CN113855727A - Preparation method of cistanche salsa formula granules - Google Patents
Preparation method of cistanche salsa formula granules Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/64—Orobanchaceae (Broom-rape family)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1682—Processes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
Abstract
The invention provides a preparation method of cistanche salsa formula granules, which comprises the steps of obtaining cistanche salsa decoction pieces, extracting, concentrating, drying and granulating to obtain cistanche salsa formula granules; the drying process comprises the following steps: adding auxiliary materials accounting for 1-25% of the weight of the decoction pieces into the clear paste with the relative density of 1.15-1.40, uniformly mixing, then carrying out reduced pressure belt drying, and crushing into fine powder after drying; the parameters of the reduced pressure belt type drying are as follows: feeding speed: 50-1000 ml/min, heating zone temperature: 50-120 ℃; cooling section temperature: 5 to 40 ℃. The product quality of the cistanche salsa formula granules prepared by the invention is excellent, and the preparation method of the invention has the advantages of high production efficiency and high powder yield.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine preparation, and in particular relates to a preparation method of cistanche deserticola formula granules.
Background
Cistanchis Herba Herba is dry succulent stem with scaly leaf of Cistanchis Herba Y.C.Ma or Cistanchis Herba C.tubulosa (Schrenk) light of Orobanchaceae, and is mainly produced in inner Mongolia, Gansu, Xinjiang, Qinghai, etc. It has effects of invigorating kidney, replenishing vital essence, loosening bowel to relieve constipation, and can be used for treating kidney yang deficiency, essence and blood deficiency, sexual impotence, infertility, soreness of waist and knees, weakness of tendons and bones, constipation due to intestinal dryness, etc. The cistanche deserticola essence is named as desert ginseng, and the main chemical components of the desert ginseng essence are phenylethanoid glycosides, iridoid glycosides, lignanoid glycosides, monosaccharides, disaccharides, polysaccharides, amino acids, polypeptides, proteins, triterpenes, sterols, polyols and the like; wherein echinacoside and verbascoside have effects of invigorating kidney, tonifying yang, resisting aging, and enhancing immunity. The herba cistanches processed with wine can avoid the side effect of diarrhea caused by intestine and enhance the functions of warming kidney and supporting yang.
The traditional Chinese medicine formula particle is prepared by carrying out water extraction, concentration, drying and granulation on single traditional Chinese medicine decoction pieces under the guidance of the traditional Chinese medicine theory, and is taken by a patient after being prepared according to the traditional Chinese medicine clinical formula. The quality level of the Chinese medicinal granule is evaluated by the consistency of three indexes of paste yield, fingerprint spectrum or characteristic spectrum, and transfer rate (or content) of main active ingredients with standard decoction (prepared by conventional method). The traditional Chinese medicine decoction inherits the characteristics of the traditional decoction, and overcomes the defects of large dosage, incapability of long-time storage and the like of the decoction; has the characteristics of small dosage, obvious drug effect, easy carrying and the like. However, the industrially produced formula particles and standard soup decoction have great difference, and different production units have different production equipment and production processes, so that the product quality is inconsistent, the drug effect is different, and different varieties have different change trends or rules in the production process due to different physical and chemical properties of the contained components. Therefore, it is important to use different equipments and process controls in the production process to achieve the same index components and efficacy with the standard decoction.
The cistanche salsa is a common clinical traditional Chinese medicine, and related reports of a preparation process of formula granules of the cistanche salsa are not seen at present. Traditional Chinese medicine formula granules are generally prepared by adopting a spray drying mode. Compared with spray drying, the belt type drying has high requirement on the density of the liquid medicine, the time cost consumption of the concentration link is higher, the liquid medicine is required to be paved on a drying belt by the belt type drying, the dried material is crushed and collected after the drying, and the operation is more complicated. However, due to the influence of the properties of cistanche salsa, the total sugar content is high, and under the condition of ensuring the contents of echinacoside and verbascoside, in order to realize industrial rapid production and avoid the problems of large viscosity, easy moisture absorption and difficult preparation of dry powder, when the formula particles are prepared by the conventional process, the spray drying mode is usually adopted by adding auxiliary materials into concentrated solution. However, even if the conventional spray drying method by adding auxiliary materials is adopted, the problems of low powder yield and unsatisfactory effective component transfer rate still exist.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problem that the cistanche salsa cannot achieve ideal effects on production efficiency, powder yield and product quality simultaneously when the formula particles are prepared by adopting the conventional process; thereby providing a preparation method of the cistanche salsa formula granules with high production efficiency, high powder yield and excellent product quality.
