CN116492396B - Preparation method of bunge cherry seed formula particles - Google Patents
Preparation method of bunge cherry seed formula particles Download PDFInfo
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- CN116492396B CN116492396B CN202310345709.4A CN202310345709A CN116492396B CN 116492396 B CN116492396 B CN 116492396B CN 202310345709 A CN202310345709 A CN 202310345709A CN 116492396 B CN116492396 B CN 116492396B
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- 241000167854 Bourreria succulenta Species 0.000 title claims abstract description 109
- 235000019693 cherries Nutrition 0.000 title claims abstract description 109
- 241000612118 Samolus valerandi Species 0.000 title claims abstract description 108
- 239000002245 particle Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 17
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 17
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 17
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 17
- 229960004853 betadex Drugs 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004945 emulsification Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000008187 granular material Substances 0.000 claims description 12
- 229920002472 Starch Polymers 0.000 claims description 11
- 235000019698 starch Nutrition 0.000 claims description 11
- 239000008107 starch Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229920001353 Dextrin Polymers 0.000 claims description 6
- 239000004375 Dextrin Substances 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 235000019425 dextrin Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 229920003081 Povidone K 30 Polymers 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000009775 high-speed stirring Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 abstract description 40
- 235000019198 oils Nutrition 0.000 abstract description 27
- 238000001035 drying Methods 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 25
- 238000003756 stirring Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 235000003487 Prunus besseyi Nutrition 0.000 description 13
- 235000005805 Prunus cerasus Nutrition 0.000 description 13
- 235000015521 Prunus fruticosa Nutrition 0.000 description 13
- 240000003462 Prunus pumila Species 0.000 description 13
- 210000000582 semen Anatomy 0.000 description 12
- 238000009472 formulation Methods 0.000 description 8
- 229920002678 cellulose Polymers 0.000 description 7
- 239000001913 cellulose Substances 0.000 description 7
- 238000007873 sieving Methods 0.000 description 6
- 238000005469 granulation Methods 0.000 description 5
- 230000003179 granulation Effects 0.000 description 5
- 239000004519 grease Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 239000010685 fatty oil Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- XUCIJNAGGSZNQT-JHSLDZJXSA-N (R)-amygdalin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O[C@@H](C#N)C=2C=CC=CC=2)O1 XUCIJNAGGSZNQT-JHSLDZJXSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 235000019750 Crude protein Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 229940089837 amygdalin Drugs 0.000 description 1
- YZLOSXFCSIDECK-UHFFFAOYSA-N amygdalin Natural products OCC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC(C#N)c3ccccc3 YZLOSXFCSIDECK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000007908 dry granulation Methods 0.000 description 1
- YGHHWSRCTPQFFC-UHFFFAOYSA-N eucalyptosin A Natural products OC1C(O)C(O)C(CO)OC1OC1C(OC(C#N)C=2C=CC=CC=2)OC(CO)C(O)C1O YGHHWSRCTPQFFC-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/736—Prunus, e.g. plum, cherry, peach, apricot or almond
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
- A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using 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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- 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
- A61P1/10—Laxatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P7/00—Drugs for disorders of the blood or the extracellular fluid
- A61P7/10—Antioedematous agents; Diuretics
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- 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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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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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- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention provides a preparation method of bunge cherry seed formula particles, which belongs to the technical field of traditional Chinese medicine preparations, and the preparation method comprises the steps of dynamically extracting bunge cherry seed medicinal materials, filtering, concentrating the obtained filtrate, adding beta-cyclodextrin for centrifugal emulsification, uniformly mixing with an adhesive, and drying the obtained paste powder aqueous solution to obtain the bunge cherry seed formula particles. The method does not need to separate the bunge cherry seed oil independently, the bunge cherry seed oil is not layered in the extracting solution, and the phenomenon that the oil flowers float on the upper layer of the extracting solution is avoided, so that the problems of bunge cherry seed oil loss and low extraction rate caused by the fact that the oil is adhered to equipment are avoided.
Description
Technical Field
The invention relates to a method for clathrating grease, in particular to a method for preparing bunge cherry seed formula particles.
