CN107898916B - Method for processing bulbus fritilariae and bulbus fritilariae preparation - Google Patents
Method for processing bulbus fritilariae and bulbus fritilariae preparation Download PDFInfo
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Abstract
The invention provides a method for processing bulbus fritilariae and a bulbus fritilariae preparation, wherein the method for processing the bulbus fritilariae comprises the following steps: (1) slicing or coarsely crushing the bulbus fritilariae, adding an ethanol extracting solution of the rosa davurica pall, and soaking for 1-2 hours at room temperature, wherein the adding amount of the ethanol extracting solution of the rosa davurica pall at least exceeds the bulbus fritilariae; (2) drying the bulbus fritilariae at 70-100 ℃ until the water content is lower than 8%; (3) and micronizing the dried bulbus fritilariae at the temperature of between 35 ℃ below zero and 25 ℃ below zero until more than 95 percent of bulbus fritilariae ultrafine powder has the particle size of 400 to 600 meshes. The bulbus fritilariae processed by the method not only can inhibit browning, increase the elution amount of alkaloid and saponin and improve the drug effect, but also has the advantages of energy conservation, low cost and high cost performance.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine processing, and particularly relates to a method for processing bulbus fritilariae and a bulbus fritilariae preparation.
Background
The bulbus fritilariae is the dry bulb of bulbus fritilariae F.cirrhosa D.Don, Fritillaria unibracteata Hsiaoet K.C.Hsia, Fritillaria kansuensis F.przewalski Maxim and Fritillaria fusiformis F.delayi Franch which belong to the traditional famous and precious Chinese medicinal materials in China. Starch is the main component of the bulbus fritillariae cirrhosae, which accounts for about 40-60% of the total mass of the bulbus fritillariae cirrhosae, the rest main components comprise cellulose, protein, fatty acid and the like, and the medicinal components of the bulbus fritillariae cirrhosae mainly comprise alkaloid, saponin, terpenes and steroid substances.
According to records in the book of Dian nan materia Medica of traditional Chinese medicine, the bulbus fritillariae cirrhosae has the functions of clearing heat, moistening lung, reducing phlegm and relieving cough. Modern pharmacological studies also confirm that the bulbus fritilariae can relax tracheal smooth muscle and has the effects of relieving asthma, relieving cough and eliminating phlegm; bulbus Fritillariae Cirrhosae has effects of lowering blood pressure, slowing heart rate, inhibiting platelet aggregation, relaxing intestinal tract contraction, slowing gastrointestinal peristalsis and resisting ulcer; in addition, Bulbus Fritillariae Cirrhosae has certain therapeutic effects on central nervous system, respiratory tract infection and tumor.
In view of the above important pharmacological actions of Chuan Bei, how to avoid the failure of active pharmaceutical ingredients in Chuan Bei and promote the dissolution of the active pharmaceutical ingredients in the Chuan Bei has important significance. The traditional processing method of the bulbus fritillariae cirrhosae is to dry the bulbus fritillariae cirrhosae at high temperature and then crush the bulbus fritillariae cirrhosae into coarse particles or slice the bulbus fritillariae cirrhosae and then dry the bulbus fritillariae cirrhosae at high temperature, and before use, the active medicine components such as alkaloid, saponin and the like are promoted to be released by adding water and decocting. The traditional processing method has great defects. Firstly, the coarse crushing or slicing cannot effectively destroy the cell wall of the tendril-leaved fritillary bulb, which is not beneficial to the dissolution of the active ingredients. Secondly, due to the high content of starch, the bulbus fritilariae is easy to brown in the drying process, and the content of active ingredients is influenced. Therefore, there is a need for an improvement of the conventional processing method of fritillaria cirrhosa.
The superfine grinding technology is a high and new technology which is rapidly developed in nearly 20 years, has unique advantages in the field of traditional Chinese medicine processing, can improve the cell wall breaking rate of traditional Chinese medicines, increase the specific surface area, and enable the particle size to reach micron order, thereby effectively improving the utilization rate of the traditional Chinese medicines and enhancing the curative effect of the medicines. The low-temperature ultramicro-pulverization technology is a novel pulverization technology developed on the basis of the ultramicro-pulverization technology, and the technology can be operated at a low temperature, so that the inactivation of heat-sensitive substances in the traditional Chinese medicinal materials can be effectively reduced, the loss of volatile components can be reduced, and the defect that polysaccharide substances are easy to adhere in the pulverization process can be avoided.
