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Sensory Properties In Consumer Products
 

Sensory Properties In Consumer Products

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Sensory Properties In Consumer Products Sensory Properties In Consumer Products Presentation Transcript

  • Controlled delivery of water-insoluble active ingredients in air from hydrogel matrices C. Dispenza 1,2 , G. Giammona 3 , M. Licciardi 3 , C. Lo Presti 1 , M. Ricca 1 , C. Spadaro 1 1 Dept. of Processing and Materials Chemical Engineering (DICPM) 2 Interdept. Research Centre on Composite Materials (CIRMAC) Dipartimento di Chimica e Tecnologie Farmaceutiche SIBPA, Palermo 17-22 September 2006 Università di Palermo logo
  • Contents: The context “ Functional” hydrogels from colloidal systems “ Functional” hydrogels obtained through ionising irradiation Release behaviour of a model fragrance Conclusions
  • Sensory properties in consumer products CONSUMER PRODUCT Informed choices Value-based choices Impulse-based choices CONSUMER BEHAVIOUR performance appearance experience
    • Foods
    • Cosmetics
    • Smoke
    • Housefield
    • Paints and coatings
    • Paper
    • Textiles
    • Automotive
    • ICT
    Major investor for research & development in the field of smart delivery of fragrances: Nissan!
    • Essential oils
    • Aroma chemicals
    • Absolutes
    • Balsams
    • Concentrated oils
    • Essences
    • Extracts
    • Resins
    • Infusions
    Polymers delivering olfactory sensations
    • Aromatic esters
    • Aliphatic esters
    • Ethers
    • Ketones
    • Alcohols
    Micelles Vesicles ACTIVE INGREDIENTS d= 100 - 600  m INCORPORATED / ENCAPSULATED INTO A POLYMER dry powders creams, foams, lotions, ect. DISPERSED/EMULSIFIED BARRIER MATERIALS DIFFERENT ARCHITECTURES FORMED BY BLOCK-COPOLYMERS IN WATER Bicontinuous phases Hexagonally packed vescicles Lamellae
    • INERT, BIOCOMPATIBLE, BIODEGRADABLE
    • HIGH LOADING CAPACITIES
      • (non equilibrium systems & processes)
    • Ensuring SYNCHRONISATION between the required TIME FOR THE SENSORIAL EFFECT and the actual RELEASE PROFILE
    • Ensuring SITE OF RELEASE RECOGNITION
    • Relatively STABLE TO STORAGE conditions over a long period of time
      • (for cosmetics: 2-3 years)
    Polymers as delivery devices, some requirements…
  • Hydrogels by definition High water content (>20% - 1000%) 3D network structure with soft consistency Elastic structure with a memorised reference configuration Linear polymer strands PHYSICAL GEL CHEMICAL GELS “ Virtual” cross-links formed by chain entanglements, electrostatic forces, hydrogen bonds T, pH, solvents + chem. reaction + chemical cross-links DISSOLUTION SWELLING + H 2 O T, pH, solvents Tridimensional polymeric networks:
  • Ionising irradiation Water + cross-linked polymer = Water + water-soluble monomers and/or polymers “ Functional” hydrogels through ionising irradiation
    • CROSSLINKING of hydrophilic MONOMERS and POLYMERS (+ X-linking agents + initiators/catalysts) by thermal activation
      • Complementary reactive groups: hydroxyl-aldehydes, amine-carboxylic acid, isocyanate-OH / NH 2 etc.
      • Reactive double bonds
    Ionising irradiation IONIZING IRRADIATION The other way… … to create reactive sites and promote reactivity! = IN SITU “FUNCTIONAL” HYDROGEL
  • “ Functional” hydrogels through ionising irradiation
    • “ Active” ingredient:
    • Water-insoluble molecules
      • heat sensitive and/or volatile
    • Water-insoluble polymers (1,2)
      • conductive polymers obtained via dispersion polymerisation
    Water- insoluble Active Ingredient Polymeric surfactant Ionising irradiation 1   C. Dispenza, C. Lo Presti, C. Belfiore, G. Spadaro, S. Piazza, Polymer, 47, 961-971, 2006. 2 C. Dispenza, M. Leone, C. Lo Presti, F. Li Brizzi, G. Spadaro, V. Vetri, Journal of Non-Crystalline Solids, 352 (2006) 3835–3840. DISPERSED “OBJECT” flavours (aromas) and fragrances
  • ‘ In-house’ developed, flexible polymer chemistry from..  - P OLY(N-2- H YDROXY E THYL)-D,L- A SPARTAMIDE PHEA Grafting of double bonds for easy of crosslinking Grafting functional groups for stimuli sensitivity Co 60 gamma irradiator ( IGS-3 at Palermo University) 60 Co 1.33 MeV 60 Co = 60 Ni + e - +  ’ 1.17 MeV DOSE : 2,5-3,5 kGy DOSE RATE : 0,5 kGy/h Gray : 1J of energy absorbed by 1 Kg of matter Experimentals PHEA + GMA = PHG PHG + water +  rays= PHG hydrogel (Derivatisation degree= 0,3) 5% wt/vol PHG/water
