CN118141767A - Wolfberry fruit formula granules and preparation method thereof - Google Patents
Wolfberry fruit formula granules and preparation method thereof Download PDFInfo
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- CN118141767A CN118141767A CN202410414785.0A CN202410414785A CN118141767A CN 118141767 A CN118141767 A CN 118141767A CN 202410414785 A CN202410414785 A CN 202410414785A CN 118141767 A CN118141767 A CN 118141767A
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- medlar
- granule
- decoction pieces
- maltodextrin
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- 239000008187 granular material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 244000241838 Lycium barbarum Species 0.000 title claims abstract description 14
- 235000015459 Lycium barbarum Nutrition 0.000 title claims abstract description 14
- 235000015468 Lycium chinense Nutrition 0.000 title claims abstract description 13
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 13
- 235000017784 Mespilus germanica Nutrition 0.000 claims abstract description 52
- 244000182216 Mimusops elengi Species 0.000 claims abstract description 52
- 235000000560 Mimusops elengi Nutrition 0.000 claims abstract description 52
- 235000007837 Vangueria infausta Nutrition 0.000 claims abstract description 52
- 238000001035 drying Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000000284 extract Substances 0.000 claims description 68
- 239000000843 powder Substances 0.000 claims description 41
- 239000005913 Maltodextrin Substances 0.000 claims description 22
- 229920002774 Maltodextrin Polymers 0.000 claims description 22
- 229940035034 maltodextrin Drugs 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 14
- 238000007908 dry granulation Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000009472 formulation Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000002671 adjuvant Substances 0.000 claims description 5
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 26
- 239000003814 drug Substances 0.000 abstract description 6
- 239000004480 active ingredient Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 4
- 229940095686 granule product Drugs 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 238000005303 weighing Methods 0.000 description 17
- 238000012546 transfer Methods 0.000 description 12
- 229930091371 Fructose Natural products 0.000 description 10
- 239000005715 Fructose Substances 0.000 description 10
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 10
- 239000003651 drinking water Substances 0.000 description 10
- 235000020188 drinking water Nutrition 0.000 description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 9
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 9
- 229930006000 Sucrose Natural products 0.000 description 9
- 230000000295 complement effect Effects 0.000 description 9
- 238000002791 soaking Methods 0.000 description 9
- 239000005720 sucrose Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 7
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 6
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 6
- 239000004677 Nylon Substances 0.000 description 6
- 229960003237 betaine Drugs 0.000 description 6
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- 239000000047 product Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 229940043376 ammonium acetate Drugs 0.000 description 2
- 235000019257 ammonium acetate Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 239000004743 Polypropylene Substances 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 206010041497 Spermatorrhoea Diseases 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 208000009205 Tinnitus Diseases 0.000 description 1
- 206010047513 Vision blurred Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
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- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
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Classifications
-
- 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
-
- 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)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
- A61K36/815—Lycium (desert-thorn)
-
- 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
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/08—Drugs for disorders of the alimentary tract or the digestive system for nausea, cinetosis or vertigo; Antiemetics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/14—Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
- A61P15/10—Drugs for genital or sexual disorders; Contraceptives for impotence
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A61P27/02—Ophthalmic agents
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- A—HUMAN NECESSITIES
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- A61P27/00—Drugs for disorders of the senses
- A61P27/16—Otologicals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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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 or 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention relates to the pharmaceutical field, in particular to medlar prescription granule and a preparation method thereof, which are characterized in that the medlar prescription granule is extracted by adopting water at 80-90 ℃ for 55-65 minutes, and the effective components in decoction pieces can be fully extracted by only one time of decoction, so that the extraction time is shortened, the quality of liquid medicine is improved, the decoction pieces are not required to be boiled in the extraction process, and the energy consumption can be saved; the water consumption for extraction is reduced by about 15% -25%, and the heat energy consumption in the concentration process is reduced. And the method of drying under reduced pressure at 50-80 ℃ is combined, so that the physical loss and the loss of active ingredients are obviously reduced, and the quality of the wolfberry fruit granule product is ensured.