A method for preparing herba cistanches formula granules comprises the following steps: obtaining herba cistanches decoction pieces, extracting, concentrating, drying, and granulating to obtain herba cistanches formula granules;
the drying process comprises the following steps: adding auxiliary materials accounting for 1-25% of the weight of the decoction pieces into the clear paste with the relative density of 1.15-1.40, then carrying out reduced pressure belt drying, and crushing into fine powder after drying;
the parameters of the reduced pressure belt type drying are as follows:
feeding speed: 50-1000 ml/min, heating zone temperature: 50-120 ℃; cooling section temperature: 5 to 40 ℃.
Preferably, in the heating zone, the temperature in one zone: 50-120 ℃, temperature of the second zone: 50-120 ℃, and three-section temperature: 50-120 ℃; the four sections are cooling sections, the four section temperature: 5-40 ℃; vacuum degree: -0.10 to-0.07 Mpa, cloth angle: 30-90 degrees.
Heating to 50-120 ℃ before carrying out reduced pressure belt drying;
the excipients include, but are not limited to, dextrin or maltodextrin.
The process parameters of the extraction step are as follows: extracting the cistanche deserticola decoction pieces by using water with the weight being 8-20 times that of the cistanche deserticola decoction pieces, wherein the extraction time is 1-3 times and 0.5-3 hours.
The using amount of the water is 10-15 times, the extraction times are 2 times, and the extraction time is 1-2 hours.
The concentration mode is decompression concentration, the concentration temperature is below 70 ℃, and the vacuum degree is-0.10 to-0.07 Mpa.
During concentration, the extracting solution obtained in the extracting step is subjected to reduced pressure concentration in heating equipment, and the heating temperature is 30-80 ℃; the heating time is 0-24 h, preferably 0-12 h. The heating equipment includes but is not limited to water bath, oil bath, steam, electric heating and other equipment; preferably, the extract obtained in the extraction step is concentrated in a water bath device; the water bath temperature of the water bath equipment is 30-80 ℃, and the water bath time is 0-24 hours, preferably 0-12 hours.
The granulation mode is dry granulation.
During dry granulation, 0-15% of auxiliary materials of cistanche deserticola decoction pieces are added and mixed, and the particle size of the prepared cistanche deserticola formula particles is 10-80 meshes.
The excipients include, but are not limited to, dextrin or maltodextrin; in the granulating process, the time for mixing after adding the auxiliary materials is 10-60 min.
The dry granulation has a compression roller gap of 0.6-2.5mm, a compression roller rotation speed of 8-50 rpm and a pressure of 80-120 bar.
The technical scheme of the invention has the following advantages:
1. the invention provides a preparation method of cistanche salsa formula granules, wherein a drying mode in a drying step is mainly optimized, the drying mode is selected to be decompression belt type drying, and the drying process is as follows: adding auxiliary materials accounting for 1-25% of the weight of the decoction pieces into the clear paste with the relative density of 1.15-1.40, then carrying out reduced pressure belt drying, and crushing into fine powder after drying; the parameters of the reduced pressure belt type drying are as follows: feeding speed: 50-1000 ml/min, heating zone temperature: 50-120 ℃; cooling section temperature: 5 to 40 ℃. According to the invention, through the optimization and limitation of the drying mode and the drying parameter conditions, the influence of the contents of the index components including echinacoside and verbascoside can be minimized, the material basis is basically not changed, and the product quality equivalent to that of a freeze drying mode is obtained; and can also effectively obtain a powder collection rate obviously higher than that of a spray drying mode; in addition, through the optimization of the parameter conditions, the production efficiency which is higher than that of all drying modes can be obtained, and the method is more suitable for large-scale industrial production.
2. The invention further optimizes the process parameters of the extraction and concentration steps, and the optimization of the process parameters can improve the paste yield, reduce the consumption of consumables and the preparation time in the extraction and concentration processes and effectively save the preparation cost under the condition of ensuring that the content of the extracted effective components is not changed.
Detailed Description
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
A preparation method of herba cistanches formula granules comprises the following specific steps:
extraction: taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank.
Concentration: concentrating under reduced pressure at 70 deg.C under vacuum degree of-0.08 Mpa to obtain fluid extract (60 deg.C) with relative density of 1.20 + -0.05.
And (3) drying: adding dextrin into the clear paste, wherein the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials is 100:5, uniformly mixing, stirring and heating to 85 ℃, drying in a pressure-reducing belt type manner, wherein the feeding speed is as follows: 80ml/min, zone temperature: 60 ℃, second zone temperature: 60 ℃, three-zone temperature: 60 ℃, four zone temperature: at 30 deg.C, vacuum degree of-0.099 Mpa, and cloth angle of 50 deg.C, and making into dry extract powder. Calculating the powder collecting rate to obtain the powder collecting rate of 81.0 percent.