Background
The semen Pruni contains amygdalin, volatile organic acid, fatty oil, crude protein, cellulose, starch, and oleic acid, wherein the fatty oil content is 58.3-74.2%, cellulose content is 24.94%, and starch content is 24.11%. The semen Pruni contains abundant oil components (i.e. fatty oil, i.e. semen Pruni oil), and has effects of moistening dryness, lubricating intestine, descending qi, and promoting diuresis. At present, the extraction of the bunge cherry seed oil mainly adopts a mode of extracting and separating grease after independent oil extraction or a mode of separating grease after conventional water extraction. Whether the oil is extracted and separated after separate oil extraction or the oil is separated after conventional water extraction, the oil is easy to adhere to equipment, and the extraction efficiency is low. The method is greatly influenced by the flattening degree of pretreatment of medicinal materials, does not independently include grease, and has the problems of large oiliness, poor powder physical properties, difficult granulation, poor solubility, poor product stability, long-term storage of rancid oil taste and the like of finished products.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of bunge cherry seed formula granules.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method comprises the steps of taking bunge cherry seed medicinal materials, dynamically extracting, filtering, concentrating the obtained filtrate, adding beta-cyclodextrin for centrifugal emulsification, uniformly mixing with an adhesive, and carrying out spray drying granulation on the obtained paste powder aqueous solution to obtain the bunge cherry seed formula particles.
Further, the weight ratio of the bunge cherry seed medicinal material to the beta-cyclodextrin is 10-20:0.4-0.7.
Further, the weight ratio of the bunge cherry seed medicinal material to the adhesive is 10-20: 0.06 to 0.1.
Further, the temperature of the dynamic extraction is 95-100 ℃ and the time is 0.5-1 h.
Further, after the concentration, the relative density of the obtained concentrated filtrate at 70 ℃ is 1.1-1.2.
Further, the centrifugal emulsification is shearing, grinding and high-speed stirring by adopting a colloid mill.
Further, the adhesive is at least one of dextrin, povidone K30, polyvinylpyrrolidone (PVP for short) and sodium carboxymethyl starch.
Further, in the dynamic extraction process, water is adopted as a solvent, wherein the weight-volume ratio of the bunge cherry seed medicinal material to the water is 10-20 kg:1L.
Further, the bunge cherry seed medicinal material is bunge cherry seed powder/bunge cherry seed particles with the diameter of 0.1-2.5 mm obtained by coarse crushing bunge cherry seed.
Further, the pore diameter of the filtering sieve is 100-500 meshes; the concentrated solution obtained after concentration is sieved by a sieve of 100-500 meshes before the beta-cyclodextrin is added.
The preparation method of the bunge cherry seed formula particle has the beneficial effects that:
because the bunge cherry seed medicinal material contains a certain amount of cellulose (about 24.94%) and starch (about 24.11%), part of cellulose and starch in the bunge cherry seed can be separated and extracted together with bunge cherry seed oil by selecting specific dynamic extraction process parameters, and the extracted part of cellulose and starch have a certain emulsification effect, so that the extracted bunge cherry seed oil is uniformly dispersed in water, the extracted bunge cherry seed oil is further in a uniform emulsification state (milky white) and the bunge cherry seed oil is ensured not to be separated out along with the progress of extraction and concentration;
according to the invention, a specific amount of beta-cyclodextrin is added into the concentrated solution, beta-cyclodextrin is matched with precipitated starch, so that the inclusion is not required after the semen pruni oil is separated independently, the semen pruni oil obtained by extraction can be successfully included only through centrifugal emulsification, and the inclusion rate is high and can reach more than 98.5%;
the method has the advantages of no need of independently extracting and separating the bunge cherry seed oil, high extraction rate, simple operation, stable product, good dissolubility, easy granulation and the like, and has the advantages of small auxiliary material consumption, simple process operation, no step with large operation difficulty and lower equipment requirement;
according to the method, the bunge cherry seed oil does not need to be separated independently, the bunge cherry seed oil is not layered in the extracting solution, and the phenomenon that oil flowers float on the upper layer of the extracting solution is avoided, so that the problems of bunge cherry seed oil loss and low extraction rate caused by the fact that the bunge cherry seed oil is adhered to equipment are avoided;
according to the method, the coarse crushed bunge cherry seed powder/bunge cherry seed particles are used as bunge cherry seed medicinal materials to be extracted, and the stirring extraction is carried out in a dynamic extraction mode, so that the extracted bunge cherry seed oil can be ensured to be uniformly dispersed in the extracting solution after being emulsified, and the extraction efficiency can be improved;
according to the invention, beta-cyclodextrin is adopted to carry out inclusion on the bunge cherry seed oil dispersed in the concentrated solution in a centrifugal emulsification mode, the problem of dissolution/dispersion of the bunge cherry seed oil is not required to be considered, and the bunge cherry seed formula particles prepared after inclusion have no oiliness and good grease stability, can avoid the generation of rancid oil taste after long-term placement, have good solubility and good powder flowability, can be directly subjected to dry granulation, and have high granulation rate.
