A precise directional processing method for increasing the content of echinacoside and verbascoside in Cistanche deserticola and its application

Abstract

The present invention belongs to the field of biomedical empowerment processing technology, and discloses a precise directional processing method and application for increasing the content of echinacoside and verbascoside in the Chinese medicinal material Cistanche deserticola. The method includes the selection, cleaning, infiltration, slicing, high-temperature drying, and packaging of Cistanche deserticola raw materials. The upper part of Cistanche deserticola is processed by vacuum freeze drying; the lower part of Cistanche deserticola is processed by temperature and humidity co-excitation technology. Existing studies have shown that there are obvious differences in the effective ingredients in Cistanche deserticola between different parts. After clarifying the distribution of echinacoside and verbascoside, the present invention specifically divides them, and then combines the physicochemical properties of the active ingredients to accurately process them using different processing methods, so as to retain and promote the conversion of its medicinal ingredients to the greatest extent, improve the quality and uniformity of Cistanche deserticola after processing, and maximize the overall value of Cistanche deserticola.

Description

Technical Field

[0001] The present invention belongs to the technical field of biomedicine empowerment processing, and in particular to a precise directional preparation method and application for increasing the content of echinacoside and verbascoside in the traditional Chinese medicinal material Cistanche deserticola. Background Art

[0002] Cistanche deserticola is known as the "desert ginseng". It is a plant that parasitizes on the roots of Haloxylon ammodendron. It has extremely high medicinal value and is a traditional precious Chinese medicinal material. Its main active ingredients are phenylethanol glycosides, including echinacoside and verbascoside. Studies have shown that verbascoside has multiple pharmacological effects such as anti-inflammatory, antioxidant, hypoglycemic and lipid-lowering, and has androgenic effects. It is an important component of Cistanche deserticola to nourish the kidney and strengthen yang. Echinacoside reduces myocardial cell apoptosis, improves cardiac function, and prevents and treats a variety of diseases by inhibiting the metabolic pathways of NADPH, ROS, and ER. Echinacoside also has extremely strong antioxidant properties, can induce and activate major endogenous antioxidant enzymes, inactivate pro-oxidases, and thus exert neuroprotective and anti-inflammatory effects.

[0003] Cistanche deserticola is in the shape of an oblate cylinder, and the upper part is more pointed than the lower part. Studies have reported that verbascoside in Cistanche deserticola is mainly concentrated in the upper part, while echinacoside is mainly concentrated in the lower part. Although both echinacoside and verbascoside have strong antioxidant capacity, the former has more phenolic hydroxyl groups, higher structural stability, and a conjugated system, which makes it have higher antioxidant capacity. In addition, as shown in the molecular structure formula below, due to the different molecular structures of echinacoside and verbascoside, the physical and chemical properties (thermal stability, etc.) of the two are also quite different, which makes the traditional processing method of mixing the whole slices and drying them uniformly have the disadvantages of low active ingredient retention conversion efficiency and poor quality uniformity.

[0004] The molecular structures of echinacoside (A) and verbascoside (B) are as follows:

[0005]

[0006] The 2020 edition of the Chinese Pharmacopoeia stipulates that the total amount of echinacoside and verbascoside in Cistanche deserticola shall not be less than 0.3%, and the total amount of echinacoside and verbascoside in Cistanche tubulosa shall not be less than 1.5%, and the moisture content of processed Cistanche deserticola shall not exceed 10%. Traditional drying methods for Cistanche deserticola mainly include sun drying, shade drying, wine drying, and hot air drying. Although these methods have low production costs, they have the problems of long time and low retention rate of effective ingredients. The Pharmacopoeia stipulates that the moisture content of processed Cistanche deserticola shall not exceed 10%. Sun drying generally takes 20-30 days, while shade drying takes 40-50 days, and is easily affected by pollutants such as dust and mold. In contrast, although vacuum freeze drying has relatively high equipment requirements and production costs, it can retain its effective ingredients to the maximum extent.

[0007] In order to improve the quality of Cistanche processing, enhance the retention and conversion efficiency of effective ingredients and shorten the production cycle, targeted drying and processing methods are adopted according to the characteristics of ingredients in different parts, and the release and conversion of active ingredients are targeted and regulated to maximize the retention and promotion of its medicinal ingredient conversion, improve the quality and uniformity of medicinal materials, and maximize the overall value of Cistanche, which is an urgent problem to be solved.

