Method for extracting rhizoma polygonati and application thereof

Abstract

The application discloses a kind of huangjing extraction method and application, it is related to the technical field of medicine preparation, the extraction method includes raw material pretreatment, multi-energy field synergistic extraction, gradient alcohol precipitation and drying screening step;Multi-energy field synergistic extraction adopts pulse ultrasonic-intermittent microwave-cellulase / pectinase complex enzyme three-energy field synchronous synergistic, control microwave, ultrasonic and enzymolysis parameter, gradient alcohol precipitation is regulated ethanol concentration in three steps.This method can significantly improve the dissolution rate of polysaccharide, total saponin and total flavone in Huangjing, and the extract can be prepared into Huangjing granules.The method and the extract can be used to prepare medicines or health foods for enhancing immunity, regulating blood sugar, regulating blood lipids, anti-fatigue and antioxidant.The process is efficient and practical.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical preparation technology, and in particular to a method for synergistic extraction of active ingredients from Polygonatum odoratum using pulsed ultrasound-microwave-enzymatic hydrolysis coupling multi-energy field, and the application of this extract in preparing Polygonatum odoratum medicinal granules. Background Technology

[0002] Polygonatum is a perennial herb belonging to the genus Polygonatum in the family Liliaceae. Its rhizome is rich in polysaccharides, saponins, flavonoids, and other active ingredients. It has traditional medicinal value, including tonifying qi and nourishing yin, strengthening the spleen and moistening the lungs, and benefiting the kidneys and replenishing essence. It is a classic tonic herb that is both food and medicine, and has broad application prospects in functional foods, cosmetics, and pharmaceuticals. Among them, the northern variety of Polygonatum sibiricum is known for its nodular shape, firm texture, rich mucilage, and stable active ingredients, making it a representative of authentic medicinal materials.

[0003] Currently, the main methods for extracting the effective components of Polygonatum include water extraction and alcohol extraction, but both have certain limitations. Traditional water extraction is simple and inexpensive, but its extraction efficiency is low, with an effective component extraction rate of only 5%-7%, and the extract contains many impurities, making subsequent separation and purification difficult. While alcohol extraction can improve the extraction rate of saponins, it is less effective at extracting polysaccharides, and the use of organic solvents increases environmental pressure and production costs. Other existing methods for extracting the effective components of Polygonatum also suffer from problems such as high extraction temperatures, long extraction times, high energy consumption, easy degradation of heat-sensitive components, and insufficient dissolution of polysaccharides and saponins. These methods struggle to simultaneously and efficiently retain multiple active ingredients, resulting in low resource utilization, uneven extract efficacy, and an inability to fully reflect the overall medicinal effects of Polygonatum, namely, "tonifying qi and nourishing yin, strengthening the spleen and moistening the lungs, and benefiting the kidneys and replenishing essence."

[0004] Ultrasonic-assisted extraction and microwave-assisted extraction enhance mass transfer through physical fields, which can improve extraction efficiency to some extent. However, when used alone, they still cannot effectively disrupt the dense structure of the Polygonatum cell wall, resulting in insufficient release of active ingredients from the cells. Furthermore, existing ultrasonic or microwave-assisted processes have not been systematically optimized for the tissue structure and component polarity of Polygonatum. The matching degree of parameters such as material-liquid ratio, ultrasonic power, temperature, and time is insufficient, often resulting in polysaccharide degradation, saponin conversion, and flavonoid loss. The extraction rate and stability are difficult to meet the requirements of large-scale production.

[0005] Therefore, developing an extraction method that can simultaneously and efficiently extract multiple active ingredients from Polygonatum odoratum, with a green and environmentally friendly extraction process and low cost, and its application, is of great significance for promoting the high-value utilization of Polygonatum odoratum resources. Summary of the Invention

[0006] To address the problems of low extraction efficiency, easy destruction of active ingredients, lack of quality control of multiple indicators, and disconnect between process and formulation in existing technologies, this invention provides a multi-energy field synergistic extraction method based on pulsed ultrasound-microwave-cellulase-pectinase complex enzymatic hydrolysis, which achieves efficient dissolution of active ingredients and structural protection, and is used to prepare Polygonatum sibiricum granules with good formability and high stability.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0008] A method for extracting Polygonatum sibiricum includes the following steps:

[0009] Step S1: Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 55-60℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 50-100 mesh sieve, and place it in a desiccator for later use;

[0010] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction 2-3 times, and combining the supernatants to obtain Polygonatum extract; placing the extract in a 90-95℃ water bath for 10-15 minutes for enzyme inactivation treatment;

[0011] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0012] Preferably, the microwave power is 100~150 W, with a working time of 3-5 seconds and an interval of 8~12 seconds.

