Cistanche deserticola honey dew and preparation method thereof

Through combined enzymatic lysis and ultrasonic extraction combined with segmented concentration technology, the problems of low extraction rate of effective ingredients and easy degradation of heat-sensitive substances in the Cistanche extraction process are solved, efficient extraction and stability improvement are achieved, and the shelf life of the product is extended.

CN120360264AInactive Publication Date: 2025-07-25AKSU DESERT HUYANG YUNYOUNONG CO LTD
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Patent Information

Application Number
CN202510560512.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-30
Publication Date
2025-07-25
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The current Cistanche extraction process has low extraction rate of active ingredients, easy degradation of heat-sensitive active substances, and high-temperature processing of honey leads to loss of enzyme activity, affecting product quality and stability.

Method used

Compound enzymatic decomposition combined with ultrasonic extraction and segmented vacuum concentration technology is used to destroy the cell wall by synergistically acting cellulase, pectinase and xylanase, combined with ultrasonic cavitation to enhance mass transfer, extract active ingredients under low temperature conditions, and reduce the loss of thermally sensitive ingredients through segmented concentration, and finally mix it with honey and composite antioxidants to improve stability.

Benefits of technology

It improves the extraction and retention rate of active ingredients in Cistanche, avoids nutritional losses caused by high temperature treatment, and enhances the stability and shelf life of the product.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the field of food processing, and particularly relates to a preparation method of cistanche honeydew. The method comprises the following steps: (1) pretreating raw materials, preparing a compound enzyme for enzymolysis, then carrying out ultrasonic extraction, and concentrating to prepare a cistanche extracting solution; and (2) uniformly mixing the cistanche extracting solution, honey and a compound antioxidant in proportion to obtain the cistanche honeydew. According to the method, enzyme-ultrasonic synergistic interaction and sectional concentration technical means are utilized, so that the extraction rate and retention rate of active ingredients in cistanche are increased, nutrient loss caused by high-temperature treatment is avoided, the stability of a final product is enhanced, and the shelf life is prolonged.
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Description

Technical Field

[0001] The present invention belongs to the field of food processing, and particularly relates to a preparation method of cistanche deserticola honeydew. Background Art

[0002] Cistanche deserticola, an annual parasitic plant, is distributed across North America and East Asia. Its unique form can often be found in the sandy soil environments of the United States and northeastern China. It is worth noting that China plays a crucial role in the global production of cistanche deserticola and is recognized as the main producing area of cistanche deserticola in the world. Cistanche deserticola has a long history of food and medicine use. Modern scientific research shows that the extracts of cistanche deserticola contain a variety of chemical components, among which alkaloids, phenyl ethanol glycosides and other components are particularly prominent. Among these components, echinacoside and acteoside (verbascoside) play a crucial role as the main active ingredients, endowing cistanche deserticola with unique value.

[0003] In the published technical solutions, there is room for optimization in the extraction process of cistanche deserticola. First, the extraction rate of active ingredients is not satisfactory. Key components such as phenyl ethanol glycosides and polysaccharides are difficult to extract efficiently, which greatly limits the full utilization of cistanche deserticola resources. Second, there are some heat-sensitive active substances in cistanche deserticola. During the conventional extraction process, due to the difficulty of temperature control, these substances are extremely prone to degradation, seriously affecting the quality and efficacy of the extracts. In addition, during the high-temperature processing stage, honey, a commonly used auxiliary material in the extraction process, will suffer a loss of enzyme activity and its flavor will also deteriorate significantly, further reducing the quality of the final product. These problems urgently require the joint efforts of scientific researchers and relevant industry practitioners to explore a more optimized and efficient extraction process to fully tap the potential value of cistanche deserticola. Summary of the Invention

[0004] The technical solution of the present invention aims at the technical problems such as low extraction rate of traditional active ingredients, easy degradation of heat-sensitive active substances, and loss of enzyme activity caused by high-temperature processing of honey, and provides a preparation method of cistanche deserticola honeydew.

[0005] The main purposes of the present invention are as follows: One, to improve the extraction efficiency and retention rate of active ingredients in cistanche deserticola; Two, to prevent the loss of nutrients caused by high-temperature treatment of honey; Three, to improve the stability of the final product and extend its shelf life.

[0006] To achieve the above purposes, the present invention adopts the following technical solutions.

