Device and method for extracting and separating dendrobium huoshanense essential oil

Abstract

The invention provides an extraction and separation device and method for dendrobium huoshanense essential oil. The method for extracting and separating the dendrobium huoshanense essential oil comprises the following steps: a, preparing raw materials: pretreating a fresh dendrobium huoshanense material, cleaning, removing impurities, and air-drying for later use, and b, performing low-temperature wall-breaking treatment: performing wall-breaking treatment on the dendrobium huoshanense material by adopting a low-temperature mechanical crushing technology so as to increase the permeability of plant cells and keep active ingredients complete. According to the extraction and separation device and method for the dendrobium huoshanense essential oil, by adopting the technical means of low-temperature wall breaking treatment, low-temperature presoaking, ultrasonic-assisted extraction, low-temperature molecular distillation and the like, it is ensured that thermosensitive active ingredients in the dendrobium huoshanense essential oil are not damaged in the extraction process, and therefore the content of active substances in the essential oil is increased; by applying the supercritical CO2 extraction technology, the problem of organic solvent residue is effectively avoided, the purity and safety of the extract are ensured, and the high-purity essential oil is obtained.

Description

Technical Field

[0001] The invention relates to the technical field of extraction and separation of essential oils, and in particular to an extraction and separation device and method for Huoshan dendrobium essential oil. Background Art

[0002] Extraction methods for Huoshan Dendrobium essential oil primarily include steam distillation, supercritical CO₂ extraction, solvent extraction, cold pressing, and microwave-assisted extraction. Steam distillation is a traditional and widely used method for extracting essential oils. It extracts volatile components by heating the oil, which is then collected through condensation. It is suitable for extracting most volatile components from plants. Its advantages include simple equipment, easy operation, and the absence of chemical solvents, making it environmentally friendly and suitable for small-scale or household essential oil extraction applications. Supercritical CO₂ extraction, using supercritical CO₂ as a solvent, can efficiently extract the active ingredients in Huoshan Dendrobium essential oil at low temperatures, making it particularly suitable for protecting heat-sensitive substances that are vulnerable to high temperatures. Furthermore, it offers excellent solubility selectivity, a high-purity extract, and no residual solvent, significantly improving the quality of the essential oil. Solvent extraction, using organic solvents (such as ethanol and n-hexane) to dissolve the essential oil components in the dendrobium, followed by evaporation to remove the solvent, allows for the efficient extraction of heat-sensitive components and is therefore suitable for large-scale industrial production.

[0003] While each of these extraction methods has its own unique advantages, they also have drawbacks. Steam distillation requires heating, which can destroy some heat-sensitive active ingredients during the extraction process, reducing the active ingredient content in the essential oil. Solvent extraction can also lead to residual solvents, compromising the purity and safety of the extract. Summary of the Invention

[0004] (1) Technical problems solved

[0005] In response to the shortcomings of the existing technology, the present invention provides an extraction and separation device and method for Huoshan Dendrobium essential oil, which solves the problem that heat-sensitive active ingredients may be destroyed during the extraction process, resulting in a decrease in the content of active substances in the essential oil; and the problem of solvent residue, which affects the purity and safety of the extract.

[0006] (2) Technical solution

[0007] To achieve the above objectives, the present invention is implemented through the following technical solutions: an extraction and separation device and method for Huoshan Dendrobium essential oil, comprising the following steps:

[0008] a. Raw material preparation: pre-treat the fresh Huoshan Dendrobium, wash and remove impurities, and air-dry for later use;

[0009] b. Low-temperature cell wall breaking: Low-temperature mechanical crushing technology is used to break the cell wall of Huoshan Dendrobium to increase the permeability of plant cells and keep the active ingredients intact;

[0010] c. Low-temperature pre-soaking: Soak the broken wall of the Huoshan Dendrobium material in pure water at a low temperature of 20-30°C for 1-2 hours to release some water-soluble active ingredients;

[0011] d. Ultrasonic-assisted extraction: Ultrasonic-assisted extraction is used under low temperature conditions to quickly release the active ingredients. The ultrasonic frequency is 20-40 kHz and the extraction time is 30-40 minutes.

