Anti-aging primordial qi-consolidating and life-prolonging pill and preparation method thereof

Abstract

The preparation method comprises the following steps: crushing raw materials, carrying out dual-frequency ultrasonic extraction in combination with a solvent to obtain a high-activity and high-oxidation-resistance component, filtering through a micro-filtration membrane, mixing an extracting solution and crushed filter residue raw materials according to a ratio, sterilizing, adding modified microcrystalline cellulose and other auxiliary materials, and mixing, so as to obtain the anti-aging body-consolidating and life-prolonging pill. And refining honey and pelleting to prepare the life-prolonging pill with high stability, good pill quality and high oxidation resistance.

Description

Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to an anti-aging Guben Yanling pill and a preparation method thereof. Background Art

[0002] Guben Yanling Pills are approved by the National Medicine Standard. This product is a large dark brown honey pill; the taste is sweet at first and then slightly bitter. The main ingredients are ginseng, ophiopogon, schisandra, asparagus, rehmannia, prepared rehmannia, yam, oriental rhizome, poria, cyathula, cornus, eucommia, costus root, polygala, cypress seed, Morinda officinalis (salted), prickly ash, calamus, salvia, cistanche, wolfberry, raspberry, lycium bark, antler glue, dodder seed, fish maw pearl, pearl, dog whip. The auxiliary material is: honey. After the above medicinal materials are dried, crushed, sterilized, mixed and processed, they are added with refined honey to make large honey pills. Functions and indications: strengthening the foundation and nourishing the essence, nourishing yin, replenishing essence, and strengthening tendons and bones. It is used for consumptive injuries, low back pain and fatigue, palpitations and insomnia, haggard skin, premature graying of hair and beard, irregular menstruation, and loss of appetite.

[0003] Studies have shown that dual-frequency ultrasound extraction is more advantageous than single-frequency ultrasound extraction, and the extraction effect is better. The key to solvent selection is to use the "like dissolves like" principle of solvents. Selecting a suitable extractant is a key and important step to obtain high-purity monomer compounds. Using water as an extractant can also extract a large amount of polysaccharides at the same time, which brings inconvenience to the subsequent separation work. Therefore, finding a suitable solvent is the research focus of this invention. Methanol has strong toxic side effects and is easy to remain in the extract during the extraction process. It cannot adapt to industrial production; ethanol is cheap and easy to obtain, easy and safe to operate, has certain antiseptic properties and can be recycled. It is mostly suitable for industrial production, but the effect is not ideal in selecting the target component for extraction.

[0004] As a new functional natural polymer compound, microcrystalline cellulose (MCC) has been increasingly valued as an excipient for food pills due to its unique physical and chemical properties. Microcrystalline cellulose is green and non-toxic, insoluble in water but dispersible in water, making it widely used in the food industry. However, due to its strong hydrophilicity, microcrystalline cellulose is difficult to disperse in general non-polar polymer molecules, which will seriously affect the comprehensive performance of pills, which greatly affects the further application of microcrystalline cellulose. Therefore, it is necessary to modify its surface to improve its dispersibility and compatibility in pills, as well as the roundness and absorption rate of pills while maintaining the excellent performance of microcrystalline cellulose itself. Summary of the invention

[0005] In order to solve the above technical problems, a specific preparation method of the anti-aging Guben Yanling Pill of the present invention is as follows:

[0006] Prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cypress seed, 60 parts of Morinda officinalis, 30 parts of Zanthoxylum bungeanum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, grind the above raw materials, add extractant according to the material-liquid ratio of 1:20 , ultrasonic extraction at 60℃, frequency of 25kHz+35kHz for 60-90min; keep the supernatant statically adsorbed by H1020 large adsorption resin for 4h, then elute the chromatography column with distilled water as eluent at a flow rate of 0.8mL / min, and collect the eluent; then dialyze the eluent in running water for 24h, the dialysis temperature is 30℃, and the water is changed every 4h; then filter through PSF ultrafiltration membrane, filter the filter residue, concentrate the filtrate to a water content of 20-30%, add ethanol to make the alcohol content reach 65%, perform alcohol precipitation treatment, and after obtaining the extract, concentrate it again to a water content of 20-30% for standby use;