[0007] A preparation method of cistanche deserticola honeydew, The method includes: (1)Pre-treat the raw materials, configure a compound enzyme for enzymatic hydrolysis, then perform ultrasonic extraction, and concentrate to obtain a cistanche deserticola extract; (2)Mix the cistanche deserticola extract, honey, and compound antioxidant evenly in proportion to obtain cistanche deserticola honeydew.

[0008] Preferably, the raw materials in step (1) are cistanche deserticola; The pre-treatment of the raw materials in step (1) is to dry and crush cistanche deserticola to 80 - 100 meshes, and then mix it evenly with a citric acid - disodium hydrogen phosphate buffer solution with a pH value of 5.2 - 5.8 according to a mass ratio of 1:(18 - 22).

[0009] Preferably, the compound enzyme in step (1) includes cellulase, pectinase, and xylanase; The dosage of the compound enzyme activity is 2000 - 2400 U / g of raw materials, and cellulase, pectinase, and xylanase are mixed according to an activity ratio of (2.5 - 3.5):1:(0.3 - 0.5).

[0010] Preferably, In the enzymatic hydrolysis process in step (1), control the enzymatic hydrolysis temperature at 40 - 50 °C and the enzymatic hydrolysis duration at 1.5 - 2.5 h.

[0011] Preferably, In the ultrasonic extraction process in step (1), control the extraction temperature at 55 - 65 °C, the ultrasonic frequency at 40 - 50 kHz, the power at 500 - 600 W, and the extraction duration at 20 - 30 min.

[0012] Preferably, The concentration in step (1) adopts multi-stage vacuum concentration. During the concentration process, control the relative vacuum degree at -0.095 - 0.050 MPa. In the first stage, control the concentration temperature at 45 - 55 °C and concentrate to 30 - 35 %VOL of the original volume. In the second stage, control the concentration temperature at 35 - 45 °C until solid matter just begins to precipitate to form a concentrated stock solution. At this time, a small amount of potable water accounting for 1 - 3 wt% of the concentrated stock solution, such as pure water, deionized water, etc., can be added during processing, and stirring can be used to accelerate the dissolution of the solid matter. It can also be restored to normal pressure to allow it to dissolve naturally, but the natural dissolution rate is slow, and even with stirring, the efficiency is relatively low, and there may be a situation where it cannot be completely dissolved. Therefore, at present, industrial production processes usually recommend adding a small amount of potable water to avoid affecting the concentration of active ingredients and as much as possible accelerate the processing efficiency to ensure both quality and quantity.

[0013] Preferably, The composite antioxidant in step (2) is a combined antioxidant of tea polyphenols and vitamin E, wherein the mass ratio of tea polyphenols to vitamin E is (1.8-2.2):1.

[0014] As a preference, In step (2), the Cistanche deserticola extract, honey and composite antioxidant are uniformly mixed in a mass ratio of 1: (1.5-2): 0.15.

[0015] As a preference, The uniform mixing process in step (2) is to obtain the Cistanche deserticola honey dew by stirring at a speed of 1500-2000 rpm for 10-20 min under the conditions of a temperature of 30-40°C and an ambient pressure of 350-400 MPa.

[0016] A kind of Cistanche honeydew.

[0017] The core of the technical solution of the present invention is to use a composite enzyme to specifically decompose the polysaccharide structure of the cell wall of Cistanche deserticola, release the intracellular active ingredients, reduce the energy consumption of subsequent extraction, and cooperate with the ultrasonic cavitation effect to enhance mass transfer, avoid the thermal decomposition of phenylethanoid glycosides under low temperature conditions, and improve the extraction rate and retention rate of the active ingredients in Cistanche deserticola.

[0018] The present invention uses a cellulase-pectinase-xylanase complex enzyme system. This system is based on the principle of precise stereo conformation matching between enzyme molecules and cell wall polysaccharides, and can specifically cut off β-1,4 glycosidic bonds, thereby effectively deconstructing the complex reticular skeleton structure of lignified cell walls. Cellulase can accurately and directionally hydrolyze the β-1,4-glycosidic bonds on the surface of microfibers by constructing β-glucan binding sites in its catalytic domain, thereby destroying the highly ordered hydrogen bond network structure of the cellulose crystal region. Weakening the stability of the cellulose structure creates favorable conditions for the subsequent release of active ingredients. Pectinase mainly acts on rhamnogalacturonan (pectin), and by cleaving the α-1,4 bonds therein, it can effectively dissociate the tightly connected intercellular layer structure at the corners of cells. As an important connection area between cells, the dissociation of the structure of the intercellular layer helps separate cells and provides a smoother path for the active ingredients to diffuse from the inside of the cell to the outside. With its unique substrate recognition ability, xylanase can specifically recognize the reducing end of the xylan main chain and hydrolyze the β-1,4-xylosidic bond through a double displacement mechanism. The hydrolysis process significantly increases the permeability of the cell wall and cell membrane, greatly promoting the dissolution of intracellular active ingredients to the outside of the cell.