[0012] e. Low temperature molecular distillation: Under vacuum conditions, the extract is initially separated using low temperature molecular distillation equipment, with the temperature controlled not to exceed 50°C to avoid destruction of heat-sensitive components;

[0013] f. Supercritical CO2 extraction: The extracted extract is subjected to supercritical CO2 extraction technology to extract essential oils at a pressure range of 15-25 MPa and a temperature controlled at 35-45°C to obtain high-purity essential oils;

[0014] g essential oil separation: the gas after supercritical CO2 extraction was condensed and separated by a condenser to obtain Huoshan Dendrobium essential oil;

[0015] h. Solvent removal: Use membrane separation technology to remove water-soluble impurities and ensure that no organic solvent remains;

[0016] i. Essential oil purification: Use molecular sieve technology to further purify the essential oil to increase the content of active ingredients in the essential oil;

[0017] j. Stabilization treatment: Antioxidant treatment of essential oils, adding natural antioxidants to improve the stability of essential oils;

[0018] k. Encapsulation treatment: Using microencapsulation technology, the essential oil is microencapsulated to reduce the volatilization and oxidation loss of active ingredients;

[0019] l. Finished product preparation: The embedded essential oil is bottled and sealed for storage as a Huoshan Dendrobium essential oil product.

[0020] m. Quality testing: Finished essential oils are tested to ensure they meet quality standards for essential oil content, purity, and stability, thereby ensuring product safety and effectiveness.

[0021] Preferably, the temperature of the low-temperature wall-breaking treatment is controlled between -10°C and 0°C to reduce the impact of high temperature on the active ingredients, and the vacuum degree in the molecular distillation process is controlled between 10-20 Pa to further lower the boiling point and reduce the degradation of heat-sensitive components.

[0022] Preferably, during the low-temperature pre-impregnation process, the immersion time is controlled to be 1.5 hours to optimize the release of active ingredients, and the power range of the ultrasonic-assisted extraction is 200-300W to ensure the extraction efficiency.

[0023] Preferably, the supercritical CO2 extraction time is controlled to be 1-2 hours to ensure that the active ingredients in the essential oil are fully extracted, and the condenser temperature after the supercritical CO2 extraction is controlled at 0-5°C to improve the recovery rate of the essential oil.

[0024] Preferably, the membrane separation technology uses a nanofiltration membrane to remove water-soluble impurities and improve the purity of the essential oil. The pore size of the molecular sieve is 0.5-1.0 nanometers to achieve efficient separation of impurities in the essential oil.

[0025] Preferably, the natural antioxidant is selected from vitamin E, rosemary extract or tea polyphenols to improve the stability of the essential oil, and the microcapsule embedding material is a mixture of gelatin and gum arabic to improve the embedding efficiency and release control of the essential oil.

[0026] Preferably, the particle size of the embedded microcapsule essential oil is in the range of 50-100 microns to facilitate the application and storage of the essential oil. The bottling process of the essential oil is carried out in an inert gas environment to reduce the occurrence of oxidation reactions. The storage temperature of the finished essential oil product is controlled at 4-10°C to increase the shelf life of the essential oil. The quality inspection includes the inspection of indicators such as the active ingredient content, heavy metal content, microbial content and antioxidant activity of the essential oil to ensure that its quality meets relevant national standards.

[0027] A device for extracting and separating Huoshan dendrobium essential oil comprises: a raw material processing device, a low-temperature wall-breaking processing device, a low-temperature prepreg tank, an ultrasonic-assisted extraction device, a low-temperature molecular distillation device, a supercritical CO2 extraction system, a condensation separation device, a membrane separation system, a molecular sieve separation device, a stabilization processing device, a microcapsule embedding device, a bottling system, and a quality detection device.

[0028] (3) Beneficial effects

[0029] The present invention provides an extraction and separation device and method for Huoshan Dendrobium essential oil, which has the following beneficial effects:

[0030] This technical solution ensures that the heat-sensitive active ingredients in Huoshan Dendrobium essential oil are not destroyed during the extraction process by adopting technical means such as low-temperature wall-breaking treatment, low-temperature pre-infusion, ultrasonic-assisted extraction and low-temperature molecular distillation, thereby increasing the active substance content of the essential oil. The application of supercritical CO2 extraction technology effectively avoids the problem of organic solvent residue, ensures the purity and safety of the extract, and obtains high-purity essential oil.

[0031] This technical solution also uses membrane separation technology, molecular sieve separation technology and microencapsulation technology to finely separate and purify essential oils, and stabilizes them by adding natural antioxidants, which significantly improves the stability and shelf life of the essential oils. The entire process of the device is carried out under low temperature and vacuum environment, minimizing oxidation reactions and ensuring the high quality of essential oil products. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a schematic diagram of the overall structure of the present invention. DETAILED DESCRIPTION

[0033] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts are within the scope of protection of the present invention.