[0007] The filter residue is washed once with a 75% ethanol solution at 80°C, and then washed on both sides with hot water at 80°C, and then dried, crushed into fine powder with a micro-powder machine, and subjected to pressure treatment in an extruder, wherein the extrusion conditions are: room temperature, 1-10Mpa, the medium is air, the pressurization time is 1-10min, and then the pressure is released instantly to obtain an extruded product, which is crushed into fine powder with a micro-powder machine and passed through a 100-140 mesh sieve;

[0008] The sterilized concentrated extract and the crushed filter residue are added to the auxiliary materials for mixing, and then refined into honey and made into pills;

[0009] The extractant is a sodium picolinate solution with a mass fraction of 50-60%.

[0010] The sterilization treatment comprises: mixing the concentrated extract and the crushed filter residue raw material in a ratio of 6:4, adding 0.1-0.3 times of vegetable oil and modified microcrystalline cellulose, stirring evenly, and placing in a wet heat sterilizer for sterilization, wherein the sterilization conditions are: temperature 121-125°C, pressure>0.2MPa, and time 15-20min;

[0011] The mass ratio of the vegetable oil to the modified microcrystalline cellulose is 1:1-3.

[0012] The modified microcrystalline cellulose comprises: adding microcrystalline cellulose and a modifier solution with a mass fraction of 30-50% in equal proportions into a three-necked flask equipped with a stirrer, rotating at a speed of 100-200RPM, stirring and reacting at 70°C for 30 minutes, stopping the reaction, adjusting the pH of the system to neutral, precipitating, filtering, washing, and drying to obtain the modified microcrystalline cellulose, and turning off the stirrer to obtain the modified microcrystalline cellulose.

[0013] The modifier is methyl 4-hydroxycinnamate.

[0014] The beneficial effects of the present invention are:

[0015] 1. The present invention relates to an anti-aging Guben Yanling Pill and a preparation method thereof, wherein the raw materials are crushed by dual-frequency ultrasound combined with solvent extraction to obtain a high-activity, high-antioxidant component, filtered through a microfiltration membrane, the extract and the crushed filter residue raw materials are mixed in proportion, sterilized and added with modified microcrystalline cellulose and other auxiliary materials, and honey is refined and pilled to prepare Yanling Pills with high stability, good pill quality and high antioxidant properties.

[0016] 2. By mixing the expanded, pressurized and crushed filter residue raw materials with the concentrated extract, the moisture in the mixture can be effectively controlled, improving the problem of the concentrated extract being too sticky and the filter residue powder being difficult to shape after being crushed. This not only facilitates the subsequent molding of pills, but also improves the absorption of the active ingredients in Yanling Pills.

[0017] 3. Dual-frequency ultrasonic extraction can produce different cavitation effects through the combination of high and low frequencies, enhancing the destruction of cell walls and making it easier for cell contents to be released. This enhanced cell destruction combined with the polarity of sodium picolinate can significantly improve the extraction efficiency of the target antioxidant components.

[0018] 4. The use of dual-frequency ultrasound combined with sodium picolinate extraction can achieve a higher extraction rate in a shorter time, reducing the time required for traditional extraction methods. This time advantage not only improves production efficiency, but also reduces energy consumption.

[0019] 5. The structural characteristics of sodium picolinate enable it to effectively dissolve polar compounds, such as polyphenols, flavonoids and other antioxidant components, which are often found in traditional Chinese medicine and have significant biological activity. Sodium picolinate can enhance the selective extraction of target compounds by forming hydrogen bonds or ionic bonds with antioxidant components in traditional Chinese medicine. This interaction promotes the dissolution of the target components, allowing them to be released more effectively from the plant matrix during the extraction process.

