Galangal essential oil and preparation method thereof
Through multi-stage temperature-controlled extraction, electrostatic adsorption purification and hierarchical condensation processes, combined with the combination of natural antioxidants and functional essential oils, the problems of insufficient purity and stability in the preparation of galangal essential oil are solved, and efficient extraction and antioxidant properties are achieved. Improved, suitable for a wide range of skin care and healthcare applications.
Patent Information
- Application Number
- CN202411496003.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2024-12-31
AI Technical Summary
In the existing preparation methods for galangal essential oil, distillation method leads to degradation of heat-sensitive components, and ethanol extraction method cannot effectively separate polar and non-polar components, resulting in insufficient purity of essential oils and residual impurities, affecting its stability and service life.
Multi-stage temperature-controlled extraction, electrostatic adsorption purification and staging condensation processes are adopted, combining natural antioxidants and functional essential oils to improve extraction efficiency and purity and enhance antioxidant performance.
It significantly improves the extraction efficiency and purity of galangal essential oil, avoids the degradation of heat-sensitive ingredients, extends the stability and service life of the product, enhances the antioxidant capacity, and is suitable for a variety of skin care and healthcare applications.
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Figure CN119220347A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of essential oil extraction and preparation, in particular to galangal essential oil and a preparation method thereof. Background Art
[0002] Galangal is a common Chinese medicinal material. Its rhizome is rich in a variety of bioactive ingredients and has a variety of pharmacological effects such as antibacterial, anti-inflammatory, and antioxidant. Galangal essential oil is an important ingredient extracted from the rhizome of Galangal and is widely used in medicines, skin care products, and health care products.
[0003] Existing methods for preparing galangal essential oil mainly include distillation extraction and ethanol extraction. The distillation extraction method evaporates the volatile components in galangal by heating and then collects them by condensation. The process is simple, but it is easy to cause the loss of heat-sensitive components. The ethanol extraction method uses ethanol as a solvent to dissolve the active ingredients in galangal and then remove the solvent by distillation to obtain essential oil. The extraction efficiency is relatively high.
[0004] The existing preparation methods of galangal essential oil have the following shortcomings: the distillation method, due to high temperature treatment, is prone to degradation of some heat-sensitive components, affecting the activity of the essential oil; although the ethanol extraction method can improve the extraction efficiency, the extraction process cannot effectively separate polar and non-polar components, resulting in more impurities in the essential oil and insufficient purity. In addition, the extraction process lacks optimization of antioxidant capacity, which makes the essential oil product prone to oxidation during storage, reducing its stability and service life. Summary of the invention
[0005] In view of the deficiencies in the prior art, the present invention provides an essential oil of galangal and a preparation method thereof. The present invention improves the extraction efficiency and purity of the essential oil of galangal through processes such as multi-stage temperature-controlled extraction, electrostatic adsorption purification and graded condensation, and avoids the degradation of heat-sensitive components. At the same time, natural antioxidants and functional essential oils are added to enhance the antioxidant properties of the essential oil, extend the stability and service life of the product, and effectively solve the problems of residual impurities and oxidation in the prior art.
[0006] To achieve the above objectives, the present invention is implemented by the following technical scheme: a galangal essential oil and a preparation method thereof, comprising the following steps:
[0007] Raw material pretreatment: the rhizomes of galangal were cut, low-temperature pretreated and treated with enzymes;
[0008] Staged temperature-controlled extraction and fractional condensation: ethanol and distilled water are used in turn for staged extraction at different temperatures, and then fractional condensation is used to collect components with different volatility;
[0009] Essential oil purification: Use electrostatic adsorption purification to remove impurities and further purify with natural organic solvents;
[0010] Adding functional materials: adding natural antioxidants and other essential oil ingredients to essential oils for compounding;
[0011] Mix well: Mix the galangal essential oil and other components evenly and let it stand.
[0012] Preferably, the raw material pretreatment includes:
[0013] Low temperature pretreatment: Cut the rhizomes of galangal into small pieces of 1 to 2 cm and precool them at 4°C for 12 to 24 hours;
[0014] Enzyme treatment: first use 0.2% to 0.5% cellulase at 45°C and pH 5.0 for 1 to 2 hours, then use 0.1% to 0.3% pectinase at 50°C and pH 4.5 for 1 hour.
[0015] Preferably, the staged temperature-controlled extraction includes:
[0016] The first stage of extraction is carried out at 70-80°C for 1-2 hours to extract the volatile components;
[0017] The second stage of extraction is carried out at 90-100°C for 1.5-2.5 hours to extract the non-volatile components;
[0018] The extracted distillation product was condensed by a graded condensation system, and the condensation temperatures were set at 30°C, 20°C and 10°C, respectively, to collect different volatile components.
[0019] Preferably, the essential oil purification comprises:
[0020] Using electrostatic adsorption purification method, the essential oil is brought into contact with the charged fiber material to adsorb and remove polar impurities, and the static time is 1 to 2 hours;
[0021] The purified essential oil is mixed with a natural organic solvent, the temperature is controlled at 40-50°C, and the treatment time is 1-3 hours.
[0022] Preferably, the ethanol and distilled water are extracted in stages at different temperatures, comprising:
[0023] Use 70% to 90% ethanol solution to perform ethanol extraction at 60°C for 2 to 3 hours;
[0024] The extraction was performed using distilled water at 90°C for 3 to 4 hours.
