The tree of perfume: the bigaradier and its essences “Citrus aurantium”

Naceur AYED*

* Naceur Ayed is Professorr Emeritus Industrial chemistry at l’INSAT (University of Carthage)

Aromatic plants store scents in their organs (flowers, fruits, leaves, bulbs, wood …). Relative extraction makes it possible to prepare a wide range of basic products for perfumery and cosmetics as well as aromatization (essential oil, hydrosol, concrete, absolute, essence …). Each type of extract borrows a specific process (hydrodistillation, steam distillation, extraction with organic solvent, mechanical extraction).

Domestically, several floral waters are traditionally produced, such as the waters of bitter orange blossoms, roses, rose hips, geraniums … and which are used for family consumption and local trade.
The industrial and domestic aromatic extracts have nutritional, cosmetic and aromatherapeutic benefits that show how much the flora records sensory qualities capitalizing on Tunisia’s natural resources.
Floral waters, essential oils, etc. … have specific compositions, characterized by sensory notes with multiple effects in addition to the feeling that it generates on the body, the atmosphere and the environment. The recorded analyzes provide a database that elucidates the properties of aromatic plant products to help set up a sustainable development plan through the promotion of a value chain of this production sector capitalizing Tunisia’s flora.

Key words: Aromatic plant, Bigaradier, Floral water, Essential oil, Olfactory note.

INTRODUCTION

Aromatic plants store scents in their organs (flowers, fruits, leaves, bulbs, wood …). Relative extraction makes it possible to prepare a wide range of basic products for perfumery and cosmetics as well as aromatization (essential oil, hydrosol, concrete, absolute, essence …). Each type of extract borrows a specific process (Hydrodistillation, steam training, extraction with organic solvent, mechanical extraction …). Several companies produce these aromatic plant extracts industrially and export them abroad to integrate perfume and perfume formulations. Domestically, many floral waters are traditionally produced, such as the waters of bitter orange blossoms, roses, rose hips, geraniums … and are used for family consumption and for local trade.
These products have nutritional, cosmetic and aromatherapeutic benefits … which show how the flora records sensory qualities capitalizing the natural resources of Tunisia. The products of the scent are strong points of Tunisia and constitute messengers of communication ensuring dialogue and sensory sharing. The bigaradier with its neroli, its small grain, its essence, its concrete, its absolute offers a bouquet of odoriferous extracts. The picking of orange blossoms creates a special atmosphere and its aroma wafts the whole city and the environment.

Citrus bigaradia :

Citrus bigaradia, bitter orange, is a tree belonging to the family Rutaceae. It is 3 to 4 meters high and has a branched trunk in a thorny branch. Originally from southern China, the bigaradier was introduced in the Mediterranean at the time of the Romans. Brought to Europe by the Arabs in the 12th century and by Europeans in the USA, Central America and South America.
It is grown in the ground in warm regions. The average production is 8 to 12 Kg of flowers per tree. In good behavior, it can reach 15 to 25 kg. In Tunisia, the bigaradier is cultivated mainly in the region of Cap Bon on a surface of 352 hectares and counts approximately 102,600 feet of which 76800 trees in production.
The average annual production is of the order of 1000 tons of orange blossoms. 50 to 60% are processed by distillation units in the region. The rest is distilled with steam by the housewives who perpetuate “the tradition of the still”: (El Kattar)

Leaf :
The oval-shaped, slightly leathery leaves, the lamina, which is 4-6 cm long and 3-4 cm wide, is articulated on a petiole 1 cm long, dilated, with a wing six to seven millimeters wide. .
By steam distillation of leaves and stems of bitter orange, we obtain the small grain, an essential oil known for its woody and floral scent and for its calming and relaxing virtues. The relative hydrolate is Me Mehkah water
Volatile solvent extraction gives the relative absolute from which, by addition of the alcohol, the concrete is obtained.

The fruit
The fruit is a fleshy berry, its bark has a rough orange-red surface. When it is ripe its juice is acid and bitter. Because of this bitterness it is consumable only prepared in jam.
Extraction by expression of bark gives the essence of bigarade from which and by addition of alcohol the concrete is obtained.

