Comparison on photo-initiators for the preparation of methacrylate monolithic columns for capillary electrochromatography

The synthesis of lauryl methacrylate monoliths for capillary electrochromatography by UV polymerization using several free-radical initiators (α,α′-azobisisobutyronitrile, 2,2-dimethoxy-2-phenylacetophenone, dibenzoyl peroxide (BPO) and lauroyl peroxide (LPO)) has been investigated. Using a 1,4-buta...

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Veröffentlicht in:Journal of Chromatography A 2010-05, Vol.1217 (19), p.3231-3237
Hauptverfasser: Bernabé-Zafón, V., Beneito-Cambra, M., Simó-Alfonso, E.F., Herrero-Martínez, J.M.
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container_end_page 3237
container_issue 19
container_start_page 3231
container_title Journal of Chromatography A
container_volume 1217
creator Bernabé-Zafón, V.
Beneito-Cambra, M.
Simó-Alfonso, E.F.
Herrero-Martínez, J.M.
description The synthesis of lauryl methacrylate monoliths for capillary electrochromatography by UV polymerization using several free-radical initiators (α,α′-azobisisobutyronitrile, 2,2-dimethoxy-2-phenylacetophenone, dibenzoyl peroxide (BPO) and lauroyl peroxide (LPO)) has been investigated. Using a 1,4-butanediol/1-propanol mixture as porogenic solvent, the influence of each initiator and its content on the morphological and electrochromatographical properties of beds was evaluated. Under their respective optimum content, satisfactory separations of a test mixture of PAHs with similar efficiencies (minimum plate heights of 8.0–12.7 μm obtained from Van Deemter plots) were achieved for the four investigated photo-initiators. The columns photo-polymerized with LPO provided the best compromise between chromatographic performance and analysis time. Moreover, this initiator showed a fine control in the column retention properties. The resulting monolithic columns exhibited a good run-to-run repeatability in the tested chromatographic parameters (RSD < 2.4%) for all initiators investigated; and satisfactory column-to-column repeatability (RSD < 6.0%), except for beds photo-polymerized with BPO (RSD < 10.8%).
doi_str_mv 10.1016/j.chroma.2009.08.075
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Using a 1,4-butanediol/1-propanol mixture as porogenic solvent, the influence of each initiator and its content on the morphological and electrochromatographical properties of beds was evaluated. Under their respective optimum content, satisfactory separations of a test mixture of PAHs with similar efficiencies (minimum plate heights of 8.0–12.7 μm obtained from Van Deemter plots) were achieved for the four investigated photo-initiators. The columns photo-polymerized with LPO provided the best compromise between chromatographic performance and analysis time. Moreover, this initiator showed a fine control in the column retention properties. The resulting monolithic columns exhibited a good run-to-run repeatability in the tested chromatographic parameters (RSD &lt; 2.4%) for all initiators investigated; and satisfactory column-to-column repeatability (RSD &lt; 6.0%), except for beds photo-polymerized with BPO (RSD &lt; 10.8%).</description><identifier>ISSN: 0021-9673</identifier><identifier>EISSN: 1873-3778</identifier><identifier>DOI: 10.1016/j.chroma.2009.08.075</identifier><identifier>PMID: 19762033</identifier><identifier>CODEN: JOCRAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>2,2-Dimethoxy-2-phenylacetophenone ; Acetophenones - chemistry ; Analytical chemistry ; Benzoyl peroxide ; Benzoyl Peroxide - chemistry ; Capillary electrochromatography ; Capillary Electrochromatography - methods ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Exact sciences and technology ; Lauroyl peroxide ; Lauryl methacrylate ; Lipid Peroxides - chemistry ; Methacrylates - chemical synthesis ; Methacrylates - chemistry ; Microscopy, Electron, Scanning ; Nitriles - chemistry ; Other chromatographic methods ; Photo-initiators ; Photochemistry - methods ; Reproducibility of Results ; UV initiation ; α,α′-Azobisisobutyronitrile</subject><ispartof>Journal of Chromatography A, 2010-05, Vol.1217 (19), p.3231-3237</ispartof><rights>2009 Elsevier B.V.</rights><rights>2015 INIST-CNRS</rights><rights>Copyright (c) 2009 Elsevier B.V. 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The resulting monolithic columns exhibited a good run-to-run repeatability in the tested chromatographic parameters (RSD &lt; 2.4%) for all initiators investigated; and satisfactory column-to-column repeatability (RSD &lt; 6.0%), except for beds photo-polymerized with BPO (RSD &lt; 10.8%).</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>19762033</pmid><doi>10.1016/j.chroma.2009.08.075</doi><tpages>7</tpages></addata></record>
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subjects 2,2-Dimethoxy-2-phenylacetophenone
Acetophenones - chemistry
Analytical chemistry
Benzoyl peroxide
Benzoyl Peroxide - chemistry
Capillary electrochromatography
Capillary Electrochromatography - methods
Chemistry
Chromatographic methods and physical methods associated with chromatography
Exact sciences and technology
Lauroyl peroxide
Lauryl methacrylate
Lipid Peroxides - chemistry
Methacrylates - chemical synthesis
Methacrylates - chemistry
Microscopy, Electron, Scanning
Nitriles - chemistry
Other chromatographic methods
Photo-initiators
Photochemistry - methods
Reproducibility of Results
UV initiation
α,α′-Azobisisobutyronitrile
title Comparison on photo-initiators for the preparation of methacrylate monolithic columns for capillary electrochromatography
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