Vacuum low-temperature distilled herbal medicine bath extraction process

Abstract

The invention relates to the technical field of medicine extraction, and discloses a vacuum low-temperature distillation herbal medicine bath fine extraction process, which comprises the following steps: 1, pretreating raw materials; step 2, crushing and mixing; step 3, vacuum low-temperature distillation; step 4, filtering treatment; step 5, concentrating and drying; and step 6, carrying out post-treatment on the extract. According to the vacuum low-temperature distillation herbal medicine bath fine extraction process, the vacuum low-temperature distillation condition is accurately controlled, so that the heat-sensitive component retention rate is greatly increased, and the medicated bath effect is enhanced; in the aspect of impurity removal, various filtering and chromatography technologies are cooperated, so that the impurity content is greatly reduced, and the use safety is guaranteed; in terms of energy consumption, low-temperature and low-pressure operation achieves great energy conservation, and large-scale production is facilitated; after the extraction process is optimized, by means of microwave, superfine grinding, ultrasonic mixing and the like, the utilization rate of the herbal medicine is remarkably increased, high-quality, high-efficiency and high-safety innovation breakthrough is brought to the herbal medicine medicated bath industry, and the method has great market competitiveness and application and popularization value.

Description

Technical Field

[0001] The invention relates to the technical field of drug extraction, in particular to a vacuum low-temperature distillation herbal medicine bath extraction process. Background Art

[0002] As people pay more and more attention to health and wellness, herbal baths are increasingly valued as a traditional health care and treatment method. With the development of science and technology and the improvement of people's quality requirements, the necessity of its extraction process has become increasingly prominent. In the natural growth process, herbs will inevitably be mixed with impurities such as soil, sand, microorganisms and residual pesticides. If untreated herbs are directly used for baths, these impurities will not only affect the use experience of the bath, such as causing skin discomfort or even allergic reactions, but may also interfere with the release and absorption of active ingredients in the herbs, making it difficult for the bath to exert the expected health and therapeutic effects; moreover, the active ingredients in herbs are often wrapped by complex structures such as cell walls. In the natural state, these ingredients are difficult to pass through the skin barrier and be effectively absorbed by the human body. Through a special extraction process, these structural constraints can be broken and the active ingredients can be enriched, thereby significantly improving the utilization rate of the herbs and enhancing the effect of the bath.

[0003] However, the existing herbal bath extraction process has many defects. The traditional distillation method is usually carried out at a relatively high temperature, which can easily lead to the destruction of heat-sensitive active ingredients in the herbs, thereby reducing the efficacy of the bath. Moreover, conventional extraction processes may not be able to effectively remove impurities and odors in the herbs, affecting the user experience and safety of the bath. In addition, the energy consumption in the extraction process is high, which is not conducive to large-scale production and sustainable development.

[0004] Therefore, a vacuum low-temperature distillation herbal medicine bath extraction process is proposed. Summary of the invention

[0005] 1. Technical issues to be resolved

[0006] In view of the shortcomings of the prior art, the present invention provides a vacuum low-temperature distillation herbal medicinal bath extraction process, which greatly improves the retention rate of heat-sensitive components and enhances the efficacy of the medicinal bath by precisely controlling the vacuum low-temperature distillation conditions; in terms of impurity removal, a variety of filtration and chromatography technologies work together to greatly reduce the impurity content and ensure safe use; in terms of energy consumption, low-temperature and low-pressure operation achieves significant energy saving, which is conducive to large-scale production; after the extraction process is optimized, the utilization rate of herbs is significantly improved with the help of microwaves, ultrafine grinding and ultrasonic mixing, etc., solving the problems raised by the background technology.