Description
Technical Field
The invention relates to the field of pharmacy, in particular to medlar prescription granules and a preparation method thereof.
Background
The fructus Lycii is dried mature fruit of Lycium barbarum L. Of Solanaceae, is a common Chinese medicinal material in the year 2020, and has effects of nourishing liver and kidney, replenishing vital essence, and improving eyesight. Clinically, the traditional Chinese medicine composition is mainly used for treating the symptoms of consumptive disease, essence deficiency, soreness of waist and knees, dizziness and tinnitus, impotence and spermatorrhea, internal heat and diabetes, blood deficiency and sallow complexion, blurred vision and the like.
The traditional Chinese medicine formula granule is prepared by extracting and concentrating single traditional Chinese medicine decoction pieces after processing according to the traditional standard, and is used for the clinical formula of the traditional Chinese medicine. It has the advantages of convenient administration, small dosage, controllable quality, easy preservation, and convenient carrying.
At present, a plurality of provinces have issued the quality standard of medlar prescription granules, wherein the standards of twenty or more provinces such as Guangdong province (Yue PFKL 20210197), sichuan province (SCYPBZ (PFKL) -2021018), jiangsu province (JS-YBZ-2021028) are basically consistent. In the standard, water is used as an extraction solvent, the prescription and the preparation amount are 1.2:1, and the total amount of fructose, D-glucose, sucrose and betaine are used as content indexes.
In the prior art, the medlar formula granule preparation process has the defects of large solvent consumption, long extraction time, low paste yield of the formula granule intermediate, low total amount of fructose, D-glucose and sucrose in the prepared formula granule, and difficult product quality meeting the standard.
Disclosure of Invention
Therefore, the invention aims to overcome the defects of large solvent consumption, long extraction time and serious loss of active ingredients in the prior art, thereby providing the medlar prescription granule and the preparation method thereof.
Therefore, the invention provides a preparation method of medlar prescription granules, which comprises the following steps:
S1, step: mixing the medlar decoction pieces with water at 80-90 ℃ to obtain a mixed solution, and decocting and extracting the mixed solution at 80-90 ℃ for 55-65 minutes to obtain an extracting solution;
S2, step: filtering and concentrating the extracting solution obtained in the step S1 to obtain fluid extract;
S3, step: mixing the fluid extract with auxiliary materials, and drying under reduced pressure at 50-80 ℃ to obtain extract powder;
S4, step: adding or not adding adjuvants into the extract powder, dry granulating, and making into fructus Lycii granule.
Further, in the mixing process of the step S1, the medlar decoction pieces are added into water which is 13-20 times of the medlar decoction pieces in mass.
Further, in the step S1, the mixture is decocted and extracted under stirring.
Further, in the step S2, the pore size of a filter screen used for filtering is not less than 200 meshes.
Further, the filtering screen comprises: at least one of a metal wire filter screen, a nylon, terylene or polypropylene filter screen.
Further, the concentrating is reduced pressure concentrating;
Preferably, the temperature of the concentration is 50-80 ℃;
Preferably, the vacuum degree of the concentration is more than or equal to-0.08 Mpa (for example, -0.08Mpa to-0.04 Mpa);
Preferably, the relative density of the extract at 55-65 ℃ is 1.20-1.26 g/ml.
Further, the vacuum degree of the reduced pressure drying is-0.08 Mpa to-0.04 Mpa.
Further, in the dry granulation process, the extrusion rotating speed is 5-10 rpm/min; the feeding rotating speed is 20-30 rpm/min; the extrusion force is 5-6 Mpa; the lateral pressure is 2-3 Mpa.
In the step S3, the auxiliary material is maltodextrin, and the mass of the maltodextrin added before the decompression drying is 20-30% of the mass of the decoction pieces.
Further, in the step S4, the auxiliary material includes one or more of maltodextrin and magnesium stearate.
Further, the mass of maltodextrin added before dry granulation is 0-20% of the mass of the decoction pieces.
The invention also provides medlar prescription granules prepared by any one of the preparation methods.
