INTRODUCTION
Research rationale
In the northern mountainous provinces, orange trees are grown in many localities throughout the provinces of Ha Giang, Tuyen Quang, Yen Bai,
Identified as a key fruit tree of a number of provinces, many projects, projects, and programs to develop growing areas, research, and apply technological processes in cultivation to increase yield and quality for orange trees crockery has been made
However, in recent years, people arbitrarily expanded the area of culturing oranges, overcoming planning barriers has many potential risks When the planning is broken, the area is massively replicated, which will lead to the immediate consequences of a sudden increase in output, and the risk of products falling into stagnation, price pressure, unsolvability Not to mention many spontaneous growers lack experience in orange care and harvesting, leading to poor fruit quality and susceptibility to pests and diseases Meanwhile, the area of citrus crops such as pomelo and sweet tangerine has grown very strongly, consumers have more choices when buying fruit for food These causes make the market price of this fruit tree much lower, plus extreme weather, prolonged heavy rain at the time of harvest, which reduces yield due to broken and damaged oranges
Currently, there are many fruit jam products such as grapes, tangerines, pomelos, strawberries on the Vietnamese market, but the products from oranges grown in Vietnam are quite a few on the market We have an abundant source of domestic orange products, but we have not taken full advantage of it
From that situation, it is necessary to research and find solutions to increase the value of oranges by taking advantage of raw materials that are poorly designed and fallen
4 oranges to avoid waste Realizing that the orange fruit contains a lot of essential oils in the peel to open up a new consumption direction for this fruit, bringing higher economic efficiency to the people who grow it
On that basis, we propose to carry out the topic: "Research on extraction process and development of products from Orange essential oil".
Research objectives
Research on the extraction process of orange essential oil and develop products from orange essential oil
Research on optimizing conditions in the extraction process of essential oils:
- Research on optimizing salt concentration in the essential oil extraction process
- Research on optimizing the ratio of water to raw materials in the process of extracting essential oils
- Research on optimizing the distillation duration of essential oils in the extraction process
Developing and perfecting products prepared from essential oils: Orange essential oil hand sanitizer.
The requirement of the research topic
- Researching and perfecting the process of extracting and preserving essential oils
- Analysis of essential oil composition after extraction
- Develop and perfect the product prepared from essential oils
The scientific and practical significance of the research topic
1.4.1 The scientific significance of the topic
- Research results of the topic will provide new scientific data on:
+ The influence of factors on the ability to extract the orange essential oil
+ Build the process of extracting essential oils with the most optimal conditions
1.4.2 The practical significance of the topic
- Help students improve their experience and skills in scientific research practice, consolidate theoretical knowledge, apply in practice to improve themselves
- From the research results of the topic, it will contribute a part to the study of the essential oil production process that brings values, health, and economic benefits to the community
LITERATURE REVIEW
The origin of orange
Orange has the scientific name Citrus sinesis Osbeck, which belongs to the genus
Citrus, family Rutaceae Oranges are native to tropical and subtropical Southeast Asia
Oranges are widely grown in warm climates, and the taste can vary from sweet to sour
The scientific name is Citrus nobilis (Reticulata X Sinensis) mainly distributed in Thailand, Cambodia, and Vietnam The main harvest season is August to December
In Vietnam, oranges are grown all over the country, mainly in the northern provinces of Vietnam such as Ha Giang, Tuyen Quang, and Yen Bai In the South of Vietnam oranges are also grown in Tam Binh (Vinh Long); Cai Be (Tien Giang), O Mon (Can Tho)…
Introduction to essential oils
Essential oils are aromatic substances or odorous substances present in certain parts of plants (such as seeds, roots, tubers, bark, flowers, leaves, fruits, oils, resins) or animals (bags of essential oils) The flora with essential oils is about 3000 species, of which 150-200 species are of industrial significance Essential oils are found in the above raw materials in very different concentrations, which can vary from parts per million to percent, and essential oils are relatively volatile
Essential oils are widely distributed in nature The amount of essential oil in the tree depends on climatic and soil conditions Plants growing in the tropics have more essential oils than in temperate regions Even within a plant, the composition and amount of essential oils in different parts are also different In addition, the amount of essential oil depends on the living environment of the plant, the method of harvesting, preservation, and extraction
Essential oils are distributed concentrated in a number of families such as Apiaceae, Asteraceae (Compositae), Burseraceae, Cupressaceae, Fabaceae, Lamiaceae (Labiatae), Laurenceae, Myrataceae, Pinaceae, Poaceae (Gramineae), Rutaceae, Zingiberaceae,…