[0008] In summary, the prior art has the following technical problems:

[0009] Firstly, the idea of ​​processing Cistanche deserticola is to slice and mix the whole part, which will cause the degradation of the unstable substance verbascoside in the upper part of Cistanche deserticola, and the quality of Cistanche deserticola after processing will be reduced and the product uniformity will be poor.

[0010] Secondly, the traditional processing technology has a long processing cycle, and the processed Cistanche has a high water content, which is easy to mold and deteriorate, and the nutrients are lost, which affects the medicinal efficacy of Cistanche.

[0011] Through the search, the following relevant patent references were found:

[0012] Comparison Patent 1:

[0013] In view of the problem that the Cistanche deserticola processed by the above-mentioned traditional processing technology has insufficient echinacoside and verbascoside content and is lower than the risk of drug quality standards, the patent disclosure document "A processing method for Cistanche deserticola slices (CN107080241A)" provides a processing method for Cistanche deserticola slices, comprising the following steps: 1. Steaming and slicing the Cistanche deserticola raw material to obtain flaky Cistanche deserticola; 2. Drying the flaky Cistanche deserticola to allow the dried flaky Cistanche deserticola to absorb concentrated liquid, and then drying the flaky Cistanche deserticola that absorbs the concentrated liquid to obtain Cistanche deserticola slices, the concentrated liquid is prepared by decocting and concentrating the processed raw materials with water, and the processed raw materials include wolfberry, cassia seed, polygonatum and licorice. The processing method provided by the present invention promotes deep biochemical reactions of the rich internal substances of Cistanche deserticola, increases the content of the two effective substances of Cistanche deserticola, and releases more functional and nutritional components.

[0014] The problems with the above patent disclosure document (CN107080241A) are: (1) the method is to uniformly process the slices of Cistanche deserticola, which may promote the degradation of verbascoside in the upper part of Cistanche deserticola; (2) although the Cistanche deserticola is first steamed, which can inactivate the enzyme, verbascoside and echinacoside cannot tolerate the high temperature of 100°C; (3) the addition of medicinal materials such as wolfberry, cassia seed, polygonatum and licorice during the processing process may have side effects on certain groups of people and reduce the audience of Cistanche deserticola slices.

[0015] Comparison Patent 2:

[0016] In view of the problem that the efficacy of Cistanche deserticola is not well exerted, the patent disclosure "A processing process for nine-steamed and nine-processed Cistanche deserticola Chinese medicinal slices (CN113440552 A)" provides a processing method for Cistanche deserticola, comprising the following steps: ① preparing pretreated Cistanche deserticola; ② preparing pretreated sheet Cistanche deserticola; ③ preparing primary processed Cistanche deserticola; ④ steaming the primary processed Cistanche deserticola, taking out the solid product, and saving the steaming liquid for standby use; ⑤ mixing the steaming liquid with the dried solid product, re-steaming the solid product absorbed with the steaming liquid, taking out the solid product, and saving the steaming liquid for standby use; ⑥ processing a total of 9 times according to the method in step ⑤, and obtaining the nine-steamed and nine-processed Cistanche deserticola Chinese medicinal slices after drying.

[0017] The problems of the above patent disclosure document (CN113440552 A) are: (1) the method mixes and slices the whole Cistanche deserticola, which may cause the degradation of the unstable substance verbascoside in the upper part of Cistanche deserticola; (2) the method steams the Cistanche deserticola 9 times, which may reduce the content of heat-insensitive echinacoside and verbascoside in the Cistanche deserticola; (3) the method of processing Cistanche deserticola is too complicated and time-consuming, which is limited to the large-scale processing and production of Cistanche deserticola.

[0018] Comparison Patent 3:

[0019] The patent publication "A Processing and Drying Process for Fresh Cistanche (CN108310065 A)" provides a method for processing and drying fresh Cistanche to solve the problem that the quality of raw medicinal materials is not up to standard due to the unreasonable processing technology of fresh Cistanche. The specific steps are: removing the floating soil on the surface of fresh Cistanche, and removing the damaged, insect-infested, rotten and deteriorated parts; sorting the pretreated fresh Cistanche according to the grade; rinsing the surface of the sorted fresh Cistanche; steaming the cleaned fresh Cistanche at a temperature of 90℃-95℃ and a time of 30min-40min; cooling the steamed Cistanche to room temperature, and drying it in the shade at below 40℃ for 50-60 days to become a dry product. The raw Cistanche processed by the method of the embodiment of the invention has a maximum content of echinacoside and verbascoside of 1.534%.