[0034] like Figure 1 As shown, the embodiment of the present invention provides an extraction and separation device and method for Huoshan Dendrobium essential oil, including: a. Raw material preparation: pre-treating the Huoshan Dendrobium fresh material, washing it to remove impurities, and air-drying it for standby use.

[0035] b. Low-temperature cell wall breaking treatment: Low-temperature mechanical crushing technology is used to break the cell wall of Huoshan Dendrobium to increase the permeability of plant cells and keep the active ingredients intact. The temperature of low-temperature cell wall breaking treatment is controlled between -10°C and 0°C to reduce the impact of high temperature on the active ingredients. The vacuum degree during the molecular distillation process is controlled between 10-20Pa to further lower the boiling point and reduce the degradation of heat-sensitive components.

[0036] c. Low-temperature pre-infusion: Soak the broken wall of the Huoshan Dendrobium material in pure water at a low temperature of 20-30°C for 1-2 hours to release some water-soluble active ingredients. During the low-temperature pre-infusion process, the soaking time is controlled at 1.5 hours to optimize the release of active ingredients. The power range of ultrasonic-assisted extraction is 200-300W to ensure extraction efficiency.

[0037] d. Ultrasonic-assisted extraction: Ultrasonic-assisted extraction is used under low temperature conditions to quickly release the active ingredients. The ultrasonic frequency is 20-40 kHz, the extraction time is 30-40 minutes, and the supercritical CO2 extraction time is controlled to 1-2 hours to ensure that the active ingredients in the essential oil are fully extracted. The condenser temperature after supercritical CO2 extraction is controlled at 0-5°C to improve the recovery rate of the essential oil.

[0038] e. Low temperature molecular distillation: Under vacuum conditions, the extract is initially separated using low temperature molecular distillation equipment, and the temperature is controlled not to exceed 50°C to avoid destruction of heat-sensitive components.

[0039] f. Supercritical CO2 extraction: The extracts from the preliminary separation are subjected to supercritical CO2 extraction technology to extract the essential oils. The pressure range is 15-25 MPa and the temperature is controlled at 35-45°C to obtain high-purity essential oils. The membrane separation technology uses nanofiltration membranes to remove water-soluble impurities and improve the purity of the essential oils. The pore size of the molecular sieve is 0.5-1.0 nanometers to achieve efficient separation of impurities in the essential oils.

[0040] g. Essential oil separation: The gas after supercritical CO2 extraction is condensed and separated by a condenser to obtain Huoshan Dendrobium essential oil.

[0041] h. Solvent removal: Use membrane separation technology to remove water-soluble impurities and ensure that no organic solvent remains.

[0042] i. Essential oil purification: Molecular sieve technology is used to further purify the essential oil to increase the content of active ingredients in the essential oil.

[0043] j. Stabilization treatment: The essential oil is subjected to antioxidant treatment and natural antioxidants are added to improve the stability of the essential oil. The natural antioxidants are selected from vitamin E, rosemary extract or tea polyphenols to improve the stability of the essential oil. The microcapsule encapsulation material is a mixture of gelatin and gum arabic to improve the encapsulation efficiency and release control of the essential oil.

[0044] k. Encapsulation treatment: The essential oil is microencapsulated using microencapsulation technology to reduce the volatilization and oxidation loss of active ingredients. The particle size of the encapsulated microcapsule essential oil is in the range of 50-100 microns, which is convenient for the application and storage of the essential oil. The bottling process of the essential oil is carried out in an inert gas environment to reduce the occurrence of oxidation reactions. The storage temperature of the finished essential oil is controlled at 4-10°C to increase the shelf life of the essential oil. Quality testing includes testing of indicators such as the active ingredient content, heavy metal content, microbial content and antioxidant properties of the essential oil to ensure that its quality meets relevant national standards.

[0045] l. Finished product preparation: The embedded essential oil is bottled and sealed for storage as a Huoshan Dendrobium essential oil product.

[0046] m. Quality testing: Finished essential oils are tested to ensure they meet quality standards for essential oil content, purity, and stability, thereby ensuring product safety and effectiveness.

[0047] A device for extracting and separating Huoshan dendrobium essential oil, characterized by comprising: a raw material processing device, a low-temperature wall-breaking processing device, a low-temperature prepreg tank, an ultrasound-assisted extraction device, a low-temperature molecular distillation device, a supercritical CO2 extraction system, a condensation separation device, a membrane separation system, a molecular sieve separation device, a stabilization treatment device, a microcapsule embedding device, a bottling system, and a quality detection device.