[0013] Preferably, the ultrasonic power of the pulsed ultrasound is 250-300W, and the duty cycle is 50%-70%.

[0014] Preferably, the extraction temperature for the synergistic extraction is 60-65℃, and the extraction time is 40-50 min.

[0015] Preferably, the material-to-liquid ratio for the synergistic extraction is 1:(30-40).

[0016] Preferably, the extractant for synergistic extraction is an acetate-sodium acetate buffer solution containing cellulase and pectinase, with a pH of 4.5 to 5.5.

[0017] Preferably, the mass ratio of cellulase to pectinase is (2.5-3.5):2; the total enzyme dosage is 1.5%~2.0% of the medicinal material weight; and the cellulase activity is ≥10000U / g and the pectinase activity is ≥5000U / g.

[0018] Preferably, the gradient alcohol precipitation specifically involves: first, adding anhydrous ethanol to bring the ethanol concentration of the system to 28-32 wt%, stirring evenly, letting it stand for 12-16 hours, and centrifuging to obtain the first precipitate and supernatant; then, adding more anhydrous ethanol to the supernatant to bring the ethanol concentration of the system to 58-62 wt%, stirring evenly, letting it stand for 12-16 hours, and centrifuging to obtain the second precipitate and supernatant; finally, adding more anhydrous ethanol to the supernatant to bring the ethanol concentration of the system to 88-92 wt%, stirring evenly, letting it stand for 12-16 hours, and centrifuging to obtain the third precipitate.

[0019] Preferably, the drying process specifically involves placing the first precipitate, the second precipitate, and the third precipitate in a vacuum drying oven and drying them to constant weight at 60-65°C and a vacuum degree of -0.08 to -0.1 MPa.

[0020] Preferably, the sieving is performed through an 80-120 mesh sieve.

[0021] Another objective of this invention is to provide a Polygonatum granule prepared from the extract obtained by the above extraction method, wherein the ingredients are formulated in the following mass ratio: 280-320 parts Polygonatum extract, 100-140 parts resistant dextrin, 50-70 parts mannitol, and 8-12 parts crospovidone, and granulation is performed using ethanol with a mass percentage concentration of 93-97% as a wetting agent.

[0022] Another object of the present invention is to provide an application of the method described above in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0023] The beneficial effects of adopting the above technical solution are as follows:

[0024] (1) This invention pioneered a synchronous and synergistic extraction process using pulsed ultrasound, intermittent microwave, and compound enzymatic hydrolysis, overcoming the limitations of simple superposition of single and dual energy fields. This process achieves multi-level directional cell wall disruption, rather than the single action of traditional physical disruption or enzymatic hydrolysis. This synergistic mechanism can reduce the mass transfer resistance of Polygonatum tissue by more than 70%, allowing three types of active ingredients with significant polarity differences—polysaccharides, steroidal saponins, and total flavonoids—to be simultaneously and efficiently dissolved. Their overall yield is significantly improved compared to the traditional water decoction method, resulting in a significant improvement in extraction efficiency.

[0025] (2) This invention achieves an extraction temperature of ≤65℃ throughout the process by using intermittent microwave output and precise control of ultrasonic duty cycle. While maintaining high extraction efficiency, it also takes into account the structural integrity of heat-sensitive components, thus solving the long-standing contradiction in the industry that "high-efficiency extraction requires high temperature and low-temperature extraction requires low efficiency." Compared with conventional single or combined ultrasonic, microwave, and enzymatic hydrolysis processes, this method achieves a molecular weight retention rate of ≥92% for Polygonatum polysaccharides and a retention rate of ≥90% for the active structures of saponins and flavonoids, significantly reducing component degradation and isomerization, and realizing the dual benefits of "high-efficiency dissolution + high-activity retention".

[0026] (3) The multi-field synergistic system of the present invention can significantly reduce the dissolution ratio of viscous impurities such as starch, mucilage, and pectin in the extract. Combined with the gradient alcohol precipitation process, the total amount of impurities in the extract is significantly reduced, the fluidity is greatly improved, and the hygroscopicity is significantly decreased. This effect is not simply achieved by removing impurities through gradient alcohol precipitation, but is the synergistic result of selective dissolution of effective components and inhibition of impurity dissolution by the multi-field system. It effectively solves the technical problems of high viscosity, difficulty in drying, easy moisture absorption, and poor formulation of Polygonatum extract, and provides a high-quality raw material basis for subsequent particle preparation.