[0019] However, for the technical solution of the present invention, it is necessary to strictly control the relative dosages of the three substrates. One lies in the substrate competition among the enzymes, with pectinase at the core, and the substrate competition relationship it forms is particularly significant. Cellulase and pectinase act on cellulose and pectin respectively. In the actual plant cell wall, components such as cellulose and pectin are intertwined with each other to form a complex network structure. During the enzymatic hydrolysis process, cellulase and pectinase may compete for the active sites due to their specific recognition of the substrates. For example, when cellulase and pectinase act on a region where cellulose and pectin are tightly connected at the same time, there will be a situation where the two enzymes compete for the substrates, thus affecting their respective enzymatic hydrolysis efficiencies. Xylanase and pectinase act on xylan and pectin respectively, and pectin and xylan may also interact with each other or jointly form certain structural regions. Therefore, substrate competition is also likely to occur between these two enzymes during enzymatic hydrolysis, resulting in the degradation efficiency of their respective substrates being affected. Moreover, the filtered xylanase may over-hydrolyze xylan, damaging its structural integrity and affecting the quality of the extract. In addition, small molecule sugars such as glucose produced by cellulase may inhibit the activities of pectinase or xylanase; products such as galacturonic acid produced by pectinase may inhibit cellulase or xylanase; products such as xylose produced by xylanase may also affect the other two enzymes. This feedback inhibition effect will further exacerbate the competition among the enzymes and reduce the enzymatic hydrolysis efficiency. Therefore, to ensure the most efficient enzymatic hydrolysis, it is necessary to relatively strictly control the dosage ratios of the three enzymes, and it is most appropriate to construct an appropriate range with pectinase as the core because pectinase has a more direct potential competition with the other two enzymes. Only when the three active enzymes cooperate synergistically can the destruction of the cell wall structure be achieved most effectively and efficiently, achieving a synergistic balance and reaching the best enzymatic hydrolysis extraction effect.

[0020] From the perspective of the target extract, in the case of effective synergy of the three enzymes, while achieving efficient enzymatic hydrolysis, it is also necessary to avoid the occurrence of over-enzymatic hydrolysis. For example, if the dosage of cellulase is too much, it may change the composition and structure of the extract. Another example is that if the dosage of xylanase is too much, it may cause over-hydrolysis of xylan, affecting the degree of polymerization and biological activity of components such as xylan in the extract.

[0021] In addition, the present invention introduces an ultrasonic cavitation field enhanced mass transfer technology. Under the action of ultrasonic waves, a large number of cavitation bubbles will be generated in the solution. When these cavitation bubbles collapse, extremely high temperatures and pressures will be generated instantaneously. Such extreme physical conditions can induce the formation of local turbulence at the boundary layer, and then generate a micro-jet effect. The powerful impact force of the micro-jet is sufficient to destroy the electrochemical diffusion layer and eliminate the resistance barrier for mass diffusion. At the same time, transient permeable pores will be formed on the cell membrane surface due to the impact of the collapse of cavitation bubbles. The appearance of these pores is like opening a "fast channel" for the exchange of substances inside and outside the cell, which is greatly beneficial to improving the transmembrane diffusion rate of intracellular substances, thereby significantly improving the extraction efficiency of the active ingredients of Cistanche deserticola.

