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

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 TechniquesEssential Oil Extraction

Cold Press

Hydro Distillation

Steam Distillation

Solvent Extraction

PRODUCTIVITY TOOLS

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

PRODUCTIVITY TOOLS

The “New” TechniqueSolvent 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” 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

PRODUCTIVITY TOOLS

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

PRODUCTIVITY TOOLS

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

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 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

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

Glassware2 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 MHGShorter Extraction Times

Recovery of Higher Boiling Compounds (pigments, flavonoids, carotenoids)

Higher Purity of Extracts

No Solvents

PRODUCTIVITY TOOLS

MHG ExtractsExtraction of Essential Oil from Rosmarinus officinalis

PRODUCTIVITY TOOLS

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.

PRODUCTIVITY TOOLS

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.

PRODUCTIVITY TOOLS

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)

PRODUCTIVITY TOOLS

Thank You!