[0025] Preferably, the added functional material comprises:
[0026] Natural antioxidant;
[0027] Lavender essential oil;
[0028] Frankincense essential oil;
[0029] Tea tree essential oil;
[0030] Panthenol;
[0031] Caprylic / capric triglyceride.
[0032] Preferably, the low temperature pretreatment further comprises:
[0033] During the soaking period, stir once every hour for 2 minutes;
[0034] The speed is controlled at 50-100 rpm.
[0035] Preferably, the electrostatic adsorption purification method comprises:
[0036] The extract is concentrated by using a rotary evaporator, the concentration temperature is controlled at 40-50°C, and the ethanol is evaporated under reduced pressure to obtain a concentrated galangal extract;
[0037] The concentrated extract is cooled and then subjected to water extraction to improve the extraction efficiency of polar components.
[0038] Preferably, the uniform mixing includes:
[0039] Adding a proper amount of emulsifier to the mixed essential oils, wherein the emulsifier is lecithin or xanthan gum from plant sources, and the added amount is 0.2% to 0.5% of the total weight;
[0040] By high-speed stirring, 1000-1500 rpm, for 5-10 minutes, emulsification is performed to make the components of the essential oil more stable and evenly distributed.
[0041] The present invention also provides an galangal essential oil, which comprises the following components in parts by weight:
[0042] Galangal essential oil 1-5%;
[0043] Lavender essential oil 0.5-2%;
[0044] Frankincense essential oil 0.5-2%;
[0045] Natural antioxidants 0.05-0.3%;
[0046] Tea tree essential oil 0.5-1%;
[0047] Panthenol 0.1-1%;
[0048] Base oil 90-98%;
[0049] Caprylic / capric triglyceride 1-5%.
[0050] The present invention provides an galangal essential oil and a preparation method thereof, which has the following beneficial effects:
[0051] 1. The present invention effectively improves the extraction efficiency and purity of galangal essential oil by combining multi-stage temperature-controlled extraction with electrostatic adsorption purification and graded condensation. The process can extract a variety of effective ingredients to the greatest extent while removing impurities, ensuring the integrity and high concentration of active ingredients in the essential oil, and improving the quality and stability of the product.
[0052] 2. The present invention enhances the antioxidant capacity of essential oils by adopting a composite formula of natural antioxidants and functional essential oils. The essential oils have free radical scavenging and reducing capabilities, thereby extending the shelf life of the product and improving its application value in skin care and medical care.
[0053] 3. The present invention greatly enhances the dispersibility and stability of essential oils through emulsification technology and uniform mixing of functional materials, ensures the uniform distribution of its components, improves the skin feel and absorption efficiency of the product, is suitable for a variety of skin care scenarios, and has broad market application prospects. BRIEF DESCRIPTION OF THE DRAWINGS
[0054] Figure 1 It is a preparation flow chart of the present invention. DETAILED DESCRIPTION
[0055] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0056] Please refer to the attached Figure 1 The embodiment of the present invention provides an essential oil of galangal and a preparation method thereof, comprising the following steps:
[0057] Raw material pretreatment: The rhizomes of galangal are cut, low-temperature pretreated and treated with enzymes. First, the freshly harvested rhizomes of galangal are washed to remove surface dirt and impurities. The purpose of cutting is to increase the contact area between the raw material and the enzyme and promote the effect of subsequent pretreatment and extraction. The cut galangal pieces are placed in a low-temperature environment of 4°C for precooling. The pretreated galangal is further treated with enzymes to destroy the plant cell walls and release the active ingredients. Through enzyme treatment, the cell walls and intercellular matrix are effectively decomposed, which greatly increases the extractability of the internal components of the galangal cells.
[0058] Staged temperature-controlled extraction and graded condensation: ethanol and distilled water are used for staged extraction at different temperatures, and then graded condensation is used to collect components with different volatilities. The staged temperature-controlled extraction combined with graded condensation technology can accurately collect different effective components in galangal according to the volatilization temperature of different components. By controlling the extraction temperature, heat-sensitive components can be protected and more effective substances that are difficult to volatilize can be extracted. Graded condensation ensures that different volatile components can be collected separately to avoid mutual interference, thereby improving the purity and accuracy of the essential oil;
[0059] Essential oil purification: Impurities are removed by electrostatic adsorption purification and further purified by natural organic solvents. Electrostatic adsorption is a physical purification method that can effectively remove polar impurities without losing the active ingredients in the essential oils. Combined with further purification by natural organic solvents, residual impurities that may affect the quality of the essential oils can be completely removed. This combined step can significantly improve the purity of the essential oils, giving the final product higher quality and a longer shelf life;
[0060] Adding functional materials: Adding natural antioxidants and other essential oil ingredients to essential oils for compounding. Compounding with other essential oils can increase the versatility of the product, making it not limited to a single efficacy, and further broaden the application range of the product;
[0061] Evenly mixed: After mixing the galangal essential oil with other components, let it stand. By stirring, the components in the essential oil can be evenly blended to avoid unevenness. By standing, the chemical balance between different essential oils and added materials can be ensured, so that the ingredients can play a more stable and efficient role in the product.
