CN114949053B - Preparation method of ephedra and apricot kernel cough relieving tablet - Google Patents

Preparation method of ephedra and apricot kernel cough relieving tablet Download PDF

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CN114949053B
CN114949053B CN202210799738.3A CN202210799738A CN114949053B CN 114949053 B CN114949053 B CN 114949053B CN 202210799738 A CN202210799738 A CN 202210799738A CN 114949053 B CN114949053 B CN 114949053B
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extract
ephedra
gypsum
drying
apricot kernel
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CN114949053A (en
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吴晓琴
付明华
胡文军
龙万江
邱玲
何俊辰
李雪梅
邓霞
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Taiji Group Sichuan Mianyang Pharmaceutical Co ltd
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Abstract

The invention discloses a preparation method of a ephedra apricot kernel cough relieving tablet, which belongs to the field of medicines, and comprises the steps of preparing ephedra herb, liquorice and part of gypsum into decoction pieces, extracting active ingredients, mixing part of extractum obtained after extraction with gypsum powder, drying, and finally, using the rest part of extractum for spray drying and granulating; the method of the invention can reduce the production procedures (alcohol granulation) and solve three problems of safety, occupational health hazard and environmental protection faced by manufacturers; but also improves the uniformity of the curative effect of the medicine, furthest promotes the decoction of the effective components of the medicinal materials and furthest improves the curative effect of the product; and the time for drying the extract can be shortened, and the energy consumption of the dried extract can be reduced, so that the production efficiency is obviously improved, and the production cost is reduced.

