CN111281901A

CN111281901A - Preparation method of liquorice formula granules

Info

Publication number: CN111281901A
Application number: CN202010298721.0A
Authority: CN
Inventors: 刘永
Original assignee: Bozhou Yizhi Health Industry Co Ltd
Current assignee: Bozhou Yizhi Health Industry Co Ltd
Priority date: 2020-04-08
Filing date: 2020-04-08
Publication date: 2020-06-16

Abstract

The invention discloses a preparation method of liquorice formula granules, which comprises the following steps: (1) crushing Glycyrrhrizae radix to obtain coarse powder with particle size of 1-5mm, adding water into the coarse powder at 30-50 deg.C, and soaking under high pressure to obtain suspension; (2) quickly freezing the suspension to below-10 ℃, forming a crushed substance by microwave oscillation after the suspension is frozen into a solid, and quickly thawing to a normal temperature state to obtain a turbid solution; (3) adding sufficient ethanol into the turbid solution, extracting for 3-6 times, mixing filtrates after each extraction, washing the residue after extraction for not less than 3 times, centrifuging at high speed, mixing the centrifugate and the filtrate, and concentrating to obtain extract; (4) drying and granulating the extract to obtain liquorice formula granules; by the method, the extraction rate of the effective components in the liquorice granules is improved, and the drug property of the obtained liquorice granules is further improved.

Description

Preparation method of liquorice formula granules

Technical Field

The invention belongs to the technical field of traditional Chinese medicine formula granules, and particularly relates to a preparation method of a liquorice formula granule.

Background

The traditional Chinese medicine formula particle is prepared by carrying out water extraction, concentration, drying and granulation on single traditional Chinese medicine decoction pieces, and is taken by patients after being prepared according to a traditional Chinese medicine clinical formula. Wherein, the liquorice formula particle is one of the most common clinical Chinese medicine formula particle varieties.

The Glycyrrhrizae radix is dried root and rhizome of Glycyrrhiza uralensis Fisch, Glycyrrhiza inflata Bat or Glycyrrhiza glabra G1 Glycyrrhiza glabra L of Leguminosae. Collected in spring and autumn, removed fibrous root, dried in the sun, and loaded in 2015 edition of Chinese pharmacopoeia, which is used for tonifying spleen and qi, clearing heat and removing toxicity, eliminating phlegm and stopping cough, relieving spasm and pain, and harmonizing the drugs. Can be used for treating weakness of spleen and stomach, asthenia, palpitation, short breath, cough, excessive phlegm, abdominal and limb spasm, pain, carbuncle, swelling, sore, and drug toxicity and strong nature. Is the most common clinical traditional Chinese medicine decoction piece. The main active ingredients of the liquorice are triterpenoid saponin compounds (glycyrrhizic acid) and flavonoid compounds (liquiritin), and the flavonoid compounds have the effects of resisting tumors, oxidation, bacteria and viruses and the like; glycyrrhizic acid has effects of protecting and treating liver, treating nephropathy and heart disease, resisting virus, and resisting bacteria. Therefore, glycyrrhizic acid and liquiritin, which are respectively used as representative components of triterpenoid saponin and flavonoid compounds in liquorice, become a liquorice content detection item in the 2015 edition of Chinese pharmacopoeia.

Disclosure of Invention

The invention aims to provide a preparation method of liquorice formula granules, which comprises the steps of crushing liquorice, pretreating under certain conditions, further extracting the crushed liquorice by adopting the method of the invention, drying and granulating, so that effective components such as liquorice brass, liquorice extract and glycyrrhetinic acid in the liquorice are better extracted, the content of the effective components is improved, and the utilization rate of the liquorice is greatly improved.

In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing a licorice root formula particle comprises the following steps:

(1) crushing Glycyrrhrizae radix to obtain coarse powder with particle size of 1-5mm, adding water into the coarse powder at 30-50 deg.C, and soaking under high pressure to obtain suspension;

(2) quickly freezing the suspension to below-10 ℃, forming a crushed substance by microwave oscillation after the suspension is frozen into a solid, and quickly thawing to a normal temperature state to obtain a turbid solution;

(3) adding sufficient ethanol into the turbid solution, extracting for 3-6 times, mixing filtrates after each extraction, washing the residue after extraction for not less than 3 times, centrifuging at high speed, mixing the centrifugate and the filtrate, and concentrating to obtain extract;

(4) and drying and granulating the extract to obtain the liquorice formula granules.