[0020] The problems of the above patent publication (CN113440552 A) are as follows: (1) the sum of the contents of echinacoside and verbascoside in the raw medicinal material of Cistanche processed by this method can reach up to 1.534%, while the sum of the contents of echinacoside and verbascoside in the upper and lower parts of Cistanche obtained by the precise processing technology of the present invention can reach 7.564%, which is about 4 times higher; (2) this method makes the steamed Cistanche dried at below 40°C for 50-60 days to become a dry product. The processing time is long, and Cistanche will also be easy to mold and deteriorate due to its high water content, resulting in the loss of its effective ingredients; (3) this method does not divide Cistanche into parts for separate processing, and the content of its effective ingredients will also be reduced due to the different physical and chemical properties of different parts.

[0021] By comparison, the patent application of the present invention is essentially different from the above-mentioned patent publications. Summary of the invention

[0022] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a precise directional processing method and application for increasing the content of echinacoside and verbascoside in Cistanche deserticola.

[0023] The technical solution adopted by the present invention to solve its technical problem is:

[0024] A precise directional processing method for increasing the content of echinacoside and verbascoside in Cistanche deserticola, the method comprising selecting Cistanche deserticola raw materials, washing, infiltrating, slicing, high-temperature drying, and packaging, and the specific steps are as follows:

[0025] (1) Selection: Select fresh Cistanche deserticola that is free of pests and diseases;

[0026] (2) Cleaning: Use running water to clean the dirt on the surface of Cistanche deserticola;

[0027] (3) Soaking: After washing, completely immerse the Cistanche deserticola in water for 18-24 hours until it becomes hard, that is, it will not feel soft when squeezed by hand;

[0028] (4) Slicing: After soaking for 18-24 hours, separate the Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola down to 25%-35% of the overall height, and the lower part is the root of the Cistanche deserticola up to 25%-35% of the overall height. Then use a slicer to cut the upper and lower parts into slices of 3 mm to 4.5 mm thick respectively.

[0029] (5) Processing of the upper part of Cistanche deserticola: The upper part is vacuum freeze-dried, and the upper Cistanche deserticola slices are pre-frozen in a -80°C freezer for 2-4 hours; vacuum is evacuated to an absolute pressure of 60Pa-70Pa, and the temperature is raised to 35-45°C, and sublimation drying is performed for 20-24 hours. The moisture content of the Cistanche deserticola slices is adjusted to 5%-8% before being discharged;

[0030] (6) Processing of the lower part of Cistanche deserticola: The lower part is processed by temperature and humidity co-excitation technology, and fresh lower Cistanche deserticola slices are pre-frozen at -80°C for 2-4 hours; vacuum the system to an absolute pressure of 60Pa-70Pa, start heating to 35-45°C, sublimation dry for 20-24 hours, and adjust the moisture content of the Cistanche deserticola slices to 5%-8% before discharging; the Cistanche deserticola slices with a moisture content of 5%-8% are placed on a plate, each containing 2.5g-3.5g, with a plate thickness of 0.3cm-0.5cm, and the drying temperature is controlled at 60-90°C. The humidity of the drying environment is not controlled, and the finished product is obtained after drying for 8h-12h;

[0031] (7) Packaging: Vacuum packed for storage.

[0032] Furthermore, the finished product is obtained after drying for 8h-12h in step (6).

[0033] Application of the method described above in increasing the content of echinacoside and verbascoside in Cistanche deserticola.

[0034] The advantages and positive effects achieved by the present invention are:

[0035] 1. Existing studies have shown that the effective ingredients in Cistanche deserticola have obvious differences in different parts. After clarifying the distribution of echinacoside and verbascoside, the present invention specifically divides them, and then uses different processing methods to accurately process them in combination with the physicochemical properties of the active ingredients, so as to retain and promote the conversion of its medicinal ingredients to the greatest extent, improve the quality and uniformity of Cistanche deserticola after processing, and maximize the overall value of Cistanche deserticola.