[0020] 6. During the extraction process, sodium picolinate can effectively reduce the solubility of impurities such as polysaccharides and lipids, which not only improves the extraction rate of the target antioxidant components, but also reduces the complexity of the subsequent purification process. By reducing the interference of impurities, the purity of the extract can be improved and the quality of the antioxidant components can be ensured.

[0021] 7. Sodium picolinate is weakly alkaline in aqueous solution and can adjust the pH value of the extract. Many antioxidant ingredients have different stability in acidic or alkaline environments. The weak alkalinity of sodium picolinate helps to protect the structure of some antioxidant ingredients and avoid degradation or inactivation caused by acidic environments, thereby improving the biological activity of the extract. In addition, the extractant components and other impurities are removed through elution and alcohol precipitation processes, thereby improving the purity of the active ingredients.

[0022] 8. The present invention uses methyl 4-hydroxycinnamate with strong hydrophilicity and adhesion to modify microcrystalline cellulose, so that the molecular chain of the microcrystalline cellulose becomes loose, the contact points are increased, and the distribution uniformity of the microcrystalline cellulose in the Yanling Pills is improved. After the modification, not only the particle size of the microcrystalline cellulose is reduced, but also a better adhesion effect is produced, which can effectively promote the uniform distribution of moisture in the material and reduce the glass transition problem caused by uneven moisture distribution.

[0023] 9. The modified microcrystalline cellulose, when used in the preparation of Yanling Pills, can exert good swelling properties and low water content, has better water holding capacity and oil holding capacity, can inhibit water evaporation and Yanling Pills shrinkage, and reduce the stress difference between the surface and the center, thereby preventing breakage and improving the storage stability of the pills. The modified microcrystalline cellulose makes the various ingredients in Yanling Pills have good compatibility, a rounded appearance, uniform particle size, a dense structure, a more delicate taste, and easy absorption. DETAILED DESCRIPTION

[0024] The present invention is further described in detail below in conjunction with the examples. The PSF ultrafiltration membrane used below has a membrane wire diameter of 1.3 mm, a length of 1150 mm (can be cut by oneself), and a filtration pore size of 0.01-0.5 μm.

[0025] Example 1

[0026] Extraction: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes bidentata, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cypress seed, 60 parts of morinda officinalis, 30 parts of zanthoxylum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, crush the above raw materials, add mass fraction according to the material-liquid ratio of 1:20 The method comprises the following steps: preparing a 55% sodium picolinate solution, and ultrasonically extracting the solution at 60°C and a frequency of 25kHz+35kHz for 75 minutes; keeping the supernatant statically adsorbed for 4 hours with a large adsorption resin of H1020, and then eluting the column with distilled water at a flow rate of 0.8mL / min, and collecting the eluate; then dialyzing the eluate in running water for 24 hours, at a dialysis temperature of 30°C, and changing the water every 4 hours; then filtering the solution through a PSF ultrafiltration membrane, filtering the filter residue, concentrating the filtrate to a water content of 25%, adding ethanol to the filtrate so that the alcohol content reaches 65%, and performing alcohol precipitation treatment to obtain an extract, and then concentrating the extract again to a water content of 25% for standby use;

[0027] Example 2

[0028] Extraction: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes bidentata, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cypress seed, 60 parts of morinda officinalis, 30 parts of zanthoxylum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, crush the above raw materials, add mass fraction according to the material-liquid ratio of 1:20 The method comprises the following steps: preparing a 50% sodium picolinate solution, and ultrasonically extracting the solution at 60°C and a frequency of 25kHz+35kHz for 90 minutes; keeping the supernatant statically adsorbed for 4 hours with a large adsorption resin of H1020, and then eluting the column with distilled water at a flow rate of 0.8mL / min, and collecting the eluate; then dialyzing the eluate in running water for 24 hours, at a dialysis temperature of 30°C, and changing the water every 4 hours; filtering the solution through a PSF ultrafiltration membrane, and filtering the filter residue, concentrating the filtrate to a water content of 20%, adding ethanol to the filtrate so that the alcohol content reaches 65%, and performing alcohol precipitation treatment to obtain an extract, and concentrating the extract again to a water content of 20% for standby use;

