Preparation process of rhizoma polygonati and fructus lycii extract

By adding dodecyl glucoside and ethanol to the extraction process of polina and wolfberry and irradiation treatment, the extraction rate of flavonoids and polysaccharides is improved, and the problem of poor effect of existing polina and wolfberry compositions is solved, achieving the realization of the realization of platinum and wolfberry compositions. It has significant tonic effects of Polygonatum and wolfberry extract.

CN119157826AActive Publication Date: 2024-12-20INST OF MEDICINAL PLANTS YUNNAN ACAD OF AGRI SCI
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Patent Information

Application Number
CN202411342965.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-25
Publication Date
2024-12-20
Estimated Expiration
2044-09-25

AI Technical Summary

Technical Problem

The existing Polygonatum and wolfberry compositions have poor effects in nourishing the spleen, moistening the lungs, promoting body fluid, calming the mind, and replenishing deficiency. How to improve its nourishing effect.

Method used

A specific preparation process is adopted, including combining dried polina and wolfberry tablets with water, dodecyl glucoside and ethanol, extracting by heating, and irradiation during the extraction process, improving the extraction rate and effectiveness of polysaccharides and flavonoids. In order to produce Polygonatum and wolfberry extract.

Benefits of technology

By improving the extraction rate and effectiveness of polysaccharides and flavonoids, the effect of Polygonatum and wolfberry extracts to replenish essence, blood and strengthen qi is enhanced, and its therapeutic effect on symptoms such as spleen and stomach qi deficiency, body fatigue, and stomach yin deficiency is enhanced.

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Abstract

The invention discloses a preparation process of rhizoma polygonati and fructus lycii extract, and belongs to the technical field of traditional Chinese medicine extraction. The preparation process comprises the following steps: adding dried and crushed polygonatum kingianum decoction pieces and Chinese wolfberry fruit decoction pieces into water, adding dodecyl polyglucoside, heating and extracting, irradiating while heating and extracting, then adding ethanol, heating and extracting, irradiating while heating and extracting, heating an extracting solution to remove ethanol, and then concentrating to obtain a concentrated solution; the rhizoma polygonati and fructus lycii extract is prepared. By adopting a specific preparation process, effective components in the polygonatum kingianum decoction pieces and the Chinese wolfberry fruit decoction pieces are fully extracted, so that the tonifying effect of the polygonatum kingianum and Chinese wolfberry fruit composition is improved. The rhizoma polygonati and fructus lycii extract extracted by the preparation process can be prepared into edible rhizoma polygonati and fructus lycii paste by directly adding honey, and the obtained rhizoma polygonati and fructus lycii paste has the effects of tonifying essence and blood and strengthening qi.
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Description

Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to a preparation process of polygonatum and wolfberry extract. Background Art

[0002] The present invention discloses a dried rhizome of Polygonatum kingianum Coll. et Hemsl Delar. ex Redoute, a plant of the Liliaceae family. The rhizome is nearly cylindrical or nearly beaded, and the nodules are sometimes irregularly rhombus-shaped, hypertrophic, and 1-3 cm in diameter. The stem is 1-3 m high, and the top is in a climbing shape. The leaves are whorled, with 3-10 leaves per whorl, strip-shaped, strip-shaped wavy needle-shaped or lanceolate, 6-25 cm long, 3-30 mm wide, and fist-shaped at the tip. The inflorescence has 2-4 flowers, the peduncle is drooping, 1-2 cm long, the pedicel is 0.5-1.5 cm long, the bracts are membranous, tiny, and usually located at the bottom of the pedicel; the perianth is pink, 18-25 mm long, and the lobes are 3-5 mm long; the filaments are 3-5 mm long, filamentous or flat on both sides, and the anthers are 4-6 mm long; the ovary is 4-6 mm long, and the style is 10-14 mm long. The berries are red, 1-1.5 cm in diameter, and contain 7-12 seeds. The flowering period is from March to May, and the fruiting period is from September to October.

[0003] Yunnan Polygonatum, a medicinal and edible herb, is the dried rhizome of Yunnan Polygonatum, a plant of the Liliaceae family. It is sweet and neutral in nature. It enters the spleen, lung, and kidney meridians. It has the effects of replenishing qi and nourishing yin, strengthening the spleen, moistening the lungs, and benefiting the kidneys. It is used for spleen and stomach qi deficiency, fatigue, insufficient stomach yin, dry mouth and poor appetite, dry cough due to lung deficiency, hemoptysis due to fatigue, insufficient essence and blood, soreness of the waist and knees, premature graying of hair, internal heat and thirst, etc.

