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Polyelectrolyte Multilayer Film Coating and Stability at the Surfaces of Oral Prosthesis Base Polymers: an in vitro and in vivo Study

O. Etienne1,2, C. Picart1, C. Taddei2, P. Keller1, E. Hubsch3, P. Schaaf3, J.C. Voegel1, Y. Haikel2, J.A. Ogier1, and C. Egles1,*

1 Institut National de la Santé et de la Recherche Médicale, Unité 595, 11, rue Humann, 67085 Strasbourg Cedex, France;
2 Faculté de Chirurgie Dentaire, Université Louis Pasteur, 1, Place de l’hôpital, 67000 Strasbourg, France; and
3 Institut Charles Sadron, UPR 22 CNRS, 6 rue Boussingault, 67083 Strasbourg Cedex, France



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Figure 1. Construction and characterization of the polyelectrolyte multilayer films. (A) Diagram of development and structure of a multilayer film based on the alternate deposition of polyanions (grey) and polycations (black). (B) Build-up of a Pre-(PGA-PLL)9 multilayer film, followed by quartz crystal microbalance (QCM) assessment. Global increase in the adsorbed mass is shown by the exponential increase in frequency shift ({Delta}f at 15 Hz, {nu} = 3). The exponential regression follows the function: y = y0 + Aexp(Bx) (with y0 = –398.7, A = 431.8, B = 0.1, R = 0.999). (C) Vertical section obtained by confocal laser scanning microscopy (CLSM) observation through a Pre-(PGA-PLL)20-PGA-PLLFITC film on a glass substrate. The film thickness is about 1 µm.

 


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Figure 2. Film presence on polymer surfaces. (A–E) Topography is observed by ESEM images (scale bars, 50 µm [x400]; inlays, 10 µm [x1600]). Below each main picture is a representation of the corresponding image of a CSLM vertical section of the polyelectrolyte film. G, comparative measurements of static contact angles. The smaller the contact angles, the greater the wettability.

 


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Figure 3. Stability of the polyelectrolyte multilayer films in saliva. (A) QCM measurements show no changes in -{Delta}f/{nu} for 1000 min in saliva, while the detergent totally removed the film in seconds (arrow). (B,C) CLSM vertical sections through a Pre-(PGA-PLL)20-PGA-PLLFITC film, after 48 hrs in 0.15 M NaCl (B) or in saliva (C). (D,E) Top view of a Pre-(PGA-PLL)20-PGA-PLLFITC film observed by fluorescent microscopy before (D) and after (E) 7 days in saliva. The film was scratched so that its integrity could be followed.

 


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Figure 4. In vivo experiments in rats. PMMA discs were coated with Pre-(PGA-PLL)20-PGA-PLLFITC film, by an automated dipping process, to ensure a full coating (A) and were sutured to the rat’s cheek (B). The CSLM image (115 x 115 µm) of the disc surfaces after 4 days in the rat’s mouth, showing the film still intact and entirely covering the disc on the mucosal side (C), while only fragments are visible on the lingual side of the specimen (D). Scale bars: 10 µm.

 





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