[0022] Another core of the technical solution of the present invention is that the loss of heat-sensitive components in the active ingredients is reduced by using segmented vacuum concentration. The segmented vacuum concentration stability control technology of the present invention is based on the principle of coordinated regulation of polymer solution phase transition kinetics and thermodynamics, and through strict control of temperature and pressure, it realizes precise intervention in the conformational evolution of polysaccharide molecules in the active ingredients and the glass transition of the solution system. In the initial concentration stage, the saturated vapor pressure difference is set to induce phase change, so that free water can escape first, and the molecular filtering effect is formed by high steam passing density, which prompts most of the free water to complete directional migration. At this stage, the dissociation barrier of free water-bound water can be broken through, while maintaining the solution temperature below the glass transition temperature of the polysaccharide molecular chain, effectively inhibiting the entanglement tendency of the molecular chain. The secondary concentration stage adopts progressive vacuum gradient regulation to reduce the water activity by reducing the kinetic energy input of the system. In addition, the free volume fraction is regulated in a vacuum environment, forcing the polysaccharide molecules to adopt an extended conformation and reduce the segment mobility, thereby blocking the random recombination path of the β-1,4-glycosidic bond.

[0023] Compared with the traditional single-stage high-temperature concentration, the present invention forms a dynamic thermal relaxation process by establishing a dual temperature window. The high-throughput dehydration in the first stage allows the system to quickly cross the critical concentration and shorten the residence time of the solution in the high reaction activity range; the second stage is operated at a subcritical temperature to construct a liquid crystal phase structure at the gas-liquid interface. The interface phase changes the water evaporation path from bulk diffusion-dominated to surface laminar flow-controlled, avoiding conformational distortion of the polymer chain caused by turbulent stretching. The synchronously formed double electric layer structure further stabilizes the colloidal system through the steric hindrance effect. The technical system in this scheme achieves the "freezing" effect of the polysaccharide molecular chain conformation during the non-equilibrium concentration process through the precise decoupling of the thermodynamic driving force and the molecular motion ability, so that the batch difference rate of the product intrinsic viscosity is small, so that the stability of the target active ingredient is improved, and the precipitation of solids is a relatively iconic macroscopic phenomenon, and it can avoid the influence of the advantages and disadvantages of different batches of Cistanche deserticola raw materials, which is convenient for industrial production to control product quality.

[0024] Then, the present invention finally mixes the Cistanche extract with honey and a composite antioxidant, which can improve the flavor characteristics of the honeydew. The natural sweetness and unique flavor of honey can optimize the flavor and taste of the honeydew. Secondly, it can also synergize with the polysaccharides and other components in the Cistanche extract to improve the efficacy of the honeydew as a whole. However, too much honey may make the solution too viscous, and may even cause some components to further precipitate during storage. Excessive use of the composite antioxidant may also cause an imbalance in the redox reaction in the system, affecting the stability of other components in the Cistanche extract.

[0025] The advantages of the technical solution of the present invention are as follows: By using the synergistic effect of enzyme-ultrasound and the segmented concentration technology, the extraction rate and retention rate of active ingredients in Cistanche deserticola are improved, the nutritional loss caused by high-temperature treatment is avoided, the stability of the final product is enhanced, and the shelf life is extended. Detailed implementation manners

[0026] The following further clearly and detailedly describes the present invention in combination with specific embodiments. Those of ordinary skill in the art will be able to implement the present invention based on these descriptions. In addition, the embodiments of the present invention involved in the following description are usually only a part of the embodiments of the present invention, rather than all the embodiments. Therefore, all other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of protection of the present invention.

[0027] Unless otherwise specified, the raw materials used in the embodiments of the present invention are all commercially available or raw materials that can be obtained by those skilled in the art; unless otherwise specified, the methods used in the embodiments of the present invention are all methods mastered by those skilled in the art.

[0028] Unless otherwise specified, the Cistanche deserticola used in the embodiments and comparative examples of the present invention is raw materials of the same batch.

[0029] Example 1: A method for preparing Cistanche deserticola honeydew The method includes: (1) After drying Cistanche deserticola, it is pulverized to 80 meshes, and then the Cistanche deserticola powder is evenly mixed with a citric acid-disodium hydrogen phosphate buffer solution with a pH of 5.5 according to a mass ratio of 1:18 to form a pretreated raw material. Cellulase, pectinase, and xylanase are evenly mixed according to an activity ratio of 2.5:1:0.3 to form a composite enzyme, and the composite enzyme is added according to an enzyme activity of 2000 U / g of raw material, and enzymolysis is carried out for 2.5 h under environmental conditions of a temperature of 40 °C to form an enzymolysis solution; (2) The enzymolysis solution is ultrasonically extracted for 30 min in an environment with a temperature of 55 °C, an ultrasonic frequency of 40 kHz, and a power of 500 W, and then after filtering and separating the solid filter residue, the filtrate is subjected to multi-stage vacuum concentration. In the first stage, the filtrate is concentrated to 30 %VOL of the original volume in an environment with a temperature of 45 °C and a relative vacuum degree of -0.095 MPa; in the second stage, it is concentrated in an environment with a temperature of 35 °C and a relative vacuum degree of -0.095 MPa until solid matter just starts to precipitate to form a concentrated stock solution, and 2 wt% of pure water based on the concentrated stock solution is added and stirred to dissolve the solid matter to form a Cistanche deserticola extract; (3) Tea polyphenols and vitamin E are evenly mixed according to a mass ratio of 1.8:1 to form a composite antioxidant; (4) Mix the extract of Cistanche deserticola, honey, and the compound antioxidant evenly at a mass ratio of 1:1.5:0.15, and stir for 20 min in an environment with a temperature of 30 °C, a pressure of 400 MPa, and a rotation speed of 1500 rpm to prepare Cistanche deserticola honeydew.