[0004] Wolfberry (Lycium chinenseMiller), a perennial woody plant of the genus Lycium in the Solanaceae family, has thin, weak, bowed or drooping branches, and is light gray; the leaves are oval; the flowers grow solitary or in pairs in the axils of leaves on long branches; the fruit is an oval berry red; the flowering period is June-July; the fruiting period is August-October.

[0005] Chinese medicine wolfberry is the dried mature fruit of the Solanaceae plant wolfberry, which is flat in nature and sweet in taste. It enters the liver meridian, kidney meridian and lung meridian. It has the effects of nourishing the liver and kidney, improving sperm and improving eyesight. It is used for liver and kidney yin deficiency, soreness of waist and knees, dizziness, blurred vision and excessive tears, consumptive cough, thirst, spermatorrhea and other symptoms.

[0006] The prior art has been about the combined use of polygonatum and wolfberry for tonifying the spleen, moistening the lungs, promoting the production of body fluids, calming the nerves, and replenishing deficiency, but the tonic effect is poor. How to improve the tonic effect of the polygonatum and wolfberry combination is a problem that technicians in this field need to solve. Summary of the invention

[0007] The purpose of the present invention is to provide a preparation process of polygonatum and wolfberry extract. By adopting a specific preparation process, the effective components in polygonatum and wolfberry are fully extracted, thereby improving the tonic effect of the polygonatum and wolfberry composition.

[0008] To achieve the above object, the present invention provides the following technical solutions:

[0009] One of the technical solutions of the present invention is to provide a preparation process of polygonatum and wolfberry extract, comprising the following steps:

[0010] Dried and crushed Yunnan polygonatum and wolfberry slices are added into water, dodecyl glucoside is added, and the extraction is carried out by heating, and irradiation is performed while the extraction is carried out by heating. Then, ethanol is added, and the extraction is carried out by heating, and irradiation is performed while the extraction is carried out. The extract is heated to remove the ethanol, and then concentrated to obtain polygonatum and wolfberry extracts.

[0011] Preferably, the mass ratio of the Yunnan Polygonatum sibiricum slices to the Chinese wolfberry slices is 10-15:5-15.

[0012] Preferably, the amount of water added is 20 to 30 times the total mass of the Yunnan Polygonatum sibiricum and Lycium barbarum slices.

[0013] Preferably, the added amount of the dodecyl glucoside is 2-3% of the total mass of the Yunnan Polygonatum sibiricum and Lycium barbarum slices.

[0014] Preferably, the temperature for heating and extraction after adding water is 95-100° C. and the time is 45-75 min.

[0015] Preferably, the irradiation dosage during heating extraction with water as the extracting liquid is 9 to 11 kGy.

[0016] The effects of the irradiation doses of 10 kGy and 9 or 11 kGy described in the examples of the present invention are not much different.

[0017] Preferably, the amount of ethanol added is such that the ethanol content of the extract is adjusted to 70-75 vol.%.

[0018] More preferably, the temperature of the heating extraction after adding ethanol is 70-80° C. and the time is 45-75 min.

[0019] Preferably, the amount of irradiation during heating extraction after adding ethanol is 6 to 8 kGy.

[0020] The effects of the irradiation doses of 7 kGy and 6 or 8 kGy described in the examples of the present invention are not much different.

[0021] The second technical solution provided by the present invention is to provide a polygonatum and wolfberry paste, which is prepared by adding honey to the polygonatum and wolfberry extract obtained by the above-mentioned preparation process.

[0022] The beneficial technical effects of the present invention are as follows:

[0023] The present invention provides a preparation process of polygonatum and wolfberry extract, wherein dodecyl glucoside is added during the extraction process, and the composite carbon contained therein is utilized to reduce the solid-liquid interfacial tension, thereby increasing the dissolution efficiency of polysaccharides and flavonoids and thus improving the extraction rate; further, by introducing irradiation treatment during the extraction process, not only the extraction rate of polysaccharides and flavonoids is enhanced, but also the effectiveness of the extracted polysaccharides is improved.