However, both the conventional superfine grinding technology and the low-temperature superfine grinding technology have great difference in the optimal technological conditions for superfine grinding of different traditional Chinese medicinal materials, and the specific processing effects are different, so that some traditional Chinese medicinal materials are even not suitable to be processed by adopting the technology due to the technical problem which is difficult to overcome. Reference 1 ("research status and thinking of superfine grinding of traditional Chinese medicine", Zhao rui zhi, 2013 research on biological particle preparation technology and industrial application technology) records: below 20 μm, the effect of reducing the particle size of the medicinal materials on increasing the dissolution of anthraquinone in rhubarb is not great; for safflower and root bark of tree peony, the superfine grinding can not increase the dissolution amount of the main components; the superfine pulverized ginseng can increase the dissolution amount of ginsenoside and polysaccharide, but has no obvious effect on improving the curative effect. In addition, after the traditional Chinese medicinal materials are subjected to ultra-refining, the physicochemical properties of the traditional Chinese medicinal materials are often changed, so that the difficulty is increased for later processing and use of the medicine. In addition, in addition to the characteristics of the traditional Chinese medicines, the superfine grinding technology, especially the low-temperature and super-temperature grinding technology, has high energy consumption and high cost, and is one of the problems encountered when the technology is applied to the traditional Chinese medicine processing.
Therefore, in order to increase the cell wall breaking rate and to increase the dissolution of the active substances, it is conceivable to process fritillaria cirrhosa by low-temperature micronization, but the following technical problems need to be solved: (1) is suitable for the low-temperature superfine grinding process conditions of the bulbus fritilariae; (2) before crushing, the brown phenomenon is easy to occur in the drying process of the bulbus fritilariae; (3) after the bulbus fritilariae is subjected to low-temperature superfine grinding, the physical and chemical properties can be changed, and the subsequent processing and utilization are not facilitated.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a method for processing bulbus fritillariae cirrhosae, by which the dissolution of alkaloid and saponin which are active medicinal ingredients of the bulbus fritillariae cirrhosae can be promoted.
The second purpose of the invention is to provide the bulbus fritillariae cirrhosae preparation prepared by the method, and the preparation has the characteristics of high active substance content, easy dissolution and the like.
In order to solve the above problems, the present invention provides a method for processing fritillaria cirrhosa, comprising the steps of:
(1) slicing or coarsely crushing the bulbus fritilariae, adding an ethanol extracting solution of the rosa davurica pall, and soaking for 1-2 hours at room temperature, wherein the adding amount of the ethanol extracting solution of the rosa davurica pall at least exceeds the bulbus fritilariae;
(2) drying the bulbus fritilariae at 70-100 ℃ until the water content is lower than 8%;
(3) and micronizing the dried bulbus fritilariae at the temperature of between 35 ℃ below zero and 25 ℃ below zero until more than 95 percent of bulbus fritilariae ultrafine powder has the particle size of 400 to 600 meshes.
Firstly, the invention adopts a low-temperature superfine grinding technology to process the bulbus fritilariae, and researches the dissolution amount and the drug effect of active drug ingredients in the bulbus fritilariae superfine powder at different temperatures and different grinding fineness. According to the experimental data shown in experimental examples 1-2 of the present specification, it is known that crushing fritillaria cirrhosa to be too fine cannot effectively increase the dissolution of active substances and improve the curative effect of fritillaria cirrhosa, and this is probably because fritillaria cirrhosa is ground to be too fine, and the charges, adhesive force and the like on the surface of the powder change, and although the particle size is smaller, the release of active ingredients is not facilitated. In addition, the leaching rate of active ingredients of the bulbus fritillariae cirrhosae is higher when the temperature is lower in the low-temperature superfine grinding process, but the leaching rates of total alkaloids and total saponins are not obviously increased along with the reduction of the temperature after the temperature is lower than-35 ℃. Therefore, after comprehensively considering the dissolution rate of active ingredients in the fritillaria cirrhosa superfine powder, the treatment efficacy and the processing cost (the lower the temperature, the smaller the particle size of the powder and the higher the processing cost), the optimal process conditions for the low-temperature superfine grinding of the fritillaria cirrhosa are finally determined as follows: micronizing the dried bulbus fritilariae at a temperature of between 25 ℃ below zero and 35 ℃ below zero until more than 95 percent of bulbus fritilariae ultrafine powder has a particle size of 400 to 600 meshes.
Secondly, in order to increase the brittleness of the materials and reduce the crushing difficulty, the materials generally need to be dried before low-temperature and over-temperature crushing, so that the water content of the materials is reduced. High-temperature heating drying is a common drying mode because the processing mode is simple and complex instruments are not needed. The bulbus fritilariae with good drying degree and low water content can be quickly obtained by using a high-temperature drying mode, but the bulbus fritilariae is easy to brown, the content of alkaloid is reduced, and the quality of the bulbus fritilariae is reduced in the heating and drying process.