[0030] Since an important core of the present invention is to avoid the influence of the heat treatment process during processing on the effectiveness of materials and components, and enzymes are a type of easily inactivated component, the present invention first detects the retention rate of enzyme activity in the product Cistanche deserticola honeydew. Referring to GB 14963-2011, the amylase and catalase activities of honey before processing are respectively detected and characterized and recorded as the enzyme activity data before processing, and the amylase and catalase activities in the finished product Cistanche deserticola honeydew are characterized. After converting the relationship between the amount of honey used in the Cistanche deserticola honeydew finished product, it is recorded as the enzyme activity data after processing (that is, converted to the enzyme activity data of the honey component in the Cistanche deserticola honeydew after processing, and other material components will not interfere with this enzyme activity data). Calculate the enzyme activity retention rate = (enzyme activity after processing / enzyme activity before processing) × 100%. The results are shown in the following table.

[0031]

[0032] It can be seen that the mixing and processing process of the extract, honey, and antioxidant of the present invention basically does not cause thermal damage to the active ingredients.

[0033] In addition, comprehensive product testing is carried out on the product Cistanche deserticola honeydew of the present invention, including product stability, physicochemical composition testing, and safety testing.

[0034] Among them, the stability test is based on the color difference test and comprehensively judged in combination with the component analysis of the physicochemical composition test. The safety test includes microbial indicators. For the microbial indicators, mainly refer to the "General Principles of Microbiological Examination of Food Hygiene in National Food Safety Standards" (GB4789.1-2016). If the standard is met, it is marked as ○.

[0035] The test is carried out in a simulated environment with a temperature of 40 °C, a relative humidity of 80%, and a light condition of 5000 lux. The product is placed in this environment for 90 d, and characterization is carried out every 30 d after the 0 d characterization.

[0036] The test results are shown in the following table.

[0037]

[0038] As can be seen from the above indicators, the honeydew product of the present invention has good safety, and on this basis, has very excellent stability. Thanks to the unique concentration and extraction process of the present invention, it can be seen that the contents of the three main active ingredients, phenyl ethanol glycosides, polysaccharides and flavonoids, after being stored for 90 days in a relatively extremely harsh storage environment, the component retention rates reach about 83.8%, 86.3% and 74.4% respectively, showing extremely high stability. Compared with the conventional cistanche deserticola extract or the finished honeydew of cistanche deserticola, in the present invention, during the extraction and concentration process, the conformation of the active ingredients is stabilized, making it not easy to cause losses. Even the loss rate after 90 days is lower than the loss rate of the conventional product after 30 days, showing very excellent stability. Moreover, in terms of the content of active ingredients, in the extraction process and the overall preparation process of the present invention, the temperature is strictly controlled and the extraction is fully and effectively realized. As a result, in the cistanche deserticola honeydew product added with honey and compound antioxidants, the contents of the three main valuable ingredients, phenyl ethanol glycosides, polysaccharides and flavonoids, are even close to those of high-quality cistanche deserticola extracts. That is, after dilution and flavoring, its actual nutritional value can even catch up with the currently commercially available high-quality cistanche deserticola concentrated extracts.