[0036] 2. The echinacoside and verbascoside in the Cistanche prepared by the directional and precise processing method of the present invention are both improved compared with those dried by the traditional processing method. The content of verbascoside in the upper part of the Cistanche dried by the traditional processing method is 11.2 mg / g, and the content of verbascoside in the upper freeze-dried Cistanche is 30.8 mg / g, which is about 1.8 times higher than that of drying; the content of echinacoside in the lower part of the Cistanche dried by the traditional processing method is 4.4 mg / g, and the content of echinacoside in the lower part of the Cistanche baked at 70°C for 8h after freeze-drying is 22.8 mg / g, which is about 4.2 times higher than that of drying. It is significantly higher than the requirement of the Chinese Pharmacopoeia that it should not be less than 3 mg / g, providing a theoretical basis and technical support for the economic value empowerment of Cistanche.

[0037] 3. The method of the present invention adopts physical methods for the targeted and precise processing of Cistanche deserticola, which can improve the contents of echinacoside and verbascoside in different parts of Cistanche deserticola in a green and safe way, and has good repeatability, simple quality control, and is suitable for large-scale production in enterprises.

[0038] 4. The Cistanche deserticola prepared by the directional and precise processing method of the present invention is used as a processing raw material, and the subsequent processing cost is low, the safety is also high, and the product has high market competitiveness.

[0039] 5. The directional and precise processing method of the Cistanche deserticola of the present invention has a processing time of 30h-52h, while the traditional processing method generally takes 20-30 days to dry. Compared with the traditional processing technology, the processing time is shortened and the content of the effective ingredients in the Cistanche deserticola is increased.

[0040] 6. The method of the present invention divides Cistanche into upper and lower parts for directional and precise processing, and uses temperature and humidity co-excitation technology to reasonably configure the drying time, temperature and other parameters, thereby increasing the contents of verbascoside in the upper part of Cistanche and echinacoside in the lower part of Cistanche, respectively, and the active ingredients are retained and converted to the greatest extent. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 The process flow chart of the precise preparation of Cistanche deserticola in the present invention;

[0042] Figure 2 Schematic diagram of the division of the parts of Cistanche deserticola in the present invention;

[0043] Figure 3 is a standard curve diagram of echinacoside in the present invention;

[0044] Figure 4 is a standard curve diagram of verbascoside in the present invention;

[0045] Figure 5 This is a comparison diagram of the active ingredients in the upper and lower parts of the freeze-dried Cistanche deserticola in the present invention;

[0046] Figure 6 This is a diagram showing the effects of different treatments on the active ingredients of the upper part of Cistanche deserticola in the present invention;

[0047] Figure 7 This is a diagram showing the effects of different treatments on the active ingredients of the lower part of Cistanche deserticola in the present invention. DETAILED DESCRIPTION

[0048] The present invention will be further described below in conjunction with the embodiments. The following embodiments are descriptive rather than restrictive, and the protection scope of the present invention cannot be limited by the following embodiments.

[0049] The various experimental operations involved in the specific embodiments are all routine techniques in the art. For parts not specially annotated in this document, ordinary technicians in the art can implement them by referring to various commonly used reference books, scientific and technological literature or related instructions, manuals, etc. before the filing date of this invention.

[0050] A precise directional processing method for increasing the content of echinacoside and verbascoside in Cistanche deserticola, the method comprising selecting Cistanche deserticola raw materials, washing, infiltrating, slicing, high-temperature drying, and packaging, and the specific steps are as follows:

[0051] (1) Selection: Select fresh Cistanche deserticola that is free of pests and diseases;

[0052] (2) Cleaning: Use running water to clean the dirt on the surface of Cistanche deserticola;

[0053] (3) Soaking: After washing, completely immerse the Cistanche deserticola in water for 18-24 hours until it becomes hard, that is, it will not feel soft when squeezed by hand;

[0054] (4) Slicing: After soaking for 18-24 hours, separate the Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola down to 25%-35% of the overall height, and the lower part is the root of the Cistanche deserticola up to 25%-35% of the overall height. Then use a slicer to cut the upper and lower parts into slices of 3 mm to 4.5 mm thick respectively.