Flower and flowering:
The bitter orange blossom is the symbol of virginity. The Grasse tradition consists in offering a garland of orange blossoms to couples who get married during the flowering of the orange bitter orange. Tradition relayed to Nabeul and Hammamet, although the necklaces and bouquets of these flowers are available at harvest time and much appreciated by lovers of their scent.

Bouquets of bitter orange flowers

The flowers are actinomorphous, of a very pure white, they are very fragrant and grouped by two or three in the axils of the leaves. The flower has five 5-8 fleshy petals with secretory pockets of essential oils. The basal part of the flower bears many stamens. Flowering depends on climatic factors. In Tunisia it usually takes place around March-April.
The distillation with water vapor (hydrodistillation) of these flowers gives, on the one hand the essential oil of orange blossom known under the name of neroli and on the other hand the hydrolat: the water of flowers of orange.
Volatile solvent extraction gives the absolute of orange blossoms from which, by addition of alcohol, the concrete is obtained.

Characterization of traditionally prepared perfumes.

Neroli Essential Oil:
This oil is obtained by steam distillation. The still is half filled with water and flowers. It is heated by injection of steam into the double bottom of the still to bring the water to a boil. The distillation can also be accelerated by injecting steam directly into the still. The water vapor formed in situ goes, by a so-called azeotropic phenomenon, to drive the volatile molecules (of low molecular weight) towards the cooling coil. This vapor condenses Hydrolat composed of aqueous phase and essential oil, will float the water and separate it inside the vase “florentin”. The yield to obtain this essence: the “neroli” is 0.1%.

Bouquets of bitter orange flowers

The flowers are actinomorphous, of a very pure white, they are very fragrant and grouped by two or three in the axils of the leaves. The flower has five 5-8 fleshy petals with secretory pockets of essential oils. The basal part of the flower bears many stamens. Flowering depends on climatic factors. In Tunisia it usually takes place around March-April.
The distillation with water vapor (hydrodistillation) of these flowers gives, on the one hand the essential oil of orange blossom known under the name of neroli and on the other hand the hydrolat: the water of flowers of orange.
Volatile solvent extraction gives the absolute of orange blossoms from which, by addition of alcohol, the concrete is obtained.
Characterization of traditionally prepared perfumes.

Industrial Bitter Orange Flower Water:
The orange blossom water is recovered during the hydrodistillation of the hydrolate separated from its neroli. When it is extracted industrially, it is considered a “by-product” whereas at the domestic level, by the traditional hydrodistillation, it is the desired product (the quantities of hydro-distilled flowers being in this case too weak to hope obtain gasoline). The quality of the orange blossom water will be expressed according to the weight of flowers used in relation to the volume of water of flowers produced. For example 1 = 1 corresponds to 1 l of water per 1 kg of flowers used. According to the codex, orange blossom water must contain at least 0.3 gr. / L. of organic compounds. Above 0.9 gr. “Eyes” are formed, a sign of maximum concentration.

Preservation of floral waters:
Floral waters are sensitive to bacteriological development. For a good conservation, it is advisable to store them protected from the light, in well filled bottles (without air) and in cool. The industrial means of decontamination are the sterilizing filtration and the passage under a UV lamp specially designed for debacterization. To prevent further contamination of these waters, only the chemical agents are effective. Phenoxyethanol and methyl para-hydroxybenzoate are used in cosmetics. Sodium benzoate and potassium sorbate are allowed as a preservative. You can add citric acid, an agent that inhibits bacteriological development, but can change the flavor. Pure Micro Forte tablets can be an elegant solution for home use. These pellets used by trotting globes, to make drinking water dubious, suppress the germs at a dose of 1 tablet per liter.

Stability in time:
The composition of orange blossom water is not stable over time. Due to their high dilution some molecules oxidize, including linalool, alpha terpineol and citronellol. On the other hand, the pink cis oxide increases, as does methyl heptenone. This molecule serves as a marker for this degradation. It is obvious that these changes in the chemical composition will affect flavor and aromatherapy properties. It is therefore necessary to avoid keeping this water of flowers of bitter orange for too long.

