A method for preparing an extract of cistanche wine by hydrothermal method

Abstract

The application discloses a kind of Cistanche wine extract water heat method preparation methods, belong to the field of liquor.This application will be dried Cistanche piece first carries out air explosion treatment, then adopts the double system negative pressure extraction of ethanol and water, obtains Cistanche extract.This method innovatively proposes air explosion pretreatment Cistanche, combines negative pressure low-temperature extraction technology effectively improves the extraction efficiency of active ingredient in Cistanche, and under optimal air explosion condition, Cistanche is compared with untreated extraction echinacoside and verbascoside extraction rate is increased by 93.5%, and polysaccharide extraction rate is increased by 92.6%.It is shown that the method of the application can be applied to the preparation of Cistanche wine extract, greatly improves the utilization efficiency of Cistanche medicinal materials, and has potential commercial application value.

Description

Technical Field

[0001] This invention belongs to the field of liqueurs, specifically relating to a hydrothermal method for preparing Cistanche deserticola wine extract. Background Technology

[0002] With the rapid development of the health industry, the application of medicinal and edible herbs in the field of health-preserving liquors continues to expand. Cistanche deserticola, a perennial parasitic herb, is a traditional and precious tonic in my country. It is sweet and salty in taste, warm in nature, and enters the kidney and large intestine meridians. It has the effects of tonifying kidney yang, nourishing essence and blood, and moistening the intestines to relieve constipation, and is known as "desert ginseng." Modern pharmacological studies have confirmed that the core active ingredients of Cistanche deserticola are phenylethanoid glycosides (with echinacoside and verbascoside as marker components), and it is also rich in iridoids, lignans, polysaccharides, flavonoids, and alkaloids, exhibiting clear pharmacological activities in anti-fatigue, anti-oxidation, neuroprotection, immune regulation, and liver and kidney protection. Cistanche deserticola has high safety for long-term consumption, making it a high-quality core raw material for the development of health-preserving liquor products.

[0003] Alcohol, as an excellent solvent for the extraction of traditional Chinese medicine, can significantly promote the dissolution of active ingredients and improve bioavailability. Cistanche deserticola wine is also a core product in the health-preserving liqueur category. Currently, the extraction technologies used in the industrial production of Cistanche deserticola wine and Cistanche deserticola extract can be divided into two main categories: traditional extraction technologies and novel auxiliary extraction technologies. However, all types of technologies have obvious limitations in actual industrial applications, making it difficult to simultaneously meet the multiple core requirements of extraction efficiency, activity retention, production cost, and scalability.

[0004] Among traditional extraction techniques, the maceration method is currently the most commonly used process in the production of Cistanche deserticola wine. It is simple to operate and can preserve the original flavor of the raw materials to the greatest extent, but it has prominent problems such as long extraction cycle, insufficient dissolution of active ingredients, and low utilization rate of medicinal materials. In particular, the cell walls of the fleshy stems of Cistanche deserticola are dense, with high contents of cellulose, hemicellulose, and lignin. The characteristic phenylethanoid glycosides are mostly found in the cell protoplasts. Conventional impregnation is difficult to break through the mass transfer barrier of the dense cell walls, and the extraction rate of its core active ingredients is generally less than 40%, resulting in a serious waste of high-quality medicinal resources. Although percolation can improve the extraction efficiency to a certain extent, it has the disadvantages of large solvent consumption, long production cycle, cumbersome operation, and difficulty in continuous industrial production. Decoction and hot reflux extraction can accelerate the dissolution of components through high temperature, but the core phenylethanoid glycosides of Cistanche deserticola have significant thermal instability. Prolonged high-temperature heating is prone to hydrolysis and oxidative degradation, resulting in a large loss of active ingredients. At the same time, polysaccharide components are prone to high-temperature gelatinization, which seriously affects the clarity of the extract and the quality of the product, making them completely unsuitable for the preparation of high-quality Cistanche deserticola extract.