[0055] (5) Processing of the upper part of Cistanche deserticola: The upper part is vacuum freeze-dried, and the upper Cistanche deserticola slices are pre-frozen in a -80°C freezer for 2h-4h; vacuum is evacuated to a system absolute pressure of 60Pa-70Pa, and the temperature is raised to 35-45°C, and sublimation drying is performed for 20-24 hours. The moisture content of the Cistanche deserticola slices is adjusted to 5%-8% before being discharged;

[0056] (6) Processing of the lower part of Cistanche deserticola: The lower part is processed by temperature and humidity co-excitation technology, and fresh lower part Cistanche deserticola slices are pre-frozen at -80°C for 2-4 hours; vacuum the system to an absolute pressure of 60Pa-70Pa, start heating to 35-45°C, sublimation dry for 20-24 hours, and adjust the moisture content of the Cistanche deserticola slices to 5%-8% before discharging; the Cistanche deserticola slices with a moisture content of 5%-8% are placed on a plate, each containing 2.5g-3.5g, with a plate thickness of 0.3cm-0.5cm, and the drying temperature is controlled at 60-90°C. The humidity of the drying environment is not controlled, and the finished product is obtained after drying for 8h-12h;

[0057] (7) Packaging: Vacuum packed for storage.

[0058] Application of the method described above in increasing the content of echinacoside and verbascoside in Cistanche deserticola.

[0059] Specifically, the relevant preparation and detection are as follows:

[0060] Example 1

[0061] A precise and directional processing method for increasing the content of echinacoside and verbascoside in the Chinese medicinal material Cistanche deserticola, see Figure 1 , including the following steps:

[0062] Select fresh, free of rot and pests and diseases, wash away the dirt on the surface with running water, soak it in water for 22 hours after washing, so that it is completely soaked and hardened; Figure 2 As shown, the upper and lower parts are divided, the upper part is the top of Cistanche downward to 25%-35% of the overall height, and the lower part is the root of Cistanche upward to 25%-35% of the overall height, and then the upper and lower parts of Cistanche are cut into slices with a thickness of 3.9 mm using a slicer. The Cistanche slices are pre-frozen in a -80°C freezer for 2h-4h; vacuumed to a system absolute pressure of 60Pa-70Pa, heated to 35-45°C, sublimation dried for 20-24 hours, and the moisture content of the Cistanche slices is adjusted to about 5%-8% before discharging.

[0063] Use a grinder to grind, take 1 g of the processed Cistanche powder and add it to a 10 mL centrifuge tube, add 5 mL of the extract, the extract is 70% methanol solution (v / v, containing 0.1% glacial acetic acid), place it at 25°C, 40 kHz frequency for 30 min, shake it for 2 h, and centrifuge it at 6000 r / min and 4°C for 20 min, take the supernatant; add 5 mL of 70% methanol solution (v / v, containing 0.1% glacial acetic acid), place it at 25°C, 40 kHz frequency for 30 min, shake it for 2 h, and centrifuge it at 6000 r / min and 4°C for 20 min, and combine the supernatants; dilute the supernatant 20 times with 70% methanol solution (v / v, containing 0.1% glacial acetic acid), and filter it with a 0.22 μm organic filter membrane.

[0064] The contents of echinacoside and verbascoside were determined by high performance liquid chromatography (General Rule 0512 of the 2020 edition of the Chinese Pharmacopoeia). Chromatographic grade echinacoside and verbascoside were prepared into a standard solution with a concentration of 2 mg / mL, and the standard solution was gradiently diluted to 15.625 μg / mL with 50% methanol (v / v), and the peak area was determined. The standard curve was drawn with the standard concentration (μg / mL) as the horizontal axis and the peak area as the vertical axis, and a linear regression calculation was performed: Echinacoside standard curve: Y1=24646x-415351, R 2 =0.997( Figure 3 ); Verbascum glycoside standard: Y2=5474x-156638, R 2 =0.9957( Figure 4 ).

[0065] The contents of echinacoside and verbascoside in Cistanche deserticola were determined by high performance liquid chromatography. Chromatographic column: kromasil C18 (250 mm × 4.6 mm, 5 μm); column temperature: 30℃; injection volume: 20 μL; phase A: aqueous solution containing 0.1% acetic acid, phase B: acetonitrile containing 0.1% acetic acid; flow rate: 1 mL / min. The solvent elution gradient of phase B was: 0min~2 min: 5%, 2min~4 min: 5%~15%, 4min~12 min: 15%~25%, 12min~18 min: 25%~35%, 18min~20min: 35%~100%, 20min~23 min: 100%, 23min~23.5 min: 100%~5%, 23.5min~26min: 5%. The detection wavelength was 330nm.