[0029] Example 3

[0030] Extraction: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes bidentata, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cypress seed, 60 parts of morinda officinalis, 30 parts of zanthoxylum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, crush the above raw materials, add mass fraction according to the material-liquid ratio of 1:20 The method comprises the following steps: preparing a 60% sodium picolinate solution, and ultrasonically extracting the solution at 60°C and a frequency of 25kHz+35kHz for 60 minutes; keeping the supernatant statically adsorbed for 4 hours with a large adsorption resin of H1020, and then eluting the column with distilled water at a flow rate of 0.8mL / min, and collecting the eluate; then dialyzing the eluate in running water for 24 hours, at a dialysis temperature of 30°C, and changing the water every 4 hours; filtering the solution through a PSF ultrafiltration membrane, and filtering the filter residue, concentrating the filtrate to a water content of 30%, adding ethanol to the filtrate so that the alcohol content reaches 65%, and performing alcohol precipitation treatment to obtain an extract, and then concentrating the extract again to a water content of 30% for standby use;

[0031] Comparative Example 1

[0032] The difference between this comparative example and Example 1 is that the 55% sodium picolinate solution extract is 55% ethanol, and the rest is the same as Example 1.

[0033] Comparative Example 2

[0034] The difference between this comparative example and Example 1 is that only a single bottle of ultrasonic extraction is used in this comparative example. The specific extraction is as follows: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cyperus arborvitae, 60 parts of Morinda officinalis, 30 parts of Zanthoxylum bungeanum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, and crush the above raw materials. A 55% mass fraction sodium picolinate solution was added at a solid-liquid ratio of 1:20, and ultrasonic extraction was performed at 60°C and a frequency of 25kHz for 75 minutes; the supernatant was kept statically adsorbed for 4 hours using H1020 macro-adsorption resin, and then the chromatography column was eluted with distilled water as the eluent at a flow rate of 0.8mL / min, and the eluent was collected; the eluent was then dialyzed in running water for 24 hours, the dialysis temperature was 30°C, and the water was changed every 4 hours; then it was filtered through a PSF ultrafiltration membrane, and the filter residue was filtered, the filtrate was concentrated to a water content of 25%, ethanol was added thereto to make the alcohol content reach 65%, and alcohol precipitation was performed to obtain an extract, which was concentrated again to a water content of 25% for standby use; the rest was the same as in Example 1.

[0035] Comparative Example 3

[0036] The difference between this comparative example and Example 1 is that the mass fraction of the sodium picolinate solution in this comparative example is different. The specific extraction is as follows: Extraction: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cyperus arborvitae, 60 parts of Morinda officinalis, 30 parts of Zanthoxylum bungeanum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, and crush the above raw materials. A 70% sodium picolinate solution was added at a material-liquid ratio of 1:20, and ultrasonic extraction was performed at 60°C and a frequency of 25kHz+35kHz for 75 minutes; the supernatant was kept statically adsorbed for 4 hours using H1020 macro-adsorption resin, and then the chromatography column was eluted with distilled water as the eluent at a flow rate of 0.8mL / min, and the eluent was collected; the eluent was then dialyzed in running water for 24 hours at a dialysis temperature of 30°C, and the water was changed every 4 hours; then the solution was filtered through a PSF ultrafiltration membrane, and the filter residue was filtered, the filtrate was concentrated to a water content of 25%, ethanol was added thereto to make the alcohol content reach 65%, and an alcohol precipitation treatment was performed to obtain an extract, which was then concentrated again to a water content of 25% for standby use; the rest was the same as in Example 1.

