Solid Phase Chemiluminescence Detection Reactors Based on in Situ Polymerized Methacrylate Materials

Abstract

In situ photopolymerized macroporous poly(glycidyl methacrylate-co-trimethylolpropane trimethacrylate) materials, which were prepared in a full factorial experimental synthesis design, were investigated as supports in solid phase chemiluminescence detection reactors. The reactors based on in situ polymerized supports showed higher light generation efficiency than packed bed reactors when evaluated in a flow system based on 1,1′-oxalyldiimidazolyl peroxyoxalate chemiluminescence detection of hydrogen peroxide, with 3-aminofluoranthene (3-AFA) as the immobilized light emitter. The results were correlated with the physical characteristics of the materials, and the efficiency was found to correlate with the amount of accessible reactive groups. A lower functionalization density was found to increase the peak area sensitivity for hydrogen peroxide in the flow system. This is explained by inner filtering. The peak height sensitivities were less influenced, indicating that the total system efficiency was limited by homogeneous reaction kinetics. The introduction of a spacer to mimic "pseudosolution" conditions of the bound 3-AFA moiety was found to decrease the light generation ability.

Preparation of methacrylate monoliths

“…One of the most popular functional monomers is glycidyl methacrylate (GMA) [9,28,37,39]. Its major advantage is the presence of reactive epoxy groups in its structure that facilitates modification in order to prepare a wide range of functional materials.…”

“…Alternatives to EDMA are diethylene and triethylene glycol dimethacrylates (DEGDMA and TEGDMA, respectively) [37,54], trimethylolpropane trimethacrylate (TRIM) [37,39,42], glycerol dimethacrylate (GDMA) [49,59], and 1,4-butanediol dimethacrylate (BDDMA) [49]. Sometimes a mixture of crosslinkers is used for preparation of the methacrylate monoliths.…”

Preparation and HPLC applications of rigid macroporous organic polymer monoliths

“…These applications cover a rather broad range from heterogenized catalysts [66, 71, 82 -87], detection [88], solid-phase extraction [41,89], polymer-supported chemistry [90,91], molecular imprinting [92 -99], to a variety of separations including gas chromatography [100], HPLC, and CEC. Most of these applications have been summarized in a recently published monograph [16].…”

Rigid Macroporous Polymer Monoliths

“…Typically, these experiments are performed using reactors packed with beads that have fluorophores bound to their surface. PontØn et al [83] have reported the use of glycidyl methacrylate-trimethylolpropane trimethacrylate (TRIM, 11) monoliths prepared by photopolymerization within a quartz tube. Both the surface area and degree of functionality of the resulting polymers could easily be adjusted by making changes in the composition of the original polymerization mixture.…”