Ginseng fruit total saponin powder and preparation method thereof

Abstract

The invention relates to the technical field of biotechnology, in particular to an extraction and filtration method of ginseng fruit total saponin powder, which specifically comprises the following steps: sequentially carrying out water extraction, pH value regulation, centrifugation, purification, concentration, drying, crushing and mixing on ginseng fruit pulp, and finally extracting to obtain the ginseng fruit total saponin powder with the yield of 0.76-0.80%. The concentration of ginsenoside Re in the ginseng fruit total saponin powder is not lower than 650 mg / g, the concentration of microorganism aerobic bacteria is smaller than or equal to 800 cfu / g, the concentration of mould and saccharomycetes is smaller than or equal to 80 cfu / g, and no Escherichia coli is detected, so that the validity period of the ginseng fruit total saponin powder is greatly prolonged and can reach 36 months in a sealed and moistureproof environment.

Description

[0001] This invention is a divisional application of the invention patent with the application number CN202310834011.9, the application date of July 7, 2023, and the invention title of the extraction and filtration method of total ginsenoside powder of ginseng fruit. Technical Field

[0002] This invention relates to the field of biotechnology, and particularly to an extraction and filtration method of total ginsenoside powder of ginseng fruit. Background Art

[0003] The fruit of ginseng is also known as ginseng seed or ginseng kernel. It is the fruit of the plant Panax ginseng C. A. Mey. of the family Araliaceae, and the fruiting period is from June to September every year. It appears in the form of a berry during the growth period and is a berry containing seeds inside. Therefore, it is more appropriate to call it ginseng berry. The ginseng berry is oblate or reniform. It is green with different depths during the growth process from the appearance of the fruit until it matures. When the seeds mature in July and August, the fruit is bright red, the size of a broad bean, and contains two semi-circular seeds. After the berry dries and the husk is removed, it is the ginseng seed. Usually, the fruit and seeds are collected at the same time, but the berry shell is mostly discarded.

[0004] Total ginsenoside powder of ginseng fruit, that is, a mixture of prototype ginsenosides, can be extracted from the fruit of ginseng and has anti-cancer effects. Total ginsenoside powder of ginseng fruit has various pharmacological effects. It has a regulatory effect on the nervous system, and the central inhibitory effect may be related to the inhibition of ATPase. Ginsenoside of ginseng stem and leaf has an androgen-like effect and can regulate the endocrine system. It has an anti-hypoxia effect, which may be related to its improvement of the hypoxia tolerance of the cerebral cortex. It has a cardiotonic effect on the cardiovascular system and is related to the increase of ATP in myocardial cells. Through long-term action, it can gradually block the transition of tumor cells from the G1 phase to the S phase and then block the transition from the S phase to the G2 phase. It can change the RAN content of tumor cells, causing changes in the characteristics of S-180 sarcoma cells, thereby inhibiting the growth of tumor cells. The protective effect on experimental liver injury may be through inducing an increase in the content of P-450 in liver microsomes, adjusting liver metabolism, anti-inflammatory and other effects on various biochemical processes, and has an antagonistic and inhibitory effect on specific inflammatory symptoms.

[0005] This invention provides an improved extraction and filtration method of total ginsenoside powder of ginseng fruit, which can reduce the content of aerobic bacteria, molds and yeasts in the extraction product while meeting the extraction efficiency of total ginsenoside powder of ginseng fruit. Summary of the Invention

[0006] This invention provides an extraction and filtration method of total ginsenoside powder of ginseng fruit, with an extraction yield reaching 0.76 - 0.80%, and at the same time reducing the content of microorganisms, so that the shelf life of the extraction product can reach 36 months.

[0007] The present invention provides an extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton, comprising the following steps:

[0008] S1. Put Solanum muricatum Aiton pulp into an extraction tank, then add water for extraction to obtain Solanum muricatum Aiton extract, and then filter the Solanum muricatum Aiton extract to obtain a roughly filtered Solanum muricatum Aiton medicinal liquid;

[0009] S2. Add CaO to the roughly filtered Solanum muricatum Aiton medicinal liquid prepared in S1 and stir. After adjusting the pH value to 9 - 10, open the steam valve, heat until the roughly filtered Solanum muricatum Aiton medicinal liquid boils and keep it boiling to obtain an alkaline Solanum muricatum Aiton medicinal liquid, and then centrifuge the alkaline Solanum muricatum Aiton medicinal liquid pump to obtain a centrifuged Solanum muricatum Aiton medicinal liquid;