Essential oils are present in different parts of the plant, such as in flowers(pink, jasmine, orange, lemon, ), in leaves (eucalyptus, mint, basil, ), in the bark (cinnamon), in the roots (ginger, turmeric, incense, ) In plants, essential oils can be available or only formed under certain conditions At that time, essential oils are not normal parts of the plant but only appear under certain conditions when some parts are dead Essential oils are the end products of metabolism and cannot be used again for the plant’s vital activity
Classification of essential oils: There are two types of pure essential oils and non-
8 pure essential oils Pure essential oils: absolutely no toxins, no chemical preservatives, so it is very safe for users and brings fast results when treated Non-pure essential oil: an essential oil is mixed from pure essential oil with other chemicals and still retains the aroma of the essential oil
2.2.2 The origin and development of essential oils
Essential oils have been known to mankind for a long time, since ancient times people have known and used plants with essential oils in dried form From the 17th to the 19th centuries, essential oils were used extensively for makeup, medicine, and industrial use to a larger extent From the 20th century to the early years of the 21st century, along with the progress of mankind and the progress of science and technology, the essential oil industry has gradually developed, essential oils have become a product
It is an indispensable product in human life and is widely applied in industries such as flavoring, food, cosmetics, pharmaceuticals
2.2.3 The physical properties and chemical composition of essential oils a The physical properties:
Essential oils usually exist in liquid form at room temperature, are fragrant, are rarely colored except for essential oils containing aluzen which are blue At room temperature, essential oils are usually liquid, with a density less than 1 (except for a few types such as cinnamon and clove essential oils, which have a density greater than
Essential oils can be evaporated., they are insoluble or very slightly soluble in water, but they make the water an auroma Essential oils are mixtures, so they do not have a certain boiling point (about 100 o C to 200 o C), essential oils are soluble in alcohol, ethers, organic solvents, and fats
To determine the physical properties of essential oils, it is common to determine
9 indexes such as density, refractive index, solubility in alcohol at 90 o at 25 o C, boiling point, polar rotational yield, and color
In terms of color, essential oils are usually colorless or pale yellow A small number of essential oils have color (e.g mugwort oil is blue, the cinnamon essential oil is dark brown) due to the presence of colored compounds that are attracted to the essential oil during extraction (e.g green due to chlorophyll, yellow due to carotenoids, etc.) The smell and taste of essential oils are mainly caused by oxidized components b The chemical composition in essential oils
Essential oil is a liquid that is purified (most commonly by steam or water distillation) from the leaves, stems, flowers, bark, roots, or other components of plants
Any essential oil has the following ingredients:
- Monoterpenes: Found in most essential oils, typically miaxene, ocimene, and laurel oil They are well air-filtered Monoterpenes are present in most essential oils
- Sesquiterpenes: Although not as volatile as monoterpenes, the typical linear and cyclic sesquiterpenes are farnesene, Zingiberene (ginger essential oil) And has a soothing effect, is anti-inflammatory, and is anti-infective
- Phenol: Some phenols are extracted from essential oils such as Thymol, Estragol, Eugenol, etc The disinfectants are mostly found in plants, stimulate the body, phenol is effective when used in small doses However, large doses can be a neurotoxin and may cause skin irritation
- Alcohols: Some important alcohols extracted from common essential oils such as Menthol, α-Terpineol, Geraniol Many alcohols are present in essential oils As an antiseptic, antibacterial, antibiotic, and tonic, it is very good for the nervous system and stimulates the immune response in the body
- Esters: The esters evaporate quickly and create a fragrance for the fragrance
Some esters present in essential oils: ethyl anthranilate, benzyl, acetate, etc Esters have antibacterial and anti-inflammatory properties
- Aldehydes: There are many aldehydes in essential oils, but now all aldehydes are obtained through chemical synthesis Only aldehydes such as cuminic, citral, and citronellal aldehydes have been extracted from natural materials Aldehydes are anti- inflammatory, with properties similar to alcohols However, high amounts of aldehydes can cause major skin irritation
Other compounds: In addition to the compounds mentioned above, in essential oils, there are compounds of the oxide group such as (eucalyptus) and amino acids (anthranilic acid), lactones (coumarin, ambrette), compounds with such as (anlylisosulfocyannat), nitrogenous compounds (methyl anthranilate)
2.2.4 The role of essential oils in plants
The issue of the role of essential oils in the life of plants has been addressed in many studies According to the concept presented in different works, the role of essential oils is concentrated in the following contents (Ph X Tanaxienco, 1985): Protecting plants from the effects of pests and diseases, covering wounds in trees prevent fungal diseases, changing the surface tension of water in plants, promote water transport, increase the efficiency of enzymatic reactions.