[0037] Comparative Example 4

[0038] The difference between this comparative example and Example 1 is that the mass fraction of the sodium picolinate solution in this comparative example is different. The specific extraction is as follows: Extraction: prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cyperus arborvitae, 60 parts of Morinda officinalis, 30 parts of Zanthoxylum bungeanum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, and crush the above raw materials. A 40% sodium picolinate solution was added at a material-liquid ratio of 1:20, and ultrasonic extraction was performed at 60°C and a frequency of 25kHz+35kHz for 75 minutes; the supernatant was kept statically adsorbed for 4 hours using a large adsorption resin of H1020, and then the chromatography column was eluted with distilled water as an eluent at a flow rate of 0.8mL / min, and the eluent was collected; the eluent was then dialyzed in running water for 24 hours at a dialysis temperature of 30°C, and the water was changed every 4 hours; then the solution was filtered through a PSF ultrafiltration membrane, and the filter residue was filtered, the filtrate was concentrated to a water content of 25%, ethanol was added thereto to make the alcohol content reach 65%, and an alcohol precipitation treatment was performed to obtain an extract, which was then concentrated again to a water content of 25% for standby use; the rest was the same as in Example 1.

[0039] Test 1: Determination of ingredient content

[0040] Determination of the content of marker ingredients: This product uses schisandra alcohol A (C24H32O7) in Schisandra chinensis as the marker ingredient, and the content shall not be less than 80 μg per gram. Determined by high performance liquid chromatography (Chinese Pharmacopoeia 2020 Edition Part IV General Rules 0512).

[0041] Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel is used as filler; methanol-water (65:35) is used as mobile phase, and the detection wavelength is 250nm. The theoretical plate number calculated based on the schisandra alcohol methyl peak should not be less than 2000.

[0042] Preparation of reference solution: Take an appropriate amount of schisandra alcohol A reference substance, weigh it accurately, and add methanol to make a solution containing 15 μg per 1 ml.

[0043] Preparation of the test solution: Take 5 ml of the extract in Example 1-3 and Comparative Example 1-4, put it in a 50 ml volumetric flask, add 18 ml of methanol, ultrasonically treat (power 250 W, frequency 20 kHz) for 20 minutes, take it out, add methanol to the scale, shake well, filter, and take the filtrate.

[0044] Determination method: Accurately pipette 10 μl of reference solution and test solution respectively, inject into liquid chromatograph, and determine.

[0045] The results are shown in Table 1.

[0046] Table 1

[0047] Group Contains schisandra chinensis as schisandra alcohol (C24H32O7) ≥ 80 μg / g Example 1 175 Example 2 173 Example 3 172 Comparative Example 1 140 Comparative Example 2 154 Comparative Example 3 169 Comparative Example 4 158

[0048] The following examples are all carried out on the basis of Example 1:

[0049] Example 4

[0050] Crushing: The filter residue is washed once with 75% ethanol solution at 80°C, and then washed on both sides with hot water at 80°C, and then dried, crushed into fine powder with a micro-powder machine, and subjected to pressure treatment in an extruder, wherein the extrusion conditions are: room temperature, 5Mpa, the medium is air, the pressurization time is 50min, and then the pressure is released instantly to obtain an extruded product, which is crushed into fine powder with a micro-powder machine and passed through a 120-mesh sieve;

[0051] Modified microcrystalline cellulose: Add microcrystalline cellulose and 40% by mass methyl 4-hydroxycinnamate solution in equal proportions into a three-necked flask equipped with a stirrer at a speed of 150 RPM. Stir and react at 70°C for 30 minutes. Stop the reaction, adjust the pH of the system to neutral, precipitate, filter, wash and dry to obtain modified microcrystalline cellulose. Turn off the stirrer.