[0062] Please see attached Figure 1 In a preferred embodiment of the present invention, the raw material pretreatment includes:
[0063] Low temperature pretreatment: Cut the rhizomes of galangal into small pieces of 1 to 2 cm and precool them at 4°C for 12 to 24 hours. This cutting method helps increase the contact area between the enzyme and the galangal cells in the subsequent processing steps, thereby improving the reaction efficiency of the enzyme. This cutting method helps increase the contact area between the enzyme and the galangal cells in the subsequent processing steps, thereby improving the reaction efficiency of the enzyme.
[0064] Enzyme treatment: First, use 0.2% to 0.5% cellulase at 45°C and pH 5.0 for 1 to 2 hours, then use 0.1% to 0.3% pectinase at 50°C and pH 4.5 for 1 hour. Cellulase is mainly used to decompose cellulose in plant cell walls. Cellulose is an important component of plant cell walls and has strong structural properties. Under the conditions of 45°C and pH 5.0, cellulase can efficiently act on cellulose and decompose it into glucose or smaller oligosaccharides, thereby rupturing the cell wall. Pectinase can degrade pectin at 50°C and pH 4.5, decomposing it into small molecules, further destroying the intercellular matrix, thereby releasing more effective ingredients. Through the decomposition of cellulase, the plant cell wall is destroyed, which greatly increases the extractability of the effective ingredients in the cell, especially the volatile components of essential oils can be more easily released from the inside of the cell.
[0065] Please see attached Figure 1 In a preferred embodiment of the present invention, the staged temperature-controlled extraction comprises:
[0066] The first stage of extraction is carried out at 70-80°C for 1-2 hours to extract volatile components. The monoterpenoid compounds and some aromatic substances in galangal have a low boiling point. Therefore, under the temperature control condition of 70-80°C, these components can be fully volatilized, which can ensure that these components are not destroyed during the extraction process and maintain their activity and purity.
[0067] The second stage of extraction is carried out at 90-100°C for 1.5-2.5 hours to extract the less volatile components. Sesquiterpenoids and other less volatile components can usually be effectively volatilized at higher temperatures. Through the high temperature environment of 90-100°C, these more stable and beneficial components can be completely extracted and collected at an appropriate condensation temperature, thereby ensuring that different types of components in galangal can be fully extracted and the extraction efficiency is maximized.
[0068] The extracted distillation product is condensed by a graded condensation system, and the condensation temperatures are set at 30°C, 20°C and 10°C, respectively, to collect different volatile components, among which 30°C is suitable for collecting low-boiling monoterpenes, 20°C is used for medium-volatile substances, and 10°C is suitable for less volatile sesquiterpenes. The graded condensation system can effectively classify and collect volatile components to avoid the problem of reduced purity caused by mixing of different volatile components.
[0069] Please see attached Figure 1 In a preferred embodiment of the present invention, essential oil purification comprises:
[0070] Using the electrostatic adsorption purification method, the essential oil is brought into contact with the charged fiber material to adsorb and remove polar impurities, and the standing time is 1 to 2 hours. The electrostatic adsorption purification method uses the electrostatic adsorption ability of the charged fiber material to attract and remove polar impurities in the essential oil. The polar impurities in the essential oil carry a charge opposite to the surface charge of the fiber material. Therefore, under the action of the electric field, these impurities will be adsorbed by the charged fiber material, thereby separating the essential oil from the impurities, thereby being able to efficiently remove polar impurities such as moisture and residues in the essential oil, and significantly improving the purity of the essential oil. At the same time, since this method is a physical adsorption method, the operation is gentle and will not damage the active ingredients in the essential oil, thereby maintaining the natural characteristics and functionality of the essential oil to the greatest extent;
[0071] The purified essential oil is mixed with a natural organic solvent, the temperature is controlled at 40-50°C, and the processing time is 1-3 hours. Ethanol has good dissolving and cleaning capabilities, and can further remove trace residual impurities in the essential oil, such as non-polar compounds, grease, etc. At the same time, ethanol is volatile and easy to recover and process. Within this temperature range, ethanol can fully dissolve trace residual substances in the essential oil, while avoiding high temperature from destroying the active ingredients of the essential oil, thereby ensuring that the residual trace impurities in the essential oil are completely removed. Combined with the use of a rotary evaporator, it can not only maintain the high purity of the essential oil, but also realize the recycling of ethanol and save costs.
[0072] Please see attached Figure 1 In a preferred embodiment of the present invention, the extraction of ethanol and distilled water at different temperatures in stages comprises:
[0073] Ethanol extraction is performed using 70% to 90% ethanol solution at 60°C for 2 to 3 hours. Ethanol is a widely used organic solvent with good polarity regulation and biocompatibility. Ethanol solutions with lower concentrations are suitable for extracting polar substances, while ethanol solutions with higher concentrations are conducive to extracting non-polar or weakly polar components. Ethanol extraction can quickly extract oils and fat-soluble compounds in galangal while maintaining the activity of effective ingredients. Ethanol, as a natural organic solvent, has low toxicity and good solubility, so it is suitable for large-scale extraction production. At the same time, under this temperature condition, the extraction efficiency and component activity can be effectively balanced to prevent the degradation of heat-sensitive components caused by high temperature;
[0074] Distilled water is used for water extraction at 90°C for 3 to 4 hours. Distilled water is a highly polar solvent and is suitable for extracting highly polar water-soluble components. By using distilled water for extraction, the effective components dissolved in water in galangal can be completely extracted, and the polar compounds that are difficult to obtain in ethanol extraction can be supplemented, thereby significantly enhancing the functionality of the final essential oil product. In addition, since water is a non-toxic and harmless natural solvent, its use will not cause any chemical residue problems, making the product safer and more environmentally friendly.