[0039] Example 2: A preparation method of cistanche deserticola honeydew, The method includes: (1) After drying cistanche deserticola, it is pulverized to 90 meshes, and then the cistanche deserticola powder is uniformly mixed with a citric acid-disodium hydrogen phosphate buffer solution with a pH of 5.5 according to a mass ratio of 1:20 to prepare a pretreatment raw material. Cellulase, pectinase and xylanase are uniformly mixed according to an activity ratio of 3:1:0.4 to prepare a compound enzyme, and the compound enzyme is added according to an enzyme activity of 2200 U / g of raw material, and enzymolysis is carried out for 2 h under the environmental condition of a temperature of 45 °C to prepare an enzymolysis solution; (2) The enzymolysis solution is ultrasonically extracted for 25 min in an environment with a temperature of 60 °C, an ultrasonic frequency of 45 kHz and a power of 550 W, and then the solid filter residue is filtered and separated, and the filtrate is subjected to multi-stage vacuum concentration. In the first stage, the filtrate is concentrated to 33%VOL of the original volume in an environment with a temperature of 50 °C and a relative vacuum degree of -0.07 MPa; in the second stage, it is concentrated in an environment with a temperature of 40 °C and a relative vacuum degree of -0.07 MPa until solid matter just begins to precipitate to form a concentrated stock solution, and 2 wt% of pure water is added to the concentrated stock solution and stirred to dissolve the solid matter to prepare a cistanche deserticola extract; (3) Tea polyphenols and vitamin E are uniformly mixed according to a mass ratio of 2:1 to prepare a compound antioxidant; (4) Mix the cistanche deserticola extract, honey, and compound antioxidant evenly at a mass ratio of 1:1.75:0.15, and stir for 15 min in an environment with a temperature of 35 °C, a pressure of 400 MPa, and a rotation speed of 1750 rpm to prepare cistanche deserticola honeydew.

[0040] Perform the same characterization on the cistanche deserticola honeydew product prepared in this example as in Example 1, and the characterization results are shown in the following table.

[0041]

[0042] Example 3: A preparation method of cistanche deserticola honeydew, The method includes: (1) Dry and crush cistanche deserticola to 100 mesh, then mix the cistanche deserticola powder with a citric acid-disodium hydrogen phosphate buffer solution with a pH of 5.5 evenly at a mass ratio of 1:22 to make a pretreatment raw material. Mix cellulase, pectinase, and xylanase evenly at an activity ratio of 3.5:1:0.5 to make a compound enzyme, and add the compound enzyme according to an enzyme activity of 2400 U / g of raw material, and enzymolyze for 1.5 h under environmental conditions of 50 °C to make an enzymolysis solution; (2) Perform ultrasonic extraction on the enzymolysis solution for 20 min in an environment with a temperature of 65 °C, an ultrasonic frequency of 50 kHz, and a power of 600 W. Then, filter and separate the solid filter residue, and perform multi-stage vacuum concentration on the filtrate. In the first stage, concentrate the filtrate to 35 %VOL of the original volume in an environment with a temperature of 55 °C and a relative vacuum degree of -0.05 MPa; in the second stage, concentrate to just start to precipitate solids to form a concentrated stock solution at a temperature of 45 °C and a relative vacuum degree of -0.05 MPa, add 2 wt% of pure water based on the concentrated stock solution and stir to dissolve the solids to make a cistanche deserticola extract; (3) Mix tea polyphenols and vitamin E evenly at a mass ratio of 2.2:1 to make a compound antioxidant; (4) Mix the cistanche deserticola extract, honey, and compound antioxidant evenly at a mass ratio of 1:2:0.15, and stir for 10 min in an environment with a temperature of 40 °C, a pressure of 400 MPa, and a rotation speed of 2000 rpm to prepare cistanche deserticola honeydew.

[0043]

[0044] Comparing Examples 2 and 3 with Example 1, the cistanche deserticola honeydew products prepared by the technical solution of the present invention have high consistency in traits and quality, stable product quality, are suitable for industrial processing and production, and can effectively ensure that the product quality can always be maintained well.

[0045] Comparative Example 1: To verify the effect of the composite enzyme system on the extraction effect, the present invention conducted a compound horizontal comparison test in the early R & D stage of the scheme. The following supplements and reproduces the compound horizontal comparison test to prove the significant effect of the composite enzyme on the extraction effect. Except for the composite enzyme, the whole processes of steps (1) and (2) in Example 2 were referred to, and the operating parameters were controlled to be the same. The specific grouping is shown in the following table.

[0046]

[0047] The prepared Cistanche deserticola extraction solutions of the above experimental groups were characterized. The characterization included the yield of active ingredients and the content of main target components. The characterization results are shown in the following table.