Influence of the metal used for the manufacture of the still:
Originally, floral water stills were made of terracotta. They were replaced by copper stills assembled with rivets themselves replaced by tin tin stills with tin solder. Aluminum pots can also be found playing the role of still. Industrial appliances are made of stainless steel.
In addition, few scientific studies were conducted to determine the influence of the nature of the raw material from which the Alembic is made on the quality of the essential oil obtained.
– Aluminum is to be banned because it generates aluminum salts toxic for the health as well as the salts of tin.
– Copper induces a green color, it can affect the chemical composition by blocking especially sulfur molecules by complexassions.
– The tinplate meanwhile, induces a red coloring.
– Copper and iron will release catalyst metal ions from the formation of free radicals. For all these reasons we will favor a good quality stainless steel (food). It will have the slightest interaction with organic molecules.

The Absolute of the Waters of Flowers:
Orange blossom water contains between 0.3 and 0.9 gr / l. of organic compounds. To extract the “Absolute Flower Water”, the flower water is brought into contact with a volatile solvent (Hexane, Cyclohexane, …) by means of a lively stirring in a tank or a passage through a column against the current. The solvent will then be charged organic molecules and after decantation, an aqueous phase having lost these compounds, is separated from an organic phase (higher because lighter) enriched in these aromatic compounds. This is concentrated in an evaporator in “Absolute Flower Water” and the solvent will be recycled. 3 tons of water of flowers will give 1 Kg of Absolute.

Concrete and absolute orange blossom
Some of the harvested flowers are transformed into concrete. For this we load in an extractor the flowers arranged on intermediate grids (to avoid packing) that is covered with a volatile solvent (usually hexane). The mixture is allowed to macerate at ambient temperature and the solvent which has been loaded with extract is then withdrawn to replace it with fresh solvent and to carry out another extraction. This operation is repeated 2 or 3 times. The fractions of extracts are combined and distilled. Once the solvent is removed, it remains in the evaporator the concrete (waxy product, orange) obtained with a yield of 0.2%. To be used in perfumery this concrete must be cleared of waxes and insoluble by recovery in cold ethanol. The concrete is stirred in ethanol, ice-cold (cooled) to -10 ° C., filtered and the filtrate which contains the absolute is concentrated in a vacuum evaporator. The yield of the absolute is about 55%.

The stills a subject of study to improve their nature and the quality of aromatic products.

Traditional stills: tinned copper, tinplate, stainless steel.

Hydrodistillation apparatus:
The traditional system:
Appliances for the hydrodistillation (Alambics) of flowers and aromatic plants are formed of kazen pots of tinned copper or tinplate, whose capital “kabous” terracotta emits a long tubular collar “jâbaâ” tinplate galvanized rectilinear cylindro-conical ending with a diameter elbow adapting to the opening of the flasks or receiving bottle of the hydrosol. This tube passes through a terracotta or metal wood tank, serving as a coolant, where the cold water must be renewed as hydrodistillation progresses. A seal placed between the lid and the pot and made of a cotton fabric ribbon “kfila”, coated with a clay slip, ensures the tightness of the system to prevent any leakage of aromas.
In Tunisia, the manufacture of stills has evolved from the traditional copper system through the vertical tinplate system to the improved stainless steel system. Each system has some peculiarities but the principle of hydrodistillation remains the same for all types of stills.
The improved stainless steel system:
This system is similar to the traditional still except that all parts are stainless steel. Its boiler is cylindrical, covered with a cap, itself, surmounted by a gooseneck connected to a tank refrigerated by a coil. The floral water accompanied by the essential oil is condensed through a bent tube and collected in the receiver.

The vertical system of tinplate (or copper)
This system consists of 3 pieces of tinplate (or copper) stacked on top of each other. The boiler is surmounted by a cap ensuring the refrigeration, this part is linked to the collector tube allowing the condensate to flow in the receiver.

Ph8: Copper still

The essence of petit grain:
The essence of petit grain is obtained by steaming. In an alembic we load the products of size of the bitter orange tree: sprigs bearing the leaves and small immature fruits (hence the name of petit grain), we pour water, and by the heated double bottom, this one , brought to a boil, is transformed into vapor thus bringing about the essence of Petit Grain. By condensation we obtain a condensate which, in the Florentine vase, will decant and give, on the one hand the Essence of Petitgrain with a yield of 0.1% and on the other hand the Eau de Brout “Meeelkah”.
As for the orange blossom water, we extract the “debrout water” with a volatile solvent and we obtain “the Absolu des Eaux de Brouts” with a yield of 1 kg for 3 tons of grazing water).