[0075] Please see attached Figure 1 In a preferred embodiment of the present invention, adding functional materials comprises:
[0076] Natural antioxidants: By adding natural antioxidants, the shelf life of galangal essential oil can be greatly extended, its chemical stability can be maintained, the active ingredients in the essential oil can be prevented from oxidizing and becoming ineffective, and the long-term use effect of the product can be ensured;
[0077] Lavender essential oil. Adding lavender essential oil not only gives galangal essential oil additional anti-inflammatory and antibacterial properties, but also enhances the aroma of the product, making it relaxing and soothing;
[0078] Frankincense essential oil. By adding frankincense essential oil, galangal essential oil will have stronger anti-inflammatory and repair functions, especially suitable for skin care, anti-aging and scar repair;
[0079] Tea tree essential oil: Tea tree essential oil is a natural antibacterial and antifungal agent that can effectively inhibit the growth of a variety of pathogenic microorganisms. It is often used to treat skin infections, acne and other problems. The addition of tea tree essential oil enhances the antibacterial and anti-inflammatory effects of galangal essential oil.
[0080] Panthenol: By adding panthenol, galangal essential oil not only has good moisturizing properties, but also can help repair the skin barrier, which is particularly suitable for the care needs of dry and sensitive skin, further improving the skin care effect of the product;
[0081] Caprylic / capric triglyceride. By adding caprylic / capric triglyceride, the user experience of galangal essential oil is greatly improved, the texture is lighter, smoother and non-greasy, and the product's absorption effect and skin feel are enhanced.
[0082] Please see attached Figure 1 In a preferred embodiment of the present invention, the low temperature pretreatment further comprises:
[0083] During the soaking period, stirring was performed once an hour for 2 minutes. During the soaking process of low temperature pretreatment, timed stirring was performed once an hour for 2 minutes each time.
[0084] The rotation speed is controlled at 50 to 100 rpm, and the stirring frequency is kept uniform to prevent excessive mechanical action from causing damage to the cells or structural destruction of the galangal, and to ensure the fluidity of the liquid and the uniform cooling of the galangal pieces. Regular stirring can improve the uniformity of soaking and the mass transfer efficiency, especially in low temperature environments, and effectively prevent the accumulation of raw materials and local uneven treatment. By controlling the stirring frequency and speed, mechanical damage caused by excessive stirring is avoided, while ensuring full contact between the soaking liquid and the raw materials, thereby maximizing the integrity of the active ingredients in the galangal and providing good prerequisites for subsequent enzyme treatment steps.
[0085] Please refer to the attached Figure 1 In a preferred embodiment of the present invention, the electrostatic adsorption purification method comprises:
[0086] The extract is concentrated by using a rotary evaporator, the concentration temperature is controlled at 40-50°C, and the ethanol is evaporated under reduced pressure to obtain a concentrated galangal extract. The rotary evaporator reduces the boiling point of ethanol by heating and reducing pressure, so that ethanol can evaporate quickly at a relatively low temperature, thereby avoiding the damage of heat-sensitive components by high temperature. By using a rotary evaporator, ethanol can be evaporated quickly and effectively, the effective ingredients therein can be recovered and the concentration of the extract can be increased. This process not only helps to reduce production costs, but also ensures that the active ingredients in the essential oil are not destroyed at low temperatures, maintaining their biological activity and stability. In addition, the recovered ethanol can be reused, further improving the sustainability of the process.
[0087] The concentrated extract is cooled and then subjected to water extraction to improve the extraction efficiency of polar components. By using a rotary evaporator, ethanol can be evaporated quickly and efficiently, the effective ingredients therein can be recovered and the concentration of the extract can be increased. This process not only helps to reduce production costs, but also ensures that the active ingredients in the essential oil are not destroyed at low temperatures, maintaining their biological activity and stability. In addition, the recovered ethanol can be reused, improving the sustainability of the process.
[0088] Please refer to the attached Figure 1 In a preferred embodiment of the present invention, mixing uniformly comprises:
[0089] Add an appropriate amount of emulsifier to the mixed essential oils, the emulsifier is lecithin or xanthan gum from plant sources, and the added amount is 0.2% to 0.5% of the total weight. Lecithin is a phospholipid compound naturally present in plants such as soybeans and sunflowers, and has good emulsification ability; xanthan gum is a natural polysaccharide produced by plant microbial fermentation, and has strong thickening and emulsification effects. Lecithin has an amphiphilic molecular structure and can form a stable emulsion layer at the interface of oil and water; xanthan gum forms a network structure through its polysaccharide molecules to enhance the viscosity and stability of the system. At the same time, the addition of the emulsifier improves the stability of the galangal essential oil and avoids the stratification phenomenon of the oil phase and other components. The plant-derived emulsifier not only has good safety, but also can improve the use of the product, ensure that the various components of the essential oil are evenly distributed in the formula, and enhance the overall texture and effect of the product;
[0090] By high-speed stirring, 1000-1500 rpm, for 5-10 minutes, emulsification is performed to make the various components of the essential oil more stable and evenly distributed. This high-speed stirring can promote the uniform dispersion of the emulsifier in the essential oil and form a stable emulsified system. After the stirring is completed, the emulsified essential oil mixture is allowed to stand for a period of time, about 30 minutes to 1 hour, to further stabilize the emulsified system. This process helps to remove tiny bubbles in the mixing process and fully combine the components in the emulsified system. Through high-speed stirring emulsification, a uniform and delicate emulsified system can be quickly formed, so that the galangal essential oil and its additional ingredients can be evenly distributed in the formula. This emulsification method improves the stability of the essential oil, prevents oil-water stratification, and extends the storage time of the product.
