CN108498624B - Preparation method of prepared rehmannia root decoction pieces and pills - Google Patents
Preparation method of prepared rehmannia root decoction pieces and pills Download PDFInfo
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Abstract
The invention relates to the field of traditional Chinese medicine preparation, and discloses a preparation method of prepared rehmannia root decoction pieces and pills, wherein the preparation method of the decoction pieces comprises the following steps: 1) cleaning and selecting; 2) washing and moistening; 3) steaming; 4) cutting; 5) and (5) drying. The preparation method of the pill comprises: A) refluxing and extracting with alcohol; B) carrying out vacuum microwave reflux treatment on the kenyaite; C) preparing cellulose-kenyaite composite aerogel powder; D) and (4) preparing pills. The prepared rehmannia root decoction pieces and pills prepared by the method have low content of ineffective components and high utilization rate of effective components. The prepared rehmannia root pill prepared by the method has a controlled release effect, is more favorable for good absorption, has better drug effect and is convenient to take.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine preparation, in particular to a preparation method of prepared rehmannia root decoction pieces and pills.
Background
Prepared rehmannia root, radix rehmanniae Praeparata, also known as rehmannia: radix rehmanniae and radix rehmanniae Preparata. Latin name:Rehmannia glutinosa (Gaetn.) Libosch. ex Fisch. et Mey。scrophulariaceae, rehmannia, cultivated in various regions at home and abroad, and the roots and stems of the plants are used as medicines. The prepared rehmannia root, a traditional Chinese medicine, is a processed product of rehmannia root, has black and glossy surface, soft and flexible quality, sweet taste and mild nature, and has the effects of nourishing yin and supplementing blood, replenishing vital essence and replenishing marrow and the like. Can be used for treating deficiency of liver-yin and kidney-yin, soreness of waist and knees, hectic fever, night sweat, nocturnal emission, internal heat, diabetes, blood deficiency, sallow complexion, cardiopalmus, menoxenia, giddiness, tinnitus, and premature gray hair.
The dried rehmannia root is prepared rehmannia root which is fumigated to be black and moist, is irregular block-shaped and has different sizes, the inside and the outside are painted black, and the product has luster and the outer surface is wrinkled and uneven. Has moist cross section, bright grease-like block in the center, high viscosity, soft texture, slight smell, and sweet taste. It is better to have a big, soft and moist root tuber, and black and glossy interior and exterior through nine times of steaming and sun drying.
The prepared rehmannia root is a general good and is generally not graded. It is better for large, heavy, soft and oily, black cross section, sweet taste. Especially, Huaiqing Dihuang produced in Henan is the best herb of the four great Huai nationalities. The radix rehmanniae Preparata can be prepared by steaming radix rehmanniae Preparata, processing with wine, processing with ginger wine, processing with fructus Amomi, and processing with charcoal of radix rehmanniae Preparata, storing in a drying container, sealing, and standing in a dry place to prevent mold and moth-eating.
In the prior art, the prepared rehmannia root is usually decocted into decoction and taken, the use of active ingredients in the medicinal materials is low, the absorption is poor, the drug effect is poor, and the decoction is needed every time of taking, so that the traditional Chinese medicine is inconvenient and is not convenient to carry. Therefore, a new prepared rehmannia root Chinese medicinal preparation which has high utilization rate of active ingredients, good absorption and convenient taking needs to be developed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of prepared rehmannia root decoction pieces and pills, and the prepared rehmannia root decoction pieces and pills have low content of ineffective components and high utilization rate of effective components. The prepared rehmannia root pill prepared by the method has a controlled release effect, is more favorable for good absorption, has better drug effect and is convenient to take.
The specific technical scheme of the invention is as follows: a preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with steam until the medicinal materials are black, taking out, and drying in the air until the medicinal materials are eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3).
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust.
Preferably, in the step 1), impurities and non-medicinal parts of the selected medicinal materials are less than or equal to 3 wt%.
The prepared rehmannia root decoction pieces prepared by the method have less impurity and non-medicinal content.
Preferably, in the step 3), the steam heating temperature is 90-100 ℃, the heating time is 6-8h, and the airing time is 6-12 h.
When steaming, the temperature and time are strictly controlled, so that the effective components in the medicinal materials are not damaged, and the retention rate of the effective components is high.
Preferably, in step 4), the slice thickness is 2-4 mm.