The orange essential oil
Orange essential oil is an essential oil produced by the cells inside the peel of an orange (Citrus sinensis fruit) Orange essential oil is a liquid, pale yellow, with a slight aroma of fresh orange, insoluble in water It is one of the most widely used essential oils in the world
2.3.1 The physical and chemical properties of orange essential oil a The physical properties of orange essential oil
Orange essential oil on the market is light yellow in color, with a slight aroma of fresh oranges
Table 2.1: Physical parameters of orange peel essential oil
Polar rotation angle 94 - 99 b The chemical properties of orange essential oil
Table 2.2: The chemical composition of orange tree
2.3.2 The role and application of orange essential oil a The role of orange essential oil
Essential oils help remove dead skin cells, keep and make skin smooth, soft and help prevent acne Essential oils help treat colds, headaches, joint diseases, treat liver and kidney problems, insomnia, detoxify the body, relax, reduce stress Essential oils create a gentle fragrance, and are completely pure for the space Essential oils are also used in the manufacture of medicines
In addition, essential oils are now used by many people to replace conventional cosmetics, because of their safety in use and almost no side effects b Applications of orange essential oil
In food technology: Essential oils play an important role in the production of confectionery and beverages Although used in extremely small amounts and in different forms, essential oils have contributed to flavoring foods and beverages, making them more appealing Recently, thanks to its superior antimicrobial activity and antioxidant capacity, in the food industry, there has also been a trend to use essential oils as a natural and safe food preservative instead of essential oils synthetic preservatives
In medicine: Essential oils are the most used pharmaceuticals in traditional medicine Each essential oil has a different chemical composition and main components, so the therapeutic activities are also different, some of which act on the central nervous system, some that stimulate digestive juices, gastric juices, and gastric juices intestines and bile Therefore, they are prepared into medicines to treat respiratory, circulatory, and digestive diseases, to treat abdominal pain, vomiting, to massage painful areas, to relieve fatigue, and to stimulate muscle activity
In the cosmetic manufacturing industry: Today, the cosmetic industry has
13 developed very strongly, essential oils are not only used directly in high-class spas, but they are also the main source of raw materials for the production of products such as Perfume, toothpaste, scented soap, shampoo, lotions, lipstick
Essential oil extraction methods
There are many methods for extracting essential oils, but regardless of the extraction method used, the production process has the following common points:
- The obtained essential oil must have the same natural aroma as the raw material
- The extraction process must be suitable for the characteristics of the raw materials
- Essential oils must be thoroughly extracted from raw materials at the lowest cost
Essential oil extraction methods are based on the following properties of essential oils:
- Attracted to steam at temperatures below 100 o C
- Easily soluble in organic solvents
- Easily absorbed in the gaseous state
Here, we go to learn about some commonly used methods to extract essential oils from plants
2.4.1 Extraction method a The basis of the method:
Based on the phenomenon of osmosis, diffusion, and dissolution of essential oils present in the raw tissues when exposed to organic solvents The extraction method is often used to separate volatile flavorings for which distillation has proven to be less
In this method, the raw materials are soaked in a suitable organic solvent, then vacuum distilled to recover the solvent, the rest is a mixture of essential oils and waxes called essential oils (called “concrete oil”) Use absolute alcohol to dissolve the
"concrete oil" and then let it cool, then the wax will solidify and be separated, the remaining liquid is steam-distilled to obtain pure essential oil (called "absolute oil")
These are also the two main product forms of aromatic substances currently circulating on the market b The factors affecting the method:
The most important factor for the success of this method is the quality and character of the solvent used, so the extraction solvent should meet the following requirements:
- Dissolve completely and quickly the aromatic components in the raw materials
- Poor solubility of other compounds such as wax, oleoresin present in raw materials
- No chemical effect with essential oils
- Do not degrade when reused many times
- Completely pure, without strange odors, non-toxic, non-corrosive to equipment, does not form explosive mixtures with air, and has poor viscosity
The boiling point is low because when distilling the extraction solution to recover the solvent, the high boiling point will affect the quality of the essential oil The boiling point of the solvent should be lower than the boiling point of the most volatile component in the essential oil In addition, there should be other additional factors such as low cost, easy-to-find supplies,
Usually, there is no solvent that satisfies all of the above conditions People use both water-insoluble solvents (such as Diethyl ether, Petroleum ether, Hexane, Chloroform ) and water-soluble solvents (such as Ethanol, Acetone ) In some specific cases, a solvent mixture is also used
This method is applicable to medicinal herbs with high essential oil content and essential oil-containing cells in the shell Extracted materials are extracted essential oils by pressing at normal temperature using endless screw presses or wedge presses The resulting part is a mixture of essential oils and pulp that can be easily separated by adding saturated brine, the essential oil will float to the top with some wax and resin involved
Use 75-80 o ethanol to dissolve the essential oil, then cool to remove the wax After evaporating under low pressure to remove the ethanol, we have an essential oil product with some resin mixed in This method can give over 90% efficiency compared to the quantified essential oil content in the laboratory
The basis of this method is based on the adsorption of aromatics by refined liquid or solid fats (vaseline, paraffin, olive oil, or tallow) People use trays 8cm deep, 60cm wide, 100cm long, the bottom is glass covered with fat to absorb aromatics The trays can be stacked on top of each other, on the surface of the tray, the ingredients are evenly arranged to extract the incense and leave it for about 12 - 72 hours depending on the type of ingredient, then change the layer of new ingredients and let them absorb 10-15 times Finally, aromatic fat is obtained Shake the fat with high ethanol to extract the essential oil, then cool to -1000C to remove all the fat that is dragged along, and then evaporate the ethanol under low pressure to collect the essential oil This technique is