[0005] Current data shows that other methods for processing Cistanche deserticola into wine include supercritical fluid extraction, Soxhlet extraction, ultrasound-assisted extraction, microwave-assisted extraction, pulsed electric field-assisted extraction, enzyme-assisted extraction, flash extraction, high-speed countercurrent chromatography, aqueous two-phase extraction, and macroporous resin separation and adsorption. However, each method has its advantages and disadvantages. Supercritical fluid extraction has a low throughput, high material consumption, and high cost, making it unsuitable for large-scale production. Soxhlet extraction is generally used in laboratory small-scale research and development. Ultrasound-assisted extraction, microwave-assisted extraction, pulsed electric field-assisted extraction, enzyme-assisted extraction, flash extraction, high-speed countercurrent chromatography, aqueous two-phase extraction, and macroporous resin separation and adsorption are generally expensive and cannot be applied on a large scale. Summary of the Invention

[0006] The purpose of this invention is to provide a hydrothermal method for preparing Cistanche deserticola wine extract. This method innovatively proposes a gas explosion pretreatment of Cistanche deserticola, combined with negative pressure low-temperature extraction technology, which effectively improves the extraction efficiency of active ingredients in Cistanche deserticola. Under optimal gas explosion conditions, the extraction rates of echinacoside and verbascoside from Cistanche deserticola are increased by 93.5% compared to untreated Cistanche deserticola, and the extraction rate of polysaccharides is increased by 92.6%. This indicates that the method of this invention can be applied to the preparation of Cistanche deserticola wine extract, greatly improving the utilization efficiency of Cistanche deserticola medicinal material and possessing potential commercial application value. Furthermore, this invention also has the advantages of high efficiency, speed, stability, and low cost in extraction.

[0007] The present invention discloses a hydrothermal method for preparing Cistanche deserticola wine extract, comprising the following steps:

[0008] Step 1: Cleaning

[0009] After slicing the Cistanche deserticola, rinse it with cold water to remove any residue at the bottom, and then dry it.

[0010] Step 2: Gas Explosion Handling

[0011] Weigh the dried Cistanche deserticola slices and transfer them to the instantaneous air explosion machine. Add a certain amount of water, seal the machine, set the operating parameters, and quickly transfer the Cistanche deserticola material out of the air explosion machine after the operation is completed.

[0012] Step 3: Impregnation Extraction

[0013] A dual-system negative pressure extraction method using ethanol and water was employed. The Cistanche deserticola material obtained by gas explosion was added to the extraction solvent and continuously extracted at low temperature under negative pressure.

[0014] Step 4: Active ingredient detection

[0015] The prepared extract was tested for the content of active ingredients, including phenylethanol glycosides, total flavonoids, and crude polysaccharides, and the extraction efficiency of active ingredients was compared with that of Cistanche deserticola extract without gas explosion treatment.

[0016] In step 2, during the gas explosion operation, weigh 100g of Cistanche deserticola slices and add water in the amount of 25~80wt.

[0017] In step 2, the gas explosion temperature is set to 110~150℃ and maintained for 5~30 minutes. After the time is up, the gas explosion machine is turned off, and the pressure is released instantaneously to complete the gas explosion. The amount of Cistanche deserticola and water added should not exceed 60~80% of the capacity of the high-pressure reactor of the gas explosion machine. The maximum pressure range monitored during the operation of the gas explosion machine is 0.35~1.0 MPa.

[0018] Furthermore, in step 2, the gas explosion temperature is 120~135℃, and the heat preservation and pressure holding time is 10~15min. This parameter range can achieve efficient cell wall disruption while avoiding thermal degradation of phenylethanoid glycosides due to prolonged high-temperature treatment, thus balancing cell wall disruption effect and activity retention.

[0019] In step 3, the extraction solvent is a 50-70% vol solvent prepared with edible alcohol, and the extraction solvent addition ratio is 0.03-0.1 kg / L.

[0020] In step 3, the extraction solvent is a 60% vol ethanol aqueous solution, and the feeding ratio is 0.03 kg / L, that is, every 10L of extraction solvent corresponds to 300g of Cistanche deserticola material after gas explosion treatment.

[0021] In step 3, the extraction temperature is 50~70℃, the negative pressure range is -0.03 to -0.05MPa, and the extraction is carried out continuously for 3 hours.