And (3) granulating: adding 24.48Kg of dextrin, and mixing uniformly; the dry granulation parameters were as follows: the total mixing time was 30 minutes, the nip was 0.6mm, the speed of the rollers was 30rpm, and the pressure was 90 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Example 2
A preparation method of herba cistanches formula granules comprises the following specific steps:
extraction: taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank.
Concentration: concentrating under reduced pressure at 70 deg.C under vacuum degree of-0.07 Mpa to obtain fluid extract (60 deg.C) with relative density of 1.20 + -0.05.
And (3) drying: adding dextrin into the clear paste, wherein the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials is 100:5, uniformly mixing, stirring and heating to 80 ℃, drying in a pressure-reducing belt type manner, and feeding speed: 60ml/min, zone temperature: 80 ℃, second zone temperature: 80 ℃, three-zone temperature: 80 ℃, four zone temperature: at 20 deg.C, vacuum degree of-0.099 Mpa, and cloth angle of 60 deg.C, and making into dry extract powder. Calculating the powder collecting rate to obtain the powder collecting rate of 84.0 percent.
And (3) granulating: adding 22.44Kg of dextrin and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 1mm, a roller speed of 30rpm and a pressure of 80 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Example 3
A preparation method of herba cistanches formula granules comprises the following specific steps:
extraction: taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank.
Concentration: concentrating under reduced pressure at 70 deg.C under vacuum degree of-0.09 Mpa to obtain fluid extract (60 deg.C) with relative density of 1.20 + -0.05.
And (3) drying: adding dextrin into the clear paste, wherein the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials is 100: 10, uniformly mixing, stirring and heating to 90 ℃, drying in a pressure-reducing belt type manner, wherein the feeding speed is as follows: 90ml/min, zone temperature: 90 ℃, second zone temperature: 90 ℃, three zone temperature: 90 ℃, four zone temperature: making into dry extract powder at 10 deg.C, vacuum degree of-0.099 Mpa, and cloth angle of 30 deg.C. And calculating the powder yield to obtain the powder yield of 90.5%.
And (3) granulating: adding 18.12Kg of dextrin and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the dextrin is added in the step to ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Example 4
The difference between the embodiment and the embodiment 3 is that the drying step is different, specifically, dextrin is added into the clear paste, and the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials is 100: 10, uniformly mixing, stirring and heating to 120 ℃, drying in a pressure-reducing belt type manner, wherein the feeding speed is as follows: 1000ml/min, zone temperature: 120 ℃, second zone temperature: 120 ℃, three-zone temperature: 120 ℃, four zone temperature: making into dry extract powder at 40 deg.C, vacuum degree of-0.08 Mpa, and cloth angle of 90 deg.C. And calculating the powder yield to obtain the powder yield of 87.4%.
Example 5
The difference between the embodiment and the embodiment 3 is that the drying step is different, specifically, dextrin is added into the clear paste, and the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials is 100: 10, uniformly mixing, stirring and heating to 100 ℃, drying in a pressure-reducing belt type manner, wherein the feeding speed is as follows: 500ml/min, zone temperature: 100 ℃, two-zone temperature: 100 ℃, three-zone temperature: 100 ℃, four zone temperature: making into dry extract powder at 5 deg.C, vacuum degree of-0.07 Mpa, and cloth angle of 70 deg.C. And calculating the powder yield to obtain the powder yield of 88.2%.
Comparative example 1
A preparation method of herba cistanches formula granules comprises the following specific steps:
taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank. Concentrating under reduced pressure at vacuum degree of-0.07-0.09 Mpa to obtain fluid extract with relative density of 1.10 + -0.05 (60 deg.C), adding Cistanchis herba decoction pieces and adjuvants at a weight ratio of 100:5, uniformly mixing the dextrin or the maltodextrin, performing spray drying, and collecting dry extract powder. Due to the fact that the weight ratio of the cistanche deserticola decoction pieces to the auxiliary materials added in the spray drying is 100:5, the drying purpose cannot be achieved due to serious tower adhesion, and powder collection is 0.
Comparative example 2
A preparation method of herba cistanches formula granules comprises the following specific steps:
taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank. Concentrating under reduced pressure at vacuum degree of-0.07-0.09 Mpa to obtain fluid extract with relative density of 1.10 + -0.05 (60 deg.C), adding Cistanchis herba decoction pieces and adjuvants at a weight ratio of 100: 10, uniformly mixing the dextrin or the maltodextrin, performing spray drying, collecting dry extract powder, and detecting. And calculating the powder yield to obtain the powder yield of 20.5%.