[0027] (4) This invention integrates multi-field extraction, alcohol precipitation purification, low-temperature drying, and formulation granulation into one process, which significantly shortens the extraction time and reduces the overall energy consumption. At the same time, the prepared Polygonatum granules have a high forming rate, high content uniformity, and significantly better stability than products produced by existing processes. The benefits of this integrated technology, which is highly efficient, low-energy, and of high finished product quality, are the overall gains resulting from the deep coupling of multi-field and formulation processes. Detailed Implementation

[0028] To enable those skilled in the art to better understand the technical solutions of the present invention and to make the above-mentioned features, objectives, and advantages of the present invention clearer and easier to understand, the present invention will be further described below with reference to embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention.

[0029] Example 1

[0030] A method for extracting Polygonatum sibiricum includes the following steps:

[0031] Step S1, Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 55℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 50-mesh sieve, and place it in a desiccator for later use;

[0032] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction twice, and combining the supernatants to obtain Polygonatum extract; placing the extract in a 90℃ water bath for 10 minutes for enzyme inactivation treatment;

[0033] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0034] The microwave power is 100W, operating for 3 seconds with an 8-second interval; the pulsed ultrasound power is 250W with a duty cycle of 50%; the co-extraction temperature is 60℃, and the extraction time is 40 minutes; the material-to-liquid ratio for co-extraction is 1:30; the extraction solution for co-extraction is an acetate-sodium acetate buffer solution containing cellulase and pectinase, with a pH of 4.5; the mass ratio of cellulase to pectinase is 2.5:2; the total enzyme dosage is 1.5% of the drug material weight; the cellulase activity is ≥10000U / g, and the pectinase activity is ≥5000U / g.

[0035] The gradient ethanol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 28 wt%, stirred evenly, and allowed to stand for 12 hours. The mixture is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 58 wt%, stirred evenly, and allowed to stand for 12 hours. The mixture is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 88 wt%, stirred evenly, and allowed to stand for 12 hours. The mixture is then centrifuged to obtain the third precipitate. The drying process involves placing the first, second, and third precipitates in a vacuum drying oven and drying them at 60°C and a vacuum of -0.08 MPa until constant weight. The sieving process involves passing the precipitate through an 80-mesh sieve.

[0036] A granule of Polygonatum sibiricum prepared from an extract obtained by the above extraction method is prepared by the following mass ratio: 280 parts Polygonatum sibiricum extract, 100 parts resistant dextrin, 50 parts mannitol, and 8 parts crospovidone, and granulation is carried out using ethanol with a mass percentage concentration of 93% as a wetting agent.

[0037] The application of the method described herein in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0038] Example 2

[0039] A method for extracting Polygonatum sibiricum includes the following steps:

[0040] Step S1, Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 56℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 60-mesh sieve, and place it in a desiccator for later use;

[0041] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction twice, and combining the supernatants to obtain Polygonatum extract; placing the extract in a 92℃ water bath for 12 minutes for enzyme inactivation treatment;

[0042] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0043] The microwave power is 120W, operating for 3.5s with a 9s interval; the pulsed ultrasound power is 260W with a duty cycle of 55%; the co-extraction temperature is 62℃, and the extraction time is 43min; the material-to-liquid ratio of the co-extraction is 1:33; the extraction solution is an acetate-sodium acetate buffer containing cellulase and pectinase, pH=4.8; the mass ratio of cellulase to pectinase is 2.7:2; the total enzyme dosage is 1.7% of the drug material weight; the cellulase activity is ≥10000U / g, and the pectinase activity is ≥5000U / g.

[0044] The gradient alcohol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 29 wt%, stirred evenly, and allowed to stand for 13 hours. The mixture is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 59 wt%, stirred evenly, and allowed to stand for 13 hours. The mixture is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 89 wt%, stirred evenly, and allowed to stand for 13 hours. The mixture is then centrifuged to obtain the third precipitate. The drying process involves placing the first, second, and third precipitates in a vacuum drying oven and drying them at 62°C and a vacuum of -0.085 MPa until constant weight. The sieving process involves passing the precipitate through a 90-mesh sieve.