To overcome this drawback, the applicant has adopted several different ways to pretreat fritillaria cirrhosa, including the use of Vc, NaHSO3The bulbus fritilariae is soaked by various treatment liquids including citric acid, puerarin, resveratrol, ethanol extract of buckwheat seeds, ethanol extract of rosa davurica pall and the like so as to reduce the browning phenomenon of the bulbus fritilariae in the drying process. Finally, the invention surprisingly found that the compounds with Vc, NaHSO3Compared with treatment solutions such as citric acid, puerarin and ethanol extract of buckwheat seeds, the brown phenomenon of the bulbus fritilariae in the high-temperature drying process is obviously reduced and the reduction of the total alkaloid content is also obviously inhibited after the soaking treatment of the ethanol extract of the rosa davurica pall. The effect of the ethanol extract of the rosa davurica pall on the aspect of inhibiting the brown of the bulbus fritilariae is basically equivalent to that of the resveratrol treatment solution, but the rosa davurica pall can be prepared in large scale by taking the rosa davurica pall as a raw material through simple extraction operation, the operation is simple, the cost is low, and the resveratrol can be obtained by a complicated separation and purification method. At present, specific raw materials of the ethanol extract of rosa davurica pall which can inhibit brown-out of fritillaria cirrhosa caused by high-temperature drying are not clear. However, no matter how the ethanol extract of the rosa davurica pall plays a role in particular, the inhibition effect on the brown-ing of the bulbus fritilariae is undoubted.
In conclusion, the method of the invention uses the ethanol extract of the rosa davurica pall to treat the bulbus fritilariae before heating and drying, which not only has good effect of inhibiting the bulbus fritilariae from browning, but also has low cost and high cost performance.
In some embodiments, the ethanol extract of rosa davurica pall is extracted by: slicing fructus Rosae Davuricae, drying, pulverizing, extracting with ethanol solution, separating solid and liquid, and decolorizing with active carbon to obtain ethanol extractive solution.
In some embodiments, the ethanol extract of rosa davurica pall is extracted by: slicing the rosa davurica pall, drying for 12-24 hours at 70-100 ℃, then crushing the rosa davurica pall, sieving with a 50-100-mesh sieve, adding 60-95% of ethanol solution according to the mass-volume ratio of 10-15 g to 100mL, leaching for 2-4 hours, carrying out solid-liquid separation, adding 1-5% of activated carbon according to the mass-volume ratio, shaking for 20-40 min, and filtering to obtain the ethanol extract of the rosa davurica pall.
In some embodiments, between step (2) and step (3), the method further comprises the steps of: crushing the bulbus fritillariae cirrhosae, sieving the crushed bulbus fritillariae cirrhosae with a 50-100-mesh sieve, adding water to dissolve the crushed bulbus fritillariae cirrhosae into bulbus fritillariae cirrhosae slurry, then carrying out high-pressure homogenization treatment on the slurry, and carrying out low-temperature freeze drying on the treated slurry.
Decocting with water is a conventional treatment method for Bulbus Fritillariae Cirrhosae decoction pieces, and can further promote release of alkaloid and saponin. However, the present invention surprisingly found that the Bulbus Fritillariae Cirrhosae ultra-fine powder subjected to low temperature ultra-fine pulverization could not increase the release of alkaloid and saponin after decocting, but rather the elution of alkaloid and saponin could be reduced, as compared with the method of directly taking with hot water or soaking, and if the Bulbus Fritillariae Cirrhosae ultra-fine powder is subjected to high pressure homogenization before ultra-fine pulverization, this phenomenon could be avoided, and the release of alkaloid and saponin during decocting could be effectively increased.
At present, the reason for the phenomenon is not clear, probably because the particle size of the bulbus fritillariae cirrhosae ultrafine powder is too fine, starch or protein is gelatinized in the decocting process, the leaching of effective substances is not facilitated, the starch and protein in the bulbus fritillariae cirrhosae are modified by high-pressure homogenization operation before ultrafine grinding, the gelatinization effect at high temperature is inhibited, and the release amount of alkaloid and saponin is increased.
In some embodiments, the specific manner of the high-pressure homogenization treatment includes: homogenizing under 20-30 MPa for 1-2 min.
In some embodiments, the method further comprises the steps of: adding an ethanol solution accounting for 30-50% of the weight of the fritillaria cirrhosa superfine powder, uniformly stirring, preparing a soft material, granulating, drying and sieving to obtain fritillaria cirrhosa granules, wherein the volume fraction of ethanol in the ethanol solution is 60-80%. The method does not add any excipient in the granulating process, not only can effectively keep all natural characteristics of the traditional Chinese medicinal materials, but also has very simple preparation process and is easy to form industrial production.
In some embodiments, the method further comprises the steps of: mixing Bulbus Fritillariae Cirrhosae superfine powder with adjuvants, and making into tablet; preferably, the auxiliary materials comprise one or more of microcrystalline cellulose, pregelatinized starch, lactose, carboxymethyl starch, calcium hydrogen phosphate, aerosil and magnesium stearate.
