2. Introduction
Essential oil lack full rounded profile
Oleoresin- represents holistic color, flavor,
taste profile
Oleoresin – complete profile
Volatile and non volatile substances
Non volatile components – flavor contributes
Recovered by suitable solvents
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
3. Solvents
• Polar solvents
– Hydroxy or carboxy
group
– Miscible with water
– Fire hazards
–Methanol ,
ethanol, acetone,
acetonitrile
• Non polar solvents
– Hydrocarbon or
chlorinated
hydrocarbon
– Limited solvent
properties
– Relatively toxic
– Methylene chloride,
ethylene chloride,
chloroform,
Hexane
Super critical Co2
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
4. Manufacturing of oleoresin
• Done by two methods
– Solvent Extraction process
– Super critical fluid extraction
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
5. Solvent Extraction
Preparation of Raw material
Exposure of material to solvent
Separation of miscella
Removal of Solvent
5R.Sorna Prema, Assistant Professor, Kongu Engineering College.
6. Preparation of raw material
• Cleaning
• Grinding
– Ensure good solvent penetration
– Smaller particle size- greater number of ruptured
cell
– Too fine particle size- slow percolation of solvent,
difficulties in recovering solvent from spent
material.
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
7. Exposure of material to solvent
• Involves three phases
• Addition of solvent to ensure even wedding of dry mass
• To allow absorption of solvent and equilibrium between
solute and solvent
• Continuous replacement of miscella with fresh solvent
• solvent/solute ratio
•Design of extractor factors influencing extraction
•Direction of flow
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
8. Separation of miscella and removal of
solvent
• Spice had high volatile compounds
• Low temperature separation – avoid loss/ damage
• High vacuum
• Desolventizing – 2 stages
• Removal of 98% of solvent – rising film, falling film, calendria
type evaporator (vacuum conditions)
• Scrubbing , sparging with nitrogen
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
9. Quality of oleoresin
• Viscous to thick- tacky paste
• Direct incorporation difficult
• Admixed with veg.oil or permitted diluent
(propylene glycol)
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
11. Super critical fluid extraction
• Separating one components from matrix using
super critical fluid
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
12. Super critical fluid
• A supercritical fluid is any substance at a
temperature and pressure above its critical point.
• It can diffuse through solids like a gas, and
dissolve materials like a liquid
• Slight changes in critical point – changes in
density, other properties
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
13. Contd…….
• 2 type of SCF
• Water
• Co2
• Ethanol / methanol – Co solvents
• CO2 -->
• non-toxic,
• Nonflammable,
• odorless,
• tasteless,
• Inert and inexpensive.
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
14. Critical Properties of SCF
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
15. Properties of SCF
• Supercritical fluids - combine properties of gases
and liquids
• Supercritical fluids can lead to reactions, which
are difficult or even impossible to achieve in
conventional solvents.
• solvent power similar to light hydrocarbons
• Solubility increases with increasing density (that
is with increasing pressure).
• Miscible with permanent gases
15R.Sorna Prema, Assistant Professor, Kongu Engineering College.
17. SUPER CRITICAL FLUID EXTRACTION PROCESS
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
18. SCE cond…..
• System contains
• CO2 Pressure vessel
• Pumps
• Pressure maintenance
• Collection
• Heating and cooling system
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
19. PUMPS
• Carbon dioxide pumped as liquid (temp 5
deg.celcius & pressure 50 bars
• Reciprocating pump or syringe pump or
diaphragm pump used
• Normally solvent incompressible
• More stroke used up to compress liquid
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
20. PRESSURE VESSEL
• Simple tube – quick fitting
• Equipped with heating
• Placed inside oven – small vessel
• Oil or electrically heated jacket – larger vessel
• Care needed – rubber seals- because CO2
dissolve rubber and rubber ruptured on
depressurization
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
21. PRESSURE MANITENANCE
• Pressure maintained from pump to pressure
vessel
• Smaller system – simple restrictor used
• Simple restrictor – capillary tube cut to length
– adjust different flow rates
• Larger system – back pressure regulators
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
22. COLLECTION
• Super critical solvent passed to the collection
vessel at lower pressure
• CO2 recycled or vent to atmosphere
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
23. HEATING AND COOLING
• Fluid is cooled before pumping and heated
after pressurization
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
24. ADVANTAGES
• Environmental improvement and reduced
product contamination
• Speed – process completed in 10- 60 mins
• Purity – SCF – non toxic, inert , readily
disposed off
• Recovery - recovery of analyte simple
• Selectivity
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R.Sorna Prema, Assistant Professor, Kongu Engineering College.
25. REFERENCES
R.Sorna Prema, Assistant Professor, Kongu
Engineering College.
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• Gary Reineccius, Flavor chemistry and
Technology, Second edition, CRC press.
• https://en.wikipedia.org/wiki/Oleoresin