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PRODUCTIVITY TOOLS
Solvent Free Microwave ExtractionThe New Way to Extract Essential Oils
Tim MichelSales ManagerMilestone Inc
PRODUCTIVITY TOOLS
Milestone apps lab, Bergamo
Milestone HQ, Bergamo Italy
Milestone R&D, Germany
• Established in 1988Headquarters in Italy, R&D and manufacturing in Germany• Over 15,000 labs use Milestone
instruments• Core technology/application:
microwave based sample prep
Milestone Worldwide
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Milestone Product Range
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Milestone’s NEOS
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Today’s Agenda
What is Solvent Free Microwave Extraction
(SFME)?
Benefits of SFME
Where does SFME technology fit best?
Other Application of the NEOS
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Traditional TechniquesEssential Oil Extraction
Cold Press
Hydro Distillation
Steam Distillation
Solvent Extraction
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Traditional TechniquesEssential Oil Extraction
Long Extraction Times
Poor Recovery
High Energy Consumed
Loss of Some Volatile Components
Thermal or Hydrolytic Degradation
Presence of Toxic Residues
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The “New” TechniqueSolvent Free Microwave Extraction (SFME)
Advantages of SFME
Shorter Extraction Times
High Purity Extracts
No Solvents – Green Chemistry
Recovery of Volatile Compounds
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The “New” TechniqueSolvent Free Microwave Extraction (SFME)
Atmospheric Pressure with No SolventsHeating of Internal WaterEssential Oils Evaporated by the In-situ WaterCooling System Condenses the VaporsExcess Water is Refluxed Back to the Extraction Vessel
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Shorter Extraction Times
Extraction of Essential Oils from Aromatic Herbs*
* Solvent-free microwave extraction of essential oils from aromatic herbs: comparison with conventional hydro-distillation. Journal of Chromatography A, 1043 (2004) 323-327.
Time (minutes) Yield (%) Time (minutes) Yield (%)
30 0.029 270 0.028
30 0.095 250 0.095
30 0.160 250 0.161
Basil
Garden Mint
Thyme
NEOS (SFME) Hydro Distillation
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Shorter Extraction Times
Extraction of Essential Oils from Orange Peel
* Solvent free microwave extraction of essential oils. Chemistry Today, Vol. 26 n.2 (2008)
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
NEOSHydro
DistillationCold
Pressing
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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
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Green ChemistryCarbon 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 SolventThe 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
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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.
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NEOS Hardware
Microwave
Control Panel
Glassware
Chiller
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Microwave
IR Sensor
Safety Micro Switches
Atmospheric Pressure
Polymer Coating
Microwave Power output
of 800 watts
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Glassware2 L and 5 L Glass Module
Extension Tube
Connecting Glass Tube
Patented Extraction Module
Glass Condenser
Chiller
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Labs Benefited by the NEOS
Research/Development
Quality Control
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Flexibility of Applications
Microwave Hydrodiffusion and Gravity (MHG)
Microwave-Accelerated Steam Distillation (MASD)
Microwave-Accelerated Dean Stark (MADS)
Microwave Integrated Soxhlet (MIS)
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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
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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.
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Microwave Hydrodiffusion and Gravity (MHG)
Higher Boiling Compounds
No Solvent
Hydrodiffusion
Falls by Earth Gravity
through Perforated Disc
Cooling System
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Benefits of MHGShorter Extraction Times
Recovery of Higher Boiling Compounds (pigments, flavonoids, carotenoids)
Higher Purity of Extracts
No Solvents
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MHG ExtractsExtraction of Essential Oil from Rosmarinus officinalis
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Flexibility of Applications
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.*
Microwave Accelerated Steam Distillation (MASD)
* 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.
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Microwave Accelerated Steam Distillation
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
MASD SD
* 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.
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SummaryAdvantages of SFME
Shorter Extraction Times High Purity ExtractsNo Solvents – Green ChemistryRecovery of Volatile Compounds
Labs Benefited by SFMEResearch/DevelopmentQuality ControlUniversities
Flexibility of NEOSMicrowave Hydrodiffusion and Gravity (MHG)Microwave-Accelerated Steam Distillation (MASD)Microwave-Accelerated Dean Stark (MADS)Microwave Integrated Soxhlet (MIS)
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Thank You!
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