In some embodiments, the method further comprises the steps of: adding 60-95% ethanol solution into the bulbus fritillariae cirrhosae superfine powder according to the mass-volume ratio of 10-15 g to 100mL, leaching for 1-3 hours, and carrying out solid-liquid separation to obtain supernatant, namely bulbus fritillariae cirrhosae extracting solution.
In some embodiments, the fritillaria cirrhosa is selected from one or more of fritillaria cirrhosa f.cirrhosa d.don, fritillaria unibracteata Hsiao et k.c.hsia, fritillaria kansuensis f.przewalski maxim, and fritillaria fusiformis f.delayayi Franch, preferably, the fritillaria cirrhosa f.cirrhosa d.don.
The invention also provides a bulbus fritilariae preparation prepared by the method. The bulbus fritilariae preparation has the advantages of high cell wall breaking rate, high dissolution rate of active ingredients and direct taking, soaking or decoction.
Compared with the prior art, the invention has the beneficial effects that:
1) after comprehensively considering the dissolution amount of active substances, the drug effect and the cost of the bulbus fritillariae cirrhosae ultrafine powder, the invention finally determines the optimal process conditions of low-temperature ultrafine crushing of the bulbus fritillariae cirrhosae: micronizing the dried bulbus fritilariae at the temperature of between 35 ℃ below zero and 25 ℃ below zero until more than 95 percent of bulbus fritilariae ultrafine powder has the particle size of 400 to 600 meshes. Under the process conditions, the dissolution amount of alkaloid and saponin of the bulbus fritillariae cirrhosae is increased, the drug effect is improved, and the advantages of energy conservation, low cost and high cost performance are achieved.
2) According to the method, the bulbus fritilariae is soaked by using the ethanol extract of the rosa davurica pall before high-temperature drying, so that the browning rate of the bulbus fritilariae in the high-temperature drying process can be effectively inhibited, and the loss of alkaloid is reduced.
3) According to the method, the bulbus fritilariae is subjected to high-pressure homogenization treatment before low-temperature superfine grinding, and the defect that the dissolution rate of alkaloid and saponin is low in the decocting process of the bulbus fritilariae superfine powder can be overcome through the treatment.
4) The bulbus fritilariae preparation has the advantages of high cell wall breaking rate, high dissolution rate of active ingredients and direct taking, soaking or decoction.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
Processing the bulbus fritilariae according to the following method:
1. cleaning: removing impurities from qualified fresh Bulbus Fritillariae Cirrhosae (F. cirrhrosa D. don), cleaning, and air drying.
2. Placing Bulbus Fritillariae Cirrhosae in a tray, drying at 70 deg.C until the water content is about 8%, stopping drying, and cooling to room temperature.
3. And coarsely pulverizing the dried Bulbus Fritillariae Cirrhosae slices with a multifunctional pulverizer to obtain coarse powder with particle size of 50 meshes.
4. Micronizing Bulbus Fritillariae Cirrhosae coarse powder at-30 deg.C with vibration type low temperature micronizer to obtain 95% or more ultrafine Bulbus Fritillariae Cirrhosae powder with particle size of about 500 meshes.
5. Uniformly mixing the bulbus fritillariae cirrhosae superfine powder, adding 60% volume concentration ethanol solution as a bonding agent, uniformly stirring with the bulbus fritillariae cirrhosae superfine powder to prepare a soft material, granulating by using a granulator, drying at 60 ℃ until the moisture content is lower than 5%, and granulating by using a 24-mesh screen to obtain qualified granules meeting the requirement on granularity, wherein the mass ratio of the bulbus fritillariae cirrhosae superfine powder to the ethanol solution is 70: 30.
6. The bulbus fritilariae particles are uniformly mixed, so that the difference of particle samples at each sampling point of the same batch of products is less than 3%.
7. Subpackaging the qualified bulbus fritilariae granules by using soaking bags according to the proportion of 3 g/bag.
Example 2
Bulbus Fritillariae Cirrhosae is processed as described in example 1, except that in step 4, 95% or more of the ultrafine Bulbus Fritillariae Cirrhosae powder has a particle size of about 400 mesh.
Example 3
Bulbus Fritillariae Cirrhosae is processed as described in example 1, except that in step 4, 95% or more of the ultrafine Bulbus Fritillariae Cirrhosae powder has a particle size of about 600 mesh.
Example 4
Bulbus Fritillariae Cirrhosae was processed as described in example 1, except that the micronization in step 4 was carried out at a temperature of-25 ℃.
Example 5
Bulbus Fritillariae Cirrhosae was processed as described in example 1, except that the temperature of micronization in step 4 was-35 ℃.
Example 6
Processing the bulbus fritilariae according to the following method:
1. cleaning: removing impurities from qualified fresh Bulbus Fritillariae Cirrhosae (F. cirrhrosa D. don), cleaning, and air drying.
