Efficient extraction method of sea-buckthorn polysaccharide
By combining low-temperature water swelling, freezing, steam explosion and ultrasonic cavitation extraction methods with ethanol microwave co-extraction, the problem of low extraction efficiency of sea buckthorn polysaccharides in existing technologies has been solved, achieving high-efficiency extraction and high yield of polysaccharides.
Patent Information
- Application Number
- CN202511486259.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-17
- Publication Date
- 2025-12-12
AI Technical Summary
In existing technologies, ultrasonic treatment during the extraction of sea buckthorn polysaccharides is insufficient to loosen the sea buckthorn tissue structure, resulting in low polysaccharide yield.
A combined extraction method involving low-temperature water swelling, freezing, steam explosion, and ultrasonic cavitation, along with microwave co-extraction with ethanol, was employed to optimize the powder structure and extraction conditions, thereby improving the polysaccharide dissolution efficiency.
It significantly improved the yield of sea buckthorn polysaccharides, achieved full dissolution and extraction of polysaccharides, and enhanced extraction efficiency.
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Figure CN121108380A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of polysaccharide extraction, in particular to a high-efficiency extraction method of sea-buckthorn polysaccharide. BACKGROUND
[0002] Sea-buckthorn is a common medicinal and edible plant with high nutritional value and biological activity. Polysaccharide is the most abundant biopolymer in nature and exists in almost all organisms. A large number of studies have shown that sea-buckthorn polysaccharide has many biological activities, such as antioxidant, anti-aging, hypoglycemic, hypolipidemic, anticoagulant, antiviral, antitumor and immunomodulatory activities, and has no toxic and side effects on normal cells of the body, which may become an ideal source of drugs.
[0003] At present, the extraction of sea-buckthorn polysaccharide is usually to crush sea-buckthorn into powder and then put it into hot solvent for ultrasonic extraction. After filtration, precipitation and drying, crude sea-buckthorn polysaccharide is obtained. However, only ultrasonic treatment cannot fully loosen the structure of sea-buckthorn, and the sea-buckthorn polysaccharide in it cannot be fully dissolved, which seriously affects the yield of sea-buckthorn polysaccharide. Therefore, a high-efficiency extraction method of sea-buckthorn polysaccharide is proposed. SUMMARY
[0004] In view of the deficiencies of the prior art, the present application provides a high-efficiency extraction method of sea-buckthorn polysaccharide. The sea-buckthorn powder is successively subjected to low-temperature water swelling, freezing and steam explosion, so that the structure of the powder becomes loose. Then, ultrasonic and air combined extraction are used to fully dissolve the polysaccharide in the powder, thereby greatly improving the yield of sea-buckthorn polysaccharide.
[0005] To achieve the above-mentioned purpose, the present application provides the following technical scheme: a high-efficiency extraction method of sea-buckthorn polysaccharide, comprising the following steps, (1) crushing and sieving sea-buckthorn dry fruits to obtain sea-buckthorn powder; (2) immersing the sea-buckthorn powder in low-temperature deionized water for swelling treatment, then filtering and freezing overnight to obtain frozen swelled powder; (3) thawing the frozen swelled powder and then subjecting it to steam explosion treatment to obtain broken wall powder; (4) putting the broken wall powder into deionized water for whole-process ultrasonic treatment, and introducing air into the deionized water during the ultrasonic treatment for combined extraction. After suction filtration, sea-buckthorn waste residue and first sea-buckthorn polysaccharide extract are obtained; (5) putting the sea-buckthorn waste residue into an ethanol solution for further extraction, and applying microwave treatment during the extraction. After the extraction is completed, the ethanol in the obtained filtrate after suction filtration is evaporated to obtain second sea-buckthorn polysaccharide extract; (6) combining the first sea-buckthorn polysaccharide extract and the second sea-buckthorn polysaccharide extract to obtain sea-buckthorn polysaccharide extract.
