CN114159394A - Preparation process of gardenia prescription granule - Google Patents

Preparation process of gardenia prescription granule Download PDF

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Publication number
CN114159394A
CN114159394A CN202111312074.5A CN202111312074A CN114159394A CN 114159394 A CN114159394 A CN 114159394A CN 202111312074 A CN202111312074 A CN 202111312074A CN 114159394 A CN114159394 A CN 114159394A
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CN
China
Prior art keywords
gardenia
preparation
prescription
prescription granule
drying
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Pending
Application number
CN202111312074.5A
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Chinese (zh)
Inventor
王光磊
何亮
魏宝林
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Shaanxi Sun Simiao High Tech Pharmaceutical Co ltd
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Shaanxi Sun Simiao High Tech Pharmaceutical Co ltd
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Priority to CN202111312074.5A priority Critical patent/CN114159394A/en
Publication of CN114159394A publication Critical patent/CN114159394A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/74Rubiaceae (Madder family)
    • A61K36/744Gardenia
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682Processes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/16Drugs for disorders of the alimentary tract or the digestive system for liver or gallbladder disorders, e.g. hepatoprotective agents, cholagogues, litholytics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P19/00Drugs for skeletal disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/08Drugs for disorders of the metabolism for glucose homeostasis
    • A61P3/10Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/12Antihypertensives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Abstract

The invention discloses a preparation process of gardenia prescription granule, relating to the technical field of preparation of traditional Chinese medicine prescription granule, comprising extraction, concentration and drying; the method comprises the following steps: step S1: taking gardenia decoction pieces, adding 8 times of drinking water, and heating to 60-80 ℃; step S2: starting a device for connecting feeding materials with an extraction tank, soaking for 60min, decocting for 2h, and filtering decoction liquid with 120 meshes; step S3: adding 6 times of water for the second time, decocting with water for 1.5h, filtering with 120 mesh sieve, and mixing filtrates; step S4: concentrating in a concentrator to obtain extract, and spray drying; step S5: adding auxiliary materials of maltodextrin and beta-cyclodextrin and uniformly mixing; step S6: drying by a spray drying method; step S7: and (4) dry granulating the dried extract powder. The technology of the invention is applied to the preparation of traditional Chinese medicine prescription granules, takes traditional Chinese medicine decoction pieces as raw materials, and is processed into a novel prescription medicine with uniform specification, uniform dosage and uniform quality standard through production processes of extraction, separation, concentration, drying, granulation, packaging and the like.