[0010] S3. Purify the centrifuged Solanum muricatum Aiton medicinal liquid prepared in S2 by column chromatography, and then successively wash the purified centrifuged Solanum muricatum Aiton medicinal liquid with water until the centrifuged Solanum muricatum Aiton medicinal liquid becomes colorless, and then perform elution to obtain a total ginsenoside extraction solution of Solanum muricatum Aiton;

[0011] S4. Place the total ginsenoside extraction solution of Solanum muricatum Aiton prepared in S3 in a concentration tank, add ethanol in the concentration tank for concentration to obtain a clear paste of total ginsenoside of Solanum muricatum Aiton;

[0012] S5. Dry the clear paste of total ginsenoside of Solanum muricatum Aiton prepared in S4, then pulverize and mix evenly to obtain total ginsenoside powder of Solanum muricatum Aiton.

[0013] According to the extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, the amount of water added to the extraction tank in S1 is 6 times the amount of Solanum muricatum Aiton pulp added, and the extraction time is 30 min.

[0014] According to the extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, the mass fraction of CaO in S2 is 0.7%, and the holding time is 30 min.

[0015] According to the extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, the conditions for column chromatography in S3 are: in a resin column with an adsorption flow rate of 3 BV / h.

[0016] According to the extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, the water consumption for washing in S3 is 10 BV, and the flow rate of water during washing is 4 BV / h;

[0017] The elution solvent is an ethanol solution with a volume fraction of 60%, the solvent consumption is 6 BV, and the flow rate of the solvent during elution is 2 BV / h.

[0018] According to the extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, in S4, the concentration tank is a single-effect evaporation concentrator, the temperature condition during concentration by the single-effect evaporation concentrator is 70-80°C, and the vacuum degree of the single-effect evaporation concentrator is 0.04-0.07 Mpa.

[0019] According to the extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, when the temperature condition of the clear paste of total ginsenoside of Solanum muricatum Aiton in S4 is 55°C, its relative density is 1.1-1.15.

[0020] According to the extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, in S5, the drying is carried out in a vacuum drying oven, and the drying conditions are as follows: the clear paste of total ginsenoside of Solanum muricatum Aiton is directly laid on the drying tray in the vacuum drying oven, the thickness of the laid paste of the clear paste of total ginsenoside of Solanum muricatum Aiton is 3-5 cm, the vacuum degree of the vacuum drying oven is 0.04-0.08 Mpa, the temperature of the vacuum drying oven is 80°C, and the drying time is 3-4 h.

[0021] According to the extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton provided by the present invention, after crushing in S5, the crushed clear paste of total ginsenoside powder of Solanum muricatum Aiton needs to be screened, and the mesh number of the sieve used during screening is 100 meshes;

[0022] The time for uniform mixing ≥ 40 min.

[0023] The present invention provides an extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton. The Solanum muricatum Aiton pulp is successively subjected to water extraction, pH adjustment, centrifugation, purification, concentration, drying, crushing and mixing, and finally total ginsenoside powder of Solanum muricatum Aiton is extracted. The yield reaches 0.76-0.80%, and the concentration of ginsenoside Re in the total ginsenoside powder of Solanum muricatum Aiton is not less than 650 mg / g. The concentration of aerobic bacteria in microorganisms ≤ 800 cfu / g, the concentration of molds and yeasts ≤ 80 cfu / g, and Escherichia coli has not been detected, greatly improving the shelf life of the total ginsenoside powder of Solanum muricatum Aiton, and it can reach 36 months in a sealed and moisture-proof environment.

[0024] Additional aspects and advantages of the present invention will be given in part in the following description, will become apparent in part from the following description, or will be understood through the practice of the present invention. Description of the Drawings

[0025] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0026] Figure 1 It is a flowchart of an extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention;

[0027] Figure 2 It is a working principle diagram of an extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton provided by the present invention. Specific embodiments

[0028] To make the objectives, technical solutions and advantages of the present invention clearer, the technical solutions in the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the present invention. Obviously, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present invention without creative efforts shall fall within the scope of protection of the present invention.

[0029] In the description of the embodiments of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing the embodiments of the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation to the embodiments of the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0030] In the description of the embodiments of the present invention, it should be noted that unless otherwise clearly specified and limited, the terms "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the embodiments of the present invention can be understood according to specific circumstances.