[0066] Contents of echinacoside and verbascoside in the upper and lower parts of freeze-dried Cistanche deserticola Figure 5 As shown in the figure, the content of echinacoside in the lower part (6.8 mg / g) is higher than that in the upper part (5.4 mg / g), but the difference is not large; the content of verbascoside in the upper part (30.8 mg / g) is higher than that in the lower part (12.6 mg / g), which shows that verbascoside is mainly concentrated in the upper part. The total amount of echinacoside and verbascoside in the upper part of freeze-dried Cistanche is 36.2 mg / g, and the total amount of echinacoside and verbascoside in the lower part is 19.4 mg / g. The content of echinacoside and verbascoside in the upper part is about 0.9 times higher than that in the lower part. It can be clearly seen that there are differences in the effective ingredients in the upper and lower parts of Cistanche, so it is very necessary to divide Cistanche into parts and carry out targeted and precise processing, which can reduce the loss of effective ingredients.

[0067] Example 2

[0068] A precise and directional processing method for increasing the content of echinacoside and verbascoside in the Chinese medicinal material Cistanche deserticola, see Figure 1 , including the following steps:

[0069] Select fresh Cistanche deserticola without rot and pests, wash the soil on the surface with running water, soak it in water for 22 hours after washing, so that it is completely soaked and hardened; separate the completely soaked Cistanche deserticola into upper and lower parts, the upper part is the top of Cistanche deserticola downward to 25%-35% of the overall height, and the lower part is the root of Cistanche deserticola upward to 25%-35% of the overall height, and then use a slicer to cut the upper and lower parts of Cistanche deserticola into slices with a thickness of 3.9 mm. Since the contact between Cistanche deserticola slices and metal will cause the loss of nutrients in them, they are baked in a glass culture dish, and the upper Cistanche deserticola slices obtained are subjected to the following four treatments:

[0070] Freeze drying: Pre-freeze the Cistanche deserticola slices in a -80°C freezer for 2h-4h; evacuate the system to an absolute pressure of 60Pa-70Pa, start heating to 35-45°C, sublimate and dry for 20-24 hours, and adjust the moisture content of the Cistanche deserticola slices to about 5%-8% before discharging to obtain freeze-dried Cistanche deserticola.

[0071] Sun drying: put 15-25g of Cistanche deserticola into each culture dish, and then dry it in a sunny place. Turn it over every other day to detect the change in water content. When the water content is less than 10%, collect the material to obtain sun-dried Cistanche deserticola.

[0072] Bake at 70°C for 8h: Place the slices of Cistanche deserticola into glass culture dishes, with 15g-25g in each dish, the thickness of the dish being 0.3cm-0.5cm, the baking temperature being 70°C, and the baking time being controlled for 8h to obtain the finished product.

[0073] Bake at 70℃ for 8h after freeze-drying (temperature and humidity co-excitation technology treatment): pre-freeze the Cistanche slices in a -80℃ freezer for 2h-4h; evacuate the system to an absolute pressure of 60Pa-70Pa, start heating to 35-45℃, sublimate and dry until the moisture content of the Cistanche slices is about 5%-8%, then discharge the material, place it in a glass culture dish and bake it with a plate thickness of 0.3cm-0.5cm, control the drying temperature at 70℃, and dry it for 8h to obtain the finished product.

[0074] The method for sample extraction and determination of echinacoside and verbascoside content is the same as that in Example 1.

[0075] like Figure 6 As shown, for the upper part of Cistanche deserticola, the contents of verbascoside after sun-drying, freeze-drying, baking at 70℃ for 8h, and freeze-drying followed by baking at 70℃ for 8h were 11.2mg / g, 30.8mg / g, 28mg / g, and 37.2mg / g, respectively. Baking at 70℃ for 8h was 1.5 times the content of verbascoside in sun-drying, and freeze-drying was 2.8 times the content of verbascoside in sun-drying, and the contents of verbascoside were significantly increased; baking at 70℃ for 8h, freeze-drying, and freeze-drying followed by baking at 70℃ for 8h increased in sequence.

[0076] The content of verbascoside in freeze-drying treatment was similar to that in baking at 70℃ for 8h after freeze-drying. However, freeze-drying treatment could better maintain the shape and nutritional components of Cistanche deserticola, while baking at 70℃ would cause the sugar in Cistanche deserticola to react with amino acids to produce Maillard toxic byproducts, which would cause certain damage to the nutritional value of Cistanche deserticola. Therefore, freeze-drying was chosen for the upper part of Cistanche deserticola.

[0077] After freeze-drying and baking at 70℃ for 8h (temperature and humidity co-excitation technology treatment), the content of verbascoside was 37.2mg / g, which was only 0.2 times higher than that of freeze-drying. From the perspective of economic cost, freeze-drying the upper part of Cistanche deserticola can not only increase the content of verbascoside but also save energy.