[0091] The present invention also provides an galangal essential oil, which comprises the following components in parts by weight:
[0092] Galangal essential oil 1-5%;
[0093] Lavender essential oil 0.5-2%;
[0094] Frankincense essential oil 0.5-2%;
[0095] Natural antioxidants 0.05-0.3%;
[0096] Tea tree essential oil 0.5-1%;
[0097] Panthenol 0.1-1%;
[0098] Base oil 90-98%;
[0099] Caprylic / capric triglyceride 1-5%.
[0100] In order to better understand the present invention, the above contents are described in detail below in conjunction with specific embodiments.
[0101] Example 1: Preparation of basic skin care type galangal essential oil
[0102] Step 1: Raw material pretreatment
[0103] Wash the fresh galangal rhizomes, cut them into small pieces of 1 to 2 cm, and pre-cool them at 4°C for 12 hours.
[0104] The enzyme treatment was carried out using 0.3% cellulase at 45°C for 1.5 hours, and then 0.2% pectinase was added and the treatment was continued at 50°C for 1 hour.
[0105] Step 2: Temperature-controlled extraction in stages
[0106] The pretreated galangal was placed in an extraction tank and extracted with 80% ethanol solution at 60°C for 2 hours.
[0107] This was followed by water extraction using distilled water at 90°C for 3 hours.
[0108] The extracted liquid passed through a graded condensation system with the condensation temperatures set at 30°C, 20°C and 10°C to collect different volatile components.
[0109] Step 3: Essential Oil Purification
[0110] The extract was brought into contact with the charged fiber material for electrostatic adsorption purification to adsorb polar impurities and allowed to stand for 1.5 hours.
[0111] The ethanol was evaporated by using a rotary evaporator under reduced pressure and controlling the temperature to 45°C to obtain concentrated galangal essential oil.
[0112] Step 4: Adding functional materials
[0113] Add 0.2% vitamin E as an antioxidant, 1% lavender essential oil and 0.5% frankincense essential oil to the essential oil and mix well.
[0114] 0.3% xanthan gum was added as an emulsifier and high-speed stirring (1200 rpm for 10 minutes) was performed to obtain a stable essential oil mixture.
[0115] Example 2: Preparation of anti-acne care type galangal essential oil
[0116] Step 1: Raw material pretreatment
[0117] The galangal was cut and precooled at 4°C for 24 hours, then treated with 0.5% cellulase at 45°C for 2 hours, and then 0.3% pectinase was added and treated at 50°C for 1 hour.
[0118] Step 2: Temperature-controlled extraction in stages
[0119] Extraction was performed using a 70% ethanol solution at 60°C for 3 hours, followed by extraction using distilled water at 90°C for 4 hours.
[0120] The extracted liquid was subjected to graded condensation, and the condensation temperatures were set to 30°C, 20°C and 10°C, respectively.
[0121] Step 3: Essential Oil Purification
[0122] After the extract is purified by electrostatic adsorption, it is subjected to rotary evaporation, and the temperature is controlled at 40° C. under reduced pressure to remove ethanol and obtain an essential oil extract.
[0123] After cooling and concentrating the extract, water extraction is performed to extract the polar components.
[0124] Step 4: Adding functional materials
[0125] Added 1% Tea Tree Essential Oil and 0.5% Panthenol to promote antibacterial, anti-inflammatory and restorative properties.
[0126] 0.3% lecithin was added as an emulsifier, and high-speed stirring (1000 rpm, 5 minutes) was performed.
[0127] Example 3: Preparation of soothing and restorative galangal essential oil
[0128] Step 1: Raw material pretreatment
[0129] After being cut, the galangal was soaked at 4°C for 12 hours, treated with 0.4% cellulase at 45°C for 1 hour, and then treated with 0.2% pectinase at 50°C for 1 hour.
[0130] Step 2: Temperature-controlled extraction in stages
[0131] The samples were extracted with 90% ethanol solution at 60°C for 2 hours and then with distilled water at 90°C for 3 hours.
[0132] The extracted liquid is condensed through a graded condensation system at temperatures of 30°C, 20°C and 10°C, respectively.
[0133] Step 3: Essential Oil Purification
[0134] After purification by electrostatic adsorption, ethanol was evaporated under reduced pressure at 50 °C by rotary evaporation to obtain a high-purity essential oil extract.
[0135] After the concentrate is cooled, the polar components are further extracted by water extraction.
[0136] Step 4: Adding functional materials
[0137] 1% frankincense essential oil, 0.5% lavender essential oil and 0.2% panthenol are added to the essential oil to promote skin repair and soothing effects.
[0138] Add 0.2% lecithin as an emulsifier and stir at high speed of 1200 rpm for 10 minutes to ensure uniform dispersion.
