Solvent Free Microwave Extraction
The New Way to Extract Essential Oils
Tim Michel
Sales Manager
Milestone Inc
PRODUCTIVITY TOOLS
Milestone Worldwide
•Established in 1988
Headquarters in Italy, R&D and
manufacturing in Germany
•Over 15,000 labs use Milestone
instruments
•Core technology/application:
microwave based sample prep
Milestone HQ, Bergamo Italy
Milestone R&D, Germany
Milestone apps lab, Bergamo
PRODUCTIVITY TOOLS
Milestone Product Range
PRODUCTIVITY TOOLS
Milestone’s NEOS
PRODUCTIVITY TOOLS
Today’s Agenda
What is Solvent Free Microwave Extraction
(SFME)?
Benefits of SFME
Where does SFME technology fit best?
Other Application of the NEOS
PRODUCTIVITY TOOLS
Traditional Techniques
Essential Oil Extraction
Cold Press
Hydro Distillation
Steam Distillation
Solvent Extraction
PRODUCTIVITY TOOLS
Traditional Techniques
Essential Oil Extraction
Long Extraction Times
Poor Recovery
High Energy Consumed
Loss of Some Volatile Components
Thermal or Hydrolytic Degradation
Presence of Toxic Residues
PRODUCTIVITY TOOLS
The “New” Technique
Solvent Free Microwave Extraction (SFME)
Advantages of SFME
Shorter Extraction Times
High Purity Extracts
No Solvents – Green Chemistry
Recovery of Volatile Compounds
PRODUCTIVITY TOOLS
The “New” Technique
Solvent Free Microwave Extraction (SFME)
Atmospheric Pressure with No Solvents
Heating of Internal Water
Essential Oils Evaporated by the In-situ Water
Cooling System Condenses the Vapors
Excess Water is Refluxed Back to the Extraction Vessel
PRODUCTIVITY TOOLS
Shorter Extraction Times
Extraction of Essential Oils
from Aromatic Herbs*
NEOS (SFME)
Hydro Distillation
Time (minutes)
Yield (%)
Time (minutes)
Yield (%)
Basil
30
0.029
270
0.028
Garden Mint
30
0.095
250
0.095
Thyme
30
0.160
250
0.161
* Solvent-free microwave extraction of essential oils from aromatic herbs: comparison with
conventional hydro-distillation. Journal of Chromatography A, 1043 (2004) 323-327.
PRODUCTIVITY TOOLS
Shorter Extraction Times
Extraction of Essential Oils
from Orange Peel
NEOS
Hydro
Distillation
Cold
Pressing
Extraction Time (minutes)
10
180
60
Yield %
0.4
0.4
0.15
Total Oxygenated Compounds (%)
1.6
0.9
1.1
Total Non Oxygenated Compounds (%)
97.4
98.5
98.2
* Solvent free microwave extraction of essential oils. Chemistry Today, Vol. 26 n.2 (2008)
PRODUCTIVITY TOOLS
High Purity Extract
Oxygenated Compounds: More valuable as they are highly
scented
Monoterpene Hydrocarbons: Less valuable to the fragrance
of essential oil
SFME has been shown to
produce higher amounts of
oxygenated compounds
than Hydro-distillation.2
2. Solvent free microwave extraction of Elletaria cardamomum L.: A multivariate study of a
new technique for the extraction of essential oil, Journal of Food Engineering, 79 (2007)
1079–1086
PRODUCTIVITY TOOLS
Green Chemistry
Carbon Emissions
“Regarding environmental
impact, the calculated quantity of
carbon dioxide rejected in the
atmosphere is higher in the case
of HD (3464 gCO2/g of essential
oil) than for SFME (200 gCO2/g of
essential oil).”1
No Solvent
The use of solvent for extractions
generates waste into the
environment. Also, no toxic
residue from solvents will be
present in extract.
1. An improved microwave Clevenger apparatus for distillation of essential oils from
orange peel, Journal of Chromatography A, 1112 (2006) 121-126
PRODUCTIVITY TOOLS
NEOS System
Solvent Free Microwave Extraction (SFME)
Laboratory of Chemistry of Natural
Substances and Food Sciences at the
Université de la Réunion, France
Partnership between Milestone and
Laboratory, which lead to the grant
European patents 1439218, 1618798 and
1629725.