[0007] (II) Technical solution

[0008] To achieve the above-mentioned purpose, the present invention provides the following technical solution: a vacuum low-temperature distillation herbal medicine bath extraction process, comprising the following steps:

[0009] Step 1: Raw material pretreatment: select fresh or dried herbal raw materials, remove impurities, moldy and insect-infested parts, weigh them according to the formula ratio, rinse them with clean water, and then dry the herbal raw materials in low-temperature drying equipment, control the temperature at 30℃-40℃, and ensure that the moisture content of the herbs is less than 8%;

[0010] Step 2: crushing and mixing, the pre-treated herbal raw materials are put into an ultra-fine grinder for crushing, and the crushing particle size is controlled at 1-30 microns. Then, the crushed herbal powder is mixed with an appropriate amount of distilled water in a mass ratio of 1:5-1:8 to form a herbal slurry;

[0011] Step 3: Vacuum low-temperature distillation, transfer the herbal slurry to a vacuum distillation device, first evacuate the device to maintain the vacuum degree between -0.08MPa and -0.06MPa, then slowly heat it up, during the heating process, heat it at a slow heating rate of 0.5℃-1℃ / min, the distillation temperature is controlled at 40℃-60℃, and the distillation process lasts for 2-4 hours. At the same time, the distillation device should be equipped with an efficient stirring device, and the stirring rate should be controlled at 50-100 rpm;

[0012] Step 4: Filtration treatment: the condensed and collected distillate is effectively filtered by combining centrifugal filtration with membrane filtration to ensure the purity of the extract;

[0013] Step 5: Concentration and drying: the filtered filtrate is transferred to a vacuum concentration device, and concentrated at a temperature of 45°C-55°C and a pressure of -0.07MPa to -0.05MPa, and the volume of the filtrate is concentrated to 1 / 4-1 / 3 of the original volume. The concentrated extract is then transferred to a vacuum drying oven, and dried at 35°C-45°C and a vacuum degree of -0.09MPa to -0.07MPa, so that the extract is finally dried into a powder or paste product;

[0014] Step 6: Post-processing of the extract: dissolve the dried medicinal bath extract powder or paste product with an appropriate amount of ethanol, and then further separate and purify it through silica gel column chromatography.

[0015] Preferably, when weighing the herbal raw materials in step 1, a high-precision electronic balance device is used, and when rinsing the herbal raw materials, clean water that meets the standards is used.

[0016] Preferably, in the step 1, microwave pretreatment can be performed after the raw material pretreatment, and the air-dried or low-temperature-dried herbal raw materials are placed in a microwave device and irradiated with microwaves at a frequency of 2450 MHz, with a power controlled at 300-600 W and an irradiation time of 2-5 minutes.

[0017] Preferably, the mixing method in step 2 is ultrasonic mixing, and the crushed herbal powder and distilled water are placed in an ultrasonic device. The cavitation effect and mechanical vibration generated by the ultrasound can quickly disperse and fully mix the powder in the liquid. The ultrasonic frequency can be set at 20-50kHz, and the processing time is 10-20 minutes.

[0018] Preferably, the filtering process in step 4 is:

[0019] First, centrifugal filtration is performed, and the distillate collected by distillation is transferred to a high-speed centrifuge, and the centrifuge speed is set to 8000-12000 rpm and the centrifugation time is 15-30 minutes;

[0020] Then membrane filtration is performed, and a microfiltration membrane with a pore size of 0.2-0.5 microns is selected for filtration, and the supernatant after centrifugation is passed through a microfiltration membrane filtration device.

[0021] Preferably, in step five, the temperature needs to be precisely controlled between 45°C and 55°C during operation, and can be monitored and adjusted in real time by a temperature control system. At the same time, the pressure needs to be stably maintained at -0.07MPa to -0.05MPa, using a high-precision pressure sensor.

[0022] Preferably, in step five, an online infrared spectrometer is provided in the distillation apparatus.

[0023] Preferably, in step six, ethanol-water mixed solutions of different proportions are selected, elution is performed at a certain flow rate, the eluate containing the target active ingredient is collected, and finally, the eluate is again concentrated under reduced pressure and vacuum dried.

[0024] Preferably, the surface of the silica gel particles used for silica gel column chromatography in step six is ​​specially modified, and functional groups having specific affinity with the target active ingredient are grafted on the surface, and the loading amount of the functional groups is 0.5-1.5 mmol / g.