[0048] While 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 these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A method for extracting and separating Huoshan Dendrobium essential oil, characterized in that: The following steps are involved: a. Raw material preparation: pre-treat the fresh Huoshan Dendrobium, wash and remove impurities, and air-dry for later use; b. Low temperature cell wall breaking treatment: Low temperature mechanical crushing technology is used to break the cell wall of Huoshan Dendrobium to increase the permeability of plant cells and keep the active ingredients intact; c. Low-temperature pre-soaking: Soak the broken wall of Huoshan Dendrobium material in pure water for 1-2 hours at a low temperature of 20-30°C to release some water-soluble active ingredients; d. Ultrasonic assisted extraction: Ultrasonic assisted extraction is used under low temperature conditions to quickly release the active ingredients. The ultrasonic frequency is 20-40kHz and the extraction time is 30-40 minutes; e. Low temperature molecular distillation: Under vacuum conditions, the extract is initially separated using low temperature molecular distillation equipment, with the temperature controlled not to exceed 50°C to avoid destruction of heat-sensitive components; f. Supercritical CO2 extraction: The extracted extract is subjected to supercritical CO2 extraction technology to extract essential oils at a pressure range of 15-25 MPa and a temperature control range of 35-45°C to obtain high-purity essential oils; g. Essential oil separation: The gas after supercritical CO2 extraction is condensed and separated by a condenser to obtain Huoshan Dendrobium essential oil; h. Solvent removal: Use membrane separation technology to remove water-soluble impurities and ensure that there is no organic solvent residue; i. Essential oil purification: Use molecular sieve technology to further purify the essential oil to increase the content of active ingredients in the essential oil; j. Stabilization treatment: Antioxidant treatment of essential oils, adding natural antioxidants to improve the stability of essential oils; k. Encapsulation treatment: Use microencapsulation technology to microencapsulate the essential oil to reduce the volatilization and oxidation loss of active ingredients; l. Finished product preparation: The essential oil after embedding treatment is bottled and sealed for storage as Huoshan Dendrobium essential oil products; m. Quality testing: Conduct quality testing on finished essential oils to ensure that they meet quality standards such as essential oil content, purity and stability to ensure the safety and effectiveness of the product.

2. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: The temperature of the low-temperature wall-breaking treatment is controlled between -10°C and 0°C to reduce the impact of high temperature on active ingredients, and the vacuum degree in the molecular distillation process is controlled between 10-20Pa to further reduce the boiling point and reduce the degradation of heat-sensitive ingredients.

3. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: During the low-temperature pre-impregnation process, the immersion time is controlled to be 1.5 hours to optimize the release of active ingredients, and the power range of the ultrasonic-assisted extraction is 200-300W to ensure the extraction efficiency.

4. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: The supercritical CO2 extraction time is controlled to be 1-2 hours to ensure that the active ingredients in the essential oil are fully extracted. The condenser temperature after the supercritical CO2 extraction is controlled at 0-5°C to improve the recovery rate of the essential oil.

5. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: The membrane separation technology uses a nanofiltration membrane to remove water-soluble impurities and improve the purity of the essential oil. The pore size of the molecular sieve is 0.5-1.0 nanometers to achieve efficient separation of impurities in the essential oil.

6. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: The natural antioxidant is selected from vitamin E, rosemary extract or tea polyphenols to improve the stability of the essential oil, and the microcapsule embedding material is a mixture of gelatin and gum arabic to improve the embedding efficiency and the release control of the essential oil.

7. A method for extracting and separating the essential oil of Dendrobium huoshanense according to claim 1, characterized in that: The particle size of the embedded microcapsule essential oil is in the range of 50-100 microns, which is convenient for the application and preservation of the essential oil. The bottling process of the essential oil is carried out in an inert gas environment to reduce the occurrence of oxidation reactions. The storage temperature of the finished essential oil product is controlled at 4-10°C to increase the shelf life of the essential oil. The quality inspection includes the inspection of indicators such as the active ingredient content, heavy metal content, microbial content and antioxidant activity of the essential oil to ensure that its quality meets relevant national standards.

8. An extraction and separation device for Huoshan Dendrobium essential oil, characterized in that: include: Raw material processing equipment, low-temperature wall breaking processing equipment, low-temperature prepreg tank, ultrasonic assisted extraction equipment, low-temperature molecular distillation equipment, supercritical CO2 extraction system, condensation separation equipment, membrane separation system, molecular sieve separation equipment, stabilization treatment equipment, microcapsule embedding equipment, bottling system, quality inspection equipment.

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