Preferably, in the step 5), the drying temperature is 65-70 ℃, the drying time is 5-6h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the method have high yield of 85-95%.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to prepare a prepared rehmannia root concentrated solution for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment, taking out and drying to obtain kenyaite powder for later use.
C) Preparing nano-cellulose into a nano-cellulose solution by using an ionic liquid, adding the kenyaite powder into the nano-cellulose solution, uniformly dispersing, stirring and heating to 60-80 ℃, and carrying out heat preservation reaction for 1-2 hours; freezing the solution at-20 deg.C to-16 deg.C for 2-4 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking radix rehmanniae Preparata concentrated solution, adding cellulose-kenyaite composite aerogel powder, stirring well, drying, adding polyvinylpyrrolidone alcohol solution to prepare mother nucleus; adding dextrin and polyvinylpyrrolidone solution, coating, and making into pill.
In the prior art, the prepared rehmannia root is usually decocted into decoction and taken, the use of active ingredients in the medicinal materials is low, the absorption is poor, the drug effect is poor, and the decoction is needed every time of taking, so that the traditional Chinese medicine is inconvenient and is not convenient to carry. Therefore, the invention firstly extracts the effective components of the prepared rehmannia root decoction pieces, and prepares the prepared rehmannia root decoction pieces into pills, and the pills are convenient to take, have the controlled release effect, high utilization rate of the effective components and good absorption.
Specifically, in the step A), the active ingredients of the prepared rehmannia root decoction pieces are extracted, and compared with the traditional decoction form, the extraction rate is higher, and the content of the active ingredients in unit mass after the prepared rehmannia root decoction pieces are prepared into pills is higher.
In the step B), the kenyaite is used as one of carrier materials of the prepared rehmannia root pills, the kenyaite is microscopically in a lamellar structure which is used as a main loading space of the medicine, but part of crystal water is filled between original ecological kenyaite lamellar layers, and the lamellar spacing is small, so that the kenyaite lamellar structure not only occupies the loading space, but also cannot be fully dispersed in the solution and is easy to agglomerate. Therefore, the invention carries out vacuum microwave radiation treatment on the kenyaite, and has the following functions: 1. microwave radiation can give molecular and atomic energy to accelerate microscopic motion of the molecules and the atoms, so that the lamella is displaced and the space between the lamellae is increased; 2. the crystal water can be effectively removed by microwave addition treatment, and a drug loading space is released; 3. the kenyaite sheet surface has a large number of hydroxyl groups, which can be activated by microwave radiation to improve its reactivity (see below for details).
In the step C), the inventor finds that the stability of drug load is not high and the slow release effect is poor by only adopting the kenyaite as the drug carrier through long-term research. And the kenyaite lamellar structures are easy to approach each other after a long time, so that large intervals cannot be kept for a long time, and the drug load is influenced. Therefore, the invention compounds the kenyaite and the cellulose in the form of aerogel, and has the following advantages: 1. according to the invention, the kenyaite is added before the nano-cellulose is crosslinked to generate gel, after the nano-cellulose is uniformly dispersed, the nano-cellulose can penetrate into layers, and then the cellulose is crosslinked, so that the cellulose among the layers can be crosslinked to form a three-dimensional network structure, and the distance between the layers is spread to serve as a framework of the aerogel. Aerogels are known to be characterized by light weight, developed pores, and large loading capacity. According to the invention, the kenyaite and the nanocellulose are prepared into the composite aerogel, and the kenyaite and the nanocellulose are self-environmental-friendly, non-toxic and harmless, so that the composite aerogel is an ideal drug carrier. 2. As mentioned above, after the vacuum microwave treatment, a large number of hydroxyl groups on the surface of the kenyaite sheet layer are activated, and can react with a plurality of active groups on the cellulose molecular chain in the cross-linking reaction. Therefore, the cellulose crosslinked between the sheet layers forms a bonding bond with the surface of the sheet layers, so that the sheet layers can keep a large distance for a long time, the stability is good, and the technical problem that the sheet layers are easy to approach after a long time is solved.
In the step D), the medicine is loaded on the composite aerogel, then the mother nucleus is prepared by polyvinylpyrrolidone alcohol solution, and then dextrin is used for coating the surface of the mother nucleus to prepare the pill. The presence of the coating can prevent the rapid dissolution and burst release of the drug when the drug is in contact with water.