PRODUCTIVITY TOOLS
NEOS Hardware
Microwave
Control Panel
Glassware
Chiller
PRODUCTIVITY TOOLS
Microwave
IR Sensor
Safety Micro Switches
Atmospheric Pressure
Polymer Coating
Microwave Power output
of 800 watts
PRODUCTIVITY TOOLS
Glassware
2 L and 5 L Glass Module
Extension Tube
Connecting Glass Tube
Patented Extraction Module
Glass Condenser
Chiller
PRODUCTIVITY TOOLS
Labs Benefited by the NEOS
Research/Development
Quality Control
PRODUCTIVITY TOOLS
Flexibility of Applications
Microwave Hydrodiffusion and
Gravity (MHG)
Microwave-Accelerated Steam
Distillation (MASD)
Microwave-Accelerated Dean
Stark (MADS)
Microwave Integrated Soxhlet
(MIS)
PRODUCTIVITY TOOLS
Microwave Hydrodiffusion and
Gravity (MHG)
Higher Boiling Compounds
The NEOS-GR for MHG is the result between
Milestone and the Université d’Avignon et des
Pays de Vaucluse, France
Led to the grant of the European patent
EP 1 955 749 A1
An Original “Upside Down” Microwave Alembic
PRODUCTIVITY TOOLS
What is Hydro Diffusion?
Hydrodiffusion is a type of Steam Distillation.
Steam comes from above sample with
Hydrodiffusion compared to Steam Distillation
where steam comes from below.
Less steam needed for the extraction, making the
process quicker.
Hydrodiffusion is less harsh than Steam Distillation
which improves the quality of the extract.
PRODUCTIVITY TOOLS
Microwave Hydrodiffusion and
Gravity (MHG)
Higher Boiling Compounds
No Solvent
Hydrodiffusion
Falls by Earth Gravity
through Perforated Disc
Cooling System
PRODUCTIVITY TOOLS
Benefits of MHG
Shorter Extraction Times
Recovery of Higher Boiling Compounds
(pigments, flavonoids, carotenoids)
Higher Purity of Extracts
No Solvents
PRODUCTIVITY TOOLS
MHG Extracts
Extraction of Essential Oil from Rosmarinus officinalis
PRODUCTIVITY TOOLS
Flexibility of Applications
Microwave Accelerated Steam Distillation (MASD)
Steam Distillation most common
technique
Sample sits above steam source
generated by microwave heating
MASD was better than Steam
Distillation in terms of Energy
Saving, Rapidity (10 min vs 90
min), Product Yield, Cleanliness
and Product Quality.*
* F. Chemat, M.E. Lucchesi, J. Smadja, L. Favretto, G. Colnaghi,
F. Visinoni, Microwave accelerated steam distillation of
essential oil from lavender: rapid, clean and environmentally
friendly approach. Analytica Chimica Acta, 2006, 555, 157-160.
PRODUCTIVITY TOOLS
Microwave Accelerated Steam
Distillation
MASD
SD
Yield %
8.86
8.75
Total Extraction Time (minutes)
10
90
Heating Time from 20-100°C (minutes)
5
30
Real Extraction Time (minutes)
5
60
* F. Chemat, M.E. Lucchesi, J. Smadja, L. Favretto, G. Colnaghi, F. Visinoni, Microwave accelerated
steam distillation of essential oil from lavender: rapid, clean and environmentally friendly approach.
Analytica Chimica Acta, 2006, 555, 157-160.
PRODUCTIVITY TOOLS
Summary
Advantages of SFME
Shorter Extraction Times
High Purity Extracts
No Solvents – Green Chemistry
Recovery of Volatile Compounds
Labs Benefited by SFME
Research/Development
Quality Control
Universities
Flexibility of NEOS
Microwave Hydrodiffusion and Gravity (MHG)
Microwave-Accelerated Steam Distillation (MASD)
Microwave-Accelerated Dean Stark (MADS)
Microwave Integrated Soxhlet (MIS)
PRODUCTIVITY TOOLS
Thank You!
PRODUCTIVITY TOOLS