[0031] In the embodiments of the present invention, unless otherwise clearly specified and limited, the first feature may be in direct contact with the second feature "above" or "below", or the first and second features may be indirectly in contact through an intermediate medium. Moreover, the first feature being "above", "over" and "on" the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply indicates that the first feature has a higher horizontal height than the second feature. The first feature being "below", "beneath" and "under" the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply indicates that the first feature has a lower horizontal height than the second feature.

[0032] In the description of this specification, the descriptions referring to terms such as "one embodiment", "some embodiments", "example", "specific example", or "some examples", etc., mean that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the embodiments of the present invention. In this specification, the schematic expressions of the above terms do not refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples. In addition, without contradiction, those skilled in the art can combine and combine the different embodiments or examples described in this specification and the features of different embodiments or examples.

[0033] The following combines Figure 1-2 the embodiments shown to describe the technical solution of the present invention:

[0034] An extraction and filtration method for total ginsenoside powder of Solanum muricatum Aiton, comprising the following steps:

[0035] S1. Put 420.0 kg of Solanum muricatum Aiton pulp into a multi-functional extraction tank, then add water for extraction to obtain Solanum muricatum Aiton extract. The water content of the multi-functional extraction tank is 6 times the total amount of Solanum muricatum Aiton pulp, and the extraction time is 30 min. Then filter the Solanum muricatum Aiton extract to obtain a roughly filtered Solanum muricatum Aiton medicinal liquid; the environmental cleanliness level during weighing and batching is the general level;

[0036] S2. Add CaO with a mass fraction of 0.7% to the roughly filtered Solanum muricatum Aiton medicinal liquid prepared in S1 and stir. After adjusting the pH value to 9 - 10, open the steam valve and heat until the roughly filtered Solanum muricatum Aiton medicinal liquid boils and keep it for 30 min to obtain an alkaline Solanum muricatum Aiton medicinal liquid. Then centrifuge the alkaline Solanum muricatum Aiton medicinal liquid pump through a plate-type sedimentation centrifuge to obtain a centrifuged Solanum muricatum Aiton medicinal liquid; the environmental cleanliness level during water extraction and concentration is the general level;

[0037] S3. Purify the centrifuged Solanum muricatum Aiton medicinal liquid prepared in S2 by column chromatography, and then sequentially wash and analyze the purified centrifuged Solanum muricatum Aiton medicinal liquid. The water consumption during washing is 10 BV, the flow rate of water during washing is 4 BV / h. After washing and eluting until colorless, perform analysis. The analysis solvent is an ethanol solution with a volume fraction of 60%, the dosage of the ethanol solution is 6 BV, and the flow rate of the ethanol solution is 2 BV / h to prepare a total ginsenoside extract of Solanum muricatum Aiton; the conditions for column chromatography purification are: a resin column with an adsorption flow rate of 3 BV / h; the environmental cleanliness level during separation is the general level;

[0038] S4. Place the total saponin extract of Solanum muricatum prepared in S3 in a single-effect evaporator of a concentration tank, add ethanol to the concentration tank for concentration. The temperature condition during concentration in the single-effect evaporator is 70 - 80°C, and the vacuum degree of the single-effect evaporator is 0.04 - 0.07 Mpa to obtain the clear paste of Solanum muricatum total saponins. When the temperature condition of the clear paste of Solanum muricatum total saponins is 55°C, its relative density is 1.1 - 1.15; the environmental cleanliness level during refining is the general level;

[0039] S5. Dry the clear paste of Solanum muricatum total saponins prepared in S4, then crush it through a high-efficiency crusher and mix it evenly through a three-dimensional mixer to obtain Solanum muricatum total saponin powder; the drying is carried out in a vacuum drying oven. The drying conditions are as follows: the clear paste of Solanum muricatum total saponins is directly laid on the drying tray in the vacuum drying oven, the paving thickness of the clear paste of Solanum muricatum total saponins is 3 - 5 cm, the vacuum degree of the vacuum drying oven is 0.04 - 0.08 Mpa, the temperature of the vacuum drying oven is 80°C, and the drying time is 3 - 4 h. Then it is crushed and mixed evenly. After crushing, the crushed Solanum muricatum total saponin powder clear paste needs to be screened. The mesh number of the sieve used during screening is 100 meshes, and the mixing time is ≥ 40 min to obtain Solanum muricatum total saponin powder; the environmental conditions in the drying chamber of the vacuum drying oven include: the cleanliness level is Class D, the temperature is 18 - 26°C, the relative humidity is 45 - 65%, and the pressure difference is a relative negative pressure;

[0040] The three-dimensional mixer is placed in the mixing chamber. The environmental conditions of the mixing chamber include: the cleanliness level is Class D, the temperature is 18 - 26°C, the relative humidity is 45 - 65%, and the pressure difference is a relative negative pressure.