[0078] Therefore, after comprehensive consideration, the upper part of Cistanche deserticola was chosen to be freeze-dried.

[0079] Example 3

[0080] A precise and directional processing method for increasing the content of echinacoside and verbascoside in the Chinese medicinal material Cistanche deserticola, see Figure 1 , including the following steps:

[0081] Select fresh Cistanche deserticola without rot and pests, wash away the soil on the surface with running water, soak it in water for 22 hours after washing, so that the Cistanche deserticola is completely soaked and hardened; separate the completely soaked Cistanche deserticola into upper and lower parts, the upper part is the top of the Cistanche deserticola downward to 25%-35% of the overall height, and the lower part is the root of the Cistanche deserticola upward to 25%-35% of the overall height, and then use a slicer to cut the upper and lower parts of the Cistanche deserticola into slices with a thickness of 3.9 mm. The obtained lower Cistanche deserticola slices are processed in the same way as in Example 2.

[0082] The method for sample extraction and determination of echinacoside and verbascoside content is the same as that in Example 1.

[0083] like Figure 7 As shown in the figure, for the lower part of Cistanche deserticola, the echinacoside content after sun-drying, freeze-drying, baking at 70℃ for 8h and freeze-dried and baked at 70℃ for 8h were 4.4mg / g, 6.8mg / g, 8.8mg / g and 22.8mg / g, respectively, and the echinacoside content increased in sequence. Among them, the 70℃ baking for 8h treatment was twice that of the sun-drying treatment, and the freeze-dried and baked at 70℃ for 8h treatment was 5.2 times that of the sun-drying treatment. The freeze-dried and baked at 70℃ for 8h treatment significantly increased the echinacoside content. In the lower part of Cistanche deserticola, the total amount of echinacoside and verbascoside after freeze-drying and 70℃ baking for 8h were 19.4mg / g and 19.9mg / g, respectively, with little difference. The total amount of echinacoside and verbascoside treated with freeze-drying and baking at 70℃ for 8h was 33.6mg / g, which was about 0.8 times higher than that treated with freeze-drying and baking at 70℃ for 8h. Therefore, the processing of the lower part of Cistanche deserticola with warm and wet co-excitation technology is more conducive to the release of echinacoside and better improves the total amount of echinacoside and verbascoside.

[0084] In Example 1 and Example 3, the upper and lower parts of Cistanche deserticola were freeze-dried in the same manner and then baked at 70°C for 8 hours. The echinacoside content in the upper and lower parts of Cistanche deserticola showed different trends. This may be due to the different active ingredients and antioxidant capacity of different parts of Cistanche deserticola. Related studies have also confirmed this. Dr. Chen Junran mentioned in the article "Analysis of the Differences in Active Ingredients and Antioxidant Activity between Different Varieties and Parts of Xinjiang Cistanche" that "the IC50 values ​​of the DPPH free radical scavenging ability of the upper, middle and lower parts of Red Willow Cistanche are 9.94, 6.57 and 5.95 mg / mL, respectively." (The IC50 value is an indicator to measure the activity of antioxidants, which stands for the "half-maximal inhibitory concentration". Specifically, the IC50 value in antioxidants refers to the concentration of antioxidants required to reduce a certain oxidation process to achieve the maximum possible effect of 50%). It is speculated that this is related to the growth and nutrient transport of Cistanche deserticola and the characteristics of the host plant, but the specific mechanism still needs further study, so different parts may have different trends after the same treatment.

[0085] At the same time, it can be seen from Examples 1 to 3 that when the lower Cistanche deserticola slices are processed in the method of the present invention, there is a synergistic effect between the freeze-drying step and the baking step, which can synergistically increase the total amount of echinacoside and verbascoside in the prepared lower Cistanche deserticola, especially the step of pre-freezing in a -80°C freezer for 2h-4h and the step of drying for 8h can significantly synergistically increase the total amount of echinacoside and verbascoside in the prepared lower Cistanche deserticola.

[0086] In summary, a precise and directional processing method for increasing the content of echinacoside and verbascoside in the Chinese medicinal material Cistanche deserticola, the optimal steps include the following steps:

[0087] Select fresh, free of rot and pests and diseases, wash away the dirt on the surface with running water, soak it in water for 22 hours after washing, so that it is completely soaked and hardened; Figure 2 As shown, the upper and lower parts are divided, the upper part is the top of Cistanche deserticola down to 25%-35% of the overall height, and the lower part is the root of Cistanche deserticola up to 25%-35% of the overall height. Then the upper and lower parts of Cistanche deserticola are cut into 3.9 mm thick slices respectively using a slicer.