Preferably, the concentration of the prepared rehmannia root concentrated solution in the step A) is 60 to 80 wt%.
Preferably, in the step B), the microwave power is 600-800W, the temperature is 100-120 ℃, and the treatment time is 20-40 min.
According to the invention, through research, the crystal water removal rate and the hydroxyl activity of the kenyaite treated under the conditions are simultaneously high.
Preferably, in the step C), the concentration of the nano-cellulose solution is 6-12wt%, and the addition amount of the kenyaite powder is 4-8% of the mass of the nano-cellulose solution.
The dosage ratio of the nano-cellulose and the kenyaite powder needs to be strictly controlled, and if the ratio is unbalanced, the loading capacity and the controlled release effect of the composite aerogel are seriously influenced.
Preferably, in the step D), the mass ratio of the prepared rehmannia root concentrated solution, the cellulose-kenyaite composite aerogel powder, the dextrin and the polyvinylpyrrolidone alcohol solution is 35-45:35-45:15-25: 1-3.
Compared with the prior art, the invention has the beneficial effects that:
1. the prepared rehmannia root decoction pieces and pills prepared by the method have low content of ineffective components and high utilization rate of effective components.
2. The prepared rehmannia root pill prepared by the method has a controlled release effect, is more favorable for good absorption, has better drug effect and is convenient to take.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 95 deg.C steam for 7 hr until the medicinal materials are black, taking out, and air drying for 7 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 3 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 68 ℃, the drying time is 5.5h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the embodiment have high yield of about 95 percent.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 70wt% for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment at 110 deg.C for 30min under the power of 700W, taking out, and drying to obtain kenyaite powder.
C) Preparing nano-cellulose into a nano-cellulose solution with the concentration of 9wt% by using an ionic liquid, adding 6% of hydroxosilicate powder by mass into the nano-cellulose solution, uniformly dispersing, stirring and heating to 70 ℃, and carrying out heat preservation reaction for 1.5 hours; freezing the solution at-16 deg.C for 3 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking 40 parts of prepared rehmannia root concentrated solution, adding 40 parts of cellulose-kenyaite composite aerogel powder, uniformly stirring, drying, and adding 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare a mother nucleus; and adding 18.5 parts of dextrin and 0.5 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The prepared rehmannia root pills (1 g) prepared by the embodiment have good roundness and hardness, no tailing and sticking phenomena, pill weight difference of less than 5 percent and dissolution time limit of not less than 30 min. Dissolution test shows that the cumulative release rate of the effective components of radix rehmanniae Preparata within 15min is about 49%.
Example 2
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 90 deg.C steam for 8 hr until the medicinal materials are black, taking out, and air drying for 6 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 2 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 65 ℃, the drying time is 6h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the embodiment have high yield of about 87%.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 60wt% for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment at 100 deg.C for 40min under the power of 600W, taking out, and drying to obtain kenyaite powder.
C) Taking nano-cellulose, preparing the nano-cellulose into a nano-cellulose solution with the concentration of 6wt% by using an ionic liquid, adding 4% of hydroxosilicate powder by mass into the nano-cellulose solution, uniformly dispersing, stirring and heating to 60 ℃, and carrying out heat preservation reaction for 2 hours; freezing the solution at-20 deg.C for 2 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking 35 parts of prepared rehmannia root concentrated solution, adding 45 parts of cellulose-kenyaite composite aerogel powder, uniformly stirring, drying, and adding 2 parts of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare a mother nucleus; then adding 17 parts of dextrin and 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The prepared rehmannia root pills (1 g) prepared by the embodiment have good roundness and hardness, no tailing and sticking phenomena, pill weight difference of less than 5 percent and dissolution time limit of not less than 30 min. Dissolution test shows that the cumulative release rate of the effective components of radix rehmanniae Preparata within 15min is about 44%.
Example 3
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 100 deg.C steam for 6 hr until the medicinal materials are black, taking out, and air drying for 6 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 4 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 70 ℃, the drying time is 5h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the embodiment have high yield of about 89%.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 80wt% for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment at 120 deg.C for 20min under the power of 800W, taking out, and drying to obtain kenyaite powder.