Preferably, in the step 1, the particle size of the coarse particles is 20-40 meshes, and the specific steps of adding water and soaking under high pressure to swell are as follows: a. directly soaking the crushed coarse particles in water for more than 2 hours; b. sealing the soaked coarse particles, introducing carbon dioxide after sealing, and introducing sufficient carbon dioxide to maintain the pressure of the soaking solution at more than 2 MPa; c. carbon dioxide was continuously introduced to maintain the above pressure.

Preferably, in step 2, the suspension is rapidly frozen under high pressure, and the swelling pressure is gradually released to normal pressure after complete freezing.

Preferably, the specific method for thawing frozen suspension after microwave disruption is as follows: mechanically crushing the frozen suspension after microwave crushing again, and uniformly spreading the crushed frozen suspension on a low-temperature heating flat plate; melting of the frozen suspension is facilitated by low temperature heating.

Preferably, the melting temperature of the low-temperature heating flat plate is 15-20 ℃.

Preferably, in step 3, the leaching comprises primary leaching, secondary leaching and tertiary leaching which are sequentially carried out; primary leaching, secondary leaching and tertiary leaching; the water adding amount of the primary leaching is 10-13 times of the weight of the solid phase, and the decocting time is 1-2 hours; the water adding amount of the secondary leaching is 7-10 times of the weight of the solid phase, and the decocting time is 0.5-1 h; the water adding amount of the three times of leaching is 5-8 times of the weight of the solid phase, and the decocting time is 0.5-1 h.

Preferably, in step 3, leaching is performed once, water is added according to a weight ratio for soaking, ethanol is added while soaking, and ethanol is gradually added in batches, so that the ethanol content is gradually increased according to a set proportion; heating to 45-60 ℃ after the first addition of ethanol, maintaining the temperature unchanged, and shaking and stirring after the second addition of ethanol; secondary leaching, namely adding water for soaking according to the weight ratio, and adding a proper amount of ethanol to ensure that the content of the ethanol in the solution is 40-60% of the highest content of the primary leaching; leaching for three times, stirring at high speed by a machine, and raising the temperature of the solution to 70-80 ℃.

Preferably, during the secondary leaching, the leaching solution is sufficiently vibrated by microwave vibration, and the interface air pressure is reduced during the secondary leaching.

Preferably, in step 4, the drying is performed by reduced pressure drying or spray drying.

Preferably, in step 4, the drying and granulating comprises the following steps: a. adding dextrin into the extract, and mixing by adopting a trough type mixing machine to obtain a mixture; b. and (3) placing the mixture into a swing granulator for granulation and molding, drying at the temperature of 60-70 ℃, and finishing granules to prepare the liquorice formula granules.

The invention has the beneficial effects that: the liquorice is crushed into coarse particles with a certain particle size, water is added for soaking under a certain temperature condition, the liquorice is further centrifuged, and a centrifuged solid phase is taken, so that water can be more fully swelled in the liquorice particles, and the main active ingredient in the liquorice is glycyrrhizic acid which is very easy to dissolve in hot water, so that certain expansion can be generated after water enters the liquorice, and particularly, when the water swells in the liquorice particles, the chemical structures of glycyrrhizic acid, glycyrrhetinic acid and the like in the liquorice can be deformed to a certain extent. On the basis, the liquorice particles are centrifuged to remove water attached to the surfaces of the liquorice so as to obtain liquorice particles with the whole skeleton stretched, and the liquorice particles are leached again according to the method, so that the extraction rate of effective components in the liquorice particles is improved, and the drug property of the obtained liquorice particles is further improved. Meanwhile, other solvents are not further used in the whole method, so that the problem that the post-purification treatment is needed under certain conditions is solved, the production efficiency is improved, and unnecessary production cost is saved.

Detailed Description

The technical solution of the present patent will be described in further detail with reference to the following embodiments.