[0088] Preparation of the upper part of Cistanche deserticola: the upper part is vacuum freeze-dried, and the upper Cistanche deserticola slices are pre-frozen in a -80℃ freezer for 2h-4h; evacuate the system to an absolute pressure of 60Pa-70Pa, start heating to 35℃-45℃, sublimate and dry for 20h-24h, and discharge the slices after adjusting the moisture content of the slices to 5%-8%.

[0089] Preparation of the lower part of Cistanche deserticola: the lower part is prepared by temperature and humidity co-excitation technology, and the fresh lower part of Cistanche deserticola slices are pre-frozen at -80°C for 2h-4h; evacuate the system to an absolute pressure of 60Pa-70Pa, start heating to 35°C-45°C, sublimate and dry for 20-24 hours, and adjust the moisture content of the Cistanche deserticola slices to 5%-8% before discharging; put the Cistanche deserticola slices with a moisture content of 5%-8% on a plate, each containing 2.5g-3.5g, and the thickness of the plate is 0.3cm-0.5cm. The drying temperature is controlled at 60°C-90°C, and the humidity of the drying environment is not controlled. The finished product is obtained after drying for 8h-12h.

[0090] By dividing Cistanche into different parts and using targeted drying and processing methods, the release and transformation of active ingredients can be targeted and regulated, so that the effective ingredients in Cistanche can be retained to the greatest extent. Therefore, it is necessary to carry out targeted and precise processing of Cistanche.

[0091] Although the embodiments of the present invention are disclosed for illustrative purposes, those skilled in the art will appreciate that various substitutions, changes and modifications are possible without departing from the spirit and scope of the present invention and the appended claims. Therefore, the scope of the present invention is not limited to the contents disclosed in the embodiments.

Claims

1. A precise and directional processing method for increasing the content of echinacoside and verbascoside in Cistanche deserticola, characterized in that: The method includes selecting Cistanche deserticola raw materials, washing, soaking, slicing, high-temperature drying, and packaging, and the specific steps are as follows: (1) Selection: Select fresh Cistanche deserticola that is free of pests and diseases; (2) Cleaning: Use running water to clean the dirt on the surface of Cistanche deserticola; (3) Soaking: After washing, completely immerse the Cistanche deserticola in water for 18-24 hours until it becomes hard, that is, it will not feel soft when squeezed by hand; (4) Slicing: After soaking for 18-24 hours, separate the Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola down to 25%-35% of the overall height, and the lower part is the root of the Cistanche deserticola up to 25%-35% of the overall height. Then use a slicer to cut the upper and lower parts into slices of 3 mm to 4.5 mm thick respectively. (5) Processing of the upper part of Cistanche deserticola: The upper part is vacuum freeze-dried, and the upper Cistanche deserticola slices are pre-frozen in a -80°C freezer for 2h-4h; vacuum is evacuated to an absolute pressure of 60Pa-70Pa, and the temperature is raised to 35°C-45°C, and sublimation drying is performed for 20h-24h. The moisture content of the Cistanche deserticola slices is adjusted to 5%-8% before discharging; (6) Processing of the lower part of Cistanche deserticola: The lower part is processed by temperature and humidity co-excitation technology, and fresh lower part Cistanche deserticola slices are pre-frozen at -80°C for 2h-4h; vacuum the system to an absolute pressure of 60Pa-70Pa, start heating to 35°C-45°C, sublimation dry for 20-24 hours, and adjust the moisture content of the Cistanche deserticola slices to 5%-8% before discharging; Cistanche deserticola slices with a moisture content of 5%-8% are placed on a plate, each containing 2.5g-3.5g, with a plate thickness of 0.3cm-0.5cm, and the drying temperature is controlled at 60°C-90°C. The humidity of the drying environment is not controlled, and the finished product is obtained after drying for 8h-12h; (7) Packaging: Vacuum packed for storage.

2. The method according to claim 1, characterized in that: The finished product is obtained after drying for 8h-12h in step (6).

3. Use of the method according to claim 1 or 2 in increasing the content of echinacoside and verbascoside in Cistanche deserticola.

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