[0006] Preferably, in step (1), the sea-buckthorn powder is extracted with petroleum ether by refluxing for 90 min to remove fat-soluble substances, and then the sea-buckthorn powder containing petroleum ether is evaporated to remove the petroleum ether.
[0007] Preferably, in step (1), the sea-buckthorn dried fruit is crushed and then passed through a 40-mesh sieve.
[0008] Preferably, in step (2), the temperature of the deionized water is 2-5 DEG C, and the swelling treatment time is 4-5 h; the freezing treatment temperature is -5 to -10 DEG C.
[0009] Preferably, in step (3), the steam explosion treatment process is as follows: the steam explosion temperature is 140-160 DEG C, the steam explosion pressure is 1-2 Mpa, and the steam explosion time is 60-100 s.
[0010] Preferably, in step (4), the ultrasonic treatment is carried out at 60-70 DEG C for 30-40 min at a frequency of 20-40 kHz; the solid-liquid ratio of the broken-wall powder and the deionized water is 1:(25-30) g / mL.
[0011] Preferably, in step (4), the air is introduced at a rate of 0.5-0.8 L / min.
[0012] Preferably, in step (5), the mass concentration of the ethanol solution is 40-60%; the extraction temperature is controlled to be 60-70 DEG C; and the solid-liquid ratio of the sea-buckthorn waste residue and the ethanol solution is 1:(15-20) g / mL.
[0013] Preferably, in step (5), the microwave treatment power is 300-400 W, and the microwave treatment time is 5-10 min.
[0014] Preferably, in step (6), the sea-buckthorn polysaccharide extract is subjected to spray drying treatment to obtain sea-buckthorn polysaccharide.
[0015] The present application provides a kind of sea-buckthorn polysaccharide efficient extraction method, compared with prior art has the following beneficial effects: The present application sequentially carries out low-temperature water swelling, freezing, steam explosion to sea-buckthorn powder, so that the structure of powder becomes loose, then uses ultrasonic and air combined extraction, can make the polysaccharide component in powder fully and fastly dissolve out, greatly improves the yield of sea-buckthorn polysaccharide.
[0016] The present application first carries out low-temperature water swelling, then carries out freezing treatment, by volume expansion to make the organizational structure of powder produce crack, is favorable to the hot steam of steam explosion when entering the organization inside of powder, so as to realize sufficient explosion, make its structure become loose enough, be favorable to the full dissolution of polysaccharide in subsequent extraction.
[0017] The present application introduces air during ultrasonic treatment, which can provide more bubble nucleus for ultrasonic cavitation, increase cavitation sites, make cavitation effect more dense and uniform, and the introduced oxygen can produce active oxygen free radicals in the high-temperature and high-pressure environment of ultrasonic cavitation, thereby assisting in the decomposition of cell wall structure or oxidation of impurities, thereby helping to release more effective ingredients.
[0018] The present application also performs ethanol combined microwave co-extraction treatment on the seabuckthorn waste residue, realizes secondary extraction of seabuckthorn polysaccharide, and increases the comprehensive yield of seabuckthorn polysaccharide. BRIEF DESCRIPTION OF DRAWINGS
[0019] The drawings described herein are used to provide further understanding of the present application, and form a part of the present application. The illustrative embodiments of the present application and their descriptions are used to explain the present application, and do not constitute an improper limitation on the present application. In the drawings: Figure 1 The scanning electron microscope images of the seabuckthorn powder, the frost expanded powder and the broken wall powder in Example 4 of the present application. DETAILED DESCRIPTION
[0020] The following examples are used to illustrate the embodiments of the present application, so that the implementation process of how to apply technical means to solve technical problems and achieve technical effects can be fully understood and implemented.