[0048]

[0049] It can be clearly seen from the above table that for the enzymatic hydrolysis extraction process of the present invention, the overall extraction yield can be extremely effectively improved. Compared with the existing yield of 40 - 60%, there is a relatively significant improvement effect. On the other hand, in the technical solutions disclosed by the current process level, the generally achievable critical concentration of phenylethanoid glycosides in the ultra-concentrated extraction solution is about 29.7%, and for polysaccharides, due to significant losses that may occur during the extraction and concentration processes, such as precipitation or conversion and decomposition, the highest concentration is about 26.2%. This is mainly due to a large amount of loss during the concentration process, and the flavonoids are generally below 5%. The present invention greatly improves the efficiency and effect of enzymatic hydrolysis extraction through composite enzymatic hydrolysis, and cooperates with an effective and unique concentration process to greatly improve the efficiency and effect of concentration. A large number of target components are effectively retained, while non-target components can be effectively removed to greatly increase the content of core target components.

[0050] It can be clearly seen from the first batch of supplementary experimental groups (Control Group 1 - Control Group 9) that, with the amount of the complex enzyme (the amount of complex enzyme in the table) remaining unchanged, different enzyme ratios will have a significant impact on the component yield of the intermediate product of the cistanche extract and the concentration of the target component. For example, with the ratio of pectinase and xylanase remaining unchanged, using too little cellulase will lead to a weakened synergistic balance effect of the enzymes, and both the overall yield and the content of the target component will decrease. Using too much cellulase will also lead to a weakened synergistic balance effect of the enzymes, but in Control Group 4, it is obvious that the polysaccharide content has decreased more significantly. Since cellulase has the ability to decompose polysaccharides, the decrease in polysaccharide content is more significant. Although the overall decrease in the yield is slightly smaller, the polysaccharide content has decreased significantly. Similarly, using too much or too little xylanase will also disrupt the synergistic balance of the enzymes, resulting in fluctuations in the yield, and a relatively unique phenomenon has occurred. Generally speaking, although xylanase theoretically also has the ability to decompose polysaccharides, its decomposition ability is weaker than that of cellulase. However, from Control Group 5 to Control Group 9, an opposite phenomenon can be found, that is, it seems that xylanase has a greater impact on the polysaccharide content, which does not conform to the original expectation. After this situation occurred and the data was repeatedly verified to be correct, the R & D personnel consulted the literature and conducted relevant verification tests and believed that this situation is indeed related to the decomposition ability of the enzymes themselves. However, due to the relationship of substrate competition between xylanase and cellulase, when the relative amount of xylanase is too much, the released polysaccharides are more likely to be decomposed by cellulase. That is, during the enzymatic hydrolysis process, xylanase restricts and to a certain extent changes the priority of the action targets of cellulase, resulting in unexpected results. It can be seen that for the technical solution of the present invention, the synergistic ratio of various enzymes in the complex enzyme should be relatively strictly controlled. The supplementary experiments in the second batch also confirmed the above conclusion to a certain extent.

[0051] Comparative Example 2: To verify the influence of the extraction and concentration process on the cistanche extract, the present invention also adopted different extraction and concentration treatment methods for extraction and concentration. Except for the extraction and concentration treatment methods, the whole processes of steps (1) and (2) in Example 2 were referred to, and the operating parameters were controlled to be the same. The specific grouping is shown in the following table.

[0052]

[0053] The cistanche extracts prepared from the above experimental groups were characterized, and the characterization included the content of the main target components. The characterization results are shown in the following table.

[0054]