[0041] Repeat the above steps 28 times to complete the extraction of Solanum muricatum total saponin powder from 11,760 kg of Solanum muricatum pulp, and obtain 89 - 94 kg of Solanum muricatum total saponin powder in the form of yellowish-brown to brownish-black powder. The yield reaches 0.76 - 0.80%. The extracted Solanum muricatum total saponin powder can be prepared into tableted medicaments. The amount of Solanum muricatum total saponin powder contained in each tablet is 25 g. The prepared medicaments can have a validity period of up to 36 months under sealed and moisture-proof conditions.

[0042] There are two multifunctional extractors in step S1, which are purchased from Changchun Pharmaceutical Machinery Factory. The output ends of the two multifunctional extractors are connected in parallel to the input end of the plate-type sedimentation centrifuge. The two multifunctional extractors are exactly the same. One of them has a volume of 3000 L and a production capacity of 2700 L per time; the model of the plate-type sedimentation centrifuge in step S2 is PSC800-NC, and its production capacity is 135 kg. It is purchased from Liaoning Zhonglian Pharmaceutical Machinery Co., Ltd.; the two multifunctional extractors and the plate-type sedimentation centrifuge are connected in series and are all set in the water extraction and centrifugation chamber;

[0043] In step S3, the resin column was purchased from Jilin Jinpeng Pharmaceutical Machinery Complete Equipment Co., Ltd., model 0.88M³; in step S4, the production capacity of the single-effect concentrator-evaporator was 1000 kg / h, and it was purchased from Jilin Jinpeng Pharmaceutical Machinery Complete Equipment Co., Ltd.; the resin column and the single-effect concentrator-evaporator were both arranged in the ethanol extraction and concentration chamber;

[0044] In step S5, the model of the vacuum drying oven was FZG-15B. A total of 4 vacuum drying ovens were arranged in the mixing and drying chamber. They were purchased from Jiangsu Fanqun Drying Equipment Factory, Changzhou Yutong Drying Equipment Factory, and Changzhou Yimin Drying Equipment Co., Ltd. Their production capacity was 60 - 100 kg / h; the model of the high-efficiency pulverizer was 30B, and it was purchased from Changzhou Yibu Drying Equipment Factory. Its production capacity was 100 - 200 kg / h. The high-efficiency pulverizer was arranged in the powder sieve chamber; the model of the three-dimensional mixer was HS-600, and they were connected in series with each other. Its production capacity was 240 kg. The three-dimensional mixer was arranged in the mixing chamber.

[0045] The intermediate product, the total ginsenosides extract of Solanum muricatum, prepared in step S3 could be sealed and stored for 12 months at room temperature; the intermediate product, the clear paste of total ginsenosides of Solanum muricatum, prepared in step S4 could be sealed and stored for 3 months under the condition of environmental temperature of -8 to 3°C.

[0046] In the method provided in this embodiment, step S6 was carried out in a Class D clean room. At the same time, after being mixed evenly in step S6, the obtained total ginsenosides powder of Solanum muricatum needed to be detected. The specific detection conditions included the following standards: the concentration of ginsenoside Re in the total ginsenosides powder of Solanum muricatum was not less than 650 mg / g, and the concentration of aerobic bacteria in microorganisms was ≤800 cfu / g, the concentration of molds and yeasts was ≤80 cfu / g, and Escherichia coli was not detected; the total ginsenosides powder meeting the above conditions was transported to the fine material warehouse for storage. The total ginsenosides powder of Solanum muricatum could be made into tablet preparations and sealed to prevent moisture for 36 months. Each tablet preparation contained 25 g of the total ginsenosides powder of Solanum muricatum.

[0047] The flow chart of an extraction and filtration method for the total ginsenosides powder of Solanum muricatum provided in this embodiment is as Figure 1 shown, and the working principle diagram is as Figure 2 shown.

[0048] The calculation method for the qualified rate of the process of the intermediate product, the clear paste of total ginsenosides of Solanum muricatum, prepared in step S4 was the mass ratio of the clear paste of total ginsenosides of Solanum muricatum to the input Solanum muricatum pulp. If the calculation result was between 2.0% and 2.8%, it was considered that the process was qualified;

[0049] In step S5, the calculation method for the qualified rate of the intermediate product obtained by crushing is the ratio of the total amount of the material after crushing to the total amount of the material before crushing. When the calculation result is ≥ 98.5%, it is considered that the process is qualified; the calculation method for the material balance rate is the ratio of the sum of the total amount of the material after crushing and the waste amount to the total amount of the material before crushing. When the material balance rate is between 98.5% and 100.0%, it is considered qualified.