  • ‘ In-house’ developed, flexible polymer chemistry from..  - P OLY(N-2- H YDROXY E THYL)-D,L- A SPARTAMIDE PHEA Grafting of double bonds for easy of crosslinking Grafting functional groups for stimuli sensitivity Co 60 gamma irradiator ( IGS-3 at Palermo University) 60 Co 1.33 MeV 60 Co = 60 Ni + e - +  ’ 1.17 MeV DOSE : 2,5-3,5 kGy DOSE RATE : 0,5 kGy/h Gray : 1J of energy absorbed by 1 Kg of matter Experimentals PHEA + GMA = PHG PHG + water +  rays= PHG hydrogel (Derivatisation degree= 0,3) 5% wt/vol PHG/water Transparent – “reversible”
  • Experimentals Effect of irradiation on chemical structure Stability prior and upon irradiation Effect of irradiation on chemical structure Insoluble fractions Swelling ratios Fragrance release behaviour CHARACTERISATIONS MATERIAL SYSTEMS Model active Tetra- HydroGeraniol (THG): 3-7 dimethyl octanol Polymeric surfactant BRIJ 58P: polyoxyethylene (20) cetyl ether Emulsions & microemulsions 20 % vol THG/water; 2 % wt/vol BriJ/water 1% vol THG/water; 3 % wt/vol BriJ/water 20 % vol THG/water; 2 % wt/vol BriJ/water + 5 %wt/vol PHG 1 % vol THG/water; 3 % wt/vol BriJ/water + 5 %wt/vol PHG Hydrogels 5 %wt/vol PHG at 2.5 kGy 5 %wt/vol PHG at 3.5 kGy 3 % wt/vol BriJ/water + 5 %wt/vol PHG 20 % vol THG/water; 2 % wt/vol BriJ/water + 5 %wt/vol PHG (stirred) 1 %vol THG/water; 3 % wt/vol BriJ/water + 5 %wt/vol PHG
  • Flux meter in out “ STATIC” HEAD-SPACE “ DYNAMIC” HEAD-SPACE GC analysis GC analysis Air supply Experimentals FRAGRANCE RELEASE BEHAVIOUR 37°C 37°C
  • Cumulative THG released, ppm “ Static” head-space release behaviour Time, [hr] 0 200 400 600 800 1000 0 10 20 30 40 50 60 0 kGy 2,5 kGy 3 ,5 kGy Head space saturation EMULSIONS 19 75 3,5 BriJ58P-PHG-water 27 65 2,5 BriJ58P-PHG-water 9 91 3,5 PHG-water 10 86 2,5 PHG-water Swelling ratio [Ws/Wd] Insoluble fraction, [%] Dose [kGy] System
  • Cumulative THG released, ppm “ Static” head-space release behaviour Time, [hr] 0 200 400 600 800 1000 0 10 20 30 40 50 60 Head space saturation EMULSIONS Cumulative THG released, ppm 0 100 200 300 400 500 600 700 800 900 0 10 20 30 40 50 60 70 Time, [hr] Head space saturation MICRO-EMULSIONS 0 kGy 2.5 kGy 3 ,5 kGy 0 kGy 2,5 kGy 3,5 kGy
  • “ Dynamic” head-space release behaviour Time, [hr] Cumulative THG released, [mg] 0 1 2 3 4 5 6 7 8 9 0 10 20 30 40 50 0 kGy 3,5 kGy 2,5 kGy Total amount of THG loaded MICRO-EMULSIONS 0.00 0.20 0.40 0.60 0.80 1.00 1.20 0 10 20 30 40 50 Time, [hr] Weight loss, [g] 0 kGy 3,5 kGy 2,5 kGy Initial weight of water + THG
  • Cumulative THG released, [mg] 4,7 4,9 5,1 5,3 5,5 5,7 5,9 30 35 40 45 50 55 Time, [hr] Re-hydration of the surface OFF ON ON OFF 2,5 kGy
      • SURFACE-REGULATED RELEASE MECHANISM
    hydration “ ON-PHASE” OF THE RELEASE “ OFF-PHASE” OF THE RELEASE de-hydration SKIN “ REVERSIBLE”!
      • SURFACE-REGULATED RELEASE MECHANISM
    • the faster the hydrogel looses water the sooner the skin is formed!
    • the looser is the polymeric network the faster is the release of water
    • water represent, by large, the main volatile component released
    0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 0 10 20 30 40 50 Time, [hr] W(t) W 0 0 kGy 3,5 kGy 2,5 kGy Dotted line: water + THG Solid line: THG
  • Conclusions: Ionising irradiation can be a stimulating tool to obtain “functional” hydrogels from water-soluble polymeric precursors. Crosslinking degree and density can be controlled by tuning irradiation conditions, thus affecting the water retention properties of the gels. Oil insoluble fragrances can be incorporated by coupling irradiation and emulsification techniques. Hydrogel formation can prevent macroscopic phase-separation of otherwise unstable systems. The hydrogel network offers a diffusion barrier to the fragrance. Water loss kinetics may be exploited for a on-off, surface hydration regulated, release behavior .
  • Controlled delivery of water-insoluble active ingredients in air from hydrogel matrices SIBPA, Palermo 17-22 September 2006 CONTACT DETAILS Clelia Dispenza Dipartimento di Ingegneria Chimica dei Processi e dei Materiali Università degli Studi di Palermo Tel +39 091 6567210 Fax+ 39 091 6567280 [email_address] THANK YOU