Description

Preparation method of ephedra and apricot kernel cough relieving tablet
Technical Field
The invention relates to the field of medicines, in particular to a preparation method of a ephedra and apricot kernel cough relieving tablet.
Background
The Ma xing zhi Ke pian has the curative effects of relieving cough, eliminating phlegm and relieving asthma. Can be used for treating acute and chronic bronchitis, and asthma.
The national food and drug administration national drug standard of the current Chinese medical standard of the Ma apricot cough relieving tablet, namely 'current national standard', namely 'wet method + ethanol + tank mixer granulation', is: 600g of ephedra, 400g of bitter apricot kernel, 1200g of gypsum and 300g of honey-fried licorice root, and the preparation method comprises the following steps: taking 60g of gypsum, and crushing the gypsum into fine powder; pulverizing the rest Gypsum Fibrosum, herba Ephedrae and radix Glycyrrhizae Preparata into coarse powder, decocting in water twice for 2 hr each time, filtering, and mixing filtrates; decocting semen Armeniacae amarum in water for 2 hr after deoiling, filtering, mixing the filtrate with the above filtrate, concentrating under reduced pressure to obtain extract with relative density of 1.10-1.15 (70deg.C), concentrating under reduced pressure to obtain dry extract, pulverizing, mixing with Gypsum Fibrosum fine powder and starch, granulating, drying, adding magnesium stearate, tabletting, and sugar coating or film coating to obtain 1000 pieces.
In the existing preparation method of the ephedra and apricot kernel cough relieving tablet, the step of concentrating under reduced pressure to dry paste is a technical gap difficult to surmount for the existing production enterprises and the reduced pressure concentration equipment or the vacuum concentration equipment due to the fact that the extract is strong in viscosity and the like, and the extract is difficult to be directly concentrated to the dry paste in practice;
in addition, in the existing preparation method of the ephedra apricot cough-relieving tablet, gypsum powder is required to be added in a granulating way, and the gypsum powder is heavy and is not easy to disperse uniformly when being mixed and granulated with extract powder and auxiliary materials (or the extract powder, gypsum powder and corn starch are mixed and granulated, and the granule/tablet is bonded because the extract powder has strong viscosity); in addition, gypsum, ephedra and honey-fried licorice root are crushed into coarse powder and then are decocted with water for two times, and for a widely applied multi-functional extraction tank, the crude powder extraction is difficult to extract when the medicinal materials are processed, and the medicinal powder is easy to wrap and agglomerate, so that the defect that the crude powder cannot be fully extracted exists.
Moreover, by adopting the traditional granulating mode, because of variety characteristics (strong viscosity), the extract powder and the corn starch are uniformly mixed and then ethanol is added for granulating so as to reduce the viscosity of the extract powder and the corn starch, the ethanol concentration during production is high, great potential safety hazards and occupational health hazards exist, and the ethanol volatilizes to cause atmospheric pollution. In addition, the traditional wet granulation method has the defects of complicated operation process and high labor intensity.
Disclosure of Invention
The invention aims to provide a preparation method of a ephedra apricot kernel cough relieving tablet so as to solve the problems.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a ephedra and apricot kernel cough relieving tablet comprises the following steps:
(1) Firstly, taking part of gypsum and crushing the gypsum into gypsum powder;
(2) Decocting herba Ephedrae, glycyrrhrizae radix and Gypsum Fibrosum with water twice, filtering, and mixing filtrates;
(3) Deoiling semen Armeniacae amarum, decocting in water, filtering, mixing the filtrate with the filtrate obtained in step (2), and concentrating under reduced pressure to obtain extract;
(4) Uniformly mixing a part of the extract obtained in the step (3) with the gypsum powder obtained in the step (1), drying under reduced pressure to obtain dry extract, and crushing into dry extract powder;
(5) Heating the rest extract in the step (3), and filtering to obtain fluid extract for later use;
(6) Spray granulating with a spray drying granulator:
placing the dry paste powder obtained in the step (4) and corn starch in a spray drying granulator, and boiling and mixing with cold air uniformly;
preheating materials: setting the air inlet temperature to be 60-80 ℃ and the material temperature to be 30-60 ℃, starting a fan and a heater to heat the material;
and (3) spray granulation: when the temperature of the material reaches 20-40 ℃, adjusting a liquid inlet valve, spraying the fluid extract obtained in the step (5) into the fluid extract under the pressure of less than or equal to 0.24Mpa, starting spraying, and starting granulating;
drying and discharging: after the spray granulation is finished, drying the granules, and discharging;
(7) Finishing and mixing: and (3) after discharging, granulating and mixing with auxiliary materials (such as magnesium stearate and the like) to obtain the finished product.
The steps of the method of the invention are the same except that the steps (2), (4), (5) and (6) are different from the traditional method (current national standard).
As a preferable technical scheme: in the step (2), the decoction pieces are: crushing gypsum into blocks, crushing ephedra into short sections of 2-3 cm, and processing licorice slices into honey-fried licorice roots.
As a preferable technical scheme: in the step (4), the mass of the extract is 74-82% of the total mass of the extract. The inventors have proved through a number of experiments that: when the mass of the extract exceeds 82%, the proportion of the granule fine powder prepared by spraying the residual extract is more than or equal to 70%, and the powder falling of the tablet does not meet the coating requirement; when the quality of the extract is lower than 74%, the residual extract is sprayed to prepare particles, so that the number of heads is increased, and the yield is reduced by 3%.
As a preferable technical scheme: in the step (4), the method of drying under reduced pressure is as follows: the materials are put into a baking tray according to the weight of 3-4 kg/tray, the pressure is less than or equal to 0.1Mpa, the vacuum degree is less than or equal to 0.05Mpa, and the drying temperature is less than or equal to 70 ℃.
As a preferable technical scheme: in the step (6), when the materials are preheated, the bag shaking function is opened at the same time.
