Gaultheria yunnanensis medicinal material superfine powder as well as preparation method and application thereof

Abstract

The invention provides a gaultheria yunnanensis medicinal material superfine powder as well as a preparation method and application thereof, and belongs to the technical field of traditional Chinese medicinal material processing. The superfine grinding method for the medicinal material of the gaultheria yunnanensis comprises the following steps: 1) taking the medicinal material of the gaultheria yunnanensis, removing impurities, grinding, and drying to obtain a pretreated raw material; 2) mixing the pretreated raw material with a solvent, and performing ultrasonic-vacuum negative pressure synergistic soaking treatment; (3) adding a compound enzyme into the solution subjected to soaking treatment, and carrying out enzymolysis treatment; and (4) filtering the solution subjected to enzymolysis in the step (3), drying filter residues, putting the dried filter residues into a low-temperature ultrafine grinder, and grinding to obtain the gaultheria yunnanensis ultrafine powder. According to the method, deep and mild wall breaking of the cell walls of the gaultheria yunnanensis is realized through three-step cooperation of physics, biology and low-temperature machinery, the extraction efficiency and the extraction speed of subsequent active ingredients can be remarkably improved, meanwhile, heat-sensitive ingredients are effectively protected, and the method has the advantages of being high in extraction rate, low in energy consumption and small in ingredient damage.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine processing technology, and in particular to an ultrafine powder of Dianbaizhu medicinal material, its preparation method and application. Background Technology

[0002] Gaultheria leucocarpa Bl. var. yunnanensis (Franch.) TZHsu, a plant belonging to the genus Gaultheria in the family Ericaceae, is a dried whole plant. It is mainly produced in Yunnan and Guizhou provinces. It has a pungent and bitter taste, and is warm in nature. It possesses the effects of dispelling wind and dampness, promoting blood circulation and relieving pain, and relieving cough and asthma. It is commonly used to treat rheumatic pain, traumatic injuries, cough, and asthma. Modern pharmacological research shows that the active ingredients of Gaultheria leucocarpa mainly include total flavonoids and volatile oils, which are the core material basis for its pharmacological effects.

[0003] The extraction efficiency of active ingredients in traditional Chinese medicine is closely related to the fineness of the powder and the degree of cell wall damage. Traditional pulverization methods have significant drawbacks: First, the heat generated by mechanical pulverization may destroy or volatilize some heat-sensitive active ingredients; second, conventional pulverization has limited particle size, resulting in a low cell wall breakage rate, making it difficult for the solvent to fully penetrate into the cells during subsequent extraction, leading to long extraction time, low extraction efficiency, and high solvent consumption; third, oxidation reactions may be triggered during pulverization, affecting the stability of the components.

[0004] While ultrafine pulverization technology can produce finer powders, the instantaneous high temperatures generated by violent collisions at room temperature are still unfavorable to heat-sensitive components, and the energy consumption is also high. Therefore, developing a pretreatment method that can deeply disrupt cell walls, protect active ingredients, and significantly improve extraction efficiency is of great significance for the high-value utilization of Yunnan white pearl medicinal materials. Summary of the Invention

[0005] The purpose of this invention is to provide a method for ultra-micro pulverization of Yunnan white pearl medicinal material. Through the synergistic effect of three steps—high-frequency ultrasound-vacuum negative pressure soaking, compound enzymatic hydrolysis, and low-temperature ultra-micro pulverization—the cell walls of the medicinal material are deeply and gently broken, thereby significantly improving the extraction rate and speed of subsequent active ingredients and effectively protecting heat-sensitive components.

[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution: This invention provides a method for ultra-fine pulverization of Yunnan white pearl medicinal material, characterized by comprising the following steps: 1) Take Yunnan white pearl medicinal material, remove impurities, pulverize and dry to obtain pretreated raw material; 2) After mixing the pretreated raw materials with the solvent, perform ultrasonic-vacuum negative pressure synergistic immersion treatment; 3) Add a compound enzyme to the soaking solution for enzymatic hydrolysis; 4) Filter the solution after enzymatic hydrolysis in step 3), dry the filter residue, and then pulverize it in a low-temperature ultrafine pulverizer to obtain Yunnan white pearl ultrafine powder.