[0045] A granule of Polygonatum sibiricum prepared from an extract obtained by the above extraction method is prepared by the following mass ratio: 290 parts Polygonatum sibiricum extract, 110 parts resistant dextrin, 55 parts mannitol, and 9 parts crospovidone, and granulation is carried out using ethanol with a mass percentage concentration of 94% as a wetting agent.

[0046] The application of the method described herein in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0047] Example 3

[0048] A method for extracting Polygonatum sibiricum includes the following steps:

[0049] Step S1: Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 58℃ until the moisture content is ≤9.0%, pulverize it and pass it through an 80-mesh sieve, and place it in a desiccator for later use;

[0050] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction 3 times, and combined supernatants to obtain Polygonatum extract; place the extract in a 93℃ water bath for 13 minutes to inactivate the enzyme;

[0051] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0052] The microwave power is 130W, operating for 4 seconds with a 10-second interval; the pulsed ultrasound power is 280W with a duty cycle of 60%; the co-extraction temperature is 63℃, and the extraction time is 45 minutes; the material-to-liquid ratio for co-extraction is 1:35; the extraction solution for co-extraction is an acetate-sodium acetate buffer solution containing cellulase and pectinase, pH=5; the mass ratio of cellulase to pectinase is 3:2; the total enzyme dosage is 1.8% of the drug material weight; the cellulase activity is ≥10000U / g, and the pectinase activity is ≥5000U / g.

[0053] The gradient ethanol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 30 wt%, stirred evenly, and allowed to stand for 14 hours. The mixture is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 60 wt%, stirred evenly, and allowed to stand for 14 hours. The mixture is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 90 wt%, stirred evenly, and allowed to stand for 14 hours. The mixture is then centrifuged to obtain the third precipitate. The drying process involves placing the first, second, and third precipitates in a vacuum drying oven and drying them at 63°C and a vacuum of -0.09 MPa until constant weight. The sieving process involves passing the precipitate through a 100-mesh sieve.

[0054] A granule of Polygonatum sibiricum prepared from an extract obtained by the above extraction method is prepared by the following mass ratio: 300 parts Polygonatum sibiricum extract, 120 parts resistant dextrin, 60 parts mannitol, and 10 parts crospovidone, and granulation is carried out using 95% ethanol as a wetting agent.

[0055] The application of the method described herein in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0056] Example 4

[0057] A method for extracting Polygonatum sibiricum includes the following steps:

[0058] Step S1, Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 59℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 90-mesh sieve, and place it in a desiccator for later use;

[0059] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction 3 times, and combined supernatants to obtain Polygonatum extract; place the extract in a 94℃ water bath for 14 min to inactivate enzymes;

[0060] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0061] The microwave power is 140W, operating for 4.5s with an 11s interval; the pulsed ultrasound power is 290W with a duty cycle of 65%; the co-extraction temperature is 64℃, and the extraction time is 48min; the material-to-liquid ratio of the co-extraction is 1:38; the extraction solution is an acetate-sodium acetate buffer containing cellulase and pectinase, pH=5.3; the mass ratio of cellulase to pectinase is 3.3:2; the total enzyme dosage is 1.9% of the drug material weight; the cellulase activity is ≥10000U / g, and the pectinase activity is ≥5000U / g.

[0062] The gradient ethanol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 31 wt%, stirred evenly, and allowed to stand for 15 hours. The mixture is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 61 wt%, stirred evenly, and allowed to stand for 15 hours. The mixture is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 91 wt%, stirred evenly, and allowed to stand for 15 hours. The mixture is then centrifuged to obtain the third precipitate. The drying process involves placing the first, second, and third precipitates in a vacuum drying oven and drying them at 64°C and a vacuum of -0.095 MPa until constant weight. The sieving process involves passing the precipitate through a 110-mesh sieve.

[0063] A granule of Polygonatum sibiricum prepared from an extract obtained by the above extraction method is prepared by the following mass ratio: 310 parts Polygonatum sibiricum extract, 130 parts resistant dextrin, 65 parts mannitol, and 11 parts crospovidone, and granulated with 96% ethanol as a wetting agent.