As a preferable technical scheme: the jitter frequency is 10 jitter times per 30 s.
As a preferable technical scheme: in the step (7), a swing type granulator is adopted for granulation.
The invention adopts a low-temperature vacuum drier to dry the extract after uniformly mixing the extract and the gypsum powder so as to reduce the viscosity of the extract and overcome the defect of heavy gypsum powder.
The improvement points of the invention mainly comprise:
(1) When the effective components of the medicinal materials are extracted, the medicinal materials are not crushed but are processed into decoction pieces meeting the preparation specification, which is more beneficial to decoction;
(2) The gypsum powder and a proper amount of extractum are dried by a low-temperature vacuum dryer, so that the adhesion of particles or the adhesion of tablets caused by the over-strong viscosity of the extractum powder can be reduced; overcomes the defect of heavy gypsum powder and improves the uniformity of the curative effect of the medicine;
(3) Mixing part of the extract with gypsum powder, and drying to obtain dry extract for 20-25 hr; compared with the traditional method that the time for concentrating all the extractum to dry extractum under reduced pressure is 35-43 hours, the method shortens the drying time of the extractum by about 15-18 hours, reduces the loss of active ingredients caused by long-time drying, thereby improving the curative effect, and also reduces the energy consumption, thereby reducing the production cost;
(4) Part of the extractum is used for spray granulation, and has the following advantages:
(a) The production process (alcohol granulation) can be reduced, three problems of safety, occupational health hazard and environmental protection faced by a production enterprise are solved, and a green process is created;
(b) The granulating and drying processes are completed in the same equipment, so that the materials can be directly prepared into granules in one step, the material transfer in the production process is reduced, and the labor intensity is reduced. The whole production process is carried out in a negative pressure closed device, so that dust pollution is avoided;
(c) The extract is used as adhesive, and the unit content of the active ingredients is increased, for example, the content transfer rate of ephedrine hydrochloride to granules in ephedra is increased (the transfer rate of traditional wet granulation is 13-21%, and the transfer rate of spray granulation by adopting the invention is 22-33%), so that the curative effect is improved.
(d) Compared with the traditional wet granulation granule fine powder, the spray granulation granule has the advantages of reduced particle size and more uniform particle size (the traditional wet granulation fine powder accounts for about 65-70 percent, and the spray granulation fine powder adopted by the application accounts for only 32-42 percent), and the fluctuation range of the weight difference is smaller (the weight difference of the traditional wet granulation tablet is +/-5 percent, and the weight difference of the spray granulation tablet adopted by the invention is +/-2.8 percent).
Compared with the prior art, the invention has the advantages that: the method of the invention can reduce the production procedures (alcohol granulation) and solve three problems of safety, occupational health hazard and environmental protection faced by manufacturers; but also improves the uniformity of the curative effect of the medicine, furthest promotes the decoction of the effective components of the medicinal materials and furthest improves the curative effect of the product; and the time for drying the extract can be shortened, and the energy consumption of the dried extract can be reduced, so that the production efficiency is obviously improved, and the production cost is reduced.
Detailed Description
The invention will be further illustrated with reference to examples.
Example 1:
a preparation method of a ephedra and apricot kernel cough relieving tablet comprises the following steps:
raw medicinal materials: 600g of ephedra, 400g of bitter apricot kernel, 1200g of gypsum and 300g of honey-fried licorice root
(1) Firstly, 60g of gypsum is taken and crushed into 100-mesh gypsum powder;
(2) Pretreating ephedra, liquorice and the rest gypsum into decoction pieces meeting the preparation specification (specifically, crushing gypsum into small pieces smaller than or equal to 8cm, crushing ephedra into short pieces with the density of 2-3 cm, processing the prepared liquorice into prepared liquorice pieces), mixing the three, adding water which is 3.57 times of the total of the three, decocting for two times each time for two hours, filtering, and combining the filtrates;
(3) Deoiling semen Armeniacae amarum, decocting in 2.6 times of water for two hours, filtering, mixing the filtrate with the filtrate obtained in step (2), and concentrating under reduced pressure to obtain extract;
(4) Uniformly mixing 82% of the extract in the step (3) with the gypsum powder in the step (1), then drying under reduced pressure (low-temperature vacuum), loading into a baking tray according to 3 kg/tray, wherein the pressure is less than or equal to 0.1Mpa, the vacuum degree is less than or equal to 0.05Mpa, the drying temperature is 70 ℃, obtaining dry paste, and crushing into dry paste powder;
(5) Heating the rest 18% of the extract in the step (3), and filtering to obtain fluid extract for later use;
(6) Spray granulating with a spray drying granulator:
putting 38.19g of the dry paste powder obtained in the step (4) and corn starch into a spray drying granulator, and boiling and mixing with cold air uniformly;
preheating materials: setting an air inlet temperature of 70 ℃, a material temperature of 50 ℃, starting a fan and a heater to heat the material, and simultaneously opening a bag shaking function, wherein the frequency is 10 times per 30 s;
and (3) spray granulation: when the temperature of the material reaches 30 ℃, adjusting a liquid inlet valve, spraying the fluid extract obtained in the step 5) by spraying the fluid extract into the spray gun at the pressure of less than or equal to 0.24Mpa, starting granulation, observing the boiling state of the material, adjusting the liquid inlet valve to prevent the material from being bonded into blocks, and ensuring a good material fluidization state until the end of spray granulation;
drying and discharging: after the spray granulation is finished, drying the granules, and discharging;
(7) Finishing and mixing: and (3) after discharging, granulating by a swing type granulator, and mixing with a proper amount of auxiliary materials such as magnesium stearate and the like.