[0052] Sterilization: Mix the concentrated extract and the crushed filter residue in a ratio of 6:4, add 0.2 times of vegetable oil and modified microcrystalline cellulose, the mass ratio of vegetable oil to modified microcrystalline cellulose is 1:2, stir evenly, and place in a wet heat sterilizer for sterilization. The sterilization conditions are: temperature 123°C, pressure>0.2MPa, time 18min;

[0053] Total mixing: Place the sterilized powder in a two-dimensional motion mixer. The amount loaded each time should not exceed two-thirds of the mixer's volume. Discharge the powder after mixing for 30 minutes. The mixing time is 1 time.

[0054] Refining honey: add 118 parts of raw honey to every 100 parts of medicinal powder, add water to the raw honey and boil it to melt it, then pass it through a 40-mesh sieve and continue heating to 117°C until the water content is 15%, the relative density is 1.38, and evenly churning fine bubbles appear.

[0055] Pill making: In a trough mixer, add refined honey to the powder while it is hot. For every 100 parts of powder, add 110 parts of refined honey. Cover and stir for 38 minutes until the color of the medicine ball is uniform, the original color of the medicine is not visible, and it is not sticky. Then introduce it into the pill making machine to make pills. Each pill should weigh 9 grams; the moisture content should be ≤14.0%.

[0056] Example 5

[0057] Crushing: The filter residue is washed once with 75% ethanol solution at 80°C, and then washed on both sides with hot water at 80°C, and then dried, crushed into fine powder with a micro-powder machine, and subjected to pressure treatment in an extruder, wherein the extrusion conditions are: room temperature, 10Mpa, the medium is air, the pressurization time is 1min, and then the pressure is released instantly to obtain an extruded product, which is crushed into fine powder with a micro-powder machine and passed through a 140-mesh sieve;

[0058] Modified microcrystalline cellulose: Add microcrystalline cellulose and 30% by mass methyl 4-hydroxycinnamate solution in equal proportions into a three-necked flask equipped with a stirrer at a speed of 200 RPM. Stir and react at 70°C for 30 minutes. Stop the reaction, adjust the pH of the system to neutral, precipitate, filter, wash and dry to obtain modified microcrystalline cellulose. Turn off the stirrer.

[0059] Sterilization: Mix the concentrated extract and the crushed filter residue in a ratio of 6:4, add 0.3 times of vegetable oil and modified microcrystalline cellulose, the mass ratio of vegetable oil and modified microcrystalline cellulose is 1:1, stir evenly, and place in a wet heat sterilizer for sterilization. The sterilization conditions are: temperature 125°C, pressure>0.2MPa, time 15min;

[0060] Total mixing: Place the sterilized powder in a two-dimensional motion mixer. The amount loaded each time should not exceed two-thirds of the mixer's volume. Discharge the powder after mixing for 30 minutes. The mixing time is 1 time.

[0061] Refining honey: add 130 parts of raw honey to every 100 parts of medicinal powder, add water to the raw honey and boil it to melt it, then pass it through a 40-mesh sieve and continue heating to 116°C until the water content is 16%, the relative density is 1.37, and evenly churning fine bubbles appear.

[0062] Pill making: In a trough mixer, add refined honey to the powder while it is hot, add 115 parts of refined honey to every 100 parts of powder. Cover and stir for 30 minutes until the color of the medicine ball is uniform, the original color of the medicine is no longer visible, and it is not sticky. Then introduce it into the pill making machine to make pills. Each pill should weigh 9.3 grams; the moisture content should be ≤14.0%.