Detailed Description
The following description of the technical solution in the embodiments of the present invention is clear and complete. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Example 1 preparation method of semen Pruni formulation granule
The embodiment is a preparation method of bunge cherry seed formula particles, and the specific preparation process comprises the following steps:
s1, taking a proper amount of bunge cherry seeds, and crushing the bunge cherry seeds into bunge cherry seed powder/bunge cherry seed particles with the particle size of 0.1-2.5 mm by a coarse crusher to serve as bunge cherry seed medicinal materials for standby.
S2, adding 10-20 kg of bunge cherry seed medicinal material (namely bunge cherry seed powder/bunge cherry seed particles) and 1L of drinking water into a dynamic extraction tank, stirring and circulating, dynamically extracting at 95-100 ℃ for 0.5-1 h (the dynamic extraction temperature in the embodiment is 100 ℃ for 1 h), centrifugally filtering the obtained extract, sieving the obtained extract by a 100-500-mesh sieve (marked as a first sieving, sieving the obtained extract by a 200-mesh sieve in the embodiment), concentrating until the relative density of the obtained concentrated filtrate is 1.1-1.2 at 70 ℃ (the relative density of the obtained concentrated filtrate is 1.15 in the embodiment), sieving the obtained concentrate by a 100-500-mesh sieve (marked as a second sieving, and sieving the obtained concentrate by a 200-mesh sieve in the embodiment).
S3, adding 0.4-0.7 kg of beta-cyclodextrin (0.5 kg of beta-cyclodextrin is added in the embodiment) into the concentrated solution, stirring and mixing uniformly at room temperature (the stirring speed is 30-50 r/min and the stirring time is 5-10 min, the stirring speed is 30r/min and the stirring time is 5min in the embodiment), and performing centrifugal emulsification through a colloid mill by shearing, grinding and high-speed stirring to obtain a liquid medicine;
wherein the rotation speed of the colloid mill is 1800-3200 r/min, the emulsification fineness is 20-50 mu m, and the rotation speed of the colloid mill in the embodiment is 2930r/min, and the emulsification fineness is 30 mu m.
S4, pumping the medicine liquid into a liquid preparation tank of a spray drying tower, adding 0.06-0.1 kg of dextrin as an adhesive (0.1 kg of dextrin is added in the embodiment), stirring uniformly at room temperature (the stirring speed is 50-100 r/min and the stirring time is 1-3 h, the stirring speed is 50r/min and the stirring time is 3h in the embodiment), and performing spray drying granulation on the obtained paste powder aqueous solution to obtain 2.20kg of bunge cherry seed formula particles (1.60 kg of bunge cherry seed oil is extracted in a folding way), and marking as Y1.
In the present invention, the method for drying the aqueous solution of the paste powder is not particularly limited, and conventional methods for drying the aqueous solution may be selected, including but not limited to vacuum drying, spray drying, freeze drying, and the like, and will not be described herein.
Examples 2-5 preparation of semen Pruni formulation particles
Examples 2 to 5 are the same as example 1, except that the raw materials and the process parameters are different, and the details are shown in table 1:
table 1 list of process parameters in examples 2 to 5
The contents of the other parts of examples 2 to 5 are the same as those of example 1, and will not be described again here.
The binder may be at least one of dextrin, povidone K30, polyvinylpyrrolidone (PVP) and sodium carboxymethyl starch, and is not limited to the above examples, but is not limited to the ratio in the above examples.
Experimental example 1 Experimental determination
Comparative examples 1 to 7 are comparative tests of the preparation process of the bunge cherry seed formulation granule of example 1, and the same batch of bunge cherry seeds as in example 1 was used as raw material, except that:
in step S1 of comparative example 1, the mixture was pulverized into 5-10 mm of semen Pruni powder/semen Pruni particles to obtain 2.11kg of semen Pruni formulation particles (1.51 kg of reduced semen Pruni oil) and marked as DY1, wherein the surface of the extract obtained after dynamic extraction was rinsed with trace oil, which may be due to insufficient pulverizing particle size, insufficient dissolution of cellulose and starch, incomplete emulsification of the extract, and further loss of subsequent semen Pruni oil due to sticking to wall and the like.