[0021] Example 1 A high-efficiency extraction method of seabuckthorn polysaccharide, comprising the following steps: (1) The seabuckthorn dry fruit is crushed and passed through a 40-mesh sieve to obtain seabuckthorn powder; (2) The seabuckthorn powder is immersed in deionized water at 3℃ for swelling treatment for 4.5h, then filtered and frozen overnight at a temperature of-8℃ to obtain a frost expanded powder; (3) The frost expanded powder is thawed and subjected to steam explosion treatment, during which the steam explosion temperature is controlled at 150℃, the steam explosion pressure is 1.5Mpa, and the steam explosion time is 85s. After the steam explosion treatment is completed, a broken wall powder is obtained; (4) The broken wall powder is placed in deionized water at a solid-liquid ratio of 1:25g / mL for full-range ultrasonic treatment, and air is introduced during the ultrasonic treatment for combined extraction. After suction filtration, seabuckthorn waste residue and first seabuckthorn polysaccharide extract are obtained. During the ultrasonic treatment, the ultrasonic treatment is carried out at 65℃ for 35min at a frequency of 30kHz. The air introduction rate is 0.6L / min; (5) the seabuckthorn waste residue is put into a 50wt% ethanol solution at a solid-liquid ratio of 1:20 g / mL, and extraction is continued at 65°C, during which microwave treatment is applied, and after the extraction is completed, the ethanol in the filtrate obtained after suction filtration is removed by evaporation to obtain secondary seabuckthorn polysaccharide extract; the power of the above-mentioned microwave treatment is 350W, and the power time of the microwave treatment is 8min; (6) the primary seabuckthorn polysaccharide extract and the secondary seabuckthorn polysaccharide extract are combined to prepare seabuckthorn polysaccharide extract, and the seabuckthorn polysaccharide extract is subjected to spray drying treatment to obtain seabuckthorn polysaccharide.
[0022] Example 2 A high-efficiency extraction method of seabuckthorn polysaccharide includes the following steps: (1) the seabuckthorn dried fruit is crushed and passed through a 40-mesh sieve to obtain seabuckthorn powder; the seabuckthorn powder is previously subjected to reflux extraction with petroleum ether for 90min to remove fat-soluble substances, and then the seabuckthorn powder containing petroleum ether is subjected to evaporation to remove the petroleum ether; (2) the seabuckthorn powder is immersed in deionized water at 5°C for swelling treatment for 4h, and then filtered and frozen overnight at a temperature of -10°C to obtain frozen and swelled powder; (3) the frozen and swelled powder is thawed and subjected to steam explosion treatment, during which the steam explosion temperature is controlled at 140°C, the steam explosion pressure is 2Mpa, and the steam explosion time is 60s, and after the steam explosion treatment is completed, the broken wall powder is obtained; (4) the broken wall powder is put into deionized water at a solid-liquid ratio of 1:30 g / mL for whole-process ultrasonic treatment, and air is introduced during the ultrasonic treatment for combined extraction, and after suction filtration, seabuckthorn waste residue and primary seabuckthorn polysaccharide extract are obtained; during the ultrasonic treatment, the ultrasonic treatment is carried out at 70°C for 40min at a frequency of 20kHz. The air introduction rate is 0.5L / min; (5) the seabuckthorn waste residue is put into a 60wt% ethanol solution at a solid-liquid ratio of 1:20 g / mL, and extraction is continued at 60°C, during which microwave treatment is applied, and after the extraction is completed, the ethanol in the filtrate obtained after suction filtration is removed by evaporation to obtain secondary seabuckthorn polysaccharide extract; the power of the above-mentioned microwave treatment is 400W, and the power time of the microwave treatment is 5min; (6) the primary seabuckthorn polysaccharide extract and the secondary seabuckthorn polysaccharide extract are combined to prepare seabuckthorn polysaccharide extract, and the seabuckthorn polysaccharide extract is subjected to spray drying treatment to obtain seabuckthorn polysaccharide.