[0007] Preferably, the pulverization in step 1) is pulverization to 10-20 mesh, and the drying is drying to a moisture content of 8%-12%.

[0008] Preferably, the solvent in step 2) is an ethanol solution with a volume fraction of 30% to 50%, and the amount used is: added at a material-to-liquid ratio of 1:10 to 20 g / mL. The ultrasonic power is 150 to 300 W, the vacuum negative pressure is -0.06 to -0.09 MPa, and the soaking time is 20 to 60 min.

[0009] Preferably, the complex enzyme in step 3) is composed of pectinase, xylanase, cellulase and β-glucosidase in a mass ratio of 1~2:0.5~1:1~3:1~2, and the total amount added is 0.5%~2% of the mass of the pretreated raw materials.

[0010] Preferably, the enzymatic hydrolysis in step 3) is a staged enzymatic hydrolysis. The pH is adjusted to 4.5~5.5. First, pectinase and xylanase are added, and the enzymatic hydrolysis time is 20~30 min. Then, cellulase and β-glucosidase are added and the enzymatic hydrolysis is carried out for 30~40 min. After the enzymatic hydrolysis is completed, the temperature is raised to 85~95℃ and kept at this temperature for 10~15 min to inactivate the enzyme.

[0011] Preferably, the drying in step 4) is to dry the filter residue to a moisture content of 5%~8%, the pulverization temperature is -40℃~-10℃, and the particle size of the pulverized material is ≤15 μm.

[0012] The present invention also provides a method for preparing Yunnan white pearl ultrafine powder by ultrafine pulverization of the aforementioned Yunnan white pearl medicinal material.

[0013] Beneficial effects: The ultrafine pulverization method provided by this invention offers the following advantages: 1. Significantly improved extraction rate: Through a synergistic system of "high-frequency ultrasound-vacuum negative pressure synergistic soaking + compound enzymatic hydrolysis + low-temperature ultrafine pulverization," a continuous process of "deep solvent penetration-complete cell wall disruption-fine particle size-enhanced dissolution" is achieved, increasing the total flavonoid extraction rate from *Phyllostachys edulis* by more than 25% compared to conventional pulverization methods. 2. High retention rate of active ingredients: Low-temperature ultrafine pulverization avoids oxidation of active ingredients caused by heat during pulverization, resulting in a total flavonoid retention rate ≥90%. 3. Shortened extraction time: After cell wall disruption, the mass transfer resistance of active ingredients is significantly reduced, shortening subsequent extraction time by more than 30%. 4. Stable and controllable process: The parameters for each step are clearly defined, suitable for industrial production, and the solvent can be recycled and reused. The compound enzyme is thoroughly inactivated, with no residual risk, meeting the environmental protection and safety requirements for traditional Chinese medicine processing. Detailed Implementation

[0014] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0015] Example 1

[0016] A method for ultra-micro pulverizing Yunnan white pearl medicinal material includes the following steps: Raw material pretreatment: Take 500g of dried Yunnan white pearl medicinal material, remove impurities and grind it to 15 mesh with a universal pulverizer, place it in a 65℃ oven and dry it to a moisture content of 10%, to obtain 480g of pretreated raw material; High-frequency ultrasound-vacuum negative pressure synergistic soaking: Mix the pretreated raw material with 40% ethanol at a material-to-liquid ratio of 1:15 g / mL (add 7200 mL of ethanol), pour into a vacuum ultrasonic reactor, evacuate to -0.075 MPa, turn on high-frequency ultrasound (frequency 150 kHz, power 200 W), and soak for 35 min. Compound enzymatic hydrolysis treatment: Adjust the pH to 4.8 with citrate-sodium citrate buffer, first add 1.5g of pectinase and xylanase (mass ratio 1:0.5), heat to 50℃, and hydrolyze for 25min. Then add 3.5g of cellulase and β-glucosidase (mass ratio 2:1.5), and hydrolyze for 60min. Then heat to 90℃ and incubate for 12min to inactivate. Low-temperature ultrafine pulverization: The filter residue was collected by filtration, dried at 65℃ to a moisture content of 6%, and then fed into a low-temperature airflow pulverizer. The residue was pulverized at -25℃ to a particle size of about 15 μm, yielding 412g of Yunnan white pearl ultrafine powder.