And (3) granulating: adding 64.44Kg of dextrin, and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Comparative example 3
A preparation method of herba cistanches formula granules comprises the following specific steps:
taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank. Concentrating under reduced pressure at vacuum degree of-0.07-0.09 Mpa to obtain fluid extract with relative density of 1.10 + -0.05 (60 deg.C), adding Cistanchis herba decoction pieces and adjuvants at a weight ratio of 100: 20, uniformly mixing the dextrin or the maltodextrin, performing spray drying, collecting dry extract powder, and detecting. And calculating the powder yield to obtain the powder yield of 25.1%.
And (3) granulating: adding 61.44Kg of dextrin and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Comparative example 4
A preparation method of herba cistanches formula granules comprises the following specific steps:
taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank. Concentrating under reduced pressure of-0.07 to-0.09 Mpa to obtain fluid extract with relative density of 1.10 + -0.05 (60 deg.C), collecting fluid extract, microwave drying, collecting dry extract powder, and detecting. And calculating the powder yield to obtain the powder yield of 87.5%.
And (3) granulating: adding 20.16Kg of dextrin and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Comparative example 5
A preparation method of herba cistanches formula granules comprises the following specific steps:
taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank. Concentrating under reduced pressure of-0.07 to-0.09 Mpa to obtain fluid extract with relative density of 1.10 + -0.05 (60 deg.C), collecting fluid extract, freeze drying, collecting dry extract powder, and detecting.
And (3) granulating: adding 17.88Kg of dextrin and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Comparative example 6
A preparation method of herba cistanches formula granules comprises the following specific steps:
extraction: taking 120kg of cistanche deserticola decoction pieces, putting into an extraction tank, adding drinking water with the amount of 12L/kg of the decoction pieces, heating to boil and extracting for 1.5h, and filtering; adding drinking water of 10L/kg, boiling for 1.5 hr, filtering, mixing the two extractive solutions, and storing in a storage tank.
Concentration: concentrating under reduced pressure at 70 deg.C under vacuum degree of-0.08 Mpa to obtain fluid extract (60 deg.C) with relative density of 1.10 + -0.05.
And (3) drying: stirring and heating the clear paste to 60 ℃, drying the clear paste by a pressure reduction belt, and feeding speed: 60ml/min, zone temperature: 40 ℃, second zone temperature: 40 ℃, three-zone temperature: 40 ℃, four zone temperature: at 5 deg.C, vacuum degree of-0.099 kpa, cloth angle of 20 °, and making into dry extract powder. And calculating the powder yield to obtain the powder yield of 71.2%.
And (3) granulating: adding 30.96Kg of dextrin, and mixing uniformly; dry granulation, total mixing: mixing was carried out for 30 minutes at a nip of 2.5mm, a roller speed of 30rpm and a pressure of 100 bar. Sieving to prepare 16-40 mesh granules, and subpackaging to obtain finished product of the cistanche deserticola formula granules, wherein the addition amount of the dextrin in the step can ensure that each gram of the cistanche deserticola formula granules is equivalent to 1.5 grams of crude drugs.
Test examples
1. Based on the data obtained in the examples and comparative examples, the cream yield (%) and the powder yield (%) were obtained, and as shown in table 1, the following were specified:
the percentage (%) of extract obtained is (weight of dry extract powder-weight of adjuvant)/amount of decoction pieces 100%
The powder collection rate (%) — actual cream yield/standard cream decoction rate × 100%.
Wherein the standard decoction preparation process comprises the following steps: taking 100g of herba cistanches decoction pieces, placing in a casserole, soaking for 30 minutes, adding water with the amount of 10 times of the decoction pieces for one decoction, boiling with strong fire, decocting with slow fire for 60 minutes, and filtering with 150-mesh filter cloth; adding water with the amount 8 times of that of decoction pieces into the second decoction, boiling the second decoction with strong fire, decocting the second decoction with slow fire for 30 minutes, and filtering the second decoction through 150-mesh filter cloth; mixing the two decoctions, concentrating at low temperature (50 deg.C) under reduced pressure until the ratio of the two decoctions is about 1:1 (relative density is 1.05-1.10), freeze drying, and collecting lyophilized powder.
2. The content of echinacoside and the content of verbascoside are measured according to the high performance liquid chromatography (China pharmacopoeia, 2020 edition general regulation 0512), and the content (%) of echinacoside, the content and the (%) of verbascoside, the powder yield (%) and the content and the transfer rate (%) are obtained by conversion, and the calculated results are shown in table 1. Wherein the content of the first and second substances,
the echinacoside content (%) is 100% of the total amount of echinacoside in the test sample/sample amount of the test sample
Acteoside content (%) -, total acteoside in the test sample/sample of the test sample 100%
Content sum (%) + The% of Echinacoside (%) + The
Content and transfer rate (%). test sample content and actual cream yield/decoction piece content and 100%.
