production of microencapsulated phenolic compounds...
TRANSCRIPT
PRODUCTION OF MICROENCAPSULATED PHENOLIC COMPOUNDS FROM OLIVE OIL INDUSTRY WASTES
USING SPRAY DRYING TECHNOLOGY
Bahar Aliakbarian, PhD
Chemical, Material and Process Engineer
MFIP13 13th International Conference
MULTIPHASE FLOW IN INDUSTRIAL PLANTS Sestri Levante (Genova), Italy; September 17-19, 2014
Department of Civil, Chemical and Environmental Engineering
INTRODUCTION (Background)
1000 kg
200 kg
450 kg 350 kg
Energy
Pellets
Anaerobic digestion
Pyrolysis
Gasification
INTRODUCTION (Background)
Olive pomace
Antioxidants
Food
Fermented milks enriched with
antioxidants
Cosmetic
«anti-aging»
creams
Exhausted pomace
Energy
Antioxidants
Free
radicals
Oxidation
reactions
-Cardiovascolar
diseas
-Neurodegenerative
desease
-Skin aging
-Inflammatory
desease
-Arthritis
-Others
Cell structural
alteration
INTRODUCTION (Background)
Prone to oxidation
Low orally absorbance
Cytotoxic in higher total dosages (though relatively
high local concentrations are required for an effect)
Low water solubility
Encapsulation is one way to :
improve bioavailability and stability
Microencapsulation (ME) is a technique in which a membrane encloses small particles of
solid, liquid or gas, to protect the core material from adverse environmental conditions
INTRODUCTION (Background)
Spray drying is a particular case of evaporation, in which small liquid droplets are rapidly (5-10 seconds) dried by a flow of hot air.
A liquid formulation containing a coating agent and the active compound in a solvent is atomized into droplets via an atomizer.
A heated process gas (air or N2) is brought into contact with the atomized feed using a gas disperser, leading to evaporation of the solvent.
As the liquid rapidly evaporates from the droplet, a particle forms and falls to the bottom of the chamber. The powder is recovered from the exhaust gases using a cyclone or a bag filter.
The rate of drying must be such that from the time the particle leaves the atomizer to the time it impinges upon the walls of the chamber, the particle is dry.
MATERIALS AND METHODS (Spray Drying)
ADVANTAGES
Simple technique, with high efficiency.
Low production costs (30-50 times cheaper than freeze-drying).
Production of high quality and stable particles.
Continuous process.
Increase of solubility of hydrophobic compound.
Used in food industry to ensure a microbiological stability of products.
DISADVANTAGES
Limited number of shell materials availability.
High air temperature can degrade heat-sensitive samples.
MATERIALS AND METHODS (Spray Drying)
MATERIALS AND METHODS (Spray Drying)
Food
Eggs, milk powder, coffee, tea, cocoa, spices, flavorings, starches, vitamins, etc.
Pharmaceutics
Antibiotics, FANS, additives, antihypertensives, etc.
Other fields
Paint pigments (toner), ceramic materials, catalyst supports, microalgae, etc.
Encapsulation of olive pomace extract to
enhance its physico-chemical properties…..
MATERIALS AND METHODS (Spray Dryer)
• High pressure and high temperature
reactor: 180 °C, 90 min, ethanol 50%
v/v
• Inlet Temperature (IT): 130 and 160 °C;
• Coating agent (MD): Maltodextrine 10
and 50 % w/v;
• Feed Flow: 5 and 10 mL/min;
• Physical Properties: moisture content,
bulk density and microstructure of
microparticles;
• Hydration properties: water solubility
index, water absorption index and
swelling capacity;
• FTIR analysis;
• Microencapsulation yield;
• Total polyphenols, Antiradical Power
and Stability tests.
RESULTS (Physical characterization of the microcapsules )
IT (°C)
MD (% w/v)
Feed flow (mL/min)
OT (°C) Moisture content (%)
Bulk density (g/mL)
130
10 5 86 ± 1 a,b 6.15 ± 0.24 b 0.19 ± 0.01 b
10 75 ± 1 c 7.03 ± 0.36 c 0.19 ± 0.02 b
50 5 87 ± 1 a,b 5.93 ± 0.37 b 0.13 ± 0.01 e
10 83 ± 1 a 6.11 ± 0.16 b, c 0.16 ± 0.01 f
160
10 5 95 ± 1 d 2.34 ± 0.31 a 0.07 ± 0.01 c
10 84 ± 1 a 2.11 ± 0.45 a 0.10 ± 0.01 d
50 5 102 ± 1 e 2.42 ± 0.29 a 0.04 ± 0.01 a
10 89 ± 1 b 2.39 ± 0.38 a 0.05 ± 0.01 a
IT (°C)
MD (% w/v)
Feed flow (mL/min)
Water Solubility
Index (%)
Water Absorption Index
(g/gDP)
Swelling Capacity (g/gDP)
130
10 5 83.82 ± 1.68 a 0.34 ± 0.02 a 2.13 ± 0.27 a,b
10 85.41 ± 2.20 a 0.33 ± 0.02 a,b 2.31 ± 0.49 a
50 5 84.67 ± 0.85 a 0.38 ± 0.01 a,c 2.49 ± 0.18 a,b
10 86.59 ± 1.59 a 0.28 ± 0.02 b 2.10 ± 0.14 a
160
10 5 79.46 ± 2.20 b 0.49 ± 0.02 d 2.43 ± 0.33 b
10 79.52 ± 1.57 b 0.58 ± 0.03 e 2.85 ± 0.16 b
50 5 83.07 ± 0.54 a,b 0.53 ± 0.01 d 3.12 ± 0.14 a,b
10 85.49 ± 1.23 a 0.40 ± 0.02 c 2.76 ± 0.31 a
RESULTS (SEM)
a) b)
c) d)
The operative conditions that generate a smaller microparticles size were MD10 and feed flow 10 mL/min, for both ITs with more than 96% of the particles in the range 0-20 μm.