[0017] Example 2

[0018] A method for ultra-micro pulverizing Yunnan white pearl medicinal material includes the following steps: Raw material pretreatment: Take 500g of dried Yunnan white pearl medicinal material, remove impurities and grind it to 10 mesh with a universal pulverizer, dry it at 60℃ until the moisture content is 8%, and obtain 475g of pretreated raw material; High-frequency ultrasound-vacuum negative pressure synergistic soaking: The pretreated raw material was mixed with 45% ethanol at a material-to-liquid ratio of 1:10 g / mL (4750 mL of ethanol was added), the vacuum degree was -0.06 MPa, the ultrasonic frequency was 100 kHz and the power was 150 W, and the soaking time was 20 min. Compound enzymatic hydrolysis treatment: Adjust the pH to 4.8 with citrate-sodium citrate buffer, first add 2g of pectinase and xylanase (mass ratio 1:1), heat to 45℃, and hydrolyze for 25min. Then add 3g of cellulase and β-glucosidase (mass ratio 2:1), and hydrolyze for 40min. Then heat to 95℃ and incubate for 10min to inactivate. Low-temperature ultrafine grinding: The filter residue was collected by filtration, dried at 60°C to a moisture content of 5%, and fed into a low-temperature airflow mill. It was then ground at -40°C to a particle size of approximately 10 μm, yielding 408g of ultrafine powder.

[0019] Example 3

[0020] A method for ultra-micro pulverizing Yunnan white pearl medicinal material includes the following steps: Raw material pretreatment: Take 500g of dried Yunnan white pearl medicinal material, remove impurities and grind it to 20 mesh with a universal pulverizer, place it in a 70℃ oven and dry it to a moisture content of 12% to obtain 485g of pretreated raw material; High-frequency ultrasound-vacuum negative pressure synergistic soaking: Mix the pretreated raw material with 50% ethanol at a material-to-liquid ratio of 1:20 g / mL (add 9700 mL of ethanol), pour into a vacuum ultrasound reactor, evacuate to a vacuum degree of -0.09 MPa, and soak for 60 min at an ultrasound frequency of 200 kHz and a power of 300 W. Compound enzymatic hydrolysis treatment: Adjust the pH to 4.8 with citrate-sodium citrate buffer, first add 1.5g of pectinase and xylanase (mass ratio 1:0.5), heat to 55℃, and hydrolyze for 25min. Then add 3.5g of cellulase and β-glucosidase (mass ratio 2:1.5), and hydrolyze for 90min. Then heat to 85℃ and incubate for 15min to inactivate. Low-temperature ultrafine grinding: The filter residue was collected by filtration, dried at 70℃ to a moisture content of 8%, and fed into a low-temperature airflow mill. It was then ground at -10℃ to a particle size of about 15μm to obtain 415 g of ultrafine powder.

[0021] Comparative Example 1

[0022] Take 500g of dried Yunnan white pearl medicinal material, remove impurities, pulverize to 15 mesh using a universal pulverizer, and dry in a 65℃ oven until the moisture content is 10%, to obtain conventionally processed Yunnan white pearl powder.

[0023] Comparative Example 2

[0024] The only difference from Example 1 is that the high-frequency ultrasonic-vacuum negative pressure synergistic immersion treatment is not performed; instead, conventional immersion treatment is used, as follows: Mix the pretreated raw material with 40% ethanol at a ratio of 1:15 g / mL (add 7200 mL of ethanol) and soak for 35 min.

