The Vine is an area within the WBWE, conceived to encourage new businesses that evolve around wine and vine industries. Using every resource, and expanding every possibility, such an initiative shows the great potential that can be developed in the sector.
Escuela de Ingenierías Industriales-Universidad de Valladolid, Valladolid, Spain (sorayarr@iq.uva.es; mjcocero@iq.uva.es)
Instituto de Tecnologia Química e Biológica, Universidade Nova de Lisboa, Oeiras, Portugal
Instituto de Biologia Experimental e Tecnológica, Oeiras, Portugal
abroBiotec – Grupo Matarromera, Valbuena de Duero, Spain
Further information about "The Vine Science Award" on http://www.worldbulkwine.com/thevine/ing/posters.html
Grape marc polyphenols encapsulation in natural origin carriers by conventional and supercritical fluid base techniques
1. THE VINE: All about the Vine, except Wine. Amsterdam, 21 & 22 November 2016
[1] González, C. M. Procedimiento de extracción de polifenoles a partir de orujo de uva procedente de destilación. Spanish Patent No. 2319032 (2007).
[2] T. Moreno, E. de Paz, I. Navarro, S. Rodríguez-Rojo, A. Matías, C. Duarte, M. Sanz-Buenhombre, M.J. Cocero. Spray Drying Formulation of Polyphenols-Rich Grape Marc Extract: Evaluation of Operating Conditions and Different Natural Carriers. Food and Bioprocess
Technology (2016) DOI 10.1007/s11947-016-1792-0
[3] M. Salgado, S. Rodríguez-Rojo, F.M. Alves-Santos, M.J. Cocero. Encapsulation of resveratrol on lecithin and b-glucans to enhance its action against Botrytis cinerea. Journal of Food Engineering 165 (2015) 13–21
Project Funded by“Marie Curie Industry-Academia Partnerships and Pathways (IAPPs)” actions of the FP7-People program
under REA Grant Agreement nº 612208
Aim: valorization of grape marc (a not very profitable byproduct of the wine industry) through the intensification of extraction
by Microwave Assisted Extraction (MAE), and formulation of its polyphenols for cosmetic, food and pharmaceutical
applications.
Framework for the transfer of knowledge (ToK) and long-term collaboration between 3 industrial and 1 academic partners.
Know more in http://winesense.eu/
High Pressure Processes
Group
Soraya Rodríguez-Rojoa* , Teresa Morenoa, Daniel Deodatoa,b,c, Ana Matiasa,b,c, Esther de Paza,c , Catarina M.M. Duarteb ,Marisa Sanzd, M.J. Coceroa
a Escuela de Ingenierías Industriales-Universidad de Valladolid, Valladolid, Spain (sorayarr@iq.uva.es; mjcocero@iq.uva.es)
b Instituto de Tecnologia Química e Biológica, Universidade Nova de Lisboa, Oeiras, Portugal
c Instituto de Biologia Experimental e Tecnológica, Oeiras, Portugal
dd abroBiotec – Grupo Matarromera, Valbuena de Duero, Spain
WP 1
WP 2
WP 3
WP 4
WP 4
WP 5
TOK
AIMS
Avoid / Reduce polyphenols degradation
Improve solubility and bioavailability in aqueous media through
development of solid stable formulations
Improve properties for incorporation into products (i.e. cosmetics, food,
nutraceutical supplements and fitofarmaceuticals)
EXTRACT:
Eminol ® [1]
TPC: 7000 – 9500 ppm GAE
TAC: 80- 130 ppm MGE
Solid content: 3 – 3,5 % w/w
CARRIER MATERIALS:
Maltodextrine (MD)
Whey Protein Isolate (WPI)
Pea Protein Isolate (PPI)
Acronyms
- TPC: Total Phenolic content
- TAC: Total Anthocyanin content
- GAE: galic acid equivalents
OPERATING CONDITIONS:
Drying gas: Hot Air
Inlet Temperature: 140°C
Outlet Temperature: 80°C
Solution flow rate: 20 mL/ min
Atomizing air pressure: 6 bar-g
ratio: 1:1 w/w
(Carrier: solid content extract ratio)
