Our Lady of Fatima University

McArthur Highway Marulas , Valenzuela City

College of Medical Technology

Isolation of Essential Oils and Synthesis of Perfume

Research Project in Organic Chemistry Dagatan, Angeline Gorospe, Angelie Lamayo, Arianne Regalado, Larry Adrian Silvestre, Ma. Cristina Solidum, Diore M. Villaviray, Nestie Bryal C. Vinco, June
Ms. Bricci Mendoza

October 15, 2012

Isolation of Essential Oils and Synthesis of Perfume Part 1: Introduction

An essential oil is the essence of a plant which produces its characteristic aroma. Essential oils are some highly volatile organic substances that can be isolated from odoriferous plants by various physical processes. The oils are usually concentrated in the seeds or flowers but may exist in other parts of the plants as well. Essential oils have been extracted from plants and spices such as allspice, almond, anise, basil, bay, caraway, cinnamon, cumin, dill, eucalyptus, garlic, jasmine, juniper, orange (and other citrus), peppermint, rose, rosemary, sassafras, sandalwood, spearmint, thyme, violet, wintergreen, and more, and valued since ancient times. Such oils were called essential because they were thought to represent the very essence of odor and flavor. Essential oils can be obtained from plants by a number of processes such as mechanical pressing and grinding, maceration, solvent extraction, distillation and concentration. In many cases a combination of processes are required for an efficient and effective isolation. Extraction processes can be by simple solvent extraction by soaking spices or flowers in water, alcohol, or oil. In this experiment we will use in the process known as steam distillation to extract the essential oil. Essential oils consist of a complex mixture of hydrocarbons, alcohols, esters, and carbonyl compounds. Some of these materials are called terpenes. Essential oils, as a group, do not need to have any specific chemical properties in common, beyond conveying characteristic fragrances. At different periods in history, essential oils have been used medicinally. Current medical applications range from skin treatments to remedies for cancer, and are often based on historical use of these oils. Medicinal claims, however, are now subject to regulation in most countries, and, as a result, have grown vaguer to stay within these regulations. Essential oils are used for flavorings, perfumes, and aromatherapy. Use of essential oils has revived in recent decades with the popularity of aromatherapy, a branch of alternative medicine which claims that the specific aromas carried by essential oils have curative effects. Oils are volatilized or diluted in carrier oil and used in massage, diffused in the air by a nebulizer or by heating over a candle flame, or burned as incense. But this time, we will use this to make a perfume. The use of plants and spices for perfume and aromatherapy has been known for thousands of years and has become a very important culture among the human races. The leaves, seeds, barks or other parts of many plants are known to have distinctively pleasant odors or flavors due to the presence of essential oils. The goal of this project is to isolate the essential oil from assigned spice, allspice, herbs and other materials then to synthesize a perfume from this extract. The isolation of the oil is done by steam distillation. The product of steam distillation is the extract with jojoba oil in the separate funnel and anhydrous sodium sulfate. The final step is to remove the sodium sulfate out of the solution by decantation.

Isolation of Essential Oils and Synthesis of Perfume PART 2 METHODOLOGY

MATERIALS NEEDED

CHEMICALS AND REAGENTS: Spices, approximately 5 g of one of the following: Cinnamon sticks Whole cloves Fennel seed Coriander Allspice, whole Cumin seed Caraway seed Black pepper

LABORATORY APPARATUS: Distillation apparatus: 150 Round bottom flask Condenser Cork Rubber tubing Iron stand Iron ring Iron clamp Bunsen burner 50 mL Erlenmeyer flask Thermometer, 250C Wire gauze 25 mL of Erlenmeyer flask Test tube, vial, or small bottle (to contain 10-15 mL of product Beaker Mortar and pestle Boiling Chips Separatory funnel Dark bottle

Herbs, such as rosemary, peppermint, thyme, lemon verbena, and more Citrus, such as lemon, orange, or grapefruit zests (larger quantities of citrus zest, such as 15 20 g, should be used for this procedure) Flowers, such as roses, jasmine, lavender, lily of the valley, violets, carnations, and more (fresh flowers should be used, exact quantities will need to be determined) Jojoba oil Distilled Water Ice Anhydrous sodium sulfate

Isolation of Essential Oils and Synthesis of Perfume

Assemble the steam distillation apparatus, as diagrammed below using a 150 mL round bottom flask and a 50 mL collection flask.

This method is usee where the sought substance is steam volatile or vaporizes with the steam. The unwanted nonvolatile fraction is left behind. It is often used in recovering essential oils from leaves, and other parts of the plant.

Obtain 5 g of a spice, flower, citrus zest, or herb. Break up any large pieces of the spice with a mortar and pestle, but do not grind the spice to a powder.

Essential oils are easily decomposed by heat so we need to break up any large pieces so we can heat them easily to prevent their decomposition.

Place the spice, and other material, into the distillation flask and add 50 mL water and boiling stone.

The ingredients will put in the flask to start the distillation with the boiling stones to accomodate the heating and prevent bumping and break up of the apparatus.

Turn on the water to the condenser, and then start heating the liquid in the flask

to provide a slow, steady rate of distillation

Continue the distillation until approximately 25 mL of distillate has been collected in the receiving flask

25 ml is the required amount of distillate to be collected.

Disassemble the apparatus, saving the liquid in the receiving flask.

The distillation is already done and will now procede to separation of essential oil from water.

Empty the water from the separatory funnel and add the liquid from the receiving flask to it.

Separatory funnel is the appropriate apparatus to get a complete separation of two liquid layers.

Isolation of Essential Oils and Synthesis of Perfume

Extract the essential oil with jojoba oil by adding 10 mL of jojoba oil to the separatory funnel. Stopper and shake well, venting every few shakes.

the essential oil will comine with the jojoba oil and the water will separate because the two liquids are immiscible with each other.

Allow the layer to separate. The jojoba oil layer will be on top.

Allow the layer to separate before drawing off each layer. The oil will be on top because it is less dense than water.

Drain the water layer into a beaker. Drain the jojoba oil layer into a 25 mL Erlenmeyer flask.

Draining the water into beaker will now separate the jojoba oil.

If the jojoba oil extract is cloudy, dry the extract with a small amount of anhydrous sodium sulfate.

The anhydrous sodium sulfate will absorbs the water from this solution.

Decant the clear jojoba oil extract into a clean, test tube or vial. Label the container. This mixture is an essential oil extract and will be used in the preparation of a perfume.

Separate the sodium sulfate from the jojoba oil by decantation.

Using a dark bottle add the jojoba oil first. Add the essential oils start with the base notes, then middle, then top, smelling as you go.

Dark bottle because perfume is very sensitive to UV light or heat.

Add 2.5 ounces of alcohol, shake for a few minutes, then let it sit for 48 hours (or up to 6 weeks-the longer it sits, the stronger the smell). Put it in a dark bottle.

Alcohol will contribute to the strong smell of the perfume.

Isolation of Essential Oils and Synthesis of Perfume Part 3 Result and Discussion