The statistics of the obtained product parameters are shown in Table 1.
Example 2:
a preparation method of a ephedra and apricot kernel cough relieving tablet comprises the following steps:
raw medicinal materials: 600g of ephedra, 400g of bitter apricot kernel, 1200g of gypsum and 300g of honey-fried licorice root
(1) Firstly, 60g of gypsum is taken and crushed into 100-mesh gypsum powder;
(2) Pretreating ephedra, liquorice and the rest gypsum into decoction pieces meeting the preparation specification (specifically, crushing gypsum into small pieces smaller than or equal to 8cm, crushing ephedra into short pieces with the density of 2-3 cm, processing the prepared liquorice into prepared liquorice pieces), mixing the three, adding water which is 3.57 times of the total of the three, decocting for two times each time for two hours, filtering, and combining the filtrates;
(3) Deoiling semen Armeniacae amarum, decocting in 2.6 times of water for two hours, filtering, mixing the filtrate with the filtrate obtained in step (2), and concentrating under reduced pressure to obtain extract;
(4) Uniformly mixing 78% of the extract in the step (3) with the gypsum powder in the step (1), then drying under reduced pressure (low-temperature vacuum), loading into a baking tray according to 3 kg/tray, wherein the pressure is less than or equal to 0.1Mpa, the vacuum degree is less than or equal to 0.05Mpa, the drying temperature is 65 ℃, obtaining dry paste, and crushing into dry paste powder;
(5) Heating the rest 22% of the extractum in the step (3), and filtering to obtain clear paste for later use;
(6) Spray granulating with a spray drying granulator:
putting 38.19g of the dry paste powder obtained in the step (4) and corn starch into a spray drying granulator, and boiling and mixing with cold air uniformly;
preheating materials: setting the air inlet temperature at 80 ℃, the material temperature at 60 ℃, starting a fan and a heater to heat the material, and simultaneously opening the bag shaking function, wherein the frequency is 10 times per 30 s;
and (3) spray granulation: when the temperature of the material reaches 40 ℃, adjusting a liquid inlet valve, spraying the fluid extract obtained in the step 5) by spraying the fluid extract into the spray gun at the pressure of less than or equal to 0.24Mpa, starting granulation, observing the boiling state of the material, adjusting the liquid inlet valve to prevent the material from being bonded into blocks, and ensuring a good material fluidization state until the end of spray granulation;
drying and discharging: after the spray granulation is finished, drying the granules, and discharging;
(7) Finishing and mixing: and (3) after discharging, granulating by a swing type granulator, and mixing with a proper amount of auxiliary materials such as magnesium stearate and the like.
The statistics of the obtained product parameters are shown in Table 1.
Example 3:
a preparation method of a ephedra and apricot kernel cough relieving tablet comprises the following steps:
raw medicinal materials: 600g of ephedra, 400g of bitter apricot kernel, 1200g of gypsum and 300g of honey-fried licorice root
(1) Firstly, 60g of gypsum is taken and crushed into 100-mesh gypsum powder;
(2) Pretreating ephedra, liquorice and the rest gypsum powder into decoction pieces meeting the preparation specification (specifically, crushing gypsum into small pieces smaller than or equal to 8cm, crushing ephedra into short pieces with the density of 2-3 cm, processing the prepared liquorice into prepared liquorice pieces), mixing the three, adding water which is 3.57 times of the total of the three, decocting for two times each time for two hours, filtering, and merging the filtrates;
(3) Deoiling semen Armeniacae amarum, decocting in 2.6 times of water for two hours, filtering, mixing the filtrate with the filtrate obtained in step (2), and concentrating under reduced pressure to obtain extract;
(4) Uniformly mixing 74% of the extract in the step (3) with the gypsum powder in the step (1), then drying under reduced pressure (low-temperature vacuum), loading into a baking tray according to 3 kg/tray, wherein the pressure is less than or equal to 0.1Mpa, the vacuum degree is less than or equal to 0.05Mpa, the drying temperature is 60 ℃, obtaining dry paste, and crushing into dry paste powder;
(5) Heating the residual 26% of the extract in the step (3), and filtering to obtain clear paste for later use;
(6) Spray granulating with a spray drying granulator:
putting 38.19g of the dry paste powder obtained in the step (4) and corn starch into a spray drying granulator, and boiling and mixing with cold air uniformly;
preheating materials: setting an air inlet temperature of 60 ℃, a material temperature of 30 ℃, starting a fan and a heater to heat the material, and simultaneously opening a bag shaking function, wherein the frequency is 10 times per 30 s;
and (3) spray granulation: when the temperature of the material reaches 20 ℃, adjusting a liquid inlet valve, spraying the fluid extract obtained in the step 5) by spraying the fluid extract into the spray gun at the pressure of less than or equal to 0.24Mpa, starting granulation, observing the boiling state of the material, adjusting the liquid inlet valve to prevent the material from being bonded into blocks, and ensuring a good material fluidization state until the end of spray granulation;
drying and discharging: after the spray granulation is finished, drying the granules, and discharging;
(7) Finishing and mixing: and (3) after discharging, granulating by a swing type granulator, and mixing with a proper amount of auxiliary materials such as magnesium stearate and the like.
The statistics of the obtained product parameters are shown in Table 1.
Comparative example 1
In this comparative example, as compared with example 2, only 71% of the extract and gypsum powder were dried in step (4), and the amount of the extract obtained in the spray granulation was 29%, and the other was the same as in example 2, and the statistics of the obtained product parameters are shown in Table 1.
Comparative example 2
In this comparative example, compared with example 2, only 90% of the extract and gypsum powder were dried in step (4), and the amount of the extract obtained in spray granulation was 10%, and the rest was the same as in example 2, and the statistics of the obtained product parameters are shown in Table 1.
Comparative example 3
In this comparative example, compared with example 2, only step (2) was still crushed according to the current national standard and then extracted, and the rest was the same as example 2, and the statistics of the obtained product parameters are shown in Table 1.
Table 1 comparison table of effects of examples and comparative examples
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.