C) Taking nano-cellulose, preparing the nano-cellulose into a nano-cellulose solution with the concentration of 12wt% by using an ionic liquid, adding 8% of hydroxosilicate powder by mass into the nano-cellulose solution, uniformly dispersing, stirring and heating to 80 ℃, and carrying out heat preservation reaction for 1 h; freezing the solution at-18 deg.C for 4 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking 45 parts of prepared rehmannia root concentrated solution, adding 35 parts of cellulose-kenyaite composite aerogel powder, uniformly stirring, drying, and adding 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare a mother nucleus; and adding 18 parts of dextrin and 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The prepared rehmannia root pills (1 g) prepared by the embodiment have good roundness and hardness, no tailing and sticking phenomena, pill weight difference of less than 5 percent and dissolution time limit of not less than 30 min. Dissolution test shows that the cumulative release rate of the effective components of radix rehmanniae Preparata within 15min is about 53%.
Example 4
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 98 deg.C steam for 8 hr until the medicinal materials are black, taking out, and air drying for 8 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 3.5 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 70 ℃, the drying time is 5h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the embodiment have high yield of about 93 percent.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 75wt% for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment at 115 deg.C under microwave power of 750W for 25min, taking out, and drying to obtain kenyaite powder.
C) Taking nano-cellulose, preparing the nano-cellulose into a nano-cellulose solution with the concentration of 8wt% by using an ionic liquid, adding 5% of hydroxosilicate powder by mass into the nano-cellulose solution, uniformly dispersing, stirring and heating to 75 ℃, and carrying out heat preservation reaction for 2 hours; freezing the solution at-16 deg.C for 3 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking 39 parts of prepared rehmannia root concentrated solution, adding 39 parts of cellulose-kenyaite composite aerogel powder, uniformly stirring, drying, and adding 0.5 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare a mother nucleus; then adding 21 parts of dextrin and 0.5 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The prepared rehmannia root pills (1 g) prepared by the embodiment have good roundness and hardness, no tailing and sticking phenomena, pill weight difference of less than 5 percent and dissolution time limit of not less than 30 min. Dissolution test shows that the cumulative release rate of the effective components of the prepared rehmannia root within 15min is about 48 percent.
Example 5
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 98 deg.C steam for 7 hr until the medicinal materials are black, taking out, and air drying for 7 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 4 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 68 ℃, the drying time is 5h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
The prepared rehmannia root decoction pieces prepared by the embodiment have high yield of about 94 percent.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 65wt% for later use.
B) Cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, placing in a vacuum microwave apparatus for vacuum microwave reflux treatment at 105 deg.C under 650W for 35min, taking out, and drying to obtain kenyaite powder.
C) Taking nano-cellulose, preparing the nano-cellulose into a nano-cellulose solution with the concentration of 10wt% by using an ionic liquid, adding 5% of hydroxosilicate powder by mass into the nano-cellulose solution, uniformly dispersing, stirring and heating to 65 ℃, and carrying out heat preservation reaction for 2 hours; freezing the solution at-16 deg.C for 3 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use.
D) Taking 35 parts of prepared rehmannia root concentrated solution, adding 37 parts of cellulose-kenyaite composite aerogel powder, uniformly stirring, drying, and adding 2 parts of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare a mother nucleus; then adding 25 parts of dextrin and 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The prepared rehmannia root pills (1 g) prepared by the embodiment have good roundness and hardness, no tailing and sticking phenomena, pill weight difference of less than 5 percent and dissolution time limit of not less than 30 min. Dissolution test shows that the cumulative release rate of the effective components of the prepared rehmannia root within 15min is about 48 percent.
Comparative example 1
A preparation method of prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part, wherein the impurities and non-medicinal part are less than or equal to 3 wt%.
2) Washing and moistening: and (4) cleaning the cleaned and selected radix rehmanniae with water, and draining the water.
3) Steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with 95 deg.C steam for 7 hr until the medicinal materials are black, taking out, and air drying for 7 hr to eighty percent dry.
4) Cutting: slicing the prepared rehmannia root processed in the step 3), wherein the slicing thickness is 3 mm.
5) And (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust. Wherein the drying temperature is 68 ℃, the drying time is 5.5h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
A method for preparing radix rehmanniae Preparata pill with radix rehmanniae Preparata decoction pieces prepared by the above method as raw materials comprises the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to obtain a prepared rehmannia root concentrated solution with the concentration of 70wt% for later use.
B) The kenyaite is taken, washed by water and ground into powder for standby.
