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C HARACTERIZATION OF S OLID L IPID N ANOPARTICLES

C HARACTERIZATION OF S OLID L IPID N ANOPARTICLES. Cécile Allais # , F. Artzner # , T. Narayanan § , T. Gulik-Krzywicki ‡ , G. Keller # and M. Ollivon # # Equipe de Physico-Chimie des Systèmes Polyphasés, UMR CNRS 8612, Faculté de Pharmacie,

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C HARACTERIZATION OF S OLID L IPID N ANOPARTICLES

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  1. CHARACTERIZATIONOFSOLIDLIPIDNANOPARTICLES Cécile Allais#, F. Artzner#, T. Narayanan§, T. Gulik-Krzywicki‡, G. Keller# and M. Ollivon# # Equipe de Physico-Chimie des Systèmes Polyphasés, UMR CNRS 8612, Faculté de Pharmacie, 5 Rue Jean-Baptiste Clément 92296 Chatenay-Malabry Cedex, France § E.S.R.F., Grenoble, France ‡Centre de Génétique Moléculaire, CNRS, Gif-sur-Yvette, France cecile.allais@cep.u-psud.fr

  2. Pharmaceutical Point of View: VECTORISATION ofPOORLY WATER-SOLUBLE DRUGS Active compounds:  Hydrophobicity  Crystallinity Characteristics : Nanometric Size: ~100nm  Lipidic Matrix: non toxic  Solid Matrix: slow release System : -model of hydrophobic molecule = CHOLESTEROL - matrix lipid = COCOA BUTTER : mixture of triglycerides

  3. SOLID LIPID NANOPARTICLES 100< d < 300 nm Low concentration of lipids: < 1% (w/w) ? Physical Characteristics: - SHAPE ? - HOMOGENEITY ? - POLYMORPHISM ? Techniques Optic Microscopy X-ray Diffraction Electronic Microcopy

  4. OPTIC MICROSCOPY IN DARK FIELD hn Light scattering Cocoa Butter/Cholesterol Nanoparticles

  5. hn OPTIC MICROSCOPY IN DARK FIELD Nanoparticles Stocked 1 Month at 4°C Nanoparticles just After Preparation at Room Temperature Spherical Particle Non Spherical Particle

  6. 100 nm 100 nm 100 nm 100 nm ELECTRONIC MICROSCOPY (T. Gulik-Krzywicki) Presence of Flat and Hemispherical Sides

  7. Cocoa Butter Polymorphism in Bulk: I < II < III < IV < V < VI[Loisel et al., 1998] 2L 3L After making at 10°C After quenching at 8°C 44.2 Å 48.2 Å 48.6 Å 54.3 Å Intensity (a.u.) I + II/III II/III + IV Intensity (a.u.) 27.15 Å 16.2 Å 16.1 Å 14.7 Å q (Å-1) q (Å-1) COCOA BUTTER POLYMORPHISM IN NANOPARTICLES (SAXS on ID2 Beamline, E.S.R.F., T. Narayanan) Cocoa Butter Nanoparticles X-ray patterns at10°C [Lipids]eau<1% (w/w)

  8. 47.8 Å 44.2 Å 47.8 Å 44 Å II/III + IV + CHOLESTEROL II/III + IV + CHOLESTEROL Intensity (a.u.) Intensity (a.u.) 34.5 Å 34.5 Å 16.1 Å 16.1 Å 17.1 Å 17.1 Å 14.5 Å 14.7 Å q (Å-1) q (Å-1) Making at 10°C Tempering at 30°C POLYMORPHISM CONTROL ? (SAXS on ID2 Beamline, E.R.S.F., T. Narayanan) CB/Cholesterol 50/50 (w/w) Nanoparticles X-ray patterns at10°C [Lipids]eau<1% (w/w)

  9. -40°C -38°C -36°C -34°C -32°C -30°C TmeltingNanoparticles< Tmelting Bulk Only 2L structures: -28°C -26°C -24°C -22°C -20°C -18°C I < II < III < IV < V < VI -16°C 2L 3L -14°C -12°C -10°C q (Å-1) POLYMORPHISM CONTROL ? (SAXS on ID2 Beamline, E.S.R.F., T. Narayanan) CB/Cholesterol 50/50 (w/w) Nanoparticles

  10. Dark-Field Microscopy Electronic Microscopy X-ray Diffraction Particle Model CONCLUSION  MultiTechniques Approach: -size -shape  Non Homogeneous Particles: microsegregation Polymorphism Study: low concentration: 1% (w/w) 2L

  11. Vacuum tube containing detector Mobile sample carrier with a capillary tube Incident X-ray beam X-RAY DIFFRACTION (T. Narayanan, E.S.R.F., Grenoble) ID 2 Beamline

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