• Title, Summary, Keyword: derivatization

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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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    • 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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Chiral Separation of ${\beta}-Blockers$ after Derivatization with a New Chiral Derivatization Agent, GATC

  • Ko, Mi-Young;Shin, Dae-Hong;Oh, Joung-Weon;Asegahegn, Workaferhaw Shibru;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.29 no.11
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    • pp.1061-1065
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    • 2006
  • A new chiral derivatization agent with sugar moiety, 2,3,4,6-tetra-O-acetyl-${\beta}$-D-galactopyranosyl isothiocyanate (GATC) was synthesized. Several ${\beta}-blockers$ were investigated for the possible separation of the enantiomers by reversed-phase HPLC after derivatization with this new chiral derivatization agent (GATC). GATC was reacted readily with ${\beta}-blockers$ at room temperature and the reaction mixture could directly be injected into the HPLC system. The corresponding diastereomers were well resolved on an ODS column with acetonitrile-ammonium acetate buffer as a mobile phase and monitored at UV 254 nm. The optimization of the derivatization procedure (concentration of GATC, reaction temperature and time) and HPLC conditions (pH and ionic strength of mobile phase) were investigated and compared with GITC.

Chiral separation of $\beta$-agonists after derivatization with a new chiral derivatization agent, GATC

  • Min, Kyeong-Il;Ko, Mi-Young;Kim, Kyeong-Ho
    • Proceedings of the PSK Conference
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    • pp.275.2-275
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    • 2003
  • Several ${\beta}$-agonists were investigated for the possible separation of the enantiomers by reversed-phase high-performance liquid chromatography after derivatization with a new chiral derivatization agent, GATC. The derivatization proceeded quantitatively within 1 h at room temperature. The corresponding diastereomers were well resolved an ODS column with acetonitrile-acetate buffers a mobile phase and monitored at UV 254nm. (omitted)

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Sensitive Determination of Alkylphenols, Chlorophenols, and Bisphenol A using GC/MS-SIM in Paper Materials (기체 크로마토그래피/질량분석기를 이용한 종이류 중 알킬페놀류, 클로로페놀류 및 비스페놀 A 정량)

  • Kim, Hyub;Kim, Jin-Ho
    • Environmental health and toxicology
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    • v.18 no.1
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    • pp.45-55
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    • 2003
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven 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 SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8%) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 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.

Part-Per-Trillion Level Determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water Samples (GC/MS-SIM 방법에 의한 수돗물 중 알킬페놀, 플로로페놀과 비스페놀 A의 ppt 정량)

  • Kim, Hyub
    • Environmental health and toxicology
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    • v.18 no.3
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    • pp.199-208
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    • 2003
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. 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 CC/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 h for SIM were 0.001∼0.050 $\mu\textrm{g}$/1 (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/1 (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). When these methods were applied to tap water samples, the range of concentrations were 22.8∼31.3 ng/1 in 2,4-dichlorophenol, 28.6∼70.3 ng/1 in pentachlorophenol, 15.2∼17.4 ng/1 in t-butylphenol, 10.8∼13.2 ng/1 in t-octylphenol and 17.6∼36.3 ng/l in bisphenol A, respectively.

Reversed-Phase High Performance and Liquid Chromatographic Separation of the Enantiomers of Terbutaline by Derivatization with 2,3,4-Tetra-o-acetyl-\beta-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Kim, Dong-Sig;Hong, Seon-Pyo;Keon, Oh-Seung
    • Archives of Pharmacal Research
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    • v.23 no.1
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    • pp.26-30
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    • 2000
  • The enantiomers of the bronchodilator terbutaline were separated by reversed-phase high performance liquid chromatograhy after derivatization with 2,3,4,6-tetra-O-acetyl-\beta-D-glucopyranosyl isothiocyanate(GITC) reagent. The derivatization proceeded quantitatively within 1 h at room temperature. The corresponding diastereomeric thiourea derivatives were well resolved on an ODS column with acetonitrile-acetate buffer as a mobile phase. Elution orders of the diastereomers were confirmed by derivatization of R-(-)-terbutaline and S-(+)-terbutaline which were collected by semi-preparative chiral HPLC using Sumichiral OA-4700 column. The native fluorescence of terbutaline was quenched by derivatization with GITC. The detection limit was 25ng when monitored at UV 278 nm.

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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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    • 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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Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1497-1504
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    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

Chiral Separation of $\beta$-Blockers after Derivatization with (-)-Menthyl chloroformate by Reversed-Phase High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Choi, Pok-Wha;Hong, Seon-Pyo;Kim, Hyun-Ju
    • Archives of Pharmacal Research
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    • v.22 no.6
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    • pp.608-613
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    • 1999
  • Optimum conditions of chiral derivatization reaction of $\beta$-blockers (acebutolol, arotinolol, betaxolol, bisoprolol, celiprolol, metoprolol and pindolol) with (-)-menthyl chloroformate were investigated for the resolution by HPLC. With more than 30 times molar excess of (-)-methyl chloroformate chiral derivatization reactions were completed within one hour at room temperature except arotinolol and celiprolol. Diastereomeric derivatives of $\beta$-blockers were well resolved on the ODS column using acetonitrile-methanol-water as a mobile phase.

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Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization

  • Pyo, Jae-Sung;Lee, Hee-Sang;Park, Yu-Jin;Jo, Ji-Yeong;Park, Yong-Hoon;Choe, Sang-Gil;Lee, Mi-Young;Lee, Jae-Sin
    • Mass Spectrometry Letters
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    • v.3 no.1
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    • pp.15-17
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    • 2012
  • Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.