[0064] The application of the method described herein in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0065] Example 5

[0066] A method for extracting Polygonatum sibiricum includes the following steps:

[0067] Step S1, Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 60℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 100-mesh sieve, and place it in a desiccator for later use;

[0068] Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction 3 times, and combined supernatants to obtain Polygonatum extract; place the extract in a 95℃ water bath for 15 minutes to inactivate the enzyme;

[0069] Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

[0070] The microwave power is 150 W, operating for 5 seconds with a 12-second interval; the pulsed ultrasound power is 300 W with a duty cycle of 70%; the co-extraction temperature is 65℃, and the extraction time is 50 min; the material-to-liquid ratio of the co-extraction is 1:40; the extraction solution is an acetate-sodium acetate buffer containing cellulase and pectinase, pH=5.5; the mass ratio of cellulase to pectinase is 3.5:2; the total enzyme dosage is 2.0% of the drug material weight; the cellulase activity is ≥10000 U / g, and the pectinase activity is ≥5000 U / g.

[0071] The gradient ethanol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 32 wt%, stirred evenly, and allowed to stand for 16 hours. The mixture is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 62 wt%, stirred evenly, and allowed to stand for 16 hours. The mixture is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 92 wt%, stirred evenly, and allowed to stand for 16 hours. The mixture is then centrifuged to obtain the third precipitate. The drying process involves placing the first, second, and third precipitates in a vacuum drying oven and drying them at 65°C and a vacuum of -0.1 MPa until constant weight. The sieving process involves passing the precipitate through a 120-mesh sieve.

[0072] A granule of Polygonatum sibiricum prepared from an extract obtained by the above extraction method is prepared by the following mass ratio: 320 parts Polygonatum sibiricum extract, 140 parts resistant dextrin, 70 parts mannitol, and 12 parts crospovidone, and granulated with 97% ethanol as a wetting agent.

[0073] The application of the method described herein in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

[0074] Comparative Example 1

[0075] A method for extracting Polygonatum sibiricum is basically the same as that in Example 5, except that traditional water decoction is used instead of multi-field synergistic extraction. The water decoction temperature is 98°C, the material-to-liquid ratio is 1:10, and the time is 3 hours.

[0076] Comparative Example 2

[0077] A method for extracting Polygonatum sibiricum is basically the same as that in Example 5, except that a single ultrasound is used instead of pulsed ultrasound-intermittent microwave, and the ultrasound power is 300W.

[0078] Comparative Example 3

[0079] A method for extracting Polygonatum sibiricum is basically the same as that in Example 5, except that a single microwave is used instead of pulsed ultrasound-intermittent microwave, and the microwave power is 150W.

[0080] Comparative Example 4

[0081] A method for extracting Polygonatum sibiricum is basically the same as that in Example 5, except that a single enzymatic hydrolysis is used instead of a pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis three-energy field.

[0082] The following experimental methods were used to analyze the components of each sample of Polygonatum sibiricum extract. The test solution was a solution with a total volume of 100 mL (the mass of Polygonatum sibiricum from northern China was 1 g) formed by dissolving each sample of Polygonatum sibiricum extract in water. The test results are shown in Table 1.

[0083] (1) Determination of Polysaccharide Content in Polygonatum sibiricum (Phenol-Sulfuric Acid Method): Accurately pipette 1.0 mL of the test solution into a stoppered test tube, add 1.0 mL of 5% phenol solution, shake well, quickly add 5.0 mL of concentrated sulfuric acid, let stand for 10 min, shake well, place in a boiling water bath for 15 min, remove and cool to room temperature; use distilled water as a blank control, and measure the absorbance at a wavelength of 582 nm. Calculate the polysaccharide content in the test sample according to the glucose standard curve.

[0084] (2) Determination of total saponin content (vanillin-perchloric acid method): Accurately pipette 1.0 mL of the test solution, evaporate to dryness in a water bath, add 0.2 mL of 5% vanillin-glacial acetic acid solution and 0.8 mL of perchloric acid, shake well, place in a 60℃ water bath for 15 min, cool in an ice bath, add 5.0 mL of glacial acetic acid, and shake well. Measure the absorbance at a wavelength of 540 nm, and calculate the total saponin content according to the diosgenin standard curve.

[0085] (3) Determination of total flavonoid content (sodium nitrite-aluminum nitrate colorimetric method): Accurately pipette 1.0 mL of the test solution, add 0.3 mL of 5% NaNO2 solution, shake well, and let stand for 6 min; add 0.3 mL of 10% Al(NO3)3 solution, shake well, and let stand for 6 min; then add 2.0 mL of 1 mol / L NaOH solution, add water to make up to 10 mL, and let stand for 15 min; measure the absorbance at a wavelength of 510 nm, and calculate the total flavonoid content according to the rutin standard curve.