[0022] Preferably, the extraction efficiency of the active ingredients in the prepared extract can reach up to 63%.

[0023] The above-mentioned hydrothermal method for preparing Cistanche deserticola extract is suitable for the efficient extraction of active ingredients from Cistanche deserticola. It belongs to the application of extracting functional components from plants and has broad application prospects in the fields of health-preserving liqueurs, functional foods, and food additives.

[0024] Compared with the prior art, the beneficial effects of the present invention are reflected in:

[0025] 1. High cell wall breaking efficiency, fundamentally breaking down the mass transfer barrier and significantly improving the utilization rate of medicinal materials. This invention uses instantaneous hydrothermal gas explosion technology to tear apart the tight cell walls and fibrous structure of Cistanche deserticola from the inside of the cells through a purely physical method. No exogenous enzymes or chemical agents are needed, ensuring high food safety. The resistance to dissolution of intracellular active ingredients in the broken-cell material is significantly reduced, and the amount of effective substances dissolved is increased compared to traditional processes, completely solving the problems of insufficient dissolution of active ingredients and low resource utilization in traditional processes.

[0026] 2. Strong process adaptability, directly compatible with existing liquor production lines. The equipment used in this invention are all industrial equipment commonly used in the food and pharmaceutical industries, requiring no additional high investment in specialized equipment. The process flow is simple and controllable, solving the problems of high difficulty in industrial scaling up of new technologies such as ultrasound, microwave, and supercritical fluid, and high equipment investment. It can be directly adapted to the large-scale production of existing liquor production lines.

[0027] 3. The extract is of excellent quality and directly suitable for the development of health-preserving liqueur products. This invention uses an ethanol-water two-phase extraction solvent consistent with the liqueur base liquor system. The resulting extract can be directly used in the blending and production of liqueur products without the need for subsequent complex solvent recovery and purification processes. This avoids the loss of active ingredients and changes in flavor caused by multiple processing steps, while also ensuring the simultaneous dissolution of active ingredients with different polarities, achieving a synergistic unity of product efficacy and flavor. Attached Figure Description

[0028] Figure 1 Figures showing the contents of echinacoside and verbascoside in Cistanche deserticola extract under different gas explosion parameters were prepared. By comparing the phenylethanoid glycoside content in the extract, when the gas explosion temperature did not exceed 140℃, the total amounts of both echinacoside and verbascoside were significantly higher than those in the untreated DZ group (35.2 mg / L). Specifically, at 130℃ (QBRC-3), the contents of both reached 68.1 mg / L, an increase of 93.5% compared to the DZ group.

[0029] Figure 2 The graph shows the crude polysaccharide content in *Cistanche deserticola* extracts prepared under different gas explosion parameters. Compared to the untreated *Cistanche deserticola* extract directly extracted (DZ, 77.3 mg / L), gas explosion temperatures below 140℃ effectively promoted the dissolution of crude polysaccharides. During the gas explosion temperature range of 110℃ to 150℃, the crude polysaccharide content showed a trend of first increasing and then decreasing, reaching a peak of 148.9 mg / L at a gas explosion temperature of 130℃, representing a 92.6% improvement in extraction efficiency compared to the DZ group. With further increases in temperature, the crude polysaccharide content decreased sharply. This was attributed to the charring of *Cistanche deserticola* under high temperature and pressure, which destroyed the structure of the crude polysaccharides.

[0030] Figure 3 Microscopic images show Cistanche deserticola treated with air explosion (QBRC-2) and untreated Cistanche deserticola. It can be seen that after air explosion treatment, most of the cell walls of Cistanche deserticola were disrupted into a disordered state, exhibiting a dispersed, blocky structure, which facilitates the release and flow of intracellular active ingredients, thereby improving extraction efficiency. Detailed Implementation

[0031] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0032] To facilitate understanding of the present invention, the technical solution of the present invention will be further described below with reference to specific embodiments. Unless otherwise specified, the materials, reagents, etc., used in the following embodiments are commercially available. Unless otherwise specified, they are generally used under conventional conditions or according to the conditions recommended by the company.