The technical scheme of the invention has the following advantages:
1. The preparation method of the medlar prescription granule provided by the invention comprises the following steps: s1, step: mixing the medlar decoction pieces with water at 80-90 ℃ to obtain a mixed solution, and decocting and extracting the mixed solution at 80-90 ℃ for 55-65 minutes to obtain an extracting solution; s2, step: filtering and concentrating the extracting solution obtained in the step S1 to obtain fluid extract; s3, step: mixing the fluid extract with auxiliary materials, and drying under reduced pressure at 50-80 ℃ to obtain extract powder; s4, step: adding or not adding adjuvants into the extract powder, dry granulating, and making into fructus Lycii granule. The effective components in the decoction pieces can be fully extracted by adopting water temperature of 80-90 ℃ for leaching extraction for 55-65 minutes only by one time of decoction, so that the extraction time is shortened, the quality of the liquid medicine is improved, the decoction pieces are not required to be boiled in the extraction process, and the energy consumption can be saved; the water consumption for extraction is reduced by about 15% -25%, and the heat energy consumption in the concentration process is reduced. And the method of drying under reduced pressure at 50-80 ℃ is combined, so that the physical loss and the loss of active ingredients are obviously reduced, and the quality of the wolfberry fruit granule product is ensured.
2. The preparation method of the medlar prescription granule provided by the invention adopts reduced pressure concentration, can utilize low-pressure steam as a heat source, has the advantages of quick removal of solvent steam, high heat transfer temperature difference, improved evaporation efficiency and effective prevention or reduction of decomposition of heat-sensitive substances. The contact between the fluid extract and the air can be reduced by adopting a decompression drying mode, so that pollution or oxidative deterioration is avoided; the dried product can form a spongy porous structure which is crisp and is easy to crush; decomposition of heat-sensitive substances can also be effectively prevented or reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a process for preparing the wolfberry fruit granules according to the embodiment of the invention.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge. The term "doubling" as used herein refers to the mass doubling.
Example 1
The embodiment provides a preparation method of medlar prescription granules, the process flow chart is shown in figure 1, and the preparation method comprises the following steps:
S1, taking 15600g of drinking water, heating to 85 ℃, adding 1200g of medlar decoction pieces, stirring and maintaining the temperature at 85 ℃ for decoction for 60 minutes to obtain an extract;
s2, filtering the extracting solution through a 200-mesh filter screen (membrane material: nylon filter cloth), and concentrating the filtrate under reduced pressure at a temperature of 75 ℃ and a vacuum degree of-0.08 Mpa to obtain an extract (or called fluid extract) with a relative density of 1.25g/ml (60 ℃);
S3, adding 300g of maltodextrin into the extract, and drying at a low temperature and under reduced pressure for 24 hours under the conditions of 65 ℃ and a vacuum degree of-0.08 Mpa to obtain extract powder;
S4, because the yield of the extract powder in the step S3 exceeds 1000g in the embodiment, auxiliary materials are not needed to be added, the extract powder dried in the step S3 is directly and uniformly mixed, and 1000g of extract powder is taken for dry granulation to prepare medlar prescription granules.
Example 2
The embodiment provides a preparation method of medlar prescription granules, which comprises the following steps:
S1, taking 19200g of drinking water, heating to 85 ℃, adding 1200g of medlar decoction pieces, stirring and maintaining the temperature at 85 ℃ for decoction for 60 minutes to obtain an extract;
S2, filtering the extracting solution through a 200-mesh filter screen (membrane material: nylon filter cloth), and concentrating the filtrate under reduced pressure at the temperature of 75 ℃ and the vacuum degree of-0.08 Mpa to obtain an extract with the relative density of 1.22g/ml (60 ℃);
S3, adding 300g of maltodextrin into the extract, and drying at a low temperature and under reduced pressure for 24 hours under the conditions of 65 ℃ and a vacuum degree of-0.08 Mpa to obtain extract powder;
s4, weighing, adding maltodextrin to complement 1000g because the yield of the extract powder in the step S3 is less than 1000g, uniformly mixing, and granulating by a dry method to obtain the medlar prescription granule.
