Luc D Randolph1, William M Palin2, Sabine Bebelman3, Jacques Devaux3, Bernard Gallez4, Gaetane Leloup5, Julian G Leprince5. 1. Louvain Drug Research Institute, Université catholique de Louvain, Brussels, Belgium; Institute of Condensed Matter and Nanosciences, Bio- and Soft- Matter, Université catholique de Louvain, Louvain-la-Neuve, Belgium; CRIBIO (Center for Research and Engineering on Biomaterials), Brussels, Belgium. Electronic address: lucrandolph@gmail.com. 2. Biomaterials Unit, University of Birmingham, College of Medical and Dental Sciences, School of Dentistry, St Chad's Queensway, Birmingham B4 6NN, UK. 3. Institute of Condensed Matter and Nanosciences, Bio- and Soft- Matter, Université catholique de Louvain, Louvain-la-Neuve, Belgium; CRIBIO (Center for Research and Engineering on Biomaterials), Brussels, Belgium. 4. Louvain Drug Research Institute, Université catholique de Louvain, Brussels, Belgium; CRIBIO (Center for Research and Engineering on Biomaterials), Brussels, Belgium. 5. Louvain Drug Research Institute, Université catholique de Louvain, Brussels, Belgium; Institute of Condensed Matter and Nanosciences, Bio- and Soft- Matter, Université catholique de Louvain, Louvain-la-Neuve, Belgium; CRIBIO (Center for Research and Engineering on Biomaterials), Brussels, Belgium; School of Dentistry and Stomatology, Université catholique de Louvain, Brussels, Belgium.
Abstract
OBJECTIVES: To test the null hypotheses that photoactive resin composites containing a Type I photoinitiator would exhibit reduced DC or increased monomer elution at substantially short curing times compared with materials based on a Type 2 ketone/amine system. METHODS: Two experimental resin composites were prepared, using either Lucirin-TPO or camphorquinone/DMAEMA. Specimens were light-cured using appropriate spectral emission that coincided with the absorption properties of each initiator using different irradiation protocols (0.5, 1, 3, 9s at 500, 1000 and 2000mW/cm(2) for Lucirin-TPO based composites and 20 or 40s at 1000mW/cm(2) for Lucirin-TPO and camphorquinone-based composites). Degree of conversion (DC) was measured by Raman spectroscopy, propagating radical concentrations were collected by means of electron paramagnetic resonance (EPR) and monomer leaching was characterized using high-performance liquid chromatography (HPLC). RESULTS: The null hypotheses were rejected, except for a single irradiation protocol (0.5s @ 500mW/cm(2)). Lucirin-TPO-based composites could cure 20 times faster and release at least 4 times less monomers in comparison to camphorquinone-based composites. At 1000mW/cm(2), and 1s irradiation time for curing times of 1s, Lucirin-TPO based composites displayed 10% higher DC. The difference in polymerization efficiency of Lucirin-TPO compared with camphorquinone-based resin composites were explained using EPR; the former showing a significantly greater yield of radicals which varied logarithmically with radiant exposure. SIGNIFICANCE: Lucirin-TPO is substantially more efficient at absorbing and converting photon energy when using a curing-light with an appropriate spectral emission and otherwise a limitation noted in several previous publications. At concentrations of 0.0134mol/L, Lucirin-TPO-based composites require a minimum light intensity of 1000mW/cm(2) and an exposure time of 1s to provide significantly improved DC and minimal elution compared with a conventional photoinitiator system. The use of a wide range of curing protocols in the current experiment has realized the significant potential of Lucirin-TPO and its impact for clinical applications, in replacement to materials using camphorquinone.
OBJECTIVES: To test the null hypotheses that photoactive resin composites containing a Type I photoinitiator would exhibit reduced DC or increased monomer elution at substantially short curing times compared with materials based on a Type 2 ketone/amine system. METHODS: Two experimental resin composites were prepared, using either Lucirin-TPO or camphorquinone/DMAEMA. Specimens were light-cured using appropriate spectral emission that coincided with the absorption properties of each initiator using different irradiation protocols (0.5, 1, 3, 9s at 500, 1000 and 2000mW/cm(2) for Lucirin-TPO based composites and 20 or 40s at 1000mW/cm(2) for Lucirin-TPO and camphorquinone-based composites). Degree of conversion (DC) was measured by Raman spectroscopy, propagating radical concentrations were collected by means of electron paramagnetic resonance (EPR) and monomer leaching was characterized using high-performance liquid chromatography (HPLC). RESULTS: The null hypotheses were rejected, except for a single irradiation protocol (0.5s @ 500mW/cm(2)). Lucirin-TPO-based composites could cure 20 times faster and release at least 4 times less monomers in comparison to camphorquinone-based composites. At 1000mW/cm(2), and 1s irradiation time for curing times of 1s, Lucirin-TPO based composites displayed 10% higher DC. The difference in polymerization efficiency of Lucirin-TPO compared with camphorquinone-based resin composites were explained using EPR; the former showing a significantly greater yield of radicals which varied logarithmically with radiant exposure. SIGNIFICANCE: Lucirin-TPO is substantially more efficient at absorbing and converting photon energy when using a curing-light with an appropriate spectral emission and otherwise a limitation noted in several previous publications. At concentrations of 0.0134mol/L, Lucirin-TPO-based composites require a minimum light intensity of 1000mW/cm(2) and an exposure time of 1s to provide significantly improved DC and minimal elution compared with a conventional photoinitiator system. The use of a wide range of curing protocols in the current experiment has realized the significant potential of Lucirin-TPO and its impact for clinical applications, in replacement to materials using camphorquinone.