Vanilla Perfume: Formulation to How Make it
Perfume is one of the cosmetics formulated from a mixture of essential oils or synthetic chemical compounds that have aromatic properties, fixatives to maintain the aroma, and solvents. Perfume is a favorite cosmetic because of its function, which is used to give fragrance to the human body, objects, or enclosed spaces, as well as an additive in various cosmetic formulations to boost a person's confidence.
The categories of perfume are divided into several types: perfume extract (20-30%), Eau de Parfum (8-15%), Eau de Toilette (4-8%), and Eau de Cologne (1-3%). The characteristic that distinguishes them from each other is based on the proportion of solvents mixed in the preparation, which will also affect the longevity of the perfume when applied.
Perfume is one of the cosmetics formulated from a mixture of essential oils or synthetic chemical compounds that have aromatic properties, fixatives to maintain the aroma, and solvents. Perfume is a favorite cosmetic because of its function, which is used to give fragrance to the human body, objects, or enclosed spaces, as well as an additive in various cosmetic formulations to boost a person's confidence. The categories of perfume are divided into several types: perfume extract (20-30%), Eau de Parfum (8-15%), Eau de Toilette (4-8%), and Eau de Cologne (1-3%). The characteristic that distinguishes them from each other is based on the proportion of solvents mixed in the preparation, which will also affect the longevity of the perfume when applied. Perfume can be formulated into three different components: top notes, which consist of 15-25% of the total composition, middle notes consisting of 30-40%, and base notes consisting of 40-55% of the final fragrance formulation. These components are formed based on the rate of evaporation of fragrance molecules into the atmosphere. Compounds in the top note are characterized by their rapid evaporation in the first 15 minutes, followed by middle notes, and finally base notes. The types of aromas commonly used for top notes include citrus, green, and fruity aromas, middle notes include floral and spicy scents, while base notes consist of woody aromas and derivatives from animal sources.
Synthesis of Compounds From Vanillin to be Used as Perfume
Indonesia is a rich country with a variety of plants that can be utilized as raw materials for perfumes. However, this potential has not been maximized. One of the plants with potential as an aromatic substance is vanilla (Vanilla planifolia A). Vanilla is known as a plant that produces vanillin contained in its fruit. Vanillin is a white powdery substance. Generally, vanillin has been utilized and used as a food and beverage additive because it has a distinctive aroma. Vanillin has a chemical name 4-hydroxy-3-methoxy benzaldehyde (C8H8O3) and belongs to the phenol compound group. Vanilla fruit can be extracted for the extraction or synthesis of menthol vanillate compounds through the oxidation stages of vanillin compounds in the fruit using AgNO3 oxidants, resulting in vanillic acid compounds which are then esterified with menthol reagents. The synthesis is carried out through the following stages:
Oxidation of vanillin compound
This oxidation is carried out through the stages of dissolving AgNO3 into NaOH solution at room temperature. After that, a dark brown Ag2O precipitate and soluble NaNO3 salt are obtained. The formed Ag2O precipitate is then filtered and washed with distilled water. Then, wet oxidation of Ag2O is carried out by adding 40 mL of distilled water, 3.93 g (97 mmol) of NaOH pellets, then stirred vigorously, and the temperature is raised. When the temperature has reached 55-60°C, 3.04 g (20 mmol) of vanillin is added and stirred vigorously for about 10 minutes. Then, the mixture is filtered with filter paper and the filtrate is acidified with concentrated sulfuric acid until crystalline vanillic acid is formed, which is insoluble anymore. The formed crystalline vanillic acid is then filtered and washed with distilled water, followed by liquid-liquid extraction using ethyl acetate and distilled water in a ratio of 1:1 (v:v). The formed organic solution is separated, then dried to obtain pure vanillic acid. The formed vanillic acid crystals are collected, and their yield is calculated, followed by a melting point test and identification using FTIR spectroscopy to observe the difference from the base compound.
Esterification of vanillin compound
The obtained vanillic acid is then taken as much as 1.5 g (0.0089 mol) and added to 2 mL (0.02 mol) of SOCl2 in a 250 mL three-neck flask. Next, the mixture is refluxed at a temperature of 45°C for 1 hour. After that, the mixture is cooled in an ice bath until the temperature reaches 10°C. Then, vanilloyl chloride is passed through the N2 gas, then menthol is added as much as 2.78 g (0.0178 mol) which is added slowly through a dropping funnel and added with 1 drop of pyridine to neutralize the remaining HCl. The mixture is refluxed again for 30 minutes. The resulting product is added with anhydrous Na2SO4 and then filtered. The obtained filtrate is weighed, and its yield is calculated and analyzed using FTIR and 1HNMR.
Organoleptic Test
The production of perfume with vanillin is then subjected to an organoleptic test to examine the synthesized compounds applied as perfume. Organoleptic testing can be performed with specific criteria, such as aroma fragrance, aroma sharpness, and preference for the resulting aroma.
Perfume Formulation
Perfume has several types, one of which is EDP (Eau de Parfum) which can be formulated through several components including top notes, middle notes, and base notes. For example, components that can be formulated are top notes (white peach), middle notes (jasmine, cherry blossom, and green tea), and base notes (sandalwood and vanilla) mixed in a chemical glass. The solution is then stirred until homogeneity is achieved, and then an evaluation test is carried out by applying the solution to aroma test strips. Formulations of fragrances that prove suitable can be further developed into formulations which are then prepared as finished products. Evaluation tests in perfume formulations are performed with the following tests:
Organoleptic Test
The organoleptic test includes evaluation of three main parameters, namely homogeneity, color uniformity, and formula consistency.
Aroma longevity test
Aroma longevity evaluation is performed by spraying the perfume solution onto aroma test strips.
Spot Test
The spot test is carried out by applying perfume to brightly colored paper, followed by measuring the diameter of the spot produced using calipers. A larger perfume spread indicates superior quality.
Hedonic Test
Hedonic evaluation is performed by panelists, where each panelist evaluates EDP samples based on their sensory perception and emotional response.
Sensory Evaluation
Sensory evaluation involves panelists assigned to evaluate perfume samples, where panelists are asked to assess the smell attributes of each sample based on their sensory sharpness. Sensory evaluation includes the assessment of aroma from perfume samples using descriptive methods.