Description

Preparation process of gardenia prescription granule
Technical Field
The invention relates to the technical field of preparation of traditional Chinese medicine formula granules, in particular to a preparation process of gardenia formula granules.
Background
The gardenia is a fruit of gardenia belonging to the family rubiaceae, belongs to the first batch of medical and edible dual-purpose resources issued by the ministry of health, has the functions of protecting liver, benefiting gallbladder, reducing blood pressure, tranquilizing, stopping bleeding, reducing swelling and the like, and is commonly used for treating diseases such as icteric hepatitis, sprain and contusion, hypertension, diabetes and the like in the traditional Chinese medicine clinical practice;
the existing preparation process of the gardenia prescription granule has poor extraction effect, the transfer rate of the geniposide in the gardenia is between 40 and 50 percent, the content is insufficient, and the product quality is influenced; therefore, a preparation process of the gardenia prescription granule is provided.
Disclosure of Invention
The invention mainly aims to provide a preparation process of gardenia prescription granules, which uses traditional Chinese medicine decoction pieces as raw materials and is processed into novel prescription medicines with uniform specification, uniform dosage and uniform quality standard through production processes of extraction, separation, concentration, drying, granulation, packaging and the like, thereby effectively solving the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation process of the gardenia prescription granule comprises an extraction process, a concentration process and a drying process;
the preparation and extraction process of the gardenia prescription granule comprises the following steps:
step S1: taking gardenia decoction pieces, adding 8 times of drinking water, and heating to 60-80 ℃ when the water temperature is high;
step S2: starting a device for connecting feeding materials with an extraction tank, soaking for 60min, decocting for 2h, and filtering decoction liquid with 120 meshes;
step S3: adding 6 times of water for the second time, decocting with water for 1.5 hr, filtering with 120 mesh sieve, mixing filtrates, and storing in an extractive solution storage tank;
the preparation and concentration process of the gardenia prescription granule comprises the following steps:
step S4: feeding the extracting solution into a concentrator, concentrating the extracting solution to obtain an extract with the relative density of 1.05-1.10 (50-65 ℃), and then performing spray drying;
step S5: adding the weighed auxiliary materials of maltodextrin and beta-cyclodextrin in time when the mixture is hot, starting stirring and mixing uniformly;
the preparation and drying process of the gardenia prescription granule comprises the following steps:
step S6: adding adjuvants, stirring, and spray drying to obtain extract;
step S7: and (4) performing dry granulation on the extract powder after spray drying to obtain the gardenia formula granules.
Preferably, the water temperature is maintained at 60 to 80 ℃ during the soaking in the step S2.
Preferably, the filtrate obtained in step S3 is the filtrate obtained in step S2 and the filtrate obtained in step S3.
Preferably, in the step S4, the concentrator controls the primary effect temperature to be 65-75 ℃ and the primary effect vacuum degree to be-0.06-0.07 Mpa; the temperature of the secondary effect is 50-60 ℃, and the vacuum degree of the secondary effect is-0.07 to-0.08 MPa.
Preferably, in the step S5, 15% of maltodextrin and 10% of beta-cyclodextrin are used.
Preferably, in the step S6, the heating steam pressure is controlled to be 0.4-0.6 Mpa, the air inlet temperature is controlled to be 140-160 ℃, the air exhaust temperature is controlled to be 75-85 ℃, the spraying pressure is controlled to be 10-14 Mpa, and the temperature in the tower is controlled to be 85-95 ℃.
The invention has the following beneficial effects:
compared with the common extraction process, the preparation process of the gardenia prescription granule has the advantages that the transfer rate of the geniposide in the gardenia is 40-50%, the transfer rate of the gardenia can be kept above 70%, the content of the geniposide is kept to the maximum extent, and the quality of the product is ensured to the maximum extent.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
Fig. 1 is a flow chart of an operation preparation method of the gardenia prescription granule preparation process of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1: the preparation process of the gardenia prescription granule comprises an extraction process, a concentration process and a drying process;
the preparation and extraction process of the gardenia prescription granule comprises the following steps:
step S1: taking gardenia decoction pieces, adding 8 times of drinking water, and heating to 60-80 ℃ when the water temperature is high;
step S2: starting a device for connecting feeding materials with an extraction tank, soaking for 60min, keeping the water temperature at 60-80 ℃ during soaking, decocting for 2h, and filtering decoction liquid by 120 meshes;
step S3: adding 6 times of water for the second time, decocting with water for 1.5 hr, filtering with 120 mesh sieve, mixing filtrates, and storing in an extractive solution storage tank;
the preparation and concentration process of the gardenia prescription granule comprises the following steps:
step S4: feeding the extracting solution into a concentrator, concentrating the extracting solution to obtain an extract with the relative density of 1.05-1.10 (50-65 ℃), and then performing spray drying; the concentrator controls the primary effect temperature to be 65-75 ℃ and the primary effect vacuum degree to be-0.06-0.07 Mpa; the double-effect temperature is 50-60 ℃, and the double-effect vacuum degree is-0.07 to-0.08 Mpa;
step S5: adding the weighed auxiliary materials of maltodextrin and beta-cyclodextrin in time when the mixture is hot, starting stirring and mixing uniformly; the proportion of maltodextrin used is 15 percent, and the proportion of beta-cyclodextrin used is 10 percent;
the preparation and drying process of the gardenia prescription granule comprises the following steps:
step S6: adding adjuvants, stirring, and spray drying to obtain extract; controlling the heating steam pressure to be 0.4-0.6 Mpa, controlling the air inlet temperature to be 140-160 ℃, the air exhaust temperature to be 75-85 ℃, the spraying pressure to be 10-14 Mpa and the temperature in the tower to be 85-95 ℃;
step S7: and (4) performing dry granulation on the extract powder after spray drying to obtain the gardenia formula granules.
In the actual operation process, the feeding sequence, the soaking time, the soaking temperature, the extraction frequency, the extraction time and the water consumption are required to be noticed in the extraction link, the concentration temperature, the relative density of the extract and the addition of auxiliary materials are required to be noticed in the concentration link, and the drying temperature is required to be noticed in the drying link;
in the scheme of the invention, because the traditional Chinese medicine formula particles are used in a national novel formula, the quality standard of the gardenia formula particles is disclosed only by the national drug administration in 2021 years, and the preparation process of the modified product at present is different from each pharmaceutical enterprise and is in a confidential stage, the preparation process of the gardenia formula particles applied at this time can not only meet the national standard, but also can reach the average value and is stable and feasible;
in order to obtain a preparation process of the gardenia prescription granule, the scheme of the invention carries out related pharmaceutical research, for example, 18 batches of gardenia medicinal materials which are selected from national main production places are subjected to quality comparison research, 18 batches of standard decoction are prepared according to the management standard of Chinese medicine decoction rooms of medical institutions, the quality comparison research is carried out, after the transfer of the effective components of the gardenia is consistent, a small test of the gardenia prescription granule is carried out, the influence factors are screened according to the time and the temperature of soaking, extracting, concentrating and spray drying, a small test product is obtained, the quality comparison research is carried out on the small test product and the standard decoction, and the test and the industrial batch production are carried out under the condition of no quality difference, so that the stable quality is ensured and the small test and the industrial batch production are in accordance with the national quality standard.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (6)