[0025] (III) Beneficial effects

[0026] Compared with the prior art, the present invention provides a vacuum low-temperature distillation herbal medicine bath extraction process, which has the following beneficial effects:

[0027] 1. The vacuum low-temperature distillation herbal medicinal bath extract process adopts vacuum low-temperature distillation technology, operates at a vacuum degree of -0.08MPa to -0.06MPa and a distillation temperature of 40℃-60℃, avoids the destruction of heat-sensitive active ingredients in herbs, retains the medicinal efficacy of herbs to the greatest extent, and significantly enhances the therapeutic and health-care effects of medicinal bath extracts, so that the medicinal bath can better play its intended role and meet the users' needs for health and wellness.

[0028] 2. The vacuum low-temperature distillation process of herbal medicinal bath extract, through a combination of centrifugal filtration and membrane filtration, as well as purification methods such as silica gel column chromatography, can comprehensively and effectively remove various impurities, pigments, odors and residual pesticides in the herbal medicinal bath extract, ensuring the purity and safety of the product, greatly reducing skin discomfort, allergic reactions and other problems caused by impurities, improving the user experience of the medicinal bath, and ensuring the health and safety of users.

[0029] 3. The vacuum low-temperature distillation herbal medicinal bath extraction process can accelerate the dissolution of active ingredients through microwave pretreatment in raw material pretreatment and ultrafine grinding and ultrasonic mixing in the grinding and mixing steps, break the constraints of herbal cell structure on the active ingredients, further improve the quality and efficacy of the medicinal bath extract, and give full play to the medicinal value of the herbs. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a process flow chart of vacuum low-temperature distillation of herbal medicinal bath extract proposed by the present invention. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments 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.

[0032] See also Figure 1 , a vacuum low-temperature distillation herbal medicine bath extraction process, comprising the following steps:

[0033] Step 1: Raw material pretreatment, select fresh or dried herbal raw materials, remove impurities, moldy and worm-eaten parts, weigh them according to the formula ratio, rinse them with clean water, and then dry the herbal raw materials with low-temperature drying equipment, control the temperature at 30℃-40℃, and ensure that the water content of the herbs is less than 8%. When weighing the herbal raw materials, use high-precision electronic balance equipment, and when rinsing the herbal raw materials, use clean and standard water; microwave pretreatment can be carried out after raw material pretreatment, place the dried or low-temperature dried herbal raw materials in a microwave equipment, and irradiate them with microwaves with a frequency of 2450MHz, control the power at 300-600W, and the irradiation time is 2-5 minutes. The thermal effect and non-thermal effect generated by microwaves can change the cell structure inside the herbs, accelerate the dissolution of effective ingredients, and also play a certain bactericidal role, reduce the impact of microorganisms on the subsequent extraction process, and improve the quality and safety of medicinal bath extracts.

[0034] Step 2: Crushing and mixing. The pre-treated herbal raw materials are placed in an ultrafine grinder for crushing. The crushing particle size is controlled at 1-30 microns. The specific surface area of ​​the herbal powder after ultrafine crushing is greatly increased, which is conducive to the dissolution of the active ingredients in the subsequent extraction process. For example, when dealing with some herbs with tighter cell structures, ultrafine crushing can better destroy the cell wall, making it easier to release the active ingredients in the cells. During operation, the working parameters of the ultrafine grinder, such as air flow speed, crushing time, etc., need to be accurately adjusted according to the characteristics of the herbs to ensure that the ideal crushing effect is achieved without destroying the active ingredients. Then, the crushed herbal powder is mixed with an appropriate amount of distilled water in a mass ratio of 1:5-1:8 to form a herbal slurry. The mixing method adopts ultrasonic mixing. The crushed herbal powder and distilled water are placed in an ultrasonic device. The cavitation effect and mechanical vibration generated by ultrasound can make the powder quickly dispersed and fully mixed in the liquid. The ultrasonic frequency can be set at 20-50kHz, and the processing time is 10-20 minutes. Compared with traditional stirring mixing, ultrasonic mixing can achieve a more uniform mixing effect in a shorter time, and can promote the initial physical and chemical reaction between some components in the herbal powder and water, which helps to improve the efficiency of subsequent distillation extraction.

