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Synthesis of a reactive polymethacrylate capillary monolith and its use as a starting material for the preparation of a stationary phase for hydrophilic interaction chromatography

Kip, Cigdem; Erkakan, Damla; Gokaltun, Aslihan; Celebi, Bekir; Tuncel, Ali


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        "affiliation": "Hacettepe Univ, Dept Chem Engn, TR-06532 Ankara, Turkey", 
        "name": "Kip, Cigdem"
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      {
        "affiliation": "Hacettepe Univ, Dept Chem Engn, TR-06532 Ankara, Turkey", 
        "name": "Erkakan, Damla"
      }, 
      {
        "affiliation": "Hacettepe Univ, Dept Chem Engn, TR-06532 Ankara, Turkey", 
        "name": "Gokaltun, Aslihan"
      }, 
      {
        "affiliation": "Hacettepe Univ, Dept Chem Engn, TR-06532 Ankara, Turkey", 
        "name": "Celebi, Bekir"
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      {
        "name": "Tuncel, Ali"
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    "description": "Poly(3-chloro-2-hydroxypropyl methacrylate-co-ethylene dimethacrylate), poly(HPMA-Cl-co-EDMA) capillary monolith was proposed as a reactive starting material with tailoring flexibility for the preparation of monolithic stationary phases. The reactive capillary monolith was synthesized by free radical copolymerization of 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl) and ethylene dimethacrylate (EDMA). The mean pore size, the specific surface area and the permeability of poly(HPMA-Cl-co-EDMA) monoliths were controlled by adjusting porogen/monomer volume ratio, porogen composition and polymerization temperature. The porogen/monomer volume ratio was found as the most effective factor controlling the porous properties of poly(HPMA-Cl-co-EDMA) monolith. Triethanolamine (TEA-OH) functionalized polymethacrylate monoliths were prepared by using the reactive chloropropyl group of poly(HPMA-Cl-co-EDMA) monolith via one-pot and simple post-functionalization process. Poly(HPMA-Cl-co-EDMA) monolith reacted with TEA-OH was evaluated as a stationary phase in nano-hydrophilic interaction chromatography (nano-HILIC). Nucleotides, nucleosides and benzoic acid derivatives were satisfactorily separated with the plate heights up to 20 mu m. TEA-OH attached-poly(HPMA-Cl-co-EDIVIA) monolith showed a reproducible and stable retention behaviour in nano-HILIC runs. However, a decrease in the column performance (i.e. an increase in the plate height) was observed with the increasing retention factor. Hence \"retention-dependent column efficiency\" behaviour was shown for HILIC mode using the chromatographic data collected with the polymer based monolith synthesized. (C) 2015 Elsevier B.V. All rights reserved.", 
    "doi": "10.1016/j.chroma.2015.04.005", 
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      "pages": "86-97", 
      "title": "JOURNAL OF CHROMATOGRAPHY A", 
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    "title": "Synthesis of a reactive polymethacrylate capillary monolith and its use as a starting material for the preparation of a stationary phase for hydrophilic interaction chromatography"
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