16 often used to extract the fragrance of flowers to obtain the product as a concentrated essential oil (“essence concentrate”) used in cosmetics
This method is based on the absorption of aromatics by fatty oils Raw materials are soaked in refined fatty oil in a device heated by steam at 45-600 o C for 1-2 hours
After each soak, take out the flowers and put them in a centrifuge to recover the oil and add new ingredients Each batch of solvent can be used to extract 10-15 times The aromatic saturated fatty oil is shaken with ethanol and then concentrated under low pressure to obtain a concentrated essential oil similar to that in the marinating method
2.4.5 Hydrodistillation method a The principle of method
This was the first method used to separate essential oils from plant materials The basis of this method is that the boiling point of the mixture will be lower than the boiling point of the components Therefore, when hydro distillation, the essential oil components will be separated at a temperature lower than the boiling point of water, thus limiting the chemical denaturation of the components in the essential oil (oxidation, pyrolysis )
During the distillation process, the steam will be penetrated into the raw tissues, then it will dissolve, diffuse and attract the organic compounds in the essential oil The distillate will meet cold at the condenser tube and be condensed and separated into 2 layers (the oil layer above and the water layer below) in the condenser system Diffusion will be easy when the cell containing the essential oil swells because the material is exposed to saturated steam for a certain time
In the case of plant tissues with non-volatile compounds (such as waxes, resins,
17 long-chain fatty acids), distillation must be carried out over a long period of time, as these compounds reduce the overall vapor pressure of the system and make diffusion more difficult
Figure 2.2: Hydrodistillation equipment b The main factors affecting distillation efficiency
State of raw materials: Extraction of essential oils by steam distillation method with ground materials gives much higher essential oil content than unground raw materials When grinding, the cells containing the essential oil are broken, the water easily penetrates into the oil bags, the essential oil easily escapes to the outside environment and the steam is responsible for drawing that essential oil out to the receiver In addition, the essential oil grinding materials obtained are transparent, colorless, and have a more natural smell than the non-ground essential oil materials, which are yellow due to prolonged heat exposure and the odor is no longer natural
Time: The longer the distillation duration, the more essential oil is obtained
However, at some point, the amount of essential oil obtained does not increase over
18 time On the other hand, prolonging the distillation duration will affect the quality of the essential oil
Temperature: High heat will decompose essential oils Therefore, when it is necessary to use superheated steam (above 1000C), it should be done in the final stage of distillation, after the volatile components have been absorbed In fact, most essential oils are less stable under heat, so the problem is to take the time to withstand high temperatures as short as possible because burning raw materials lose the natural aroma of the essential oils
Amount of water: If the amount of water is too much, some of the polar essential oil components will dissolve into the water If the amount of water is too small, it is not enough to dissolve the colloids and salts surrounding the essential oil bag c Advantages and disadvantages of the distillation method
Advantages: The technical process is relatively simple Compact equipment, easy to manufacture During distillation, it is possible to separate the components in the mixture by condensing each part over time Does not require auxiliary materials such as impregnation and absorption methods Relatively fast time Distillation can be carried out with essential oil components that can withstand high temperatures Able to thoroughly separate essential oils in raw materials
METHOD
Material
- Sanh orange peel from Ham Yen, Tuyen Quang.
Chemicals used for research
Penetrates into the tissues of the raw material, dissolving, diffusing, and attracting the organic compounds in the essential oil
2 NaCl Increases the permeability of water in the cell, increasing the polarity of the solution.
Equipment and tools used for research
Table 3.2: Equipments and tools used for research
Distillation pot 2L Erlenmeyer flask (250ml)
Pear extraction funnel (250ml) Measuring cup, measuring tube
Filter Paper Pipet (1ml, 2ml, 5ml, 10ml) Along with other equipment and tools for research in the addiction laboratory of the Department of Biotechnology - Food Science
Scope, place, and time of the research
- Research on the extraction process of essential oils and develop products from orange essential oil from oranges purchased in Sanh orange Ham Yen, Tuyen Quang orchards
- Location: Laboratory of the Faculty of Biotechnology - Food Technology, Thai Nguyen University of Agriculture and Forestry
Research content
Experiment 1: Research on optimizing salt concentration in the essential oil extraction process
Experiment 2: Research on optimizing the ratio of water to raw materials in the process of extracting essential oils
Experiment 3: Research on optimizing the distillation duration of essential oils in the extraction process
Content 2: Analysis of the chemical composition of orange essential oil
Content 3: Develop and perfect the product prepared from essential oil
- Using pure essential oils and some additives to develop orange essential oil hand sanitizer product
Figure 3.1: Essential oil distillation equipment
Handle Reseach the ratio of raw material incubation water
Reseach the distillation duration Hydrodistillation
Reseach the concentration of NaCl, soaking time
The expected extraction process of orange essential oil by Hydrodistillation method 24 3.7 Experimental set-up method
Figure 3.2: Flowchart of the expected orange essential oil extraction process
Natri Sulfate (Na₂SO₄) Dehydrate
Essential oil Decant Crude oil Dissociation
From the diagram we give the basic steps in the distillation of essential oils as follows:
Step 1: Prepare materials: orange peel has been pretreated:
Take 10kg of oranges, wash them to remove dirt, bacteria and peel off the skin (1kg of oranges get 300g of peel)
After the shell has been cleaned, it is crushed and added with the amount of NaCl, the ratio of water / raw materials soaking time has been optimized
Step 2: Carry out distillation and collection of the essential oil mixture:
The shells after being crushed and added to the optimal conditions will be put into the distillation pot and conduct essential oil distillation
After the distillation of essential oils is finished, use an extractor to collect the extracted crude oil
Step 3: Processing after obtaining the amount of crude oil:
Use Na2SO4 to absorb all the water and impurities from the raw essential oil