Claims (5)

1. The preparation method of the ephedra and apricot kernel cough relieving tablet is characterized by comprising the following steps of:
(1) Firstly, taking part of gypsum and crushing the gypsum into gypsum powder;
(2) Decocting herba Ephedrae, glycyrrhrizae radix and Gypsum Fibrosum with water twice, filtering, and mixing filtrates;
(3) Deoiling semen Armeniacae amarum, decocting in water, filtering, mixing the filtrate with the filtrate obtained in step (2), and concentrating under reduced pressure to obtain extract;
(4) Uniformly mixing a part of the extract obtained in the step (3) with the gypsum powder obtained in the step (1), and then drying under reduced pressure to obtain dry extract, and crushing the dry extract into dry extract powder, wherein the mass of the obtained extract is 74-82% of that of the total extract;
(5) Heating the rest extract in the step (3), and filtering to obtain fluid extract for later use;
(6) Spray granulating with a spray drying granulator:
placing the dry paste powder obtained in the step (4) and corn starch in a spray drying granulator, and boiling and mixing with cold air uniformly;
preheating materials: setting the air inlet temperature to be 60-80 ℃ and the material temperature to be 30-60 ℃, starting a fan and a heater to heat the material;
and (3) spray granulation: when the temperature of the material reaches 20-40 ℃, adjusting a liquid inlet valve, spraying the fluid extract obtained in the step 5) under the pressure of less than or equal to 0.24Mpa, starting spraying, and starting granulating;
drying and discharging: after the spray granulation is finished, drying the granules, and discharging;
(7) Finishing and mixing: discharging, granulating, and mixing with adjuvants;
wherein, in the step (2), the decoction pieces are: crushing gypsum into blocks, crushing ephedra into short sections of 2-3 cm, and processing licorice slices into honey-fried licorice roots;
the formula of the ephedra and apricot kernel cough relieving tablet comprises the following components: 600g of ephedra, 400g of bitter apricot kernel, 1200g of gypsum and 300g of honey-fried licorice root, wherein the gypsum obtained in the step (1) is 60g.
2. The method for preparing the ephedra and apricot kernel cough relieving tablet according to claim 1, which is characterized in that: in the step (4), the method of drying under reduced pressure is as follows: the materials are put into a baking tray according to the weight of 3-4 kg/tray, the pressure is less than or equal to 0.1Mpa, the vacuum degree is less than or equal to 0.05Mpa, and the drying temperature is less than or equal to 70 ℃.
3. The method for preparing the ephedra and apricot kernel cough relieving tablet according to claim 1, which is characterized in that: in the step (6), when the materials are preheated, the bag shaking function is opened at the same time.
4. The method for preparing the ephedra and apricot kernel cough relieving tablet according to claim 3, which is characterized in that: the jitter frequency is 10 jitter times per 30 s.
5. The method for preparing the ephedra and apricot kernel cough relieving tablet according to claim 1, which is characterized in that: in the step (7), a swing type granulator is adopted for granulation.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103512998A (en) * 2013-09-10 2014-01-15 张文臣 Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof

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CN104435216A (en) * 2014-11-26 2015-03-25 黑龙江省智诚医药科技有限公司 Ephedra and apricot cough relieving traditional Chinese medicine dispersible tablet and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103512998A (en) * 2013-09-10 2014-01-15 张文臣 Chinese ephedra medicinal material, and content determination method of three alkaloids in preparation thereof

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* Cited by examiner, † Cited by third party
Title
中药颗粒剂制粒工艺现状和展望;胡启飞等;《世界科学技术(中医药现代化)》;第14卷(第6期);2212-2216 *

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