1. The preparation process of the gardenia prescription granule is characterized by comprising an extraction process, a concentration process and a drying process;
the preparation and extraction process of the gardenia prescription granule comprises the following steps:
step S1: taking gardenia decoction pieces, adding 8 times of drinking water, and heating to 60-80 ℃ when the water temperature is high;
step S2: starting a device for connecting feeding materials with an extraction tank, soaking for 60min, decocting for 2h, and filtering decoction liquid with 120 meshes;
step S3: adding 6 times of water for the second time, decocting with water for 1.5 hr, filtering with 120 mesh sieve, mixing filtrates, and storing in an extractive solution storage tank;
the preparation and concentration process of the gardenia prescription granule comprises the following steps:
step S4: feeding the extracting solution into a concentrator, concentrating the extracting solution to obtain an extract with the relative density of 1.05-1.10 (50-65 ℃), and then performing spray drying;
step S5: adding the weighed auxiliary materials of maltodextrin and beta-cyclodextrin in time when the mixture is hot, starting stirring and mixing uniformly;
the preparation and drying process of the gardenia prescription granule comprises the following steps:
step S6: adding adjuvants, stirring, and spray drying to obtain extract;
step S7: and (4) performing dry granulation on the extract powder after spray drying to obtain the gardenia formula granules.
2. The preparation process of gardenia prescription granule according to claim 1, wherein the water temperature is kept at 60-80 ℃ while soaking in the step S2.
3. The process of claim 1, wherein the step S3 is performed by combining the filtrates of step S2 and step S3.
4. The gardenia prescription granule preparation process of claim 1, characterized in that in the step S4, the concentrator controls the primary effect temperature to be 65-75 ℃, the primary effect vacuum degree to be-0.06-0.07 Mpa; the temperature of the secondary effect is 50-60 ℃, and the vacuum degree of the secondary effect is-0.07 to-0.08 MPa.
5. The process of claim 1, wherein in step S5, maltodextrin is used at a ratio of 15% and beta-cyclodextrin is used at a ratio of 10%.
6. The preparation process of the gardenia prescription granule according to claim 1, wherein in the step S6, the heating steam pressure is controlled to be 0.4-0.6 Mpa, the air inlet temperature is controlled to be 140-160 ℃, the air exhaust temperature is controlled to be 75-85 ℃, the spraying pressure is controlled to be 10-14 Mpa, and the temperature in the tower is controlled to be 85-95 ℃.
CN202111312074.5A 2021-11-08 2021-11-08 Preparation process of gardenia prescription granule Pending CN114159394A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115212244A (en) * 2022-07-28 2022-10-21 黑龙江中医药大学 Honeysuckle formula particle prescription and preparation process thereof

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