Step 4: Decanting and collecting pure essential oil:
To settle the above mixture was obtained and filtered with filter paper to obtain the pure essential oil
Store essential oils in glass jars, tightly closed to avoid evaporation, exposure to direct light Store refrigerated at 0-5 o C
3.7.1 Experiment 1: Research on optimizing NaCl concentration in soaking water during extraction of orange essential oil
Research experiments to optimize different concentrations of NaCl to find the
26 right concentration of NaCl to obtain the most efficient volume of essential oil
According to references, NaCl has a good effect in the process of separating and extracting essential oils because NaCl has the effect of increasing the permeability of water in cells, increasing the polarity of the solution, thereby reducing the interaction force between the less polar essential oil constituents and water Therefore, the essential oil will be easily separated during the distillation process Investigating the concentration of added NaCl to help build a graph of the relationship between the concentration of orange peel essential oil extraction Therefore, we conducted this experiment to evaluate whether salt has a good effect on the extraction of orange peel essential oil
Step1: Take 200g of processed orange peel into the blender, add a quantity of distilled water with the ratio of water/material selected in these experiments: 5/1 Add NaCl to different concentrations: 0%, 1.5%, 3%, 4.5%, 5%, respectively
Step 2: Then, grind the ingredients for 1 minute
Step 3: Transfer all the blended ingredients into the distillation pot and distill the mixture for 60 minutes The mixture after heating will evaporate and pass through the condenser tube Here, the essential oil will condense when it is cold, then it will separate into 2 layers: the floating layer is the essential oil, the bottom layer is the water
Step 4: Read the volume of e-liquid separated on the marked condenser tube and then compare From there, choose the appropriate NaCl concentration
The above experiment was repeated 3 times The total number of experiments was 15 Experimental results after optimization were used for subsequent experiments
From there, choose the appropriate concentration of NaCl
Table 3.3: Expected results in the research on optimizing NaCl concentration in soaking water
Formula NaCl concentration (%) Obtained essential oil volume (ml)
3.7.2 Experiment 2: Research on optimizing the water/material ratio in the extraction process of orange essential oil
Water has the effect of penetrating into the raw tissues, then it will dissolve, diffuse and attract the organic compounds in the essential oil, creating conditions for the essential oil to escape more easily If the solvent volume is too small, the essential oil will not diffuse well into the solution, making the distillation duration longer and the longer the heat exposure time will turn yellow and the quality of the essential oil will decrease The percentage of water more or less affects the yield of essential oil
Experiment: Determine the amount of water added when soaking to evaluate the ability to separate essential oils in the raw materials, this is an important factor affecting the efficiency of the distillation process Therefore, determining the amount of water added also determines the optimal distillation duration of the product
This experiment is conducted with the amount of water/material changing in the following ratios: 3/1; 4/1; 5/1; 6/1; 7/1
Step 1: Take 200g of treated orange peel into the grinder, add a quantity of
28 distilled water, in which the ratio of water/material changes: 3/1, 4/1, 5/1, respectively
6/1, 7/1 (v/w) with appropriate NaCl content determined from previous experiments
Step 2: Crush for 1 minute to crush the sample, increase the contact area with the water environment to promote the diffusion of essential oils
Step 3: Transfer all the crushed ingredients into the distillation pot and distill the mixture for 60 minutes
Step 4: Read the volume of crude oil separated on the condenser tube (with volumetric markings) and compare the volume of essential oil obtained at different concentrations as above From there, choose the appropriate water/ingredient ratio
The above experiment was repeated 3 times The total number of experiments was 15 Experimental results after optimization were used for subsequent experiments
From there, choose the appropriate water/ingredient ratio
Table 3.4: Expected results in research on optimizing the water/material ratio
Formula Ratio of water/material Obtained essential oil volume (ml)
3.7.3 Experiment 3: Research on optimizing the distillation duration of orange essential oil
Distillation duration plays a role in determining the amount of essential oil obtained If distillation duration is too short, the extracted essential oil is not completely exhausted or it still exists in the secretory cells, thus reducing the volume of essential
29 oil obtained On the contrary, when distillation exceeds the optimal time, it is both times consuming, energy-consuming and more seriously, the quality of the obtained essential oil is also significantly reduced Therefore, we conduct this experiment, to determine the appropriate distillation duration
After determining the concentration of the optimal parameters: NaCl concentration and ratio of water/material We continue to conduct the experimental batch to determine the distillation duration
Experimental distillation of raw materials with variable time intervals from 30 minutes, 60 minutes, 90 minutes, from 120 minutes, 150 minutes, etc The distillation duration starts from when the first drop of essential oil drops into the extraction flask
Attention should be paid to regular monitoring and recording every 15 minutes until the volume of crude oil obtained on the extraction flask can no longer increase At that time, proceed to stop the distillation process and record the volume of essential oil along with the time of distillation at the time when the oil can no longer increase
The above experiment was repeated 3 times The total number of experiments was 15 Experimental results after optimization were used for subsequent experiments
From that choose the appropriate distillation duration
Table 3.5: Expected results in the research on optimizing the distillation duration
Formula Distillation duration (mins) Obtained essential oil volume (ml)
The results of each of the above experiments are the average of 3 parallel determinations
Data processing using MS Excel 2016 software
Draw graphs using Excel 2016 software
3.7.5 Analysis of components in orange peel essential oil by GC-MS method
Detecting the presence of components in orange peel essential oil at the laboratory of Institute of Life Sciences - Thai Nguyen University on gas chromatography-mass spectrometry The identification of components in essential oils is done by using the pre-installed software on the machine to compare the full-MS and MS/MS spectra of each component separated on the chromatogram with the standard spectra available in the spectrum library