[0086] Table 1. Component Analysis Results of Polygonatum Extract

[0087]

[0088] As can be seen from the data in Table 1, Example 5, which uses a pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis three-energy field synchronous synergistic extraction method, showed that the contents of Polygonatum polysaccharide (25.99%), total saponins (7.65%), and total flavonoids (0.61%) were significantly higher than those of the comparative examples. Among them, the contents of the three components in Comparative Example 1 (traditional water decoction method) were the lowest, while the contents of the components in Comparative Example 2 (single ultrasound), Comparative Example 3 (single microwave), and Comparative Example 4 (single enzymatic hydrolysis) were between those of Example 5 and Comparative Example 1. This fully demonstrates that the multi-energy field synergistic extraction process can significantly improve the dissolution rate of active ingredients in Polygonatum compared with traditional water decoction and single extraction methods.

[0089] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of this invention is defined by the appended claims and their equivalents.

Claims

1. A method for extracting Polygonatum sibiricum, characterized in that, Includes the following steps: Step S1: Raw material pretreatment: Take the northern chicken head polygonatum medicinal material, clean and slice it, vacuum dry it at 55-60℃ until the moisture content is ≤9.0%, pulverize it and pass it through a 50-100 mesh sieve, and place it in a desiccator for later use; Step S2, Multi-field Synergistic Extraction: Simultaneous synergistic extraction using pulsed ultrasound-intermittent microwave-cellulase / pectinase complex enzymatic hydrolysis in three energy fields; centrifugation, repeated extraction 2-3 times, and combining the supernatants to obtain Polygonatum extract; placing the extract in a 90-95℃ water bath for 10-15 minutes for enzyme inactivation treatment; Step S3, gradient alcohol precipitation and drying and sieving: Cool the enzyme-inactivated extract to room temperature, and then perform gradient alcohol precipitation, drying and sieving in sequence to obtain fine powder of Polygonatum extract.

2. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The microwave power is 100~150 W, with a working time of 3~5 seconds and an interval of 8~12 seconds.

3. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The pulsed ultrasound has an ultrasonic power of 250-300W and a duty cycle of 50%-70%.

4. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The extraction temperature for the synergistic extraction is 60-65℃, and the extraction time is 40-50 min.

5. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The material-to-liquid ratio for the synergistic extraction is 1:(30-40).

6. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The extractant for the synergistic extraction is an acetate-sodium acetate buffer solution containing cellulase and pectinase, with a pH of 4.5-5.5; the mass ratio of cellulase to pectinase is (2.5-3.5):2; the total enzyme dosage is 1.5%-2.0% of the drug material weight; the cellulase activity is ≥10000U / g and the pectinase activity is ≥5000U / g.

7. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The gradient ethanol precipitation process is as follows: first, anhydrous ethanol is added to bring the ethanol concentration of the system to 28-32 wt%, stirred evenly, and allowed to stand for 12-16 hours. The system is then centrifuged to obtain the first precipitate and supernatant. Next, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 58-62 wt%, stirred evenly, and allowed to stand for 12-16 hours. The system is then centrifuged to obtain the second precipitate and supernatant. Finally, anhydrous ethanol is added to the supernatant to bring the ethanol concentration of the system to 88-92 wt%, stirred evenly, and allowed to stand for 12-16 hours. The system is then centrifuged to obtain the third precipitate.

8. The method for extracting Polygonatum sibiricum according to claim 1, characterized in that, The drying process specifically involves placing the first, second, and third precipitates in a vacuum drying oven and drying them to constant weight at 60-65°C and a vacuum of -0.08 to -0.1 MPa; the sieving process involves passing the precipitates through an 80-120 mesh sieve.

9. A Polygonatum sibiricum granule prepared from an extract obtained by the extraction method according to any one of claims 1-8, characterized in that, The ingredients are formulated according to the following mass ratio: 280-320 parts of Polygonatum extract, 100-140 parts of resistant dextrin, 50-70 parts of mannitol, and 8-12 parts of crospovidone. Granulation is carried out using ethanol with a mass percentage concentration of 93-97% as a wetting agent.

10. The application of the method according to any one of claims 1-8 in the preparation of pharmaceuticals or health foods that enhance immunity, regulate blood sugar, regulate blood lipids, combat fatigue, and have antioxidant properties.

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