[0063] Example 6

[0064] Crushing: The filter residue is washed once with 75% ethanol solution at 80°C, and then washed on both sides with hot water at 80°C, and then dried, crushed into fine powder with a micro-powder machine, and subjected to pressure treatment in an extruder, wherein the extrusion conditions are: room temperature, 1Mpa, the medium is air, the pressurization time is 10min, and then the pressure is released instantly to obtain an extruded product, which is crushed into fine powder with a micro-powder machine and passed through a 100-mesh sieve;

[0065] Modified microcrystalline cellulose: Add microcrystalline cellulose and 50% by mass methyl 4-hydroxycinnamate solution in equal proportions into a three-necked flask equipped with a stirrer at a speed of 100 RPM. Stir and react at 70°C for 30 minutes. Stop the reaction, adjust the pH of the system to neutral, precipitate, filter, wash and dry to obtain modified microcrystalline cellulose. Turn off the stirrer.

[0066] Sterilization: Mix the concentrated extract and the crushed filter residue in a ratio of 6:4, add 0.1 times of vegetable oil and modified microcrystalline cellulose, the mass ratio of vegetable oil and modified microcrystalline cellulose is 1:1-3, stir evenly, and place in a wet heat sterilizer for sterilization. The sterilization conditions are: temperature 121°C, pressure>0.2MPa, time 20min;

[0067] Total mixing: Place the sterilized powder in a two-dimensional motion mixer. The amount loaded each time should not exceed two-thirds of the mixer's volume. Discharge the powder after mixing for 30 minutes. The mixing time is 1 time.

[0068] Refining honey: add 105 parts of raw honey to every 100 parts of medicinal powder, add water to the raw honey and boil it to melt it, then pass it through a 40-mesh sieve and continue heating to 118°C until the water content is 14%, the relative density is 1.39, and evenly churning fine bubbles appear.

[0069] Pill making: In a trough mixer, add refined honey to the powder while it is hot, add 105 parts of refined honey for every 100 parts of powder. Cover and stir for 45 minutes until the color of the medicine ball is uniform, the original color of the medicine is no longer visible, and it is not sticky. Then introduce it into the pill making machine to make pills. Each pill should weigh 8.7 grams; the moisture content should be ≤14.0%.

[0070] Comparative Example 5

[0071] The difference between this comparative example and Example 4 is that the modified microcrystalline cellulose is chitosan, and the rest is the same as Example 4.

[0072] Comparative Example 6

[0073] The difference between this comparative example and Example 4 is that the microcrystalline cellulose is not modified, and the rest is the same as Example 4.

[0074] Comparative Example 7

[0075] The difference between this comparative example and Example 4 is that the amount of methyl 4-hydroxycinnamate added is different. Specifically, the modified microcrystalline cellulose is as follows: microcrystalline cellulose and a 60% by mass methyl 4-hydroxycinnamate solution are added in equal proportions to a three-necked flask equipped with a stirrer, the speed is 150 RPM, and the reaction is stirred at 70° C. for 30 minutes, the reaction is stopped, the pH of the system is adjusted to neutral, precipitation, filtration, washing, and drying are performed to obtain modified microcrystalline cellulose, and the stirrer is turned off to obtain; the rest is the same as Example 4.

[0076] Comparative Example 8

[0077] The difference between this comparative example and Example 4 is that the amount of methyl 4-hydroxycinnamate added is different. Specifically, the modified microcrystalline cellulose is as follows: microcrystalline cellulose and a 20% by mass methyl 4-hydroxycinnamate solution are added in equal proportions to a three-necked flask equipped with a stirrer, the speed is 150 RPM, and the reaction is stirred at 70° C. for 30 minutes, the reaction is stopped, the pH of the system is adjusted to neutral, precipitation, filtration, washing, and drying are performed to obtain modified microcrystalline cellulose, and the stirrer is turned off to obtain; the rest is the same as Example 4.

[0078] Test 2: The quality of Yanling Pills was evaluated using roundness and dissolution time as indicators. The results are shown in Table 2 below.