[0023] Example 3 A high-efficiency extraction method of seabuckthorn polysaccharide includes the following steps: (1) The sea buckthorn dry fruit is crushed and passed through a 40-mesh sieve to obtain sea buckthorn powder; the sea buckthorn powder is previously extracted with petroleum ether by reflux extraction for 90 min to remove fat-soluble substances, and then the sea buckthorn powder containing petroleum ether is evaporated to remove the petroleum ether; (2) The sea buckthorn powder is immersed in deionized water at 2°C for swelling treatment for 5 h, then filtered and frozen overnight at a temperature of -5°C to obtain a frozen and swelled powder; (3) The frozen and swelled powder is thawed and subjected to steam explosion treatment, during which the steam explosion temperature is controlled at 160°C, the steam explosion pressure is 1 MPa, and the steam explosion time is 100 s; after the steam explosion treatment is completed, a broken cell wall powder is obtained; (4) The broken cell wall powder is placed in deionized water at a solid-liquid ratio of 1:30 g / mL for whole-process ultrasonic treatment, and air is introduced during the ultrasonic treatment to perform combined extraction; after suction filtration, sea buckthorn waste residue and a first sea buckthorn polysaccharide extract are obtained; during the ultrasonic treatment, the treatment is carried out at 60°C for 30 min at a frequency of 40 kHz. The air introduction rate is 0.8 L / min; (5) The sea buckthorn waste residue is placed in a 40 wt% ethanol solution at a solid-liquid ratio of 1:15 g / mL for further extraction at 70°C, during which microwave treatment is applied; after the extraction is completed, the ethanol in the obtained filtrate after suction filtration is evaporated to obtain a second sea buckthorn polysaccharide extract; the power of the microwave treatment is 300 W, and the power time of the microwave treatment is 10 min; (6) The first sea buckthorn polysaccharide extract and the second sea buckthorn polysaccharide extract are combined to obtain a sea buckthorn polysaccharide extract, and the sea buckthorn polysaccharide extract is subjected to spray drying treatment to obtain sea buckthorn polysaccharide.
[0024] Example 4 A high-efficiency extraction method of sea buckthorn polysaccharide, comprising the following steps: (1) The sea buckthorn dry fruit is crushed and passed through a 40-mesh sieve to obtain sea buckthorn powder; the sea buckthorn powder is previously extracted with petroleum ether by reflux extraction for 90 min to remove fat-soluble substances, and then the sea buckthorn powder containing petroleum ether is evaporated to remove the petroleum ether; (2) The sea buckthorn powder is immersed in deionized water at 3°C for swelling treatment for 4.5 h, then filtered and frozen overnight at a temperature of -8°C to obtain a frozen and swelled powder; (3) The frozen and swelled powder is thawed and subjected to steam explosion treatment, during which the steam explosion temperature is controlled at 150°C, the steam explosion pressure is 1.5 MPa, and the steam explosion time is 85 s; after the steam explosion treatment is completed, a broken cell wall powder is obtained; (4) The broken wall powder is put into deionized water according to the solid-liquid ratio of 1:25 g / mL for ultrasonic treatment, and air is introduced during the ultrasonic treatment to carry out combined extraction. After suction filtration, seabuckthorn waste residue and first seabuckthorn polysaccharide extract are obtained. During the ultrasonic treatment, the ultrasonic treatment is carried out at 65°C with a frequency of 30 kHz for 35 min. The air inlet rate is 0.6 L / min; (5) The seabuckthorn waste residue is put into 50 wt% ethanol solution according to the solid-liquid ratio of 1:20 g / mL for further extraction at 65°C, during which microwave treatment is applied. After the extraction is completed, the ethanol in the filtrate obtained after suction filtration is evaporated to obtain secondary seabuckthorn polysaccharide extract. The power of the above-mentioned microwave treatment is 350 W, and the power time of the microwave treatment is 8 min; (6) The first seabuckthorn polysaccharide extract and the secondary seabuckthorn polysaccharide extract are combined to obtain seabuckthorn polysaccharide extract, and the seabuckthorn polysaccharide extract is subjected to spray drying treatment to obtain seabuckthorn polysaccharide.
[0025] Combined scanning electron microscopy Figure 1 It can be known that the surface morphology of the seabuckthorn powder is relatively flat and smooth; the structure of the freeze-swollen powder begins to crack; and the structure of the broken wall powder has become very loose, which is helpful for the full dissolution of polysaccharides.