Example 1

A method for preparing a licorice root formula particle comprises the following steps:

(1) crushing Glycyrrhrizae radix into coarse particles with particle size of 1-5mm, adding water into the coarse particles at 30-50 deg.C, and soaking under high pressure to obtain suspension;

Specifically, in step 1, the particle size of the coarse particles obtained after crushing may not be required, for example, in order to further improve the water-holding capacity of the coarse particles and enable the water swollen in the particles to better improve the overall supporting skeleton, the particle size of the coarse particles is preferably 20-40 mesh. From the viewpoint of further removing water on the surface of the coarse particles and improving the overall skeleton, the obtained coarse particles are soaked and swollen to facilitate the extraction of the later substances.

In this embodiment, the specific steps of soaking and swelling the coarse particles with water under high pressure are as follows: a. directly soaking the crushed coarse particles in water for more than 2 hours; b. sealing the soaked coarse particles, introducing carbon dioxide after sealing, and introducing sufficient carbon dioxide to maintain the pressure of the soaking solution at more than 2 MPa; c. carbon dioxide was continuously introduced to maintain the above pressure.

Specifically, for better soaking and expanding, the granule needs to absorb more moisture as much as possible, the expanding effect is improved by increasing the pressure, and water is pressed into the granule through high pressure, so that the granule can absorb more water, and the expanding effect is improved.

In addition, in the invention, in the water for promoting the expansion of the particles, a certain content of carbon dioxide is pressed in a high-pressure mode, namely, gases such as carbon dioxide are dissolved in the water and then expanded, and a large amount of carbon dioxide gas is pressed into the particles, so that the gas can quickly escape after the particles are crushed and pressure tested at the later stage, and the escape efficiency of effective substances is improved.

According to the above, after a large amount of gas is pressed into the particles, the suspension is rapidly frozen to prevent the dissolved gas from escaping, thereby affecting the later escape effect, and in order to reduce the gas escape as much as possible, the suspension is optionally frozen in a high-pressure environment, i.e. in step 2, the suspension is rapidly frozen under high-pressure conditions, and the expansion pressure is gradually released to normal pressure after complete freezing.

In order to enhance the freezing effect, the freezing effect should be enhanced as quickly as possible, and in the present embodiment, it is preferable to provide a low-temperature environment and completely freeze the suspension by quenching to avoid gas diffusion due to a decrease in solubility in the low-temperature environment.

In this embodiment, the providing of the low temperature environment can be performed in the same manner as the selected gas, for example, if the dissolved gas selected in this embodiment is carbon dioxide, then the providing of the low temperature environment can select fixed or liquid carbon dioxide as the cooling source, which has the advantages that on one hand, the low temperature environment can be formed through the volatilization of the solid or liquid carbon dioxide, and on the other hand, a good gas atmosphere can be formed when the gas volatilizes, so as to reduce the volatilization of the gas. After the suspension is completely frozen to form a solid, the suspension is completely crushed by microwave crushing, so that the crushing grade can be improved, and the crushing effect can be controlled.

In the present embodiment, a specific method for thawing a frozen suspension after microwave disruption is as follows: mechanically crushing the frozen suspension after microwave crushing again, and uniformly spreading the crushed frozen suspension on a low-temperature heating flat plate; melting of the frozen suspension is facilitated by low temperature heating.

In the aforesaid, the dull and stereotyped melting temperature of low temperature intensification is between 15 ~ 20 ℃, through the temperature that control melts, avoids quick intensification to lead to gaseous still just taking place a large amount of effuses before not dissolving, consequently, in this embodiment, through carrying out mechanical crushing once more, can improve kibbling effect, later melts again, and with temperature control in normal atmospheric temperature range, through keeping this temperature range unchangeably make the solid after freezing to melt fast.

After the thawing is completed, the gas can be quickly dissipated due to the normal temperature and pressure, the effective substances in the gas can be carried out in the escape process, and the plant tissues with the strength greatly reduced due to the repeated change of pressure and temperature can be damaged when the gas is quickly escaped, so that the extraction efficiency of the effective substances is improved.

The leaching times can be adjusted according to actual conditions, for example, in the preferred embodiment of the present invention, the leaching in step 2 comprises a primary leaching, a secondary leaching and a tertiary leaching which are sequentially performed.

The leaching conditions are not limited, however, in the preferred embodiment of the invention, in combination with