[0079] Table 2

[0080] Group Average roundness Dissolution time (min) Example 4 0.99 5.2 Example 5 0.98 5.3 Example 6 0.98 5.5 Comparative Example 5 0.68 6.9 Comparative Example 6 0.75 6.6 Comparative Example 7 0.94 5.8 Comparative Example 8 0.92 6.2

Claims

1. A method for preparing an anti-aging Guben Yanling Pill, characterized in that: Prepare 60 parts of ginseng, 60 parts of ophiopogon, 60 parts of schisandra, 60 parts of asparagus, 60 parts of rehmannia, 60 parts of prepared rehmannia, 60 parts of yam, 30 parts of oriental rhizome, 60 parts of tuckahoe, 60 parts of achyranthes bidentata, 60 parts of cornus, 60 parts of eucommia, 60 parts of costusroot, 30 parts of polygala, 60 parts of cypress seed, 60 parts of Morinda officinalis, 30 parts of zanthoxylum, 30 parts of calamus, 120 parts of salvia miltiorrhiza, 120 parts of cistanche, 45 parts of wolfberry, 45 parts of raspberry, 45 parts of lycium bark, 30 parts of antler glue, 120 parts of dodder seed, 30 parts of fish maw pearl, 9 parts of pearl and 25 parts of dog whip, grind the above raw materials, add extractant according to the material-liquid ratio of 1:20, and extract by ultrasonic at 60°C and frequency of 25 kHz+35 kHz for 60-90 min; the supernatant was kept statically adsorbed with H1020 large adsorption resin for 4 hours, and then distilled water was used as eluent to elute the chromatography column at a flow rate of 0.8 mL / min, and the eluent was collected; the eluent was then dialyzed in running water for 24 hours, the dialysis temperature was 30°C, and the water was changed every 4 hours; then it was filtered through a PSF ultrafiltration membrane, and the filter residue was filtered, and the filtrate was concentrated to a water content of 20-30%, ethanol was added to it to make the alcohol content reach 65%, and alcohol precipitation was performed to obtain the extract, and then it was concentrated again to a water content of 20-30% for standby use; The filter residue is washed once with 75% ethanol solution at 80°C, and then washed on both sides with hot water at 80°C, and then dried, crushed into fine powder with a micro-powder machine, and subjected to pressure treatment in an extruder, wherein the extrusion conditions are: room temperature, 1-10Mpa, the medium is air, the pressurization time is 1-10min, and then the pressure is released instantly to obtain an extruded product, which is crushed into fine powder with a micro-powder machine and passed through a 100-140 mesh sieve; The sterilized concentrated extract and the crushed filter residue are added to the auxiliary materials for mixing, and then refined into honey and made into pills. The extractant is a sodium picolinate solution with a mass fraction of 50-60%.

2. The method for preparing the anti-aging Guben Yanling Pills according to claim 1, characterized in that: The sterilization treatment comprises: mixing the concentrated extract and the crushed filter residue raw material in a ratio of 6:4, adding 0.1-0.3 times of vegetable oil and modified microcrystalline cellulose, stirring evenly, and placing in a wet heat sterilizer for sterilization, wherein the sterilization conditions are: temperature 121-125°C, pressure>0.2MPa, and time 15-20min; The mass ratio of the vegetable oil to the modified microcrystalline cellulose is 1:1-3.

3. The method for preparing the anti-aging Guben Yanling Pills according to claim 2, characterized in that: The modified microcrystalline cellulose comprises: adding microcrystalline cellulose and a modifier solution with a mass fraction of 30-50% into a three-necked flask equipped with a stirrer in equal proportions, with a rotation speed of 100-200RPM, stirring and reacting at 70°C for 30 minutes, stopping the reaction, adjusting the pH of the system to neutral, precipitating, filtering, washing, and drying to obtain the modified microcrystalline cellulose, and turning off the stirrer to obtain the modified microcrystalline cellulose.

4. The method for preparing the anti-aging Guben Yanling Pills according to claim 3, characterized in that: The modifier is methyl 4-hydroxycinnamate.