2. Slicing the bulbus fritilariae by using a slicer to obtain bulbus fritilariae slices with uniform thickness.
3. Preparing an ethanol extracting solution of the rosa davurica pall: slicing the rosa davurica pall, drying for 12h at 70 ℃, crushing the dried sample by using a multifunctional sample crusher, sieving the crushed sample by using a 80-mesh sieve, adding 75% ethanol solution according to the mass-volume ratio of 1g to 10mL, leaching for 3 h, then carrying out solid-liquid separation, adding 5% mass fraction of active carbon, shaking for 30min, and filtering to obtain the ethanol extract of the rosa davurica pall.
4. Adding ethanol extractive solution of fructus Rosae Davuricae into Bulbus Fritillariae Cirrhosae tablet, and soaking Bulbus Fritillariae Cirrhosae tablet at room temperature for 30min, wherein the ethanol extractive solution is preferably added in an amount larger than that of Bulbus Fritillariae Cirrhosae tablet.
5. After the treatment, the bulbus fritilariae slices are dried, placed in a tray, put into a dryer and dried at 70 ℃ until the water content is about 5 percent, and then the drying is stopped and the temperature is cooled to the room temperature.
6. And coarsely pulverizing the dried Bulbus Fritillariae Cirrhosae slices with a multifunctional pulverizer to obtain coarse powder with particle size of 50 meshes.
7. Micronizing Bulbus Fritillariae Cirrhosae coarse powder at-30 deg.C with vibration type low temperature micronizer to obtain Bulbus Fritillariae Cirrhosae superfine powder with average fineness of about 500 meshes.
8. Uniformly mixing the bulbus fritillariae cirrhosae superfine powder, adding 70% volume concentration ethanol solution as a bonding agent, uniformly stirring with the bulbus fritillariae cirrhosae superfine powder to prepare a soft material, granulating by a granulator, drying at 60 ℃ until the moisture content is lower than 5%, and granulating by a 24-mesh screen to obtain qualified granules meeting the requirement of granularity, wherein the mass ratio of the bulbus fritillariae cirrhosae superfine powder to the ethanol solution is 70: 30.
9. The bulbus fritilariae particles are uniformly mixed, so that the difference of particle samples at each sampling point of the same batch of products is less than 3%.
10. Packaging qualified Bulbus Fritillariae Cirrhosae granules with soaking belt at a ratio of 3 g/bag.
Example 7
Processing the bulbus fritilariae according to the following method:
1. cleaning: removing impurities from qualified fresh Bulbus Fritillariae Cirrhosae (F. cirrhrosa D. don), cleaning, and air drying.
2. Slicing the bulbus fritilariae by using a slicer to obtain bulbus fritilariae slices with uniform thickness.
3. Preparing an ethanol extracting solution of the rosa davurica pall: slicing the rosa davurica pall, drying for 24 hours at 70 ℃, crushing the dried sample by using a multifunctional sample crusher, sieving the crushed sample by using a 50-mesh sieve, adding 75% ethanol solution according to the mass-volume ratio of 1g to 10mL, leaching for 3 hours, then carrying out solid-liquid separation, adding 5% mass fraction of active carbon, shaking for 30 minutes, and filtering to obtain the ethanol extract of the rosa davurica pall.
4. Adding ethanol extractive solution of fructus Rosae Davuricae into Bulbus Fritillariae Cirrhosae tablet, and soaking Bulbus Fritillariae Cirrhosae tablet at room temperature for 30min, wherein the ethanol extractive solution is preferably added in an amount larger than that of Bulbus Fritillariae Cirrhosae tablet.
5. After the treatment, the bulbus fritilariae slices are dried, placed in a tray, put into a dryer and dried at 70 ℃ until the water content is about 5 percent, and then the drying is stopped and the temperature is cooled to the room temperature.
6. And coarsely pulverizing the dried Bulbus Fritillariae Cirrhosae slices with a multifunctional pulverizer to obtain coarse powder with particle size of 50 meshes.
7. Dissolving the coarse powder of the bulbus fritilariae with 3 times of volume of water, grinding into slurry to obtain bulbus fritilariae slurry, and then homogenizing for 2 minutes by a homogenizer under the pressure of 30 MPa.
8. And (3) freeze-drying the slurry subjected to high-pressure homogenization treatment at the temperature of-40 ℃ for 36 hours.
9. Micronizing at-30 deg.C with a vibration type low temperature micronizer to obtain superfine powder of Bulbus Fritillariae Cirrhosae with average fineness of about 500 meshes.
10. Uniformly mixing the bulbus fritillariae cirrhosae superfine powder, adding 80% volume concentration ethanol solution as a bonding agent, uniformly stirring with the bulbus fritillariae cirrhosae superfine powder to prepare a soft material, granulating by using a granulator, drying at 70 ℃ until the moisture content is lower than 5%, and granulating by using a 24-mesh screen to obtain qualified granules meeting the requirement on granularity, wherein the mass ratio of the bulbus fritillariae cirrhosae superfine powder to the ethanol solution is 80: 20.
