Solvent Free Microwave Extraction The New Way to Extract Essential Oils Tim Michel Sales Manager Milestone Inc Welcome to Solvent Free Microwave Extraction Webinar. My name is Melissa Lightner, and I am an applications chemist here at Milestone.

Milestone HQ, Bergamo Italy Milestone apps lab, Bergamo 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 Microwave based sample preparation is core technology. Milestone R&D, Germany Milestone apps lab, Bergamo

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Milestone’s NEOS We saw a need for a fast, more advanced technology for essential oil extraction, so we developed the NEOS which uses SFME

Today’s Agenda What is Solvent Free Microwave Extraction (SFME)? Benefits of SFME Where does SFME technology fit best? Other Application of the NEOS

Traditional Techniques Essential Oil Extraction Cold Press Hydro Distillation Steam Distillation Solvent Extraction

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 these techniques can suffer from long extraction times, poor recovery, high energy consumes, loss of some volatile components, thermal or hydrolytic degradation, and presence of toxic residues in the extracts. Traditional tech. effective, but challenges associated with them. SFME addresses these issues.

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

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 SFME is performed at atmospheric pressure; the method involves placing the sample in the microwave reactor, without any added solvents. The internal heating of the water within the sample distends its cells and leads to rupture of the glands and oleiferous receptacles. This process thus frees essential oils, which are evaporated by the in-situ water, then a cooling system, condenses the vapors which are collected separately. The excess water is refluxed back to the extraction vessel in order to restore the in-situ water to the sample; once the essential oils have been collected they can be analyzed directly by GC-MS without any clean-up.

Shorter Extraction Times Extraction of Essential Oils from Aromatic Herbs* NEOS (SFME) Hydro Distillation Time (minutes) Yield (%) 30 0.029 270 0.028 0.095 250 0.160 0.161 Basil Garden Mint Thyme 8 to 9 times faster with the NEOS when compared to Hydro distillation. * Solvent-free microwave extraction of essential oils from aromatic herbs: comparison with conventional hydro-distillation. Journal of Chromatography A, 1043 (2004) 323-327.

Shorter Extraction Times Extraction of Essential Oils from Orange Peel Hydro Distillation Cold Pressing NEOS Extraction Time (minutes) 10 180 60 Yield % 0.4 0.15 Total Oxygenated Compounds (%) 1.6 0.9 1.1 Total Non Oxygenated Compounds (%) 97.4 98.5 98.2 3 hours with Hydrodistillation and 1 hour with Cold Pressing, and even with cold pressing you are getting over 60% less yield than with NEOS SFME and Hydrodistilllation. * Solvent free microwave extraction of essential oils. Chemistry Today, Vol. 26 n.2 (2008)

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

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. Over 17x less carbon dioxide released into the atmosphere with SFME 1. An improved microwave Clevenger apparatus for distillation of essential oils from orange peel, Journal of Chromatography A, 1112 (2006) 121-126

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. The NEOS system is based on Solvent Free Microwave Extraction (SFME) for rapid extraction of essential oils from aromatic herbs, spices and seeds. SFME technology was developed at the Laboratory of Chemistry of Natural Substances and Food Sciences at the Université de la Réunion, France. The NEOS system is the result of the partnership between Milestone and this laboratory, which lead to the grant European patents 1439218, 1618798 and 1629725.

NEOS Hardware Microwave Control Panel Glassware Chiller 4 areas we are going to look at that make the SFME that make it efficient, easy to use and safe.

Microwave Microwave Power output of 800 watts IR Sensor Safety Micro Switches Atmospheric Pressure Polymer Coating Microwave Power output of 800 watts As a microwave sample prep company, we make sure our microwaves safe.

Glassware 2 L and 5 L Glass Module Extension Tube Connecting Glass Tube Patented Extraction Module Glass Condenser Chiller

Labs Benefited by the NEOS Research/Development Quality Control

Flexibility of Applications Microwave Hydrodiffusion and Gravity (MHG) Microwave-Accelerated Steam Distillation (MASD) Microwave-Accelerated Dean Stark (MADS) Microwave Integrated Soxhlet (MIS)

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 The NEOS-GR is the result of a partnership between Milestone and the Université d’Avignon et des Pays de Vaucluse, France, which lead to the grant of the European patent EP 1 955 749 A1. This green extraction technique is an original “upside down” microwave alembic combining microwave heating and earth gravity at atmospheric pressure.

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. Hydro Diffusion method for extraction of oils is a type of steam distillation and is only different in the way in which steam is enters the container of the still. In hydro diffusion, steam is fed in from the top onto the botanical material while in the case of steam distillation, steam is fed from the bottom. In this way the steam can saturate the plants more evenly and in less time than with steam distillation. The condensation of the oil containing steam mixture occurs below the area in which the botanical material is held. The main advantage of this method over steam distillation is that less steam is used hence shorter processing time and therefore a higher oil yield. This method is also less harsh on the botanical material

Microwave Hydrodiffusion and Gravity (MHG) Higher Boiling Compounds No Solvent Hydrodiffusion Falls by Earth Gravity through Perforated Disc Cooling System This method involved placing plant material in a microwave reactor, without adding any solvent or water. The physical phenomenon, know as hydrodiffusion, allows the extract (water and essential oil) diffused outside the plant material, to drop by earth gravity out of the microwave reactor and fall through a perforated disc. A cooling system outside the microwave oven cools the extract continuosly, thus the water and essential oils are collected and separated in a flask. Whereas traditional process are carried out within 3 h, solvent free microwave hydrodiffusion plus gravity requires no more 30 min.

Benefits of MHG Shorter Extraction Times Recovery of Higher Boiling Compounds (pigments, flavonoids, carotenoids) Higher Purity of Extracts No Solvents

Extraction of Essential Oil from Rosmarinus officinalis MHG Extracts Extraction of Essential Oil from Rosmarinus officinalis Key things, extraction time, and oxygenated compounds.

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.

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) 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.

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) There are many different types of labs that can be benefited by Milestone’s NEOS with Solvent Free Microwave Extraction. These benefits include significantly shorter extraction times, quality extractions, environmentally friendly extractions, and great recovery. The flexibility of applications are an added benefit to labs who may have several groups within the company looking at the NEOS for different purposes.

Thank You!