-149
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    • 2003
  • A new technique is proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert.-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6∼105.2 % (isoBOC derivatization) and 97.6∼484.5 % (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001∼0.050 $\mu\textrm{g}$/l (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/l (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). The derivative methods and their application to tap water samples will be disscussed.

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Determination of fungicides in wines by solid-phase extraction and gas chromatography with mass selective detection (고체상 추출법과 GC/MS를 이용한 포도주 중의 fungicides 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.438-442
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    • 2003
  • The fungicides, used for grape growth and remained in the wine products from domestic and foreign countries such as vinclozolin, dichlofluanid, penconazole, procymidone were quantitatively analyzed after solid-phase extraction using a GC/MS-SIM method. The results obtained were as follows: for all the samples, the content of procymidone was in the range from 2.2 to $76.1{\mu}g/L$, recoveries 81.3-93.1 %, and standard deviation 1.4-3.4 %.

Selective Concentration and Determination of Phenol and Chlorophenols by Solid Phase Extraction

  • Jung, Min-Woo;Lee, Dai Woon;Paeng, Ki-Jung
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.535-538
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    • 1995
  • This study employs the variety of mixtures of XAD resin and active carbons as concentration base for solid phase extraction (SPE) which has been widely used to preconcentrate and purify phenol and chlorophenols in determination of environmental water samples. In this study, we employed variety of mixtures of copolymer based XAD-4 resin with active carbons. This cartridges shows advantages of both materials, such as better affinity to phenol by active carbon and better mechanical stabilities from XAD resin. The better enrichment factor, pretreatment time, recoveries and limit of detection (LOD) were achieved by the attempts to pack precolumns with both meterials for preconcentration.

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On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

Determination of Histamine in a Pharmaceutical Preparation after Clean-Up by Solid- Phase Extraction

  • Kim, Chang-Soo;Kim, Naml-Lee;Jeong, Min-Gyo;Hong, Seung-Hwa;Moon, Dong-Cheul
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.397.1-397.1
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    • 2002
  • A human immune globulin preparation (histobulin\ulcorner) are made to bind a small amount of histamine (0.15 $\mu$g) to the protein (12 mg) to increase the resistance of histamine susceptibility in the treatment of allergic diseases. Strict control of histamine content of the drug are required since intake of histamine might result in hypo- or hypertension. headache. or anaphylactic shock syndromes. HPLC analytical method with pre-column fluorescent derivatizalion after clean-up by solid-phase extraction (SPE) was developed. (omitted)

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Characterization of Natural Organic Matter in Spring Water

  • Yoo, Hee-Jin;Choi, Yoon-Ji;Cho, Kun
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.90-94
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    • 2020
  • Interest in aspects of industrialization relating to human health has increased. Accordingly, the use of labels such as 'natural foods' and 'organic ingredients' has become more widespread, and greater emphasis is being placed on improving quality of life. Water is an essential element for human life, and water quality has a significant impact on human health. However, technology that can precisely determine the substances present in water is still lacking. This study was conducted to establish a complete mass spectrometry process, from pretreatment to analysis, to measure and characterize natural organic matter (NOM) in Korean spring water samples. Salts and other matrices were removed from the samples using solid-phase extraction (SPE) with two different columns (PPL and C18). After establishing an accurate analysis method, the experimental results were evaluated based on Van Krevelen diagrams and analysis of molar O/C and H/C ratios. The method for characterizing NOM introduced herein should facilitate evaluation of water quality.