In the step S2 of the comparative example 2, conventional water extraction is adopted, water and oil of the extracting solution are obviously layered, the subsequent inclusion operation cannot be directly carried out, and the bunge cherry seed formula particles are not obtained.
The dynamic extraction temperature in step S2 of comparative example 3 was 60℃to give 1.84kg of the dwarf cherry seed formulation granule (1.24 kg of the reduced dwarf cherry seed oil), designated DY3. The trace oil flowers float on the surface of the extracting solution obtained after dynamic extraction, which is probably caused by insufficient dissolution of cellulose and starch due to insufficient extraction temperature, and the extracting solution is not completely emulsified, so that the subsequent bunge cherry seed oil is lost due to the problems of wall sticking and the like. And it can also be seen that the total amount of the prepared bunge cherry seed formula particles is obviously reduced, so that the extraction rate of bunge cherry seed oil is obviously reduced, and the phenomenon that bunge cherry seed oil is not completely extracted into the extracting solution possibly caused by the reduction of dynamic extraction temperature is caused.
In step S2 of comparative example 4, the concentrated filtrate obtained was concentrated to a relative density of 1.3 at 70℃to give 2.14kg of a dwarf cherry seed formulation granule (1.54 kg of reduced dwarf cherry seed oil) labeled DY4.
In step S3 of comparative example 5, the amount of beta-cyclodextrin added was 0.2kg, yielding 1.89kg of a dwarf cherry seed formula granule (1.49 kg of reduced dwarf cherry seed oil), labeled DY5, and the surface of the obtained dwarf cherry seed formula granule DY5 was sticky and oily. It can be seen that the prepared bunge cherry seed formula particles DY5 have oiliness, probably due to the fact that the amount of beta-cyclodextrin is too small, bunge cherry seed oil is not completely included; meanwhile, the total amount of the prepared bunge cherry seed formula particles is reduced, so that the bunge cherry seed oil possibly has wall sticking in the drying process, and the bunge cherry seed oil is lost.
In step S3 of comparative example 6, conventional stirring was performed at a stirring speed of 2930r/min instead of a colloid mill to obtain 2.06kg of the dwarf cherry seed formula particles (1.46 kg of the reduced and extracted dwarf cherry seed oil), marked as DY6, and the surfaces of the obtained dwarf cherry seed formula particles DY6 were sticky and oily. It can be seen that the prepared bunge cherry seed formula particles DY6 have oiliness, probably because common stirring can not completely cover bunge cherry seed oil; meanwhile, the total amount of the prepared bunge cherry seed formula particles is reduced, so that the bunge cherry seed oil possibly has wall sticking in the drying process, and the bunge cherry seed oil is lost.
The dextrin was added in the step S4 of comparative example 7 in an amount of 0.02kg to obtain 2.03kg of the dwarf cherry seed formula granule (1.51 kg of the dwarf cherry seed oil was folded and extracted), and the resultant dwarf cherry seed formula granule DY7 had sticky hands and oily surfaces.
Eleven groups of bunge cherry seed formula particles Y1-Y5 and DY1, DY 2-DY 7 are taken for respectively measuring inclusion rate, and the specific method is as follows:
and (3) taking 10g of corresponding bunge cherry seed formula particles (namely, the amount of the bunge cherry seed formula particles weighed during determination of inclusion rate is 10 g), washing with a proper amount of petroleum ether (60-90 ℃) to remove oil attached to the surfaces of the bunge cherry seed formula particles, filtering, placing the obtained solid phase in a rope extractor, adding a proper amount of petroleum ether (60-90 ℃) to extract the bunge cherry seed particles through heating and reflux for 5 hours until the bunge cherry seed oil is completely extracted, collecting an extracting solution, placing the extracting solution in an evaporation dish dried to constant weight, evaporating the extracting solution on a water bath at a low temperature, drying the extracting solution at 100 ℃ for 1 hour, displacing the extracting solution in a dryer, cooling the extracting solution for 30 minutes, precisely weighing, and calculating to obtain the bunge cherry seed oil content in the bunge cherry seed formula particles during determination of the inclusion rate.