The fruit:
Fruit alone the skin is valued. By expression the fresh zest (pericardium) will give the essential oil of bigarade. The yield is 0.35%. The extraction operation, formerly manual, is now carried out by machines such as peeler, smoke machine, Brown, etc.
This essence is used in the aroma industry and in the perfume industry. Because of its high content of coumarins and psoralens its use is regulated by IFRA.
Dried zest is used by the food industry, mainly by liqueurs and beverage drink manufacturers. The button: dried is used in herbal tea and for the preparation of the infusion called “white coffee”.

The industrial stil

In perfumery
In perfumery, Neroli, the Orange Blossom Absolute and the Petit Grain Essence are used. Neroli is used in association with the absolute in “Eau de Cologne”. It is also found, alone in the “Eau de Toilette” masculine or associated with the absolute in the “Eau de Toilette” feminine. The essence of petit grain is, in turn, used mainly in personal hygiene products: shampoo, bubble bath, shower gel, soap, as well as in industrial perfumery in detergents and other detergents. For the absolutes of the waters one uses that of flowers in waters of feminine toilet and that of browse for its notes chypres, oriental and leathers in certain perfumes.

A Nabeulian alcohol-free perfume: “EL MAJMOUA”

Composition:

Aromatic plants:
Pelargonium rosat: Atrchia
Rosa canica: Nesri
RosaDamascena: Ward
Citrus aurentum: Zahar
Alaegnusaugustifolia: Zanzfour

Fumigation Products: Atractylisgum: ded
Clove Clove: Oud Kronfel
AquilariaAgollocha: oud kmeri
Incense: Bkhour
Musk: Mesk
Amber: Ambar
Myrrh: Mestekeh

In aromatherapy:
Neroli is sought for its neuro-tonic properties, very effective in the treatment of nervous breakdown. It is a rebalancing (anti-blues) that makes it much better in the skin. It is also a tonic of the general system. It is also used to help with childbirth.
On the other hand, it has anti-infectious, bacterial and parasitic properties (interesting for children and babies who have worms because by its non-toxicity it has no side effects). It is used orally, cutaneously or respiratory.
The absolute, in addition to the properties of neroli, has an antioxidant power due to the presence of flavonoids.
The water of flowers is interesting in case of conjunctivitis, it can be used to wash the eyes of babies and also to help them to sleep and have calm nights.
The essence of petit grain is an anti-infectious, antispasmodic and regenerative skin tissue. It will be used for wounds, coughing fits and muscle spasms.
In food flavors:
Bitter oranges are mainly used for “marmalade” or bitter orange jam. They are also used in confectionery and for the flavoring of liqueurs and non-alcoholic beverages. The orange blossom water is used in the preparation of the traditional pastry of North Africa.

In cosmetics and care and hygiene products:
Cosmetics, hygiene, care and massage products are available on the international and Tunisian market based on extracts of bitter orange.

Neroli
It is in the middle of spring that many regions across Tunisia enjoy the sublime scent of bitter orange and especially the region of Cap Bon. The blooming of the bitter orange and other aromatic trees boosts the traditional activity of hydrodistillation. In addition to artisanal systems with low production capacity, industrial units, with copper or stainless steel stills, produce different species. The most popular herbs are rose bush, rosehip, bitter orange and geranium. The annual supply of aromatic hydrolate, essences, concretes and absolutes is drawn from it. All are used in the composition of perfumes and aromas of cosmetic and therapeutic products.
Neroli produced by distilleries in the Nabeul region is partially exported in the raw state. How much would be desired refining this product to increase its added value!
The legend of neroli: Neroli is the oil extracted from the flowers of bitter orange. It is named after an Italian legend who says that the wife of a prince named nerol gave his name to neroli. She used it to perfume the water of her bath as well as her gloves.