The high performance liquid chromatography is as follows:
chromatographic conditions and system applicability experiments take octadecylsilane chemically bonded silica as a filler (the column length is 100mm, the inner diameter is 2.1mm, and the particle size is 1.7 mu m); acetonitrile is taken as a mobile phase A, 0.1 percent formic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the flow rate was 0.4ml per minute; the column temperature was 35 ℃; the detection wavelength was 330 nm. The theoretical plate number is not less than 5000 calculated according to echinacoside peak.
Preparing reference substance solution by respectively weighing appropriate amount of echinacoside and verbascoside, and adding 10% ethanol to obtain 0.2mg echinacoside solution per 1ml and 0.01mg verbascoside solution per 1 ml.
Preparing a test solution, grinding an appropriate amount of the test solution, weighing about 0.4g of the test solution precisely, placing the test solution in a conical flask with a plug, precisely adding 25ml of 10% ethanol, sealing the plug, weighing, carrying out ultrasonic treatment (power of 250W and frequency of 40kHz) for 10 minutes, cooling, weighing again, supplementing the lost weight with 10% ethanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain the test solution.
The determination method comprises precisely sucking 5 μ l of reference solution and sample solution respectively, injecting into liquid chromatograph, and determining.
TABLE 1
The results of the examples and the comparative examples show that the comprehensive efficiency of the powder collection rate, the content and the production efficiency of the vacuum belt type drying is better than that of other drying modes, and particularly, the drying time is greatly saved on the aspect of the production efficiency.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The preparation method of the cistanche salsa formula granules is characterized by comprising the following steps: obtaining herba cistanches decoction pieces, extracting, concentrating, drying, and granulating to obtain herba cistanches formula granules;
the drying process comprises the following steps: adding auxiliary materials accounting for 1-25% of the weight of the decoction pieces into the clear paste with the relative density of 1.15-1.40, then carrying out reduced pressure belt drying, and crushing into fine powder after drying;
the parameters of the reduced pressure belt type drying are as follows:
feeding speed: 50-1000 ml/min, heating zone temperature: 50-120 ℃; cooling section temperature: 5 to 40 ℃.
2. The method of claim 1, wherein the granules are heated to 50-120 ℃ before drying under reduced pressure;
the excipients include, but are not limited to, dextrin or maltodextrin.
3. The method for preparing cistanche salsa formula particles according to claim 1 or 2, wherein the process parameters of the extraction step are as follows: extracting the cistanche deserticola decoction pieces by using water with the weight being 8-20 times that of the cistanche deserticola decoction pieces, wherein the extraction time is 1-3 times and 0.5-3 hours.
4. The method for preparing the cistanche tubulosa formula particle according to claim 3, wherein the amount of water is 10-15 times, the number of extraction times is 2, and the extraction time is 1-2 h.
5. The method for preparing Cistanchis herba granule according to any one of claims 1-4, wherein the concentration is under reduced pressure, concentration temperature is below 70 deg.C, and vacuum degree is-0.10 to-0.07 Mpa.
6. The method for preparing cistanche salsa formula particles according to any one of claims 1-4, wherein during the concentration, the extract obtained in the extraction step is subjected to reduced pressure concentration in heating equipment, and the heating temperature is 30-80 ℃; the heating time is 0-24 h, preferably 0-12 h.
7. The method for preparing the cistanche salsa formula particle according to any one of claims 1-6, wherein the granulation mode is dry granulation.
8. The method for preparing cistanche tubulosa formula particles according to claim 7, wherein 0-15% of auxiliary materials of cistanche tubulosa decoction pieces are added and mixed during dry granulation, and the particle size of the prepared cistanche tubulosa formula particles is 10-80 meshes.
9. The method of claim 8, wherein the excipients include, but are not limited to, dextrin or maltodextrin; in the granulating process, the time for mixing after adding the auxiliary materials is 10-60 min;
the dry granulation has a compression roller gap of 0.6-2.5mm, a compression roller rotation speed of 8-50 rpm and a pressure of 80-120 bar.
10. A cistanche salsa formula particle, characterized by being prepared by the preparation method of the cistanche salsa formula particle according to any one of claims 1 to 9.
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| CN107744510A (en) * | 2017-10-25 | 2018-03-02 | 广东罗浮山国药股份有限公司 | A kind of preparation method of micro-pill type granule |
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