[0025] Comparative Example 3

[0026] The only difference from Example 1 is that no compound enzymatic hydrolysis treatment is performed.

[0027] Comparative Example 4

[0028] The only difference from Example 1 is that the compound enzymatic hydrolysis process does not involve stepwise enzymatic hydrolysis. The specific process is as follows: Adjust the pH to 4.8 with citrate-sodium citrate buffer, add 5g of pectinase, xylanase, cellulase and β-glucosidase (mass ratio 1:0.5:2:1.5), heat to 50℃ and enzymatically hydrolyze for 85min; then heat to 90℃ and incubate for 12min to inactivate.

[0029] Comparative Example 5

[0030] The only difference from Example 1 is that the ultrafine grinding process is carried out at room temperature (25°C).

[0031] Experimental Example 1

[0032] Five g of each of the Yunnan white pearl powder prepared in Examples 1-3 and Comparative Examples 1-5 were taken, and the content of total flavonoids was determined. The total flavonoid content was determined by the aluminum nitrate-sodium nitrite colorimetric method (calculated as rutin) according to the method in the pharmacopoeia. The results are shown in Table 1 below.

[0033] Table 1. Results of total flavonoid content in Yunnan white pearl powder of each group

[0034] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for ultra-fine pulverization of Yunnan white pearl medicinal material, characterized in that, Includes the following steps: 1) Take Yunnan white pearl medicinal material, remove impurities, pulverize and dry to obtain pretreated raw material; 2) After mixing the pretreated raw materials with the solvent, perform ultrasonic-vacuum negative pressure synergistic immersion treatment; 3) Add a compound enzyme to the soaking solution for enzymatic hydrolysis; 4) Filter the solution after enzymatic hydrolysis in step 3), dry the filter residue, and then pulverize it in a low-temperature ultrafine pulverizer to obtain Yunnan white pearl ultrafine powder.

2. The method for ultrafine pulverization of Yunnan white pearl medicinal material as described in claim 1, characterized in that, The pulverization mentioned in step 1) refers to pulverizing to 10-20 mesh, and the drying refers to drying to a moisture content of 8%-12%.

3. The method for ultrafine pulverization of Yunnan white pearl medicinal material as described in claim 1, characterized in that, The solvent in step 2) is an ethanol solution with a volume fraction of 30% to 50%, and the amount used is 1:10 to 20 g / mL. The ultrasonic power is 150 to 300 W, the vacuum negative pressure is -0.06 to -0.09 MPa, and the soaking time is 20 to 60 min.

4. The method for ultrafine pulverization of Yunnan white pearl medicinal material as described in claim 1, characterized in that, The complex enzyme mentioned in step 3) is composed of pectinase, xylanase, cellulase and β-glucosidase in a mass ratio of 1~2:0.5~1:1~3:1~2, and the total amount added is 0.5%~2% of the mass of the pretreated raw materials.

5. The method for ultrafine pulverization of Yunnan white pearl medicinal material as described in claim 1, characterized in that, The enzymatic hydrolysis process described in step 3) is a staged enzymatic hydrolysis. The pH is adjusted to 4.5~5.

5. First, pectinase and xylanase are added, and the enzymatic hydrolysis time is 20~30 min. Then, cellulase and β-glucosidase are added, and the enzymatic hydrolysis time is 30~40 min. After the enzymatic hydrolysis is completed, the temperature is raised to 85~95℃ and kept at this temperature for 10~15 min to inactivate the enzyme.

6. The method for ultrafine pulverization of Yunnan white pearl medicinal material as described in claim 1, characterized in that, The drying in step 4) is to dry the filter residue to a moisture content of 5%~8%, the pulverization temperature is -40℃~-10℃, and the particle size of the pulverized residue is ≤15 μm.

7. A method for preparing Dianbaizhu ultrafine powder by ultrafine pulverization of medicinal material according to any one of claims 1 to 6.

Images