[0139] Example 4: Preparation of anti-aging galangal essential oil
[0140] Step 1: Raw material pretreatment
[0141] The galangal pieces were cut and precooled at 4°C for 24 hours, treated with 0.4% cellulase at 45°C for 1.5 hours, and then treated with 0.3% pectinase at 50°C for 1 hour.
[0142] Step 2: Temperature-controlled extraction in stages
[0143] Extraction was performed using 80% ethanol at 60°C for 2.5 hours, followed by extraction using distilled water at 90°C for 3.5 hours.
[0144] A graded condensation system was used with the temperatures controlled at 30°C, 20°C and 10°C to collect different volatile components in sequence.
[0145] Step 3: Essential Oil Purification
[0146] After the extract was purified by electrostatic adsorption, it was concentrated by rotary evaporator with the temperature set at 45°C to remove ethanol.
[0147] After the concentrated liquid is cooled, water extraction is performed to improve the extraction efficiency of polar antioxidant substances.
[0148] Step 4: Adding functional materials
[0149] 0.3% Vitamin E is added as an antioxidant, 1% Frankincense essential oil and 0.5% Tea Tree essential oil are used to promote anti-aging and antibacterial effects.
[0150] 0.4% xanthan gum was added for emulsification, and high-speed stirring was performed at 1500 rpm for 5 minutes.
[0151] Comparative experiment 1: Extraction efficiency test experiment
[0152] Experimental purpose: To verify whether the preparation method of galangal essential oil in the present invention can significantly improve the extraction efficiency.
[0153] Experimental setup:
[0154] Experimental group (method of the present invention): using a staged temperature-controlled extraction method, combined with ethanol extraction, water extraction, multi-stage condensation and electrostatic adsorption purification.
[0155] Control group 1: only ethanol extraction was used without multi-stage extraction or electrostatic adsorption purification.
[0156] Control group 2: Only water extraction was used, without ethanol extraction and other complex purification steps.
[0157] Control group 3: traditional distillation extraction method without staged temperature control, electrostatic adsorption or water extraction.
[0158] Experimental materials and equipment:
[0159] 100 g fresh galangal rhizome (same for each group).
[0160] 70% to 90% ethanol solution (used in the experimental group and control group 1).
[0161] Distilled water (used in experimental group and control group 2).
[0162] Distillation extraction equipment, rotary evaporator, graded condensation system, electrostatic adsorption equipment, etc.
[0163] Experimental steps:
[0164] Raw materials preparation:
[0165] The galangal raw materials in each group were standardized, cut into small pieces of 1 to 2 cm, and pre-treated at low temperature to ensure the consistency of the raw materials.
[0166] Extraction process:
[0167] Experimental group: The process of the present invention was adopted, using 70% ethanol for extraction at 60°C for 2 hours, performing temperature-controlled extraction in stages, and then performing water extraction (90°C, 3 hours), and concentrating by electrostatic adsorption and rotary evaporation.
[0168] Control group 1: extraction with 70% ethanol at 60°C for 3 hours without water extraction or electrostatic adsorption purification.
[0169] Control group 2: Extraction with distilled water at 90°C for 4 hours without ethanol extraction or staged temperature control.
[0170] Control group 3: conventional distillation extraction was performed for 3 hours using conventional distillation extraction equipment without any other treatment.
[0171] Extract collection:
[0172] The galangal essential oil extracted from each group was weighed, and the mass of the extract of each group was recorded.
[0173] Calculate the extraction efficiency:
[0174] The calculation formula of extraction efficiency is: extraction efficiency = (extract mass / raw material mass) × 100%.
[0175] The extraction efficiency of each group was recorded and the data were collated.
[0176] The comparative experimental data are shown in Table 1:
[0177] Table 1 Extraction efficiency comparison experimental data
[0178] Group Raw material mass (g) Extract mass (g) Extraction efficiency (%) Experimental Group 100 4.5 4.5 Control group 1 100 3.1 3.1 Control group 2 100 2.7 2.7 Control group 3 100 2.2 2.2 Experimental Group 100 4.4 4.4 Control group 1 100 3.0 3.0 Control group 2 100 2.6 2.6 Control group 3 100 2.1 2.1 Experimental Group 100 4.6 4.6 Control group 1 100 3.3 3.3 Control group 2 100 2.9 2.9 Control group 3 100 2.5 2.5
[0179] From the data in Table 1, we can get:
[0180] The experimental group of the present invention has a significant advantage in extraction efficiency. The staged temperature-controlled extraction method combined with multiple purification technologies greatly improves the extraction efficiency of essential oils compared to a single extraction method (such as ethanol extraction and distillation extraction). In particular, under the extraction method combining multiple solvents, more effective ingredients can be extracted from Alpinia galanga.
[0181] Comparative experiment 2: Essential oil purity test experiment
[0182] Experimental purpose: To verify whether the multi-stage extraction method, electrostatic adsorption purification, graded condensation and rotary evaporation process in the present invention can effectively improve the purity of essential oils.
[0183] Experimental setup:
[0184] Experimental group (method of the present invention): multi-stage temperature-controlled extraction, electrostatic adsorption purification, graded condensation, and rotary evaporator concentration extraction processes were adopted.
[0185] Control group 1: The traditional ethanol extraction method was used without electrostatic adsorption and multi-stage purification.