[0024] The polygonatum sibiricum and wolfberry extracts obtained by the preparation process of the present invention can be directly added with honey to prepare edible polygonatum sibiricum and wolfberry paste, and the obtained polygonatum sibiricum and wolfberry paste has the effects of replenishing essence and blood and strengthening qi. DETAILED DESCRIPTION

[0025] Now, various exemplary embodiments of the present invention are described in detail, and this detailed description should not be considered as a limitation of the present invention, but should be understood as a more detailed description of certain aspects, characteristics and embodiments of the present invention. It should be understood that the terms described in the present invention are only for describing specific embodiments and are not used to limit the present invention.

[0026] In addition, for the numerical range in the present invention, it is understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. The intermediate value in any stated value or stated range, and each smaller range between any other stated value or intermediate value in the range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0027] Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the invention pertains. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein may also be used in the practice or testing of the present invention.

[0028] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0029] The Yunnan polygonatum decoction pieces and wolfberry decoction pieces used in the examples of the present invention and the comparative examples are both Chinese medicinal decoction pieces from the same origin and the same batch, wherein the Yunnan polygonatum decoction pieces are the Yunnan polygonatum decoction pieces that have been steamed and processed nine times.

[0030] Example 1

[0031] Preparation of Polygonatum sibiricum and Lycium barbarum extract:

[0032] The Yunnan polygonatum slices and wolfberry slices dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.5g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0033] Example 2

[0034] Preparation of Polygonatum sibiricum and Lycium barbarum extract:

[0035] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and then 7g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 75vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0036] Example 3

[0037] Preparation of Polygonatum sibiricum and Lycium barbarum extract:

[0038] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.6g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 75vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0039] Comparative Example 1

[0040] Preparation of Polygonatum sibiricum and Lycium barbarum extract (the difference from Example 1 is that the addition of dodecyl glucoside is omitted):

[0041] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water were added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. After reflux extraction, the extract was cooled and filtered. Ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0042] Comparative Example 2

[0043] Preparation of polygonatum and wolfberry extract (the difference from Example 1 is that the irradiation dose selected for the two heating refluxes is 10 kGy):

[0044] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.5g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 10kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0045] Comparative Example 3

[0046] Preparation of polygonatum and wolfberry extract (the difference from Example 1 is that the irradiation dose selected for the two heating refluxes is 7 kGy):

[0047] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.5g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 7kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0048] Comparative Example 4

[0049] Preparation of polygonatum and wolfberry extract (the difference from Example 1 is that the irradiation dose selected for the two heating refluxes is 15 kGy):

[0050] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.5g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 15kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 15kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0051] Comparative Example 5

[0052] Preparation of polygonatum and wolfberry extract (the difference from Example 1 is that the irradiation dose selected for the two heating refluxes is 5 kGy):

[0053] The Yunnan polygonatum slices and wolfberry dried at 60°C were crushed separately, 15g of the crushed Yunnan polygonatum slices and 10g of wolfberry slices were taken, 500mL of water was added, and 0.5g of dodecyl glucoside was added, and refluxed at 100°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 5kGy. The extract was cooled to below 60°C, ethanol was added to adjust the ethanol content in the extract to 70vol.%, and refluxed at 80°C for 60min. During the reflux extraction, electron irradiation was performed using a high-energy electron accelerator with an irradiation dose of 5kGy. After reflux extraction, the extract was cooled and filtered. The ethanol was first distilled out of the filtrate at 78°C, and then concentrated at 100°C to a relative density of 1.3mg / mL to obtain a polygonatum and wolfberry extract.

[0054] The polygonatum sibiricum and wolfberry extracts prepared in Examples 1-3 and Comparative Examples 1-5 were weighed, and the results are shown in Table 1.

[0055] Table 1

[0056]

[0057] The total weight of total flavonoids and total weight of total polysaccharides in the polygonatum and wolfberry extracts prepared in Examples 1-3 and Comparative Examples 1-5 were measured, and the results are shown in Table 2. The determination method is to freeze-dry each group of extracts, and the samples obtained after drying are respectively subjected to total flavonoid content determination and total polysaccharide content determination, and the total weight of total flavonoids and total polysaccharides in the extracts are calculated; wherein, the total flavonoid content is determined by aluminum chloride colorimetry using rutin as a reference substance, and the total polysaccharide content is determined by phenol-sulfuric acid method.

[0058] Table 2

[0059]

[0060] It can be seen from Table 2 that if the addition of dodecyl glucoside is omitted, the extraction rates of total flavonoids and total polysaccharides are reduced. Changing the irradiation dose during extraction will also affect the extraction rates of total flavonoids and total polysaccharides.