The chemical composition of orange essential oil was determined by Gas chromatography-mass spectrometry GC/MS
3.7.6 Research, develop and perfect some products from orange essential oil
Using pure essential oils to develop antiseptic hand sanitizer products formulated with pure essential oils: Antiseptic hand sanitizer products are formulated with ingredients regulated by the Ministry of Health and recommended WHO ingredients for the ingredients in hand sanitizers
Use pure essential oils to develop disinfectant sprays formulated with pure essential oils:
- Disinfectant spray products are formulated with ingredients specified by the Ministry of Health and WHO recommendations for ingredients in disinfectant spray solutions
- The product is packed with the packaging design, label, and content according to the national standard on cosmetic products and stated on the label as a test product
RESULTS
Research on factors affecting the extraction process of essential oils and perfecting the
4.1.1 Research results on optimizing NaCl concentration in soaking water during extraction of orange essential oil
To study the effect of NaCl concentration on the content of essential oil extracted from orange essential oil After referring to other studies, we grinded the raw materials for 1 minute and added NaCl with different concentrations and then distilled the essential oil After distillation is completed, measure the volume of essential oil, the results obtained are shown in Table 4.1
Table 4.1: Effect of NaCl concentration in soaking water on the volume of essential oil obtained
Formula NaCl concentration (%) Obtained essential oil volume (ml)
("-" sign means that no essential oil can be obtained and will be explained below)
Figure 4.1: The volume of essential oil obtained at different concentrations of NaCl
From the result table 4.1, we see that, when increasing the concentration of NaCl to 4%, the highest amount of essential oil (4ml) is obtained And when continuing to increase the concentration of NaCl to 6%, 8%, no essential oil is obtained
From the result table 4.1, we have the following chart:
Figure 4.2: Graph of the volume of essential oil obtained at different concentrations of NaCl
The volume of essential oil obtained (ml)
But when continuing to increase the concentration of NaCl to 6% and 8%
Because we initially used a small distillation flask (2-liter capacity), at the same time, during the preliminary processing of the ingredients, there was a mixture of citric acid, so increasing the concentration of NaCl will affect the boiling point of the distillation flask, and material being pushed up the distillation pipeline leads to no essential oil being obtained
Therefore, we chose the formula of NaCl concentration 4% as the point to obtain the best volume of essential oil and used this result for the next experiments
4.1.2 Research results on optimizing the ratio of water/material in the extraction process of orange essential oil
To study the effect of water/material ratio on extracted essential oil content, we grind the raw materials for 1 min and add 4% NaCl was determined in the previous experiment We then add different proportions of water to the fixed raw material and then proceed to distill the essential oil The results obtained are shown in table 4.2
Table 4.2: Effect of water/material ratio on the volume of obtained essential oil
Formula Ratio of water/material Obtained essential oil volume (ml)
Figure 4.3: The volume of essential oil obtained at different water/material ratio
From result table 4.2, we see that the ratio of water/material 4/1 obtained the largest volume of essential oil is 4.13ml Among formulas 1, 3, 4, the difference is not significant, respectively 3.8ml, 3.53ml, 3.67ml But when it comes to formula 5 with a water ratio of 7/1, the amount of essential oil obtained is significantly reduced than 3.1ml
From the result table 4.2, we have the following chart:
Figure 4.4: Graph of the volume of essential oil obtained at different water/material ratio
The volume of essential oil obtained (ml)
Based on the chart above, we can see that the volume of essential oil obtained increases as the ratio of water / ingredients increases and reaches the largest volume at the ratio of water / ingredients is 4/1 The volume of essential oil obtained will decrease as the water/material ratio continues to increase Because when increasing the amount of water, the ingredients remain the same, the boiling time is longer, leading to a decrease in the amount of essential oil obtained in the same time between recipes
Therefore, we chose the formula of water-to-material ratio 4/1 as the point to obtain the best volume of essential oil and used this result for the next experiments
4.1.3 Research results on optimizing the distillation duration of orange essential oil
After studying the appropriate concentration of NaCl for distillation of orange essential oil is 4%, the ratio of water/material is 4/1 We investigated the effect of distillation duration on the yield of essential oil Process raw materials with optimal conditions and conduct essential oil distillation with defined time conditions for essential oil distillation The obtained results are shown in Table 4.3
Table 4.3: Effect of distillation duration on the volume of essential oil obtained
Formula Essential oil distillation duration
Figure 4.5: The volume of essential oil obtained at different distillation duration
From Table 4.3, the results show that the amount of orange essential oil obtained increased rapidly in the first 45 minutes to 3.73ml After that, the amount of essential oil obtained increased slowly and reached a maximum when distilling for 60 minutes was 4.17ml and when distilling up to 75 minutes, no more essential oil was obtained
From the result table 4.3 we have the following chart:
Figure 4.6: Graph of the volume of essential oil obtained at different distillation duration
Essential oil distillation duration (minutes) The volume of essential oil obtained (ml)
Based on the chart above, we can see that initially, the amount of raw materials is large, the essential oil is high, the diffusion and evaporation speed is high, so the amount of essential oil obtained increases rapidly From the 60th minute to the 75th minute onwards, the amount of essential oil in the raw materials is exhausted, so the amount of essential oil obtained will be reduced
Therefore, in the study period from 15 minutes to 75 minutes, we chose the 60- minute formula as the point to obtain the best volume of essential oil and use this result for the next experiments
Complete the process of extracting essential oils from Sanh orange peels
From the research results that have been optimized, we have completed the extraction process of orange peel essential oil shown in figure 3.2 as follows:
Water/material (v/w): 4/1 Grinding time: 1 minute
Figure 4.7: Complete orange essential oil extraction process
Explain the process of distilling orange essential oil:
Step 1: Prepare and preliminary process materials:
The raw material used for the distillation process is Sanh orange peel The orange peel will be preliminarily processed and washed A batch of essential oil distillation requires about 200g of raw material
When purchasing oranges, it is necessary to remove crushed and rotten fruits to avoid reducing the use-value of orange peels and reducing the effectiveness of the obtained essential oil
When washing the shell, it is necessary to wash and remove the stains and impurities on the shell (wear gloves and masks when preliminary processing to ensure the safety of samples and workers to avoid contamination)
Peel off the flesh of the fruit and remove only the rind
After being preliminarily processed, the orange peel is ground with water so that the ratio of water/material is 4/1 (v/w) Blend ingredients for 1 minute
Since the essential oils in plants are usually located in the tissues of the plant, the grinding of the material is intended to release the essential oils from the tissues Since then, when conducting distillation, the essential oil is easy to escape, helping to shorten the distillation process time to achieve high efficiency If we grind the materials smaller, the efficiency of breaking down the cell tissue is higher, but it is easy to clog the steam pipe (essential oil + water) and the small porosity also affects the distillation process
Therefore, it is necessary to grind the material to the right size to achieve the highest efficiency
After being crushed, the orange peel material will be soaked in a solution of NaCl (4%) The purpose of this stage is to make the essential oil penetrate from the bag to the outside, making the distillation process more thorough
Raw materials after being soaked will be put into the distillation device So that the material is on the support plate, separated from the bottom layer of the distillation flask The material contained in the device does not exceed 85% of the device capacity, avoiding the phenomenon of foaming and overflowing to the cooling pipe Do not put the ingredients too tightly as this will make it difficult for the steam to evenly distribute all the materials The material should also not be too liquid, too porous because that will make it easier for the vapors to follow the voids out without contacting the whole material When the ingredients are put into the distillation flask, it is necessary to close the lid of the pot tightly to avoid evaporation and loss of essential oils during the distillation process Then install and turn on the cooling system
Conduct distillation and collection of essential oils:
At the beginning of the oil distillation process, we can apply a large amount of heat to boil the distilled water After about 10 minutes, the distillation flask starts to boil, and then the steam wraps the essential oil out to the cooling tube and out to the extraction vessel, we get a mixture of water and essential oil Essential oils lighter than water will float to the top of the water the first 60 minutes of heating is the time when the oil comes out the most Then lower the temperature, maintain the pot at a sufficient boiling temperature because when at high temperature, the essential oil will easily decompose
Therefore, it is necessary to monitor the distillation flask temperature meter and
42 maintain it at 95-100 o C During the distillation process, care should be taken to adjust the condensate temperature so that it is in the range of 30-40 o C (by adjusting the cooling water rate) Because if the condensate is too hot, it will increase the solubility of the essential oil in the water and evaporate the essential oil To check if the distillation process is finished or not, we can use a glass plate to catch some condensate, if there is still oil on the glass, the distillation process is not finished
After the distillation is complete, close the valve providing cooling water, turn off the stove, let it cool for 15-30 minutes, open the lid and remove the residue, then clean the equipment with clean water before continuing to refill the new batch
The mixture of steam and essential oil is released into the condenser tube of the distillation device Under the effect of water in the condenser tube with low temperature, it will convert the above mixture from a vapor to a liquid form and then flow into the condenser of the device
Leave the resulting mixture in the condenser until completely separate into two phases: the essential oil lighter than water will be at the top, the water will be at the bottom Open the drain valve on the extractor to let the essential oil flow into the receiver to collect the crude oil
Dehydrate with excess anhydrous Na2S04 because it has the feature of absorbing water Add excess anhydrous Na2S04 to the raw essential oil container, add and shake well until crystals of Na2S04 salt are observed starting to separate
Step 8: Decant - Collect essential oils:
To decant the above mixture Allow the above essential oil (which has been anhydrous with Na2SO4) to flow through a glass funnel lined with a layer of filter paper, pour it slowly through the funnel, avoiding the spillage of essential oils, there is a glass jar below to store essential oils
Preservation: Essential oils that have been removed from the water are kept in glass jars, tightly closed to avoid evaporation, and avoid direct exposure to light and air
Results of determining the chemical composition of orange essential oil
The chemical composition of orange essential oil was determined by gas chromatography-mass spectrometry GC/MS The results of the analysis of the essential oil samples are shown in the figure below:
Table 4.4: Results of GC/MS analysis of Ham Yen orange peel essential oil
4.4 Research develop and complete product from orange essential oil
Orange essential oil hand sanitizer:
The ingredients used in the product meet the national standards for the quality of cosmetic products and the ingredients on the packaging have been identified and tested
44 based on the database of the Ministry of Health
The ingredients to prepare the product referenced and developed from WHO (as shown in table 4.5)
Table 4.5: Substances composition in orange essential oil hand sanitizer
Uses of components in the hand sannitizer from orange essential oil:
- Ethyl hydroxy peroxide (H202): kill bacteria - Essential oils: create the scent, kill bacteria - Glycerol: moisturize the skin
Figure 4.8: Oragne essential oil hand sanitizer
The product is transparents, without color or sediment, and has a distinctive orange essential oil aroma When used, it is not viscous and does not create pain
- Helps to clean the air / surrounding environment, kill bacteria, antibacterial, eliminate odors
- The product is colorless, clear, without sediment, has a characteristic scent of orange oil, is not harmful to the respiratory tract, and protects the environment
- The product has been tested according to the standards of the Ministry of Health, the standards of WHO
Compared with similar products on the market, their effects are similar, but the ratio of ingredients in the solution and scent in the product is not the same.