[0033] Example 1:

[0034] The hydrothermal method for preparing Cistanche deserticola wine extract in this embodiment is as follows:

[0035] Take 100g of dried Cistanche deserticola slices and transfer them to an instantaneous gas explosion machine. Add 75mL of water, fix the machine in place, and set the operating parameters: temperature 110℃, holding time 10min. Turn on the power to perform the gas explosion. Immediately after the operation is complete, turn off the power and open the valve to release the gas-exploded Cistanche deserticola. Repeat the above experiment three times. Combine the gas-exploded Cistanche deserticola slices, transfer them to a non-woven bag, and place them in a 100L explosion-proof basket extraction machine. Add 10L of 60% vol extraction solvent (prepared from commercially purchased edible alcohol diluted with deionized water). Extract continuously at 65℃ under reduced pressure to boiling for 3 hours. After extraction, collect the extract and name it QBRC-1.

[0036] Example 2:

[0037] The hydrothermal method for preparing Cistanche deserticola wine extract in this embodiment is as follows:

[0038] Take 100g of dried Cistanche deserticola slices and transfer them to an instantaneous gas explosion machine. Add 75mL of water, fix the machine in place, and set the operating parameters: temperature 120℃, holding time 10min. Turn on the power to perform the gas explosion. Immediately after the operation is complete, turn off the power and open the valve to release the gas-exploded Cistanche deserticola. Repeat the above experiment three times. Combine the gas-exploded Cistanche deserticola slices, transfer them to a non-woven bag, and place them in a 100L explosion-proof basket extraction machine. Add 10L of 60% vol extraction solvent (prepared from commercially purchased edible alcohol diluted with deionized water). Extract continuously at 65℃ under reduced pressure to boiling for 3 hours. After extraction, collect the extract and name it QBRC-2.

[0039] Example 3:

[0040] The hydrothermal method for preparing Cistanche deserticola wine extract in this embodiment is as follows:

[0041] Take 100g of dried Cistanche deserticola slices and transfer them to an instantaneous gas explosion machine. Add 75mL of water, fix the machine in place, and set the operating parameters: temperature 130℃, holding time 10min. Turn on the power to perform the gas explosion. Immediately after the operation is complete, turn off the power and open the valve to release the gas-exploded Cistanche deserticola. Repeat the above experiment three times. Combine the gas-exploded Cistanche deserticola slices, transfer them to a non-woven bag, and place them in a 100L explosion-proof basket extraction machine. Add 10L of 60% vol extraction solvent (prepared from commercially purchased edible alcohol diluted with deionized water). Extract continuously at 65℃ under reduced pressure to boiling state for 3 hours. After extraction, collect the extract and name it QBRC-3.

[0042] Example 4:

[0043] The hydrothermal method for preparing Cistanche deserticola wine extract in this embodiment is as follows:

[0044] Take 100g of dried Cistanche deserticola slices and transfer them to an instantaneous gas explosion machine. Add 75mL of water, fix the machine in place, and set the operating parameters: temperature 140℃, holding time 10min. Turn on the power to perform the gas explosion. Immediately after the operation is complete, turn off the power and open the valve to release the gas-exploded Cistanche deserticola. Repeat the above experiment three times. Combine the gas-exploded Cistanche deserticola slices, transfer them to a non-woven bag, and place them in a 100L explosion-proof basket extraction machine. Add 10L of 60% vol extraction solvent (prepared from commercially purchased edible alcohol diluted with deionized water). Extract continuously at 65℃ under reduced pressure to boiling for 3 hours. After extraction, collect the extract and name it QBRC-4.

[0045] Example 5:

[0046] The hydrothermal method for preparing Cistanche deserticola wine extract in this embodiment is as follows:

[0047] Take 100g of dried Cistanche deserticola slices and transfer them to an instantaneous gas explosion machine. Add 75mL of water, fix the machine in place, and set the operating parameters: temperature 150℃, holding time 10min. Turn on the power to perform the gas explosion. Immediately after the operation is complete, turn off the power and open the valve to release the gas-exploded Cistanche deserticola. Repeat the above experiment three times. Combine the gas-exploded Cistanche deserticola slices, transfer them to a non-woven bag, and place them in a 100L explosion-proof basket extraction machine. Extract continuously at 65℃ under reduced pressure until boiling for 3 hours. After extraction, collect the extract and name it QBRC-5.