[0035] Step 3: Vacuum low-temperature distillation, transfer the herbal slurry to a vacuum distillation device, first evacuate the device to maintain the vacuum degree between -0.08MPa and -0.06MPa, then slowly heat it up, and during the heating process, heat it at a slow heating rate of 0.5℃-1℃ / min, which helps to maintain the stability of the ingredients in the herbs and prevent the decomposition or deterioration of the ingredients due to rapid temperature changes. The distillation temperature is controlled at 40℃-60℃, and the distillation process lasts for 2-4 hours. At the same time, the distillation device should be equipped with an efficient stirring device, and the stirring rate is controlled at 50-100 rpm to ensure that the herbal slurry is heated evenly and promote the full evaporation of the active ingredients. Through this operation, under low temperature and vacuum environment, the active ingredients in the herbs can be evaporated at a lower temperature, avoiding the destruction of heat-sensitive ingredients, and evaporating the volatile active ingredients and some semi-volatile ingredients in the herbs, which are condensed and collected in the condenser;

[0036] Step 4: Filtration treatment. The distillate collected by condensation is effectively filtered by combining centrifugal filtration and membrane filtration to ensure the purity of the extract. The filtration process is as follows: first, centrifugal filtration is performed to transfer the distillate collected by distillation to a high-speed centrifuge. The centrifuge speed is set to 8000-12000 rpm and the centrifugation time is 15-30 minutes. Under the action of high-speed centrifugal force, most of the larger particle impurities in the distillate, such as incompletely distilled herbal residues, mud and sand, will be deposited at the bottom of the centrifuge due to the centrifugal force, thereby achieving preliminary Separation; then membrane filtration is carried out, and a microfiltration membrane with a pore size of 0.2-0.5 microns is selected for filtration. The supernatant after centrifugation passes through the microfiltration membrane filtration device. Driven by a certain pressure difference, tiny particle impurities, some colloid substances and some large molecular impurities in the solution will be retained by the microfiltration membrane, while the effective ingredients can pass through the microfiltration membrane to enter the next process. It can comprehensively and effectively remove various impurities in the herbal bath extract, ensure the purity and safety of the product, provide high-quality raw materials for subsequent concentration and drying processes, and ensure the quality of the final bath product.

[0037] Step 5: Concentration and drying. The filtered filtrate is transferred to a vacuum concentration device and concentrated at a temperature of 45°C-55°C and a pressure of -0.07MPa to -0.05MPa. The filtrate volume is concentrated to 1 / 4-1 / 3 of the original volume. The concentrated extract is then transferred to a vacuum drying oven and dried at 35°C-45°C and a vacuum degree of -0.09MPa to -0.07MPa. The extract is finally dried into a powder or paste product. During the operation, the temperature must be accurately controlled between 45°C and 55°C. It can be monitored and adjusted in real time through a temperature control system. Too high a temperature may cause the heat-sensitive components in the extract to denature or decompose, reducing the efficacy of the medicinal bath extract; too low a temperature will slow down the concentration rate, affecting production efficiency. At the same time, The pressure needs to be stably maintained at -0.07MPa to -0.05MPa, and high-precision pressure sensors and regulating valves are used to ensure this. Excessive pressure fluctuations may cause violent boiling of the solution, resulting in material loss or even damage to the equipment. In addition, the internal components of the concentration device, such as the evaporating coil, condenser, etc., should be checked regularly to ensure that they are clean and scale-free to maintain good heat exchange efficiency and ensure the smooth progress of the concentration process. An online infrared spectrometer is installed in the distillation device, which can monitor the changes in the active ingredients of the herbal slurry during the distillation process in real time, and feed the data back to the control system. The control system automatically adjusts the distillation temperature, vacuum degree and stirring rate based on the feedback data to ensure that the extraction rate of key active ingredients is maintained at the optimal level, and the fluctuation range of the extraction rate of the active ingredients is controlled within ±5%.