[0055] From the above data, it can be clearly seen that the extraction and concentration process will have a greater impact on the Cistanche extract. Among them, the concentration of group 1 shows that the content of phenylethanol glycosides and polysaccharides has a certain impact, but it is relatively controllable. However, in the additional yield characterization settlement, it is shown that the yield of the standard group is about 73.2%, while the yield of the concentration of group 1 has a significant decrease to about 63.2%. In addition, a significant impact is found, that is, after the Cistanche extract of group 1 is concentrated according to the scheme of Example 2, it is made into the product Cistanche honey dew. During the 90-day storage process similar to the embodiment, the decrease in its components is significantly improved, which is higher than that of Example 2. The retention rates of its phenylethanol glycosides, polysaccharides and flavonoids are only about 71.3%, 75.0% and 66.7%, respectively, indicating that it may still have an unknown mechanism. And the concentration of group 2, its concentration process is carried out under normal pressure, and the content of the main target components produced is greatly reduced. This is mainly due to the poor concentration and separation effect of some non-target extract components during the concentration process, resulting in more non-target components, such as flavor and volatile components. If such components are not significantly affected in the general scheme, the target product of the present invention can be directly taken or taken, and the flavor and taste of the honeydew are good. Some of the flavor and volatile components contained in Cistanche deserticola are "incompatible" with honey, resulting in the flavor and taste of the final product honeydew. Decrease and deterioration, thus, in addition to the significant decrease in the content of the target component, it also ultimately leads to a decrease in the sensory quality of the product. In the first stage of the multi-stage vacuum concentration process, a higher concentration temperature was used in the concentration group 3. Although the concentration efficiency was improved, it can be clearly seen that a significant component loss was produced. Although the concentration group 4 used a lower concentration temperature, in terms of the total yield of the components in the extract and the content of the target components, there seems to be no significant difference with the standard group, and the single-stage concentration can reduce the process difficulty. However, in fact, after the Cistanche extract of 4 groups was concentrated according to the scheme of Example 2 to prepare the product Cistanche honey dew, the decline of its components was significantly improved during the 90-day storage process similar to the embodiment, especially the retention rate of polysaccharide components was only about 69.8%, and the loss rate was extremely high. This is mainly because the present invention achieves the "freezing" effect of the polysaccharide molecular chain conformation during the non-equilibrium concentration process through the precise decoupling of the thermodynamic driving force and the molecular motion ability, so that the batch difference rate of the product intrinsic viscosity is small, the stability of the target active ingredient is improved, and the product has stable properties and a longer effective shelf life.

Claims

1. A preparation method of Cistanche deserticola honeydew, characterized in that, the method comprises: (1) Pretreating the raw materials, configuring a composite enzyme for enzymatic hydrolysis, then performing ultrasonic extraction, and concentrating to obtain a Cistanche deserticola extract; (2) Mixing the Cistanche deserticola extract, honey and a composite antioxidant evenly in proportion to obtain the Cistanche deserticola honeydew.

2. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the raw materials in step (1) are Cistanche deserticola; the pretreatment of the raw materials in step (1) is to dry and crush the Cistanche deserticola to 80-100 meshes, and then mix it evenly with a citric acid-disodium hydrogen phosphate buffer solution with a pH value of 5.2-5.8 according to a mass ratio of 1:(18-22).

3. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the composite enzyme in step (1) includes cellulase, pectinase and xylanase; the active dosage of the composite enzyme is 2000-2400 U / g of raw materials, and cellulase, pectinase and xylanase are mixed according to an active ratio of (2.5-3.5):1:(0.3-0.5).

4. The preparation method of Cistanche deserticola honeydew according to claim 1 or 3, characterized in that, the enzymatic hydrolysis process in step (1) controls the enzymatic hydrolysis temperature at 40-50 °C and the enzymatic hydrolysis duration at 1.5-2.5 h.

5. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the ultrasonic extraction process in step (1) controls the extraction temperature at 55-65 °C, the ultrasonic frequency at 40-50 kHz, the power at 500-600 W, and the extraction duration at 20-30 min.

6. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the concentration in step (1) adopts multi-stage vacuum concentration. During the concentration process, the relative vacuum degree is controlled at -0.095-0.050 MPa, and the first stage controls the concentration temperature at 45-55 °C and concentrates to 30-35 %VOL of the original volume. The second stage controls the concentration temperature at 35-45 °C until solids just start to precipitate.

7. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the composite antioxidant in step (2) is a combined antioxidant of tea polyphenols and vitamin E, and the mass ratio of tea polyphenols to vitamin E is (1.8-2.2):

1.

8. The preparation method of Cistanche deserticola honeydew according to claim 1 or 7, characterized in that, the Cistanche deserticola extract, honey and composite antioxidant in step (2) are mixed evenly according to a mass ratio of 1:(1.5-2):0.

15.

9. The preparation method of Cistanche deserticola honeydew according to claim 1, characterized in that, the mixing evenly process in step (2) is carried out under the conditions of a temperature of 30-40 °C and an environmental pressure of 350-400 MPa, and stirred at a rotation speed of 1500-2000 rpm for 10-20 min to obtain the Cistanche deserticola honeydew.

10. A Cistanche deserticola honeydew prepared by any of the methods according to claims 1 to 9.