[0061] The antioxidant activities of the dried extracts of polygonatum and wolfberry prepared in Examples 1-3 and Comparative Examples 1-5 were measured.

[0062] Determination of hydroxyl radical (·OH) scavenging ability: 1 g of freeze-dried extract of each group was dissolved in 1 L of 30 vol.% ethanol solution, 0.5 mL of the prepared solution was taken, and 6 mmol·L -1 Ferrous sulfate 1mL, 6mmol·L -1 Hydrogen peroxide 2mL, 6mmol·L -1 1 mL of salicylic acid was mixed and placed in a 37°C water bath for 30 min. The solution was adjusted to zero with distilled water and the absorbance was measured at 510 nm and recorded as A.样品 ; Distilled water replaces the extract, recorded as A 空白 ; Distilled water replaces hydrogen peroxide and is recorded as A 对照 ; Calculate the OH removal rate according to formula (1), and the results are shown in Table 4.

[0063] Determination of DPPH free radical (DPPH·) scavenging ability: 1 g of freeze-dried extract of each group was dissolved in 1 L of 30 vol.% ethanol solution, 0.5 mL of the prepared solution was taken, and 0.5 mmol·L -1 3.5 mL of DPPH solution was mixed and allowed to stand at room temperature in the dark for 30 min; the solution was adjusted to zero with anhydrous ethanol and the absorbance was measured at 517 nm and recorded as A 样品 ; Distilled water replaces the extract, recorded as A 空白 ; Anhydrous ethanol replaces DPPH, recorded as A 对照 ; DPPH clearance rate was calculated according to formula (1), and the results are shown in Table 4.

[0064] Clearance rate (%) = [A 空白 -(A 样品 -A 对照 )] / A 空白 ×100% Formula (1)

[0065] Table 3 The scavenging activity of the dried extracts of each group of hydroxyl radicals

[0066]

[0067]

[0068] Table 4 The scavenging activity of DPPH free radicals of each group of dried extracts

[0069]

[0070] From the results in Tables 3 and 4, it can be seen that the antioxidant capacity of the samples obtained in the experimental groups without irradiation or with too large or too small irradiation doses is significantly reduced, indicating that the correct dose of irradiation helps to improve the antioxidant effect of the product. The antioxidant capacity of the freeze-dried extract mainly comes from polysaccharides. The antioxidant data of Comparative Example 2 and Examples 1-3 show that the irradiation dose of 9 to 11 kGy mainly affects the effectiveness of polysaccharides.

[0071] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A preparation process of polygonatum and wolfberry extract, characterized in that: The following steps are involved: Dried and crushed Yunnan polygonatum and wolfberry slices are added into water, dodecyl glucoside is added, and the extraction is carried out by heating, and irradiation is performed while the extraction is carried out by heating. Then, ethanol is added, and the extraction is carried out by heating, and irradiation is performed while the extraction is carried out. The extract is heated to remove the ethanol, and then concentrated to obtain polygonatum and wolfberry extracts.

2. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: The mass ratio of the Yunnan Polygonatum cyrtonema decoction pieces to the wolfberry decoction pieces is 10-15:5-15.

3. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: The amount of water added is 20 to 30 times the total mass of the Yunnan Polygonatum sibiricum and Lycium barbarum slices.

4. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: The added amount of the dodecyl glucoside is 2-3% of the total mass of the Yunnan polygonatum sibiricum decoction pieces and the wolfberry decoction pieces.

5. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: After adding water, the temperature of heating extraction is 95-100°C and the time is 45-75 minutes.

6. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: When water is used as the extracting liquid for heating extraction, the amount of irradiation is 9 to 11 kGy.

7. The preparation process of polygonatum and wolfberry extract according to claim 1, characterized in that: The amount of ethanol added is to adjust the ethanol content of the extract to 70-75 vol.%.

8. The preparation process of polygonatum and wolfberry extract according to claim 7, characterized in that: After adding ethanol, the temperature of heating extraction is 70-80°C and the time is 45-75 minutes.

9. The preparation process of polygonatum sibiricum and wolfberry extract according to claim 1, characterized in that: The amount of irradiation during heating extraction after adding ethanol is 6 to 8 kGy.

10. A polygonatum and wolfberry paste, characterized in that: The extract of polygonatum and wolfberry prepared by the preparation process according to any one of claims 1 to 9 is prepared by adding honey.

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