11. The bulbus fritilariae particles are uniformly mixed, so that the difference of particle samples at each sampling point of the same batch of products is less than 3%.
12. Packaging qualified Bulbus Fritillariae Cirrhosae granules with soaking belt at a ratio of 3 g/bag.
Example 8
Bulbus Fritillariae Cirrhosae was processed by the method described in example 7, except that the pressure of the high homogenization treatment in step 7 was 20 MPa.
Example 9
Bulbus Fritillariae Cirrhosae was processed by the method described in example 7, except that the pressure of the high-pressure homogenization treatment in step 7 was 25 MPa.
Comparative example 1
Processing the bulbus fritilariae according to the following method:
1. cleaning: removing impurities from qualified fresh Bulbus Fritillariae Cirrhosae (F. cirrhrosa D. don), cleaning, and air drying.
2. Placing Bulbus Fritillariae Cirrhosae in a tray, drying at 70 deg.C until the water content is about 8%, stopping drying, and cooling to room temperature.
3. And coarsely pulverizing the dried Bulbus Fritillariae Cirrhosae slices with a multifunctional pulverizer to obtain coarse powder with particle size of 50 meshes.
4. Uniformly mixing the bulbus fritillariae cirrhosae superfine powder, adding 60% volume concentration ethanol solution as a bonding agent, uniformly stirring with the bulbus fritillariae cirrhosae superfine powder to prepare a soft material, granulating by using a granulator, drying at 70 ℃ until the moisture content is lower than 5%, and granulating by using a 24-mesh screen to obtain qualified granules meeting the requirement on granularity, wherein the mass ratio of the bulbus fritillariae cirrhosae superfine powder to the ethanol solution is 60: 40.
5. The bulbus fritilariae particles are uniformly mixed, so that the difference of particle samples at each sampling point of the same batch of products is less than 3%.
6. Packaging qualified Bulbus Fritillariae Cirrhosae granules with soaking belt at a ratio of 3 g/bag.
Comparative examples 2 to 8
Comparative examples 2 to 8 Bulbus Fritillariae Cirrhosae processed by the method described in example 1 is different in that 95% or more of the ultrafine Bulbus Fritillariae Cirrhosae powder in step 4 has a particle size of about 100 mesh, 200 mesh, 300 mesh, 700 mesh, 800 mesh, 900 mesh, and 1000 mesh, respectively.
Comparative examples 9 to 14
Comparative examples 9 to 14 Bulbus Fritillariae Cirrhosae processed by the method described in example 1 was characterized in that the temperatures for the low-temperature micronization in step 4 were-10 ℃, -15 ℃, -20 ℃, -40 ℃, -45 ℃ and-50 ℃.
Comparative examples 15 to 20
Comparative examples 15-20 bulbus fritilariae was processed according to the method described in example 6, with the only difference that steps 3-4 were: vc treatment liquid (0.1g/L) and NaHSO are respectively prepared by 0.1M phosphate buffer3Adding the treatment liquid (0.2g/L), citric acid treatment liquid (15g/L), puerarin treatment liquid (0.001mol/L), resveratrol treatment liquid (0.1mol/L) and ethanol extract of buckwheat seeds into the bulbus fritilariae tablets, and treating for 30 minutes if the bulbus fritilariae tablets are submerged. Wherein the ethanol extract of buckwheat seeds is obtained by the following steps: peeling buckwheat seeds, drying at 80 ℃ for 12 hours, crushing, sieving with a 80-mesh sieve, and mixing the powder according to the mass-volume ratio of 10 g: adding 100ml of the extract into 60% ethanol solution, leaching for 3 hours, and performing solid-liquid separation to obtain ethanol extract of buckwheat seeds.
Comparative examples 21 to 24
Comparative examples 21 to 24 Bulbus Fritillariae Cirrhosae was processed by the method described in example 7, except that the treatment pressure for high-pressure homogenization in step 7 was 10MPa, 40MPa, 50MPa, and 60MPa, respectively.
Experimental example 1
The elution amount of total alkaloids and total saponins in the fritillaria cirrhosa granules in examples 1-5 and comparative examples 1-14 is detected, and specific detection results are shown in table 1 and table 2, wherein table 1 shows elution amount of total alkaloids and total saponins in fritillaria cirrhosa granules with different particle sizes, and table 2 shows content of total alkaloids and total saponins in fritillaria cirrhosa granules with different temperatures.