Example 3
The embodiment provides a preparation method of medlar prescription granules, which comprises the following steps:
S1, taking 24000g of drinking water, heating to 85 ℃, adding 1200g of medlar decoction pieces, stirring and maintaining the temperature at 85 ℃ for decoction for 60 minutes to obtain an extract;
S2, filtering the extracting solution through a 200-mesh filter screen (membrane material: nylon filter cloth), and concentrating the filtrate under reduced pressure at the temperature of 75 ℃ and the vacuum degree of-0.08 Mpa to obtain an extract with the relative density of 1.23g/ml (60 ℃);
S3, adding 300g of maltodextrin into the extract, and drying at a low temperature and under reduced pressure for 24 hours under the conditions of 65 ℃ and a vacuum degree of-0.08 Mpa to obtain extract powder;
s4, because the mass of the extract powder obtained in the step S3 of the embodiment exceeds 1000g, auxiliary materials are not required to be added, the extract powder dried in the step S3 is directly and uniformly mixed, and 1000g of extract powder is taken and then subjected to dry granulation to obtain the medlar prescription granule.
Example 4
The embodiment provides a preparation method of medlar prescription granules, the process flow chart is shown in figure 1, and the preparation method comprises the following steps:
S1, taking 15600g of drinking water, heating to 85 ℃, adding 1200g of medlar decoction pieces, stirring and maintaining the temperature at 85 ℃ for decoction for 60 minutes to obtain an extract;
S2, filtering the extracting solution through a 200-mesh filter screen (membrane material: nylon filter cloth), and concentrating the filtrate under reduced pressure at the temperature of 75 ℃ and the vacuum degree of-0.08 Mpa to obtain an extract with the relative density of 1.20g/ml (60 ℃);
S3, adding 300g of maltodextrin into the extract, and drying at a low temperature and under reduced pressure for 24 hours under the conditions of 80 ℃ and a vacuum degree of-0.08 Mpa to obtain extract powder;
s4, weighing, adding maltodextrin to complement 1000g because the yield of the extract powder in the step S3 is less than 1000g, uniformly mixing, and granulating by a dry method to obtain the medlar prescription granule.
Example 5
The embodiment provides a preparation method of medlar prescription granules, the process flow chart is shown in figure 1, and the preparation method comprises the following steps:
S1, taking 15600g of drinking water, heating to 85 ℃, adding 1200g of medlar decoction pieces, stirring and maintaining the temperature at 85 ℃ for decoction for 60 minutes to obtain an extract;
S2, filtering the extracting solution through a 200-mesh filter screen (membrane material: nylon filter cloth), and concentrating the filtrate under reduced pressure at the temperature of 75 ℃ and the vacuum degree of-0.08 Mpa to obtain an extract with the relative density of 1.24g/ml (60 ℃);
s3, adding 300g of maltodextrin into the extract, and drying at a low temperature and under reduced pressure for 24 hours under the conditions of a temperature of 50 ℃ and a vacuum degree of-0.08 Mpa to obtain extract powder;
s4, because the yield of the extract powder in the step S3 exceeds 1000g in the embodiment, auxiliary materials are not needed to be added, the extract powder dried in the step S3 is directly and uniformly mixed, 1000g of the extract powder is taken and then is subjected to dry granulation, and the medlar prescription granule is prepared.