The bunge cherry seeds in the corresponding examples or comparative examples are taken as bunge cherry seed medicinal materials, bunge cherry seed oil is extracted by adopting a corresponding dynamic extraction method, solid phase matters are obtained by freeze drying, and the solid phase matters are extracted in a Soxhlet extractor, precisely weighed, and the oil quantity of the dynamically extracted bunge cherry seeds is obtained. It should be noted that, in each example or comparative example, the dynamic extraction process parameter for obtaining the amount of oil of the dynamically extracted bunge cherry seed is the same as that in the corresponding example or comparative example when calculating the inclusion rate, i.e. the dynamic extraction process parameter for obtaining the amount of oil of the dynamically extracted bunge cherry seed is the same as that in example 1 when calculating the inclusion rate, and so on.
Dynamic extraction of the total amount of the bunge cherry seed oil= (bunge cherry seed medicinal material dosage/calculation of dynamic extraction of bunge cherry seed oil quantity Shi Yuli seed medicinal material dosage when preparing bunge cherry seed formula granules) ×dynamic extraction of bunge cherry seed oil quantity;
the total oil content of the bunge cherry seed formula particle= (total amount of bunge cherry seed formula particle/amount of bunge cherry seed formula particle weighed when determining inclusion rate) ×bunge cherry seed oil content in bunge cherry seed formula particle when determining inclusion rate;
inclusion ratio (%) = (total oil content of the bunge cherry seed formula granule/total amount of dynamic extraction bunge cherry seed oil) ×100%;
the specific results are shown in the following table:
table 2 table of the results of determination of inclusion rate of particles of the cherry seed formula
Group of | Inclusion rate (%) |
Y1 | 100.0 |
Y2 | 99.1 |
Y3 | 98.5 |
Y4 | 99.5 |
Y5 | 98.9 |
DY1 | 92.6 |
DY3 | 94.2 |
DY4 | 89.2 |
DY5 | 52.4 |
DY6 | 67.7 |
DY7 | 86.9 |
It can be seen that although the total amount of the bunge cherry seed formulation particles prepared in comparative examples 4, 5, 6 and 7 is not low, the calculated inclusion rate is significantly reduced after the surface oil is removed again. The inclusion rate of the bunge cherry seed formula particles prepared in comparative examples 1 and 3 is relatively good, but the total amount of the bunge cherry seed formula particles prepared correspondingly is low. The total amount of the prepared bunge cherry seed formula particles is relatively high in inclusion rate.
In addition, it was found that the inclusion ratio of β -cyclodextrin to the binder was increased during inclusion, and the oil inclusion rate was improved. However, the proportion of the bunge cherry seed oil in the inclusion compound can be reduced by adopting more beta-cyclodextrin; with more binder, wall sticking occurs when dry formulation particles are prepared. The invention can achieve higher inclusion rate by adopting proper component proportion and process method without increasing the dosage of beta-cyclodextrin and adhesive.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (3)
1. The preparation method is characterized in that the preparation method is that the bunge cherry seed medicinal material is dynamically extracted for 0.5-1 h at the temperature of 95-100 ℃, the obtained filtrate is concentrated, the relative density of the obtained concentrated filtrate is 1.1-1.2 at the temperature of 70 ℃, beta-cyclodextrin is added for centrifugal emulsification, and then the mixture is uniformly mixed with an adhesive, and the obtained paste powder aqueous solution is dried, so that the bunge cherry seed formula particle is obtained;
in the dynamic extraction process, the adopted solvent is water, wherein the weight-volume ratio of the bunge cherry seed medicinal material to the water is 10-20 kg:1L;
the bunge cherry seed medicinal material is bunge cherry seed powder/bunge cherry seed particles which are prepared by coarse crushing bunge cherry seed into 0.1-2.5 mm;
the weight ratio of the bunge cherry seed medicinal material to the beta-cyclodextrin is 10:0.35-0.5;
the weight ratio of the bunge cherry seed medicinal material to the adhesive is 10-20: 0.06-0.1;
the centrifugal emulsification is realized by shearing, grinding and high-speed stirring by a colloid mill.
2. The method of claim 1, wherein the binder is at least one of dextrin, povidone K30, polyvinylpyrrolidone, and sodium carboxymethyl starch.
3. The method for preparing the bunge cherry seed formula granules according to claim 1, wherein the pore diameter of the filtering sieve is 100-500 meshes; the concentrated solution obtained after concentration is sieved by a sieve with 100-500 meshes before the beta-cyclodextrin is added.
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