[0038] Step six: post-treatment of the extract, dissolving the dried medicinal bath extract powder or paste product with an appropriate amount of ethanol, and then further separating and purifying it through silica gel column chromatography, selecting ethanol-water mixed solutions in different proportions, eluting at a certain flow rate, collecting the eluate containing the target active ingredient, and finally, decompressing and concentrating the eluate and vacuum drying it again to obtain a medicinal bath extract product with higher purity, thereby enhancing its efficacy and stability in medicinal bath applications; the surface of the silica gel particles used for silica gel column chromatography has been specially modified, and functional groups with specific affinity to the target active ingredients have been grafted on its surface, and the loading amount of the functional groups is 0.5-1.5mmol / g. The modified silica gel can significantly enhance the selective adsorption and separation effect of the target active ingredient, thereby increasing the purity of the target active ingredient by 20%-30% on the original basis.

[0039] In summary, the vacuum low-temperature distillation herbal medicinal bath extraction process selects mugwort, lavender and honeysuckle as herbal raw materials and formulates them in a mass ratio of 3:2:1. First, the raw materials are pretreated to carefully remove impurities, mildew and insect-eaten parts. After being accurately weighed by a high-precision electronic balance, they are rinsed with clean water that meets the standards, and then dried at 35°C using low-temperature drying equipment to a moisture content of less than 8%.

[0040] Then the raw materials are crushed and mixed. The pretreated raw materials are placed in an ultrafine grinder. According to the characteristics of these herbs, the air flow velocity is set to 180m / s and the crushing time is set to 8 minutes, so that the crushing particle size reaches 1-30 microns. Then, ultrasonic mixing is used to place the crushed herbal powder and distilled water in an ultrasonic device at a mass ratio of 1:6. The ultrasonic frequency is set to 30kHz and the processing time is 15 minutes to form a uniform herbal slurry.

[0041] Then vacuum low-temperature distillation is carried out, and the herbal slurry is transferred to a vacuum distillation device, evacuated to -0.07MPa, and slowly heated to 50°C at a rate of 0.8°C / min. The distillation process lasts for 3 hours, while the stirring device speed is maintained at 80 rpm. After the distillation is completed, the distillate is condensed and collected.

[0042] For the filtration treatment, the distillate was first centrifuged at 10,000 rpm for 20 minutes in a high-speed centrifuge, and then a microfiltration membrane with a pore size of 0.3 μm was selected to perform membrane filtration at a pressure difference of 0.2 MPa.

[0043] During the concentration and drying stage, the filtrate is concentrated to 1 / 4 of its original volume in a reduced pressure concentration device at a temperature of 50°C and a pressure of -0.06MPa, and then transferred to a vacuum drying oven and dried into a powdery product at 40°C and a vacuum degree of -0.08MPa.

[0044] Finally, the extract was post-processed, and the dried powder was dissolved with an appropriate amount of ethanol, and eluted with a mixed solution of ethanol-water (7:3) at a flow rate of 2 ml / min through silica gel column chromatography, and the target active ingredient eluate was collected, and then concentrated and vacuum dried again. After testing, the purity of the active ingredient in the final product reached 85%, and the impurity content was less than 0.5%, which fully proved the effectiveness and stability of the process of the present invention in this embodiment, and can provide high-quality refined raw materials for medicinal bath products.

[0045] The feasibility and superiority of the present invention are further demonstrated through specific implementation, providing more abundant reference basis for actual production application.

[0046] It should be noted that the term "comprises" or any other variation thereof is intended to cover non-exclusive inclusion, so that a process, method, article, or device that includes a series of elements includes not only those elements, but also includes other elements that are not explicitly listed, or also includes elements inherent to such process, method, article, or device. In the absence of further restrictions, an element defined by the sentence "comprises a ..." does not exclude the presence of other identical elements in the process, method, article, or device that includes the element.