Comparative example 1
The comparative example provides a preparation method of medlar prescription granule, which is basically the same as that of the example 1, and the difference is only that the operation of the step S1 and the step S4 is different, and the yield of extract powder of the step S3 is different, and the step S1 of the comparative example is as follows: 15600g of drinking water is taken, heated to 70 ℃, added with 1200g of medlar decoction pieces, stirred and kept at the temperature of 70 ℃ for 60 minutes to obtain an extracting solution. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 2
The comparative example provides a preparation method of medlar prescription granule, which is basically the same as that of the example 1, and the difference is only that the operation of the step S1 and the step S4 is different, and the yield of extract powder of the step S3 is different, and the step S1 of the comparative example is as follows: 15600g of drinking water is taken, 1200g of medlar decoction pieces are added, soaked for 30 minutes, heated to boiling (98-100 ℃), and decocted for 60 minutes at the temperature to obtain extract. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 3
The comparative example provides a preparation method of medlar prescription granule, which is basically the same as that of the example 1, and the difference is only that the operation of the step S1 and the step S4 is different, and the yield of extract powder of the step S3 is different, and the step S1 of the comparative example is as follows: 15600g of drinking water is taken, 1200g of medlar decoction pieces are added, heated to boiling (98-100 ℃), and decocted for 60 minutes at the temperature to obtain an extracting solution. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 4
The comparative example provides a preparation method of medlar prescription granule, which is basically the same as that of the example 1, and the difference is only that the operation of the step S1 and the step S4 is different, and the yield of extract powder of the step S3 is different, and the step S1 of the comparative example is as follows: 15600g of drinking water is taken, 1200g of medlar decoction pieces are put into the kettle, soaked for 30 minutes, heated to boiling (98-100 ℃), kept at the temperature for one time of decoction for 60 minutes, 8400g of drinking water is taken from the residues after one time of decoction, heated to boiling (98-100 ℃), kept at the temperature for two times of decoction for 30 minutes, and the extracts obtained by the two times of decoction are combined. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 5
The comparative example provides a preparation method of medlar granules, which is basically the same as that of the example 1, except that the decoction time in the step S1 is shortened from 60 minutes to 30 minutes. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 6
The comparative example provides a preparation method of wolfberry fruit granules, which is basically the same as that of example 1, except that the low-temperature reduced-pressure drying in the step S3 is replaced by spray drying, and in the spray drying process, the inlet temperature is controlled to be 200 ℃ and the outlet temperature is controlled to be 100 ℃. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Comparative example 7
This comparative example provides a preparation method of a wolfberry fruit granule formulation, which is substantially the same as in example 1, except that the drying temperature of the low-temperature reduced-pressure drying in step S3 is adjusted to 40 ℃.
Comparative example 8
This comparative example provides a preparation method of wolfberry fruit granule formulation, which is basically the same as that of example 1, except that the drying temperature of low-temperature reduced-pressure drying in step S3 is adjusted to 100 ℃.
Comparative example 9
This comparative example provides a preparation method of a wolfberry fruit granule formulation, which is substantially the same as in example 1, except that the drying temperature of the low-temperature reduced-pressure drying in step S3 is adjusted to 120 ℃. In the step S4, after weighing, the yield of the extract powder in the step S3 of the comparative example is less than 1000g, maltodextrin is added to complement 1000g, and after uniform mixing, the medlar prescription granule is prepared by dry granulation.
Experimental example 1
And (3) measuring the extract yield of the wolfberry extract powder obtained in the step S3 of each example and comparative example, the content and the content transfer rate of each index component in the extract powder and the formula particles, and evaluating the standard compliance of the content of each index component in the formula particles.
(1) The method for calculating the paste yield and the content transfer rate comprises the following steps:
paste yield% = weight of extract powder g/decoction piece weight g×100%;
The content transfer rate = (content mg/g of active ingredient in extract powder x weight g/1000 of extract powder)/(content% g/g of active ingredient in decoction pieces x weight g) x 100%.
(2) The content is detected by high performance liquid chromatography, and is specifically as follows:
1) The total amount of fructose, D-glucose and sucrose is determined by high performance liquid chromatography (China Pharmacopeia 2020 edition general rule 0512).
Chromatographic conditions and System applicability test zwitterionic hydrophilic interaction silica gel is used as filler (refer to chromatographic column Poroshell HILIC-Z, column length 100mm, inner diameter 2.1mm, particle size 2.7 μm); acetonitrile is taken as a mobile phase A, 0.01mol/L ammonium acetate solution (pH value is adjusted to 4 by glacial acetic acid) is taken as a mobile phase B, water is taken as a mobile phase C, and gradient elution is carried out according to the specification in the following table; the flow rate is 0.30ml per minute; the column temperature is 30 ℃; detected with an evaporative light scattering detector. The theoretical plate number should be not less than 1000 calculated as fructose peak.