Neroli: Characteristics

 

 

Citrus bigaradia / aurantium

 

Family Rutaceae
Origin of the bitter orange Southern China, introduced to the Mediterranean at the time of the Romans.
Obtaining Distillation of the fresh flowers of the bitter orange
Yield 1 kg for 1 ton of flowers
Density 0,866 to 0,876
Refractive index 1,470 to 1,474
Acid index 2 maximum
Ester index 28 to 50
Rotating power +6° to +11°
Odour Suave (pleasant), flowery
Division

 

Tunisia, Mediterranean Basin, Florida

Neroli: aromatic profile

Compound Neroli

(bigaradier de France)* (%)

Neroli

dEgypte (%)

Neroli of unspecified

origin (%)

Alpha pinene  

35.0

4.26 0.8
Camphene 5.50
Dipentene
Paraffine C-27
Sabinene 2.55
Beta pinene 8.67 15.0
Myrcene 2.15 1.6
Delta 3 carene 2.46
Limonène 22.43 16.1
Trans ocimène 6. O
Terpinene 4.14
p-cymene trace
Terpineol 2.0 (alpha) 1.87 3.0 (alpha)
Linalol 30.0 2.52 30.6
Acetate de linalyle 7.0 0.87 9.1
Geraniol  

 

4.0

1.02 2.0
Nerol 6.97 (y compris farnesol, non identifié) 0.2

 

Geranyle Acetate  

4.0

 

3.74 2.9 1,5 à 4
Neryle Acetate 1.7 1 à 3
Citronellol 1.87 0.2
Citral 2.41
Beta citral 1.87
Nerolidol 6.0 7.6 1 à 9 (trans)
Farnesol Voir nerol 4.0
Antranilate de Methyle 0.6 1.89 0.3 0,1 à 1
Indole < 0.1 0.1
Acide Acetique, palmitique 0.1
Aldheyde décyclique  

 

 

11.2

Acide phenylacetique
Acide benzoique
Farnesol
Jasmone

Properties and uses of neroli

Cosmetics:
Neroli has an anti-aging effect due to its high ceramide content. On the other hand, because of its pure natural origin, it perfectly respects the epidermis and gives it great efficiency and excellent tolerance. Neroli is tonic, it strengthens and strengthens the muscles of the face to give them strength. It is mainly suitable for dry and sensitive skin.

Perfumery:
Neroli is used all over the world in both colognes and the most expensive perfumes. It gives them an extremely fresh, rich, floral and fine smell.

Aromatherapy:

Aromatherapy is the art of healing with the aroma of essential oils of plants
Aromatic. Its purpose is to strengthen and stimulate the natural defense system present in each organism.
The essential oil, neroli, has properties, anti-infectious, energizing and toning of the nervous system, liver and pancreas. It promotes sleep. It is an antidepressant, it improves the venous capillary circulation, decongests the uterus and regulates the heart. This oil is regenerative at the cellular level, deodorant, antispasmodic, antiseptic, bactericidal, aphrodisiac, hypnotic soft, rebalancing and soothing in the emotional disorders. It is used in children in case of over-excitement or difficulty falling asleep. Neroli is indicated in local applications for acne, it is used against depression, used for care of dry, devitalized or wrinkled skin and normal skin

AGROALIMENTARY:

Neroli is used in the manufacture of certain food flavors. The fruits of the common bitter orange are used in confectionery. They go into the making of bitter orange jam, the “Dundee” very popular in Britain. The Nabeulian family uses a recipe of jam of petals of flowers of bitter orange, a real delight.
The specification and expertise of aromatic materials through the probes revealing natural scents make it possible to monitor the quality of these aromatic products

 

Benefits of essential oils of bitter orange

 

Conclusion

Man has been naturally seduced by everything that belongs to the olfactory.
This article has been devoted to the aromatic plants of the Tunisian terroirs which are described without forgetting their extraction processes allowing to obtain the extracts whose exquisite perfumes are sought to please and make the life pleasant by their odoriferous, culinary and pharmaceutical qualities.
The floral waters, essential oils, etc. … have specific compositions, characterized by sensory notes with multiple effects in addition to the feeling that it generates on the body, the atmosphere and surrounding.
The recorded analyzes provide a database that elucidates the properties of aromatic plant products to help set up a sustainable development plan through the promotion of a value chain of this production sector capitalizing Tunisia’s flora.

Leave a Reply

Your email address will not be published.