CONCLUSIONS AND DISCUSSION
Conclusions
From the above studies, I built the process of distilling essential oils by steam distillation with the following optimal ratios:
- The ratio of water/material is 4/1 (v/w)
- The distillation duration is 60 minutes
And the product obtained is orange peel essential oil with some properties such as: transparent, yellow, with a strong aroma of orange peel essential oil
After that, we developed product lines from orange essential oil: pure essential oil used as an essential oil, hand sanitizer and disinfectant spay.
Discussion
Due to the limited research time, there are still many unfinished works, so in the coming time we will continue to study the remaining works:
- Research on extracting the first extract from the remaining parts of the orange tree such as leaves, fruits,
- Conduct surveys on the quality of input materials
- Continue to develop and innovate products from orange essential oil
- Continue to study the extraction of orange peel essential oil on an industrial scale
Le Thi Anh Dao, Dr Dang Van Lieu (2007) Thực hành hóa hữu cơ Pedagogical
Le Van Dang (2005) Chuyên đề một số hợp chất tự nhiên Ho Chi Minh City National University Publishing House
Le Pham Tan Quoc, Vo Ai My, Trinh Thi Minh Nguyet (2014) Nghiên cứu tách chiết tinh dầu từ vỏ cam sành (Citrus sinensis (l) osbeck)
Le Ngoc Thach (2003) Tinh dầu Ho Chi Minh City National University Publishing
Nguyen Dac Phat (2010) Nghiên cứu chiết xuất tinh dầu từ vỏ bưởi Năm Roi (Citrus grandis ( L ) Osbeck var grandis) bằng phương pháp chưng cất lôi cuốn hơi nước
Faculty of Processing, Nha Trang University
Nguyen Thi My Dung (2001) Nghiên cứu tách chiết và ứng dụng dịch chiết vỏ quả cam, quýt ở Quảng Nam làm chất ức chế ăn mòn kim loại
Nguyen Van Minh (2011) Các phương pháp sản xuất tinh dầu Electronic newspaper - Oil and Oilseed Research Institute - Science and Technology Newsletter
Pham Thi My Lan (2012) Nghiên Cứu Chiết Xuất Tinh Dầu Từ Vỏ Quả Quất Băng Phương Pháp Chưng Cất Lôi Hơi Nước
Vuong Ngoc Chinh (2005) Hương liệu mỹ phẩm Ho Chi Minh City National
Tran Xuan Ngach (2007) Bài giảng môn học nguyên liệu sản xuất thực phẩm
University of Danang, University of Science and Technology - Faculty of Chemical Engineering
Nguyen Van Ninh (2003) Nghiên cứu chiết rút tinh dầu từ một số loại quả Faculty of Processing, Nha Trang University
Baker , R.T and Smith , H.G (1912) A Research On The Eucalypts Of Tasmania And
Horst Surburg and Johannes Panten (2006) Common fragrance and flavor matterials
Thavanapong, N (2006) The essential oil from peel and flower or Citrus Maxima
Master Thesis, Dept Pharmacology, Silpakorn University Ahmad, M.M., Salim-ur-rehman, Anjum, F.M., Bajwa, E.E (2006) Comparative physical examination of various Citrus pell essential oil Int J Agri Biol., Vol 8, No
Atti Santos, A C., Serafini, L A., Moyna, P., (2005) Extraction of Essential Oils from
Lime (Citrus latifolia Tanaka) by Hydrodistillation and Supercritical Carbon Di- oxide
Brazilian Archives of Biology and Technology, Vol.48 (1), p 155-160
CRC (1981-1982) Handbook of Chemistry and Physics 62 nd edition
Dharmawan, J.,(2008) Characterization of Volatile Compounds in selected Citrus
Fruits from Asia Doctor Thesis, Dept Chemistry, NUS, Singapore
Sun, J., (2007) D-Limonene: Safety and Clinical Applications Alt Med Review, Volume 12, No.3, p.259-264
Merk & Co Inc Rahway (1989) The Merk Index Vol 1,2 – N.J.U.S.A
Ph D-D Van Nostrand Company (2008) The Essential Oil Vol 1, 2, 3 Ernest Guenther
Appendix 1: Some table of data of the research experiments to optimize the conditions in the extraction of essential oils
Table of appendix 1: The volume of essential oil was obtained at different NaCl concentration ratios
Obtained essential oil volume (ml)
Error 1 st 2 nd 3 rd Average
("-" sign means that no essential oil can be obtained)
Table of appendix 2: The volume of essential oil was obtained at different water/material ratios
Formula Ratio of water/material
Obtained essential oil volume (ml)
Error 1 st 2 nd 3 rd Average
Table of appendix 3: The volume of essential oil was obtained at different distillation ratios
Obtained essential oil volume (ml)
Erorr 1 st 2 nd 3 rd Average
Appendix 2: Some pictures during the extraction of orange essential oil
Figure of appendix 1: Sanh orange used in the study
Figure of appendix 2: Oranges were peeled and ground
Figure of appendix 3: Put the ingredients into the device and then proceed to distillation