Preparing reference solution, respectively taking fructose reference, D-glucose reference, sucrose reference, and appropriate amount, precisely weighing, placing into a measuring flask, adding 70% methanol for dissolving, and making into mixed solution containing fructose 8mg, D-glucose 7mg, and sucrose 0.5mg per 1 ml.
The preparation of the test solution comprises grinding proper amount of the sample, precisely weighing about 1g, placing into a conical flask with a plug, precisely adding 70% methanol 50ml, weighing, ultrasonic treating (power 250W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking, filtering, and collecting the filtrate.
The measuring method comprises the steps of precisely sucking 0.5 mu l of reference substance solution and 1.0 mu l of sample solution respectively, injecting 1 mu l of sample solution into a liquid chromatograph, measuring, and calculating by using an external standard two-point logarithmic equation to obtain the final product.
2) Betaine is measured by high performance liquid chromatography (China pharmacopoeia 2020 edition general rule 0512).
Chromatographic conditions and System applicability test octadecylsilane chemically bonded silica was used as filler (column length 150mm, inner diameter 2.1mm, particle size 1.6 μm); acetonitrile-0.02 mol/L ammonium acetate solution (pH value is adjusted to 3 by glacial acetic acid) (volume ratio is 86:14) is used as mobile phase; the flow rate is 0.40ml per minute, and the column temperature is 30 ℃; the evaporative light scattering detector detects. The theoretical plate number should be not less than 3000 calculated as betaine peak.
Preparation of control solution betaine control is prepared by weighing appropriate amount of control, adding methanol to obtain solution containing betaine 160 μg per 1 ml.
The preparation of the sample solution comprises taking a proper amount of the sample, grinding, taking about 0.5g, precisely weighing, placing into a conical flask with a plug, precisely adding 50ml of 50% methanol, weighing, performing ultrasonic treatment (power is 250W and frequency is 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
The measuring method comprises precisely sucking 1 μl of reference solution and 2 μl of test solution, respectively, injecting 2 μl of test solution into a liquid chromatograph, measuring, and calculating by external standard two-point logarithmic equation.
The test results of each example, comparative example and reference example are shown in tables 1 and 2.
Table 1 results of detection of extract powder of examples and comparative examples
Table 2 results of testing examples, comparative examples formulation particles
As can be seen from comparison of the results of examples 1,2 and 3, the extraction of different water-added amounts is adopted, the paste yield, the content of index components and the content transfer rate are not obviously different, and the content of index components in the formula particles all meet the standard, so that the water-added amount is within the range of 13-20 times, and the extraction and preparation effects are basically consistent.
As is clear from comparison of the results of examples 1, 4 and 5, the index component content in the formulation particles prepared by drying at 50 ℃, 65 ℃ and 80 ℃ meets the standard, so that the drying temperature can be 50 ℃ to 80 ℃, and especially the index component content at 50 ℃ to 65 ℃ is higher.
As can be seen from the comparison of the results of the example 1 and the comparative example 1, the invention adopts the hot water temperature soaking extraction at 85 ℃ and compared with the hot water temperature soaking extraction at 70 ℃, not only improves the paste yield, but also improves the content and the content transfer rate of the two index components.
As can be seen from the comparison of the results of the example 1, the comparative example 2 and the comparative example 3, the invention adopts 85 ℃ hot water temperature soaking extraction, compared with the conventional cold water soaking re-heating extraction and cold water non-soaking heating extraction, not only shortens the extraction process period, but also improves the extraction rate, the index component fructose, the total content of D-glucose and sucrose and the content transfer rate.
As can be seen from the comparison of the results of the example 1 and the comparative example 4, the method adopts the hot water at 85 ℃ for one-time soaking and extraction, and compared with the conventional cold water soaking and the heating and extraction for two times, the method obviously shortens the extraction process period and reduces the water consumption; meanwhile, due to the reduction of water consumption, the period of the concentration process is shortened, the concentration period is shortened, and the stability of index components can be ensured.