[0050] In step S5, the calculation method for the qualified rate of the intermediate product obtained by mixing is the ratio of the total amount of the material after mixing to the total amount of the material after crushing. When the calculation result is ≥ 99.5%, it is considered that the process is qualified; the calculation method for the material balance rate is the ratio of the sum of the total amount of the material after mixing and the waste amount to the total amount of the material after crushing. When the material balance rate is between 99.8% and 100.0%, it is considered qualified.

[0051] In this embodiment, the production cycle of the weighing and batching stage in the preliminary preparation is ≤ 1 day, the production cycle of the water extraction stage of the extraction tank is ≤ 8 days, the production cycle of the drying stage is ≤ 1 day, the production cycle of the crushing stage is ≤ 1 day, and the production cycle of the mixing stage is ≤ 1 day.

[0052] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the present invention in each embodiment.

Claims

1. A preparation method of total ginsenoside powder of Solanum muricatum Aiton, characterized in that, It includes the following steps: S1. Put the sapodilla fruit pulp into an extraction tank, then add water for extraction to obtain a sapodilla fruit extract, and then filter the sapodilla fruit extract to obtain a roughly filtered sapodilla fruit medicinal liquid; S2. Add CaO to the roughly filtered sapodilla fruit medicinal liquid prepared in S1 and stir. After adjusting the pH value to 9 - 10, open the steam valve, heat until the roughly filtered sapodilla fruit medicinal liquid boils and maintain it to obtain an alkaline sapodilla fruit medicinal liquid, and then centrifuge the alkaline sapodilla fruit medicinal liquid pump to obtain a centrifuged sapodilla fruit medicinal liquid; S3. Subject the centrifuged sapodilla fruit medicinal liquid prepared in S2 to column chromatography purification, and then sequentially wash the purified centrifuged sapodilla fruit medicinal liquid with water. After eluting until the centrifuged sapodilla fruit medicinal liquid is colorless, perform desorption to obtain a total saponin extract of sapodilla fruit; S4. Place the total saponin extract of sapodilla fruit prepared in S3 in a concentration tank, add ethanol to the concentration tank for concentration to obtain a clear paste of total saponin of sapodilla fruit; S5. Dry the clear paste of total saponin of sapodilla fruit prepared in S4, then pulverize and mix evenly to obtain a powder of total saponin of sapodilla fruit.

2. The extraction and filtration method of the total ginsenoside powder of Solanum muricatum Aiton as claimed in claim 1, wherein In S1, the amount of water added to the extraction tank is 6 times the amount of sapodilla fruit pulp added, and the extraction time is 30 min.

3. The extraction and filtration method of the total ginsenoside powder of Solanum muricatum Aiton according to claim 1, characterized in that In S2, the mass fraction of CaO is 0.7%, and the maintenance time is 30 min.

4. The extraction and filtration method of total ginsenoside powder of Solanum muricatum Aiton as claimed in claim 1, wherein The conditions for the column chromatography in S3 are: in a resin column with an adsorption flow rate of 3 BV / h.

5. The extraction and filtration method of the total ginsenoside powder of Solanum muricatum Aiton according to claim 1, characterized in that, In S3, the water consumption for washing is 10 BV, and the flow rate of water during washing is 4 BV / h; The solvent for desorption is an ethanol solution with a volume fraction of 60%, the solvent consumption is 6 BV, and the flow rate of the solvent during desorption is 2 BV / h.

6. The extraction and filtration method of the total ginsenoside powder of Solanum muricatum Aiton as claimed in claim 1, wherein, In S4, the concentration tank is a single - effect concentration evaporator. The temperature condition for concentration in the single - effect concentration evaporator is 70 - 80 °C, and the vacuum degree of the single - effect concentration evaporator is 0.04 - 0.07 Mpa.

7. The extraction and filtration method of the total ginsenoside powder of Solanum muricatum Aiton as claimed in claim 1, wherein, When the temperature condition of the clear paste of total saponin of sapodilla fruit in S4 is 55 °C, its relative density is 1.1 - 1.

15.

8. A total ginsenoside powder of Solanum muricatum Aiton, characterized in that, Prepared by the preparation method according to any one of claims 1 - 7.

9. Application of the powder of total saponin of sapodilla fruit according to claim 8 in food or pharmaceutical additives.

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