[0026] Comparative Example 1 A high-efficiency extraction method of seabuckthorn polysaccharide includes the following steps: (1) The seabuckthorn dry fruit is crushed and passed through a 40-mesh sieve to obtain seabuckthorn powder. The seabuckthorn powder is previously subjected to reflux extraction with petroleum ether for 90 min to remove fat-soluble substances, and then the seabuckthorn powder containing petroleum ether is evaporated to remove the petroleum ether; (2) The seabuckthorn powder is immersed in 3°C deionized water for swelling treatment for 4.5 h, and then filtered to obtain swelled powder; (3) The swelled powder is subjected to steam explosion treatment, during which the steam explosion temperature is controlled at 150°C, the steam explosion pressure is 1.5 MPa, and the steam explosion time is 85 s. After the steam explosion treatment is completed, broken wall powder is obtained; Steps (4)-(6) are the same as in Example 4.
[0027] Comparative Example 2 A high-efficiency extraction method of seabuckthorn polysaccharide includes the following steps: (1) The seabuckthorn dry fruit is crushed and passed through a 40-mesh sieve to obtain seabuckthorn powder. The seabuckthorn powder is previously subjected to reflux extraction with petroleum ether for 90 min to remove fat-soluble substances, and then the seabuckthorn powder containing petroleum ether is evaporated to remove the petroleum ether; (2) The seabuckthorn powder is immersed in 3°C deionized water for swelling treatment for 4.5 h, and then filtered and frozen overnight at a temperature of -8°C to obtain freeze-swollen powder; (3) freeze-thawing the frost-swollen powder to obtain broken-wall powder; Steps (4)-(6) are the same as in Example 4.
[0028] Comparative Example 3 A high-efficiency extraction method of seabuckthorn polysaccharide, comprising the following steps: Steps (1)-(3) are the same as in Example 4; (4) the broken-wall powder is put into deionized water at a solid-liquid ratio of 1:25 g / mL for whole-process ultrasonic treatment, and after suction filtration, seabuckthorn waste residue and seabuckthorn polysaccharide extract are obtained; during the ultrasonic treatment, the treatment is carried out at 65℃ for 35 min at a frequency of 30 kHz; Steps (5)-(6) are the same as in Example 4.
[0029] Comparative Example 4 A high-efficiency extraction method of seabuckthorn polysaccharide, comprising the following steps: (1) the seabuckthorn dried fruit is crushed and passed through a 40-mesh sieve to obtain seabuckthorn powder; the seabuckthorn powder is previously subjected to reflux extraction with petroleum ether for 90 min to remove fat-soluble substances, and then the seabuckthorn powder containing petroleum ether is evaporated to remove the petroleum ether; (2) the seabuckthorn powder is immersed in deionized water at 3℃ for swelling treatment for 4.5 h, and then filtered and frozen overnight at a temperature of -8℃ to obtain frost-swollen powder; (3) the frost-swollen powder is subjected to steam explosion treatment after thawing, during which the steam explosion temperature is controlled at 150℃, the steam explosion pressure is 1.5 MPa, and the steam explosion time is 85 s, and after the steam explosion treatment is completed, broken-wall powder is obtained; (4) the broken-wall powder is put into deionized water at a solid-liquid ratio of 1:25 g / mL for whole-process ultrasonic treatment, and air is introduced during the ultrasonic treatment for combined extraction, and after suction filtration, seabuckthorn waste residue and seabuckthorn polysaccharide extract are obtained; during the ultrasonic treatment, the treatment is carried out at 65℃ for 35 min at a frequency of 30 kHz. The air introduction rate is 0.6 L / min; (5) the seabuckthorn polysaccharide extract is subjected to spray drying treatment to obtain seabuckthorn polysaccharide.