[0186] Control group 2: only water extraction process was used without other purification steps.
[0187] Control group 3: using conventional distillation without multi-stage condensation, electrostatic adsorption or rotary evaporator treatment.
[0188] Experimental materials and equipment:
[0189] Fresh galangal rhizome (100g / group).
[0190] Gas chromatography-mass spectrometry (GC-MS).
[0191] Graded condensation system, rotary evaporator, electrostatic adsorption equipment, ethanol solution and distilled water, etc.
[0192] Experimental steps:
[0193] Raw material handling:
[0194] The raw materials of galangal were standardized for all groups, ensuring that 100 g of galangal rhizome was used in each group.
[0195] Extraction process:
[0196] Experimental group: A multi-stage temperature-controlled extraction method was used, combining 70% ethanol and water extraction, and after graded condensation (30°C, 20°C, and 10°C) and electrostatic adsorption purification, the solvent was removed by rotary evaporation to obtain the essential oil.
[0197] Control group 1: Traditional ethanol extraction was performed at 60°C for 3 hours without electrostatic adsorption or condensation treatment.
[0198] Control group 2: Extraction was performed using only distilled water at 90°C for 4 hours without any other purification treatment.
[0199] Control group 3: extraction by traditional distillation for 3 hours without other purification steps.
[0200] Purity analysis:
[0201] Gas chromatography-mass spectrometry (GC-MS) was used to detect the main chemical components in each group of samples, and the percentage content of each group of target components (such as monoterpenes and sesquiterpenes) was recorded.
[0202] The target components include α-terpineol, β-phellandrene, eucalyptol, etc. The proportion of the target components in each group to the total essential oil was calculated to evaluate the purity of the essential oil.
[0203] Result recording and analysis:
[0204] Record the content ratio of the target component in each group of essential oils and calculate the purity of the essential oils;
[0205] The difference in purity between the present invention and each control group was analyzed to verify the effect of the process of the present invention.
[0206] The comparative experimental data are shown in Table 2:
[0207] Table 2 Comparative experimental data of galangal essential oil purity
[0208]
[0209] From the data in Table 2, we can get:
[0210] The average purity of the experimental group of the present invention reached 94.67%, indicating that impurities were effectively removed through multi-stage temperature-controlled extraction, electrostatic adsorption purification and graded condensation processes, and the content of the main components in the extract was significantly improved, thereby verifying the innovation and effectiveness of the present invention in improving the purity of essential oils.
[0211] Comparative experiment 3: Antioxidant performance test experiment
[0212] Experimental purpose: To verify whether the multi-stage extraction process and the addition of functional materials of the present invention can effectively improve the antioxidant capacity of essential oils.
[0213] Experimental setup:
[0214] Experimental group (method of the present invention): using the multi-stage temperature-controlled extraction, electrostatic adsorption purification and graded condensation process of the present invention, the functional materials include antioxidant ingredients such as vitamin E, lavender essential oil, frankincense essential oil, tea tree essential oil, etc.
[0215] Control group 1: Only ethanol extraction was used without adding any antioxidants or functional essential oils.
[0216] Control group 2: Only natural antioxidants (such as vitamin E) were added, and no other functional essential oils (such as lavender essential oil, frankincense essential oil, etc.) were added.
[0217] Control group 3: Traditional distillation extraction method without adding antioxidants or other functional materials.
[0218] Experimental materials and equipment:
[0219] Fresh galangal rhizome (100g / group).
[0220] DPPH reagent, used for free radical scavenging ability test.
[0221] FRAP reagent, used for testing the iron ion reducing antioxidant capacity.
[0222] UV-Vis spectrophotometer was used to measure absorbance.
[0223] Experimental steps:
[0224] Raw material handling:
[0225] The rhizomes of Alpinia officinalis in each group were standardized (100 g per group) to ensure consistent experimental conditions.
[0226] Extraction process:
[0227] Experimental group: The method of the present invention was used in combination with staged temperature-controlled extraction, electrostatic adsorption purification, graded condensation and the addition of functional materials (vitamin E, lavender essential oil, frankincense essential oil, tea tree essential oil, etc.).
[0228] Control group 1: ethanol extraction method was used without adding any antioxidants.
[0229] Control group 2: ethanol extraction method was used, and only 0.2% vitamin E was added as an antioxidant.
[0230] Control group 3: Extracted using traditional distillation method without adding any antioxidants or functional materials. DPPH free radical scavenging ability test: Prepare 0.1mM DPPH solution, mix each group of galangal essential oil samples with DPPH solution in a 1:1 ratio, and react in the dark for 30 minutes.
[0231] The absorbance of each sample at 517 nm was measured using a UV-visible spectrophotometer, and the free radical scavenging rate was calculated:
[0232]
[0233] Among them, A 对照 is the absorbance of DPPH blank solution, A 样品 is the absorbance of the sample after reaction with DPPH.
[0234] FRAP Antioxidant Capacity Test:
[0235] FRAP reagent was prepared, and each group of galangal essential oil samples was mixed with FRAP reagent in a 1:1 ratio and reacted at 37°C for 30 minutes.
[0236] The absorbance of the sample was measured at 593 nm using a spectrophotometer and the reducing capacity was calculated.
[0237] Data recording and analysis:
[0238] The DPPH free radical scavenging rate and FRAP value of each group of samples were recorded, and the differences in antioxidant capacity of each group of samples were analyzed.