[0048] Comparative Example 1:

[0049] Take 300g of dried Cistanche deserticola slices, transfer them to a non-woven bag, and then transfer them to a 100L explosion-proof hanging basket extraction machine. Add 10L of 60% vol extraction solvent (prepared from commercially purchased edible alcohol diluted with deionized water), and extract continuously at 65℃ under reduced pressure to boiling for 3 hours. After extraction, collect the extract and name it DZ.

[0050] Example 6: Detection of phenylethyl glycosides (echinacoside and verbascoside) and crude polysaccharides in Cistanche deserticola extract

[0051] (a) Detection of phenylethanoid glycoside content in extract

[0052] According to the 2025 edition of the Chinese Pharmacopoeia, high-performance liquid chromatography (HPLC) was used for determination. An appropriate amount of well-mixed sample was weighed, filtered through a membrane, and then analyzed using the HPLC.

[0053] The content of phenylethanoid glycosides is calculated using the formula:

[0054] Where: the total amount of target substance in the sample W (mg / L), the concentration of target substance in the sample test solution C (mg / L), the concentration of target substance in the blank control C0 (mg / L), the volume of the final volume V (ml), the dilution factor N, and the sample volume m (ml).

[0055] (II) Method for detecting crude polysaccharide content in extract

[0056] Weigh 5g of the sample, add 5mL of water, vortex, then add 20mL of anhydrous ethanol, sonicate for 30min, centrifuge, wash the precipitate with 80% ethanol for 30min, centrifuge again, add water to the precipitate, sonicate for 90min, and bring the volume to 50mL. Take the solution, add to 1mL, add 1mL of phenol solution, add 5mL of sulfuric acid, and let stand for 10min. Mix well, incubate in a 30℃ water bath for 20min, and determine the colorimetric value at 490nm. The crude polysaccharide content of the sample is calculated as follows:

[0057]

[0058] The mass m1 of crude polysaccharide in the sample solution (converted from the absorbance value of the spectrophotometer), the total volume V1 (mL) of the treatment solution, the mass m (g) of the sample, and the total volume V1 (mL) of the treatment solution.

Claims

1. A hydrothermal method for preparing Cistanche deserticola wine extract, characterized in that: The dried Cistanche deserticola slices were first subjected to gas explosion treatment, and then extracted using a dual-system negative pressure extraction of ethanol and water to obtain Cistanche deserticola extract.

2. The preparation method according to claim 1, characterized in that... Includes the following steps: Step 1: Cleaning After slicing the Cistanche deserticola, rinse it with cold water to remove the residue at the bottom, and then dry it. Step 2: Gas Explosion Handling Weigh the dried Cistanche deserticola slices and transfer them to the instantaneous air explosion machine. Add a certain amount of water, seal the machine, set the operating parameters of the air explosion machine, and quickly transfer the Cistanche deserticola material out of the air explosion machine after the operation is completed. Step 3: Impregnation Extraction A dual-system negative pressure extraction method using ethanol and water was employed. The Cistanche deserticola material obtained by gas explosion was added to the extraction solvent and continuously extracted at low temperature under negative pressure to obtain Cistanche deserticola extract.

3. The preparation method according to claim 2, characterized in that: In step 2, during the gas explosion operation, weigh 100g of Cistanche deserticola slices and add 25~80wt% of water.

4. The preparation method according to claim 2, characterized in that: In step 2, the gas explosion temperature is set to 110~150℃ and maintained for 5~30 minutes.

5. The preparation method according to claim 4, characterized in that: In step 2, the gas explosion temperature is 120~135℃, and the heat preservation and pressure holding time is 10~15min.

6. The preparation method according to claim 2, characterized in that: In step 3, the extraction solvent is a 50-70% vol solvent prepared with edible alcohol, and the extraction solvent addition ratio is 0.03-0.1 kg / L.

7. The preparation method according to claim 6, characterized in that: In step 3, the extraction temperature is 50~70℃, the negative pressure range is -0.03 to -0.05MPa, and the extraction is carried out continuously for 3 hours.

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