Operating parameters [3]
- T drying chamber: 60 – 70 °C
- Flow CO2: 10 kg/h
- Gas/liquid: 30 w/w
-High process yield (% solid recovery): up to 80% (WPI & MD). Except for PPI (ca. 20%)
- High encapsulation efficiency (TPC, TAC) from 70% (PPI) to 100% (MD)
- Increase in specific ORAC values (by mg GAE) from 28.5% (MD) to 50% (WPI)
- Residual moisture content from 7 % (PPI) to 11% (WPI). Water activity values below the
threshold for microbial growth inhibition (aw < 0.61%)
Materials
EMINOL ®
Carriers:
- Lecithin
- Modified OSA starch
- Barley β-glucan
GRAPE
MARC
AQUEOUS
EXTRACT
NATURAL
CARRIERS
DRYING AND
CO-PRECIPITATION:
2 ALTERNATIVE
PROCESSES:
Spray drying
PGSS drying FORMULATED
PHENOLIC
EXTRACT
FINAL APPLICATION:
INCORPORATION
INTO PRODUCTS
CHEMICAL AND MORPHOLOGICAL ANALYSISFORMULATION
MD
Dv,0.5 : 15 μm
PPI
Dv,0.5 : 46 μm
WPI
Dv,0.5:9.4 μm
PRINCIPLE
Alternative supercritical CO2 based process to reduce polyphenols
degradation and loss of antioxidant capacity by temperature and
the presence of oxygen during processing. Phenolic & carrier
solution is mixed at high pressure and temperature (95 bar & 125
°C) for short time before expansion into the drying chamber.
Expansion of CO2 improves atomization and drying, and lower
processing temperatures (from 40 – 70 ° C) are used, depending
on Gas to Liquid ratio and solid content of the feed. It allows
processing solutions with low Tg (i.e. high sugar contents such as
extracts derived from fruit residues).
RELEASE PROFILES
- Immediate release of TPC and TAC except for WPI formulation
(controlled by Fickian diffusion, Korsmeyer-Peppas Model)
- Incomplete release in all cases:
- MD and F/D and PPI: max.80%., being lower in intestinal
simulated fluid (an external gastric capsule would be
required in oral administration) .
- Proteins, especially, WPI show lower release %, possible
due to binding with the phenolic compounds
CELULAR ANTIOXIDANT ACTIVITY [2]
- Cell Model: Human colon Caco-2
- High cell viability for extract and formulated products (> 95%)
- Higher CAA for WPI formulation. No CAA por pure WPI:
WPI as carrier may enhance penetration trough cell membrane
and increase bioavailability of grape marc bioactives
STABILITY
6-month stability test at 25°C in dark and light (350 lux):
- No significant changes in TPC and moisture content
- Significant loss of ORAC over time (44-73% of initial value)
- Significant loss of TAC over time, especially for WPI (>50%)
- No difference between light and dark conditions
2-weeks accelerated stability test at 40 and 60°C
- No significant effects in TPC and ORAC values, only in TAC
- Lowest degradation of TAC in PPI even at 60°C = color stability
- Spray Dried formulations: Tests for anti-aging and skin lightening properties (enzymatic and cell based assays) in cosmetic applications
- PGGS-drying formulations: Antioxidant cellular activity test to verifiy the increased chemical antioxidant activity (ORAC)
First order
kinetic model
for TAC
degradation
RESULTS
No significant effect of the carrier material:
- High encapsulation efficiency (ca. 100%) for TPC & TAC
- Increase in specific ORAC values (by mg GAE) higher than 200%
- Morphology: small microparticles in agglomerated form
- MGE: malvidin-3-glucoside
equivalents
- F/D: Freeze drying sample
FORMULATION
OSA-starch
Dv,0.5 : 34 μm
Particle size according to laser difraction measurements in dry sate
β-glucan
Dv,0.5 : 7.2 μm
Particle size according to laser difraction measurements in dry sate