[0047] 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 vacuum low-temperature distillation herbal medicine bath extraction process, characterized in that: The following steps are involved: Step 1: Raw material pretreatment: select fresh or dried herbal raw materials, remove impurities, moldy and insect-infested parts, weigh them according to the formula ratio, rinse them with clean water, and then dry the herbal raw materials in low-temperature drying equipment, control the temperature at 30℃-40℃, and ensure that the moisture content of the herbs is less than 8%; Step 2: crushing and mixing, the pre-treated herbal raw materials are put into an ultra-fine grinder for crushing, and the crushing particle size is controlled at 1-30 microns. Then, the crushed herbal powder is mixed with an appropriate amount of distilled water in a mass ratio of 1:5-1:8 to form a herbal slurry; Step 3: Vacuum low-temperature distillation, transfer the herbal slurry to a vacuum distillation device, first evacuate the device to maintain the vacuum degree between -0.08MPa and -0.06MPa, then slowly heat it up, during the heating process, heat it at a slow heating rate of 0.5℃-1℃ / min, the distillation temperature is controlled at 40℃-60℃, and the distillation process lasts for 2-4 hours. At the same time, the distillation device should be equipped with an efficient stirring device, and the stirring rate should be controlled at 50-100 rpm; Step 4: Filtration treatment: the condensed and collected distillate is effectively filtered by combining centrifugal filtration with membrane filtration to ensure the purity of the extract; Step 5: Concentration and drying: the filtered filtrate is transferred to a vacuum concentration device, and concentrated at a temperature of 45°C-55°C and a pressure of -0.07MPa to -0.05MPa, and the volume of the filtrate is concentrated to 1 / 4-1 / 3 of the original volume. The concentrated extract is then transferred to a vacuum drying oven, and dried at 35°C-45°C and a vacuum degree of -0.09MPa to -0.07MPa, so that the extract is finally dried into a powder or paste product; Step 6: Post-processing of the extract: dissolve the dried medicinal bath extract powder or paste product with an appropriate amount of ethanol, and then further separate and purify it through silica gel column chromatography.

2. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: In the step 1, when weighing the herbal raw materials, a high-precision electronic balance device is used, and when rinsing the herbal raw materials, clean water that meets the standards is used.

3. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: In the step 1, microwave pretreatment can be performed after the raw material pretreatment, and the air-dried or low-temperature-dried herbal raw material is placed in a microwave device and irradiated with microwaves at a frequency of 2450 MHz, with a power controlled at 300-600 W and an irradiation time of 2-5 minutes.

4. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: The mixing method in step 2 adopts ultrasonic mixing, and the crushed herbal powder and distilled water are placed in an ultrasonic device. The cavitation effect and mechanical vibration generated by ultrasound can quickly disperse and fully mix the powder in the liquid. The ultrasonic frequency can be set at 20-50kHz, and the processing time is 10-20 minutes.

5. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: The filtering process in step 4 is as follows: First, centrifugal filtration is performed, and the distillate collected by distillation is transferred to a high-speed centrifuge, and the centrifuge speed is set to 8000-12000 rpm and the centrifugation time is 15-30 minutes; Then membrane filtration is performed, and a microfiltration membrane with a pore size of 0.2-0.5 microns is selected for filtration, and the supernatant after centrifugation is passed through a microfiltration membrane filtration device.

6. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: In step 5, the temperature needs to be precisely controlled between 45°C and 55°C during the operation, and can be monitored and adjusted in real time through a temperature control system. At the same time, the pressure needs to be stably maintained at -0.07MPa to -0.05MPa, using a high-precision pressure sensor.

7. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: In the step 5, an online infrared spectrometer is arranged in the distillation apparatus.

8. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: In the step six, ethanol-water mixed solutions of different proportions are selected, elution is performed at a certain flow rate, and the eluate containing the target effective ingredient is collected. Finally, the eluate is again concentrated under reduced pressure and vacuum dried.

9. The vacuum low-temperature distillation herbal medicine bath extraction process according to claim 1, characterized in that: The surface of the silica gel particles used for silica gel column chromatography in step six is ​​specially modified, and functional groups having specific affinity with the target active ingredients are grafted onto the surface, and the loading amount of the functional groups is 0.5-1.5 mmol / g.

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