C) Taking 40 parts of prepared rehmannia root concentrated solution, adding 40 parts of hydroxosilate powder, uniformly stirring, drying, and adding 1 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% to prepare mother nucleus; and adding 18.5 parts of dextrin and 0.5 part of polyvinylpyrrolidone alcohol solution with the concentration of 5wt% for coating, and preparing into pills.
The pill (1 g) prepared from radix rehmanniae Preparata prepared by this comparative example has dissolution time of 20-25 min. Dissolution test shows that the cumulative release rate of the effective components of radix rehmanniae Preparata within 15min is above 68%.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (7)
1. A method for preparing a prepared rehmannia root pill, which is characterized by comprising the following steps:
A) taking prepared rehmannia root decoction pieces, crushing, performing reflux alcohol extraction, and concentrating to prepare a prepared rehmannia root concentrated solution for later use;
B) cleaning the kenyaite with water, grinding into powder, dispersing into ethanol solution, and placing in a vacuum microwave apparatus for vacuum microwave reflux treatment, wherein the microwave power is 600-800W, the temperature is 100-120 ℃, and the treatment time is 20-40 min; taking out and drying to obtain the kenyaite powder for later use;
C) preparing nano-cellulose into a nano-cellulose solution by using an ionic liquid, adding the kenyaite powder into the nano-cellulose solution, uniformly dispersing, stirring and heating to 60-80 ℃, and carrying out heat preservation reaction for 1-2 hours; freezing the solution at-20 deg.C to-16 deg.C for 2-4 days, taking out, thawing at normal temperature, and washing to remove unreacted impurities to obtain cellulose-kenyaite composite wet gel; replacing the solvent in the cellulose-kenyaite composite wet gel with alcohol, drying by supercritical carbon dioxide fluid, and finally grinding to obtain cellulose-kenyaite composite aerogel powder for later use; the concentration of the nano-cellulose solution is 6-12wt%, and the addition amount of the kenyaite powder is 4-8% of the mass of the nano-cellulose solution;
D) taking radix rehmanniae Preparata concentrated solution, adding cellulose-kenyaite composite aerogel powder, stirring well, drying, adding polyvinylpyrrolidone alcohol solution to prepare mother nucleus; adding dextrin and polyvinylpyrrolidone alcohol solution, coating, and making into pill;
the preparation method of the prepared rehmannia root decoction pieces comprises the following steps:
1) cleaning and selecting: cleaning rehmanniae radix to remove impurities and non-medicinal part;
2) washing and moistening: cleaning the cleaned and selected dried rehmannia root with water, and draining;
3) steaming: separating the drained radix rehmanniae, placing in a steaming container, heating with steam until the medicinal materials are black, taking out, and drying in the air to eight dry;
4) cutting: slicing the prepared rehmannia root processed in the step 3);
5) and (3) drying: drying the sliced radix rehmanniae Preparata, and sieving to remove dust.
2. The preparation method according to claim 1, wherein in step 1), the impurity and non-medicinal part of the selected medicinal material are less than or equal to 3 wt%.
3. The preparation method according to claim 1, wherein in the step 3), the steam heating temperature is 90-100 ℃, the heating time is 6-8h, and the airing time is 6-12 h.
4. The method according to claim 1, wherein in step 4), the slice thickness is 2 to 4 mm.
5. The preparation method according to claim 1, wherein in the step 5), the drying temperature is 65-70 ℃, the drying time is 5-6h, and the water content of the dried medicinal material is less than or equal to 13 wt%.
6. The method of claim 1, wherein the concentration of the prepared rehmannia root concentrate in step A) is 60 to 80 wt%.
7. The method according to claim 1, wherein the mass ratio of the prepared rehmannia root concentrate, the cellulose-kenyaite composite aerogel powder, the dextrin and the polyvinylpyrrolidone alcohol solution in step D) is 35-45:35-45:15-25: 1-3.
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| 水羟硅钠石的制备与表征;戈明亮等;《化工进展》;20141231;第33卷(第12期);第3309-3312页，尤其是第3309页和第3310页左栏第1-2段 * |
| 纤维素基气凝胶材料及其应用研究进展;张鑫等;《中国材料进展》;20170831;第36卷(第7-8期);第512-520页，尤其是第513页左栏第1段，右栏倒数第2段，第514页右栏第2段，第519页左栏第1段 * |
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