As is clear from comparison of the results of comparative examples 2 and 4, the conventional soaking and boiling decoction methods have the problem of long decoction time in addition to the soaking time, and if the decoction time is shortened, the paste yield may be reduced, and the content of the effective components in the formulation particles may not meet the product standard.
As can be seen from the comparison of the results of the example 1 and the comparative example 5, the invention adopts the hot water at 85 ℃ for 60 minutes of extraction, and compared with the hot water at 85 ℃ for 30 minutes of extraction, not only improves the paste yield, but also improves the content and the content transfer rate of the two index components.
As can be seen from the comparison of the results of example 1 and comparative example 6, the invention adopts low-temperature and reduced-pressure drying, and compared with spray drying, not only ensures higher paste yield, but also ensures that the total content of fructose, D-glucose and sucrose serving as index components and the content transfer rate of the two index components are at higher level.
As is clear from the comparison of the results of examples 1, 4, 5 and 7, the dry extract powder obtained by the invention is dried at 50-80 ℃ and 40 ℃ and meets the requirements of the powder chemical properties, and the contents of the two index components and the total content transfer rate of fructose, D-glucose and sucrose are at higher level.
As can be seen from the comparison of the results of examples 1,4, 5, 8 and 9, the invention adopts drying at 50-80 ℃ and drying at 100 ℃ and 120 ℃ to ensure that the total content and the content transfer rate of fructose, D-glucose and sucrose are at higher level and the betaine content and the content transfer rate are at higher level.
In conclusion, the preparation process of the medlar formula granule is improved, the extraction process and the drying process parameters are adjusted, the extraction process period is shortened, the water consumption for production is reduced, and the index component content in the prepared formula granule accords with the standard of finished products, so that theoretical basis can be provided for popularization to mass production.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. The preparation method of the medlar prescription granule is characterized by comprising the following steps:
S1, step: mixing the medlar decoction pieces with water at 80-90 ℃ to obtain a mixed solution, and decocting and extracting the mixed solution at 80-90 ℃ for 55-65 minutes to obtain an extracting solution;
S2, step: filtering and concentrating the extracting solution obtained in the step S1 to obtain fluid extract;
S3, step: mixing the fluid extract with auxiliary materials, and drying under reduced pressure at 50-80 ℃ to obtain extract powder;
S4, step: adding or not adding adjuvants into the extract powder, dry granulating, and making into fructus Lycii granule.
2. The method for preparing the medlar prescription granule as claimed in claim 1, wherein, in the mixing process of the step S1, medlar decoction pieces are added into water which is 13-20 times of the medlar decoction pieces in mass.
3. The method of claim 1 or 2, wherein in step S1, the wolfberry fruit granules are extracted by decocting with stirring.
4. The method for preparing a granule according to any one of claims 1 to 3, wherein in step S2, the pore size of the filter screen used for the filtration is not less than 200 mesh.
5. The method of preparing a wolfberry fruit granule according to any one of claims 1 to 4, wherein the concentration is reduced pressure concentration;
Preferably, the temperature of the concentration is 50-80 ℃;
Preferably, the vacuum degree of the concentration is more than or equal to-0.08 Mpa;
preferably, the relative density of the fluid extract is 1.20-1.26 g/ml at 55-65 ℃.
6. The method for preparing the medlar formulation granule according to any one of claims 1 to 5, wherein the vacuum degree of the reduced pressure drying is-0.08 Mpa to-0.04 Mpa.
7. The method for preparing a granule according to any one of claims 1 to 6, wherein in step S3, the adjuvant is maltodextrin, and the mass of maltodextrin added before drying under reduced pressure is 20% -30% of the mass of the decoction pieces.
8. The method of claim 1-7, wherein in step S4, the adjuvant comprises one or more of maltodextrin and magnesium stearate.
9. The method according to any one of claims 1 to 8, wherein in step S4, maltodextrin is added to the tablet before dry granulation in an amount of 0-20% of the tablet mass.
10. The wolfberry fruit granules according to any of claims 1 to 9.
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