The specific detection method of the total alkaloid elution amount comprises the following steps: soaking 5g of bulbus fritillariae cirrhosae particles in 100mL of 70 ℃ drinking water for 15min, then carrying out solid-liquid separation, evaporating the obtained liquid to dryness on a water bath, dissolving the residue with a small amount of chloroform, evaporating to dryness, dissolving the residue with 10mL of diethyl ether, adding 10mL of 0.001mol/L standard sulfuric acid solution, carefully removing the diethyl ether on the water bath, adding 15mL of newly-boiled cooled distilled water, using methyl red as an indicator, dripping back with 0.002mol/L standard sodium hydroxide solution, and changing the solution at the end point of titration from red to yellow. The alkaloid content is calculated according to the following formula:
the percentage content of the total alkaloids is 2MVm 100%/(1000W), wherein M-mole concentration of standard sulfuric acid solution, V-milliliter number of consumed standard sulfuric acid solution, W-gram number of sample, and M-molecular weight of the fritillaria cirrhosa alkali (calculated as sibiricin, 429).
The specific detection of the total saponin elution amount is as follows: soaking 5g of bulbus fritillariae cirrhosae ultrafine powder in 100mL of drinking water at 70 ℃ for 15min, then carrying out solid-liquid separation, evaporating the obtained liquid on a water bath to dryness, dissolving residues with 20mL of methanol, adding 50mL of diethyl ether, mixing uniformly, placing in a refrigerator overnight, pouring out supernate, dissolving precipitates with 10mL of diethyl ether by heating with 30mL of methanol after washing, filtering with a vertical melting hourglass funnel which is dried to constant weight, adding 50mL of diethyl ether into filtrate, placing in the refrigerator overnight, filtering with the vertical melting glass hourglass funnel, draining, drying in vacuum at 60 ℃ to constant weight, weighing, subtracting the weight of the funnel to obtain the content of total saponins in the sample, and calculating the mass fraction of the total saponins in the sample.
TABLE 1 elution amounts of Total alkaloid and Total Saponin in Bulbus Fritillariae Cirrhosae granules of different particle sizes
TABLE 2 elution amounts of Total alkaloid and Total Saponin in Bulbus Fritillariae Cirrhosae granules at different pulverization temperatures
Experimental example 2
The fritillary bulb particles of examples 1-5 and comparative examples 1-14 were tested for antitussive and expectorant effects:
1. cough-inducing Guinea pig citric acid experiment
About 200 + -50 g of guinea pigs were divided into 20 groups of 3 animals, and the groups were assigned to the blank control group, examples 1 to 5, and comparative examples 1 to 14, respectively. Taking 1g of the bulbus fritillariae cirrhosae particles in examples 1-5 and comparative examples 1-14, adding 5mL of water to prepare bulbus fritillariae cirrhosae suspension, performing intragastric administration on mice for 5 days according to the ratio of 3 times per day, wherein drinking water is used as a blank control, and performing intragastric administration on control mice. After 1h after the end of the 5 th day administration, each group was challenged with a 17.5% citric acid spray, and after 30s, the number of coughs in the guinea pigs within 5min was observed and recorded (see table 3 for specific test results).
2. Rat capillary sputum excretion experiment
SD rats were randomly divided into 20 groups of 3 rats each corresponding to a blank control group, examples 1 to 5 and comparative examples 1 to 14, respectively. Taking 1g of bulbus fritillariae cirrhosae particles described in examples 1-5 and comparative examples 1-14, adding 5mL of water to prepare bulbus fritillariae cirrhosae micro-suspension, performing intragastric administration on rats for 3 times per day for 5 days, after administration for 1h on the 5 th day, anesthetizing 25% urethane according to 1g/kg, fixing the back, exposing trachea, inserting a glass capillary tube with the diameter of 0.5mm into the position of the 3 rd ring cartilage ring below the thyroid cartilage ring, collecting sputum for 2h, and analyzing the length of each group of sputum in 2h and the quality of the sputum in unit time by taking the length of the sputum as an index (the specific detection result is shown in Table 3).
TABLE 3 cough and asthma relieving effects of Chuan Bei mu Ke Li
Experimental example 3
1. The browning degree of the bulbus fritilariae after high-temperature drying in the examples 1 and 6 and the comparative examples 15-19 is detected: grinding 1g of Bulbus Fritillariae Cirrhosae before and after drying into homogenate, adding 10ml of distilled water, fixing volume to the maximum capacity of centrifuge tube, centrifuging at 4000rpm for 20min, and collecting supernatant. Measuring absorbance at 460nm on ultraviolet spectrophotometer by absorbance method, and determining browning degree as OD460Before drying-OD460After dryingThe specific test results are shown in Table 5.
2. Detecting the content of total alkaloids and saponins in the leaching solution: taking 5g of the bulbus fritillariae cirrhosae particles in examples 1 and 6 and comparative examples 15-19, adding 100ml of warm water with the temperature of 70 ℃, soaking for 15 minutes, carrying out solid-liquid separation, and detecting the elution amount of total alkaloids and saponins in a leaching solution, wherein the specific detection method is shown in experimental example 1, and the specific detection results are shown in table 4.