IT 130°C, MD 10 % (w/v), feed flow 10 mL/min
IT 130°C, MD 50 % (w/v), feed flow 10 mL/min
IT 160°C, MD 10 % (w/v), feed flow 10 mL/min
IT 160°C, MD 50 % (w/v), feed flow 5 mL/min
RESULTS (FTIR)
a
b
c
MD without extract
IT130, MD10, FF 10 mL/min
Dried extract
IT (°C)
MD (% w/v)
Feed flow (mL/min) TP
(mgCAE/gDP) ARP
(mgDPPH˙/mLextract) Microencapsulation
Yield (%)
130
10
5 27.7 ± 1.7 b 8.0 ± 1.1 c 65.5 ± 4.1 a, b
10 39.5 ± 4.9 c 13.3 ± 1.7 d 93.7 ± 0.4 c
50
5 4.5 ± 0.3 a 1.5 ± 0.8 a 54.3 ± 4.1 a
10 6.2 ± 0.4 a 2.7 ± 0.5 a 72.6 ± 0.6 b
160
10
5 26.0 ± 1.2 b 5.8 ± 0.3 b 61.6 ± 2.9 a, b
10 26.0 ± 1.5 b 7.5 ± 0.8 c 60.4 ± 3.6 a, b
50
5 4.8 ± 0.5 a 2.0 ± 0.2 a 58.0 ± 7.1 a, b
10 4.4 ± 0.3 a 1.4 ± 0.8 a 50.8 ± 4.8 a
RESULTS (Total Polyphenols, Antiradical Power, Yield)
TP content is maximum (39.5±4.9 mgCAE/gDP) at IT130, MD10 with a feed flow of 10 mL/min; The higher ARPs were found in microparticles with MD10 and feed flow equal to 10 mL/min; Microencapsulation yields are higher than 50 % for all samples, and the maximum yield is for the microparticles obtained at IT130, MD10 and feed flow 10 mL/min.
RESULTS (Stability)
a
b bb
b bb
b
c cc
0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
40.00
45.00
0 1 2 3 4 5 6 8 10 24 48
TP (m
g CAE/g DP
)
Time (h)
a
a,b,c a,b,c,d b,c,db,c,d
b,c,d
b,c,d,g
a
a,b,c,d a,b,c,d
b,c,d d,g c,d,g
e,g
a
a,bb,c,d
e,f e,f f f
0.00
10.00
20.00
30.00
40.00
50.00
0 1 7 14 21 28 70
TP(m
g CAE/g
DP)
Time (days)
Dark Sunlight Lamp light
aa,b,c,d a,b,c,d
a,b,c,da a,b a,b,c,d
a
a,b,c,d a,b,c,da,b,c,d
c,d a,b,c,dd,e
aa,b,c a,b,c,d
a,b,c,d
c,d,e
b,c,d
e
0.00
10.00
20.00
30.00
40.00
50.00
0 1 7 14 21 28 70
TP(m
g CAE/g
DP)
Time (days)
T=5 °C T=25 °C T=45 °Ca
b
c
Conclusions
• An increase from IT130 to IT160 leads to lower moisture content and bulk density, causes a higher degradation of the spherical structure of the particles and resulted to lower TP and ARP.
• Increasing MD concentration causes lower bulk density and higher size of the powders.
• The highest microencapsulation yield was obtained at IT130, MD10 and feed flow equal to 10 mL/min. At these conditions notable TP content (39.5±4.9 mgCAE/gDP) and ARP (13.3±1.7 mgDPPH˙/mLextract) were obtained, along with a high ME (75.9±3.3 %), and small particle sizes.
The product obtained shows good stability at storage conditions and remarkable antioxidant properties, and can be considered a new potential source for integration in novel food or pharmaceutical products.
ACKNOWLEDGMENTS…
Prof. Patrizia PEREGO- University of Genova Prof. Roberto BOTTER- University of Genova Dr. Marco PAINI- PhD student- University of Genova Dr. Alessandro Alberto CASAZZA- PhD- University of Genova Dr. Alberto Lagazzo- PhD- University of Genova