[0030] Yield of seabuckthorn polysaccharide The calculation method of the yield of seabuckthorn polysaccharide is: the mass of the initial seabuckthorn powder is weighed and recorded as M 1 ; the mass of the seabuckthorn polysaccharide obtained by spray drying is weighed and recorded as M 2 ; the yield of seabuckthorn polysaccharide in Examples 1-4 and Comparative Examples 1-4 is calculated respectively, and the calculation formula is: yield (%) = M 2 / M 1 X 100%. The specific calculation results are shown in Table 1.
[0031] Table 1: Yield of seabuckthorn polysaccharide From Table 1, it can be seen that: (1) Compared with Example 4, Comparative Example 1 was not subjected to freezing treatment, and the powder structure was relatively dense and complete, which was not conducive to the entry of hot steam during subsequent steam explosion treatment, affecting the explosion effect and resulting in a decrease in the dissolution amount of polysaccharide.
[0032] (2) Compared with Example 4, steam explosion treatment was not used in Comparative Example 2, and the powder structure was in a non-loose state, which was not conducive to the sufficient dissolution of polysaccharide.
[0033] (3) Compared with Example 4, air was not introduced during ultrasonic extraction in Comparative Example 3, which finally reduced the yield of seabuckthorn polysaccharide.
[0034] Although the embodiments of the present application have been shown and described, it can be understood by those of ordinary skill in the art that various changes, modifications, replacements and modifications can be made to these embodiments without departing from the principles and spirits of the present application, and the scope of the present application is defined by the appended claims and their equivalents.
Claims
1. A highly efficient extraction method for sea buckthorn polysaccharides, characterized in that, Includes the following steps: (1) The dried sea buckthorn fruit is crushed and sieved to obtain sea buckthorn powder; (2) The sea buckthorn powder was soaked in low-temperature deionized water for swelling treatment, then filtered and frozen overnight to obtain frozen swollen powder; (3) After the frozen and thawed powder is thawed, it is subjected to steam explosion treatment to obtain cell wall broken powder; (4) The cell wall broken powder was placed in deionized water for full ultrasonic treatment, and air was introduced during the ultrasonic treatment for combined extraction. After filtration, sea buckthorn waste residue and sea buckthorn polysaccharide extract were obtained. (5) The sea buckthorn residue was placed in an ethanol solution for further extraction. Microwave treatment was applied during the extraction. After the extraction was completed, the filtrate obtained by vacuum filtration was evaporated to remove the ethanol and a secondary sea buckthorn polysaccharide extract was obtained. (6) Combine the primary and secondary sea buckthorn polysaccharide extracts to obtain the sea buckthorn polysaccharide extract.
2. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (1), the sea buckthorn powder is first extracted by reflux extraction with petroleum ether for 90 minutes to remove fat-soluble substances, and then the sea buckthorn powder containing petroleum ether is evaporated to remove petroleum ether.
3. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (1), the dried sea buckthorn fruit is crushed and then passed through a 40-mesh sieve.
4. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (2), the temperature of the deionized water is 2~5℃, the swelling treatment time is 4~5h, and the freezing treatment temperature is -5~-10℃.
5. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (3), the steam explosion treatment process is as follows: the steam explosion temperature is 140~160℃, the steam explosion pressure is 1~2Mpa, and the steam explosion time is 60~100s.
6. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (4), the ultrasonic treatment is performed at 60~70℃ and at a frequency of 20~40kHz for 30~40min; the ratio of the cell wall-breaking powder to the deionized water is 1:(25~30)g / mL.
7. The efficient extraction method for sea buckthorn polysaccharides according to claim 6, characterized in that, In step (4), the air flow rate is 0.5~0.8L / min.
8. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (5), the mass concentration of the ethanol solution is 40-60%; the extraction temperature is controlled at 60-70℃; and the ratio of sea buckthorn waste residue to ethanol solution is 1:(15-20)g / mL.
9. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (5), the power of the microwave treatment is 300~400W, and the power treatment time is 5~10min.
10. The efficient extraction method for sea buckthorn polysaccharides according to claim 1, characterized in that, In step (6), the sea buckthorn polysaccharide extract is spray-dried to obtain sea buckthorn polysaccharide.