TABLE 4 brown-out and dissolution test of active substance of Sichuan fritillary bulb
Experimental example 4
Taking 5g of the bulbus fritillariae cirrhosae granules in examples 1, 7-9 and comparative examples 20-23, adding 150mL of water, decocting for 10 minutes, carrying out solid-liquid separation, and detecting the elution amount of total alkaloids and total saponins in a decoction, wherein the specific detection method is shown in experiment example 1, and the specific detection result is shown in Table 5.
TABLE 5 elution amount of Total alkaloid and Total Saponin in Bulbus Fritillariae Cirrhosae granule in decoction
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method of processing fritillaria cirrhosa, comprising the steps of:
(1) slicing or coarsely crushing the bulbus fritilariae, adding an ethanol extracting solution of the rosa davurica pall, and soaking for 1-2 hours at room temperature, wherein the adding amount of the ethanol extracting solution of the rosa davurica pall at least exceeds the bulbus fritilariae;
(2) drying the bulbus fritilariae at 70-100 ℃ until the water content is lower than 8%;
(3) micronizing the dried bulbus fritilariae at the temperature of between 35 ℃ below zero and 25 ℃ below zero until the particle size of more than 95 percent of bulbus fritilariae micropowder is within the range of 400-600 meshes;
between step (2) and step (3), the method further comprises the steps of: crushing the bulbus fritillariae cirrhosae, sieving the crushed bulbus fritillariae cirrhosae with a 50-100-mesh sieve, adding water to dissolve the crushed bulbus fritillariae cirrhosae into bulbus fritillariae cirrhosae slurry, then carrying out high-pressure homogenization treatment on the slurry, and carrying out low-temperature freeze drying on the treated slurry;
the specific mode of the high-pressure homogenization treatment comprises the following steps: homogenizing under 20-30 MPa for 1-2 min.
2. The method according to claim 1, wherein the ethanol extract of rosa davurica pall is extracted by: slicing fructus Rosae Davuricae, drying, pulverizing, extracting with ethanol solution, separating solid and liquid, and decolorizing with active carbon to obtain ethanol extractive solution.
3. The method according to claim 2, wherein the ethanol extract of rosa davurica pall is extracted by:
slicing the rosa davurica pall, drying for 12-24 hours at 70-100 ℃, then crushing the rosa davurica pall, sieving with a 50-100-mesh sieve, adding 60-95% by volume of ethanol solution according to the mass-volume ratio of 10-15 g to 100mL, leaching for 2-4 hours, carrying out solid-liquid separation, adding 1-5% by mass of activated carbon, shaking for 20-40 min, and filtering to obtain the ethanol extract of the rosa davurica pall.
4. A method according to any of claims 1-3, characterized in that the method further comprises the steps of: adding 30-50% by weight of ethanol solution with the volume fraction of 60-80% into the bulbus fritillariae cirrhosae ultrafine powder, uniformly stirring, preparing a soft material, granulating, drying and sieving to obtain bulbus fritillariae cirrhosae granules.
5. A method according to any of claims 1-3, characterized in that the method further comprises the steps of: mixing Bulbus Fritillariae Cirrhosae superfine powder with adjuvants, and making into tablet.
6. The method of claim 5, wherein the excipients comprise one or more of microcrystalline cellulose, pregelatinized starch, lactose, carboxymethyl starch, dibasic calcium phosphate, aerosil, magnesium stearate.
7. A method according to any of claims 1-3, characterized in that the method further comprises the steps of: adding 60-95% ethanol solution into the bulbus fritillariae cirrhosae superfine powder according to the mass-volume ratio of 10-15 g to 100mL, leaching for 1-3 hours, and carrying out solid-liquid separation to obtain supernatant, namely bulbus fritillariae cirrhosae extracting solution.
8. The method of any one of claims 1-3, wherein the Bulbus Fritillariae Cirrhosae is selected from Bulbus Fritillariae CirrhosaeF.cirrhosaDon and Fritillaria unibracteataF. unibracteataHsiao et K.C. Hsia, fritillary bulb of Gansu provinceF. przewalskiiMaxim, and Fritillaria fusiformisF. delavayiOne or more of Franch.
9. The method of any one of claims 1-3, wherein the Bulbus Fritillariae Cirrhosae is Bulbus Fritillariae CirrhosaeF.cirrhosaD.Don。
10. A fritillary bulb preparation prepared by the method according to any one of claims 1 to 9.
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| 川贝母鳞茎褐变的生理因子变化及其褐变抑制;张泽锦;《中国优秀硕士学位论文全文数据库——农业科技辑》;20110430(第4期);摘要第1页第3段，正文第6页第1段、第9页第4、5段 * |
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