[0239] The comparative experimental data are shown in Table 3:
[0240] Table 3 Comparative experimental data on antioxidant properties of galangal essential oil
[0241] Group DPPH free radical scavenging rate (%) <![CDATA[FRAP value (μmol Fe 2+ / g)]]> Experimental Group 87.2 320.5 Control group 1 51.3 165.8 Control group 2 73.4 275.2 Control group 3 45.8 150.1 Experimental Group 88.5 330.0 Control group 1 50.1 170.3 Control group 2 74.2 268.7 Control group 3 46.7 158.6 Experimental Group 86.9 315.4 Control group 1 52.6 160.7 Control group 2 71.8 280.0 Control group 3 47.3 149.3
[0242] From the data in Table 3, we can get:
[0243] The average DPPH free radical scavenging rate of the experimental group was 87.53%, and the average FRAP value was 321.97 μmol Fe 2+ / g, compared with the control group without adding antioxidants, the antioxidant capacity was significantly improved. This is because the experimental group not only adopted a staged temperature-controlled extraction process, but also added a variety of antioxidant ingredients. These ingredients significantly enhanced the antioxidant capacity of the essential oil, which can effectively remove free radicals and reduce oxidants, thereby enhancing its antioxidant capacity.
[0244] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing galangal essential oil, characterized in that: The following steps are involved: Raw material pretreatment: the rhizomes of galangal were cut, low-temperature pretreated and treated with enzymes; Staged temperature-controlled extraction and fractional condensation: ethanol and distilled water are used in turn for staged extraction at different temperatures, and then fractional condensation is used to collect components with different volatility; Essential oil purification: Use electrostatic adsorption purification to remove impurities and further purify with natural organic solvents; Adding functional materials: adding natural antioxidants and other essential oil ingredients to essential oils for compounding; Mix well: Mix the galangal essential oil and other components evenly and let it stand.
2. The method for preparing galangal essential oil according to claim 1, wherein: The raw material pretreatment comprises: Low temperature pretreatment: Cut the rhizomes of galangal into small pieces of 1 to 2 cm and precool them at 4°C for 12 to 24 hours; Enzyme treatment: first use 0.2% to 0.5% cellulase at 45°C and pH 5.0 for 1 to 2 hours, then use 0.1% to 0.3% pectinase at 50°C and pH 4.5 for 1 hour.
3. The method for preparing galangal essential oil according to claim 1, characterized in that: The staged temperature-controlled extraction comprises: The first stage of extraction is carried out at 70-80°C for 1-2 hours to extract the volatile components; The second stage of extraction is carried out at 90-100°C for 1.5-2.5 hours to extract the non-volatile components; The extracted distillation product was condensed by a graded condensation system, and the condensation temperatures were set at 30°C, 20°C and 10°C, respectively, to collect different volatile components.
4. The method for preparing galangal essential oil according to claim 1, wherein: The essential oil purification comprises: Using electrostatic adsorption purification method, the essential oil is brought into contact with the charged fiber material to adsorb and remove polar impurities, and the static time is 1 to 2 hours; The purified essential oil is mixed with a natural organic solvent, the temperature is controlled at 40-50°C, and the treatment time is 1-3 hours.
5. The method for preparing galangal essential oil according to claim 3, characterized in that: The ethanol and distilled water are subjected to phased extraction at different temperatures, comprising: Use 70% to 90% ethanol solution to perform ethanol extraction at 60°C for 2 to 3 hours; The extraction was performed using distilled water at 90°C for 3 to 4 hours.
6. The method for preparing galangal essential oil according to claim 1, characterized in that: The added functional materials include: Natural antioxidant; Lavender essential oil; Frankincense essential oil; Tea tree essential oil; Panthenol; Caprylic / capric triglyceride.
7. The method for preparing galangal essential oil according to claim 2, characterized in that: The low temperature pretreatment further comprises: During the soaking period, stir once every hour for 2 minutes; The speed is controlled at 50-100 rpm.
8. The method for preparing galangal essential oil according to claim 4, characterized in that: Electrostatic adsorption purification methods include: The extract is concentrated by using a rotary evaporator, the concentration temperature is controlled at 40-50°C, and the ethanol is evaporated under reduced pressure to obtain a concentrated galangal extract; The concentrated extract is cooled and then subjected to water extraction to improve the extraction efficiency of polar components.
9. The method for preparing galangal essential oil according to claim 1, characterized in that: The uniform mixing comprises: Adding a proper amount of emulsifier to the mixed essential oils, wherein the emulsifier is lecithin or xanthan gum from plant sources, and the added amount is 0.2% to 0.5% of the total weight; By high-speed stirring, 1000-1500 rpm, for 5-10 minutes, emulsification is performed to make the components of the essential oil more stable and evenly distributed.
10. An essential oil of galangal, characterized in that: A method for preparing galangal essential oil according to any one of claims 1 to 9, wherein the galangal essential oil comprises the following components in parts by weight: Galangal essential oil 1-5%; Lavender essential oil 0.5-2%; Frankincense essential oil 0.5-2%; Natural antioxidants 0.05-0.3%; Tea tree essential oil 0.5-1%; Panthenol 0.1-1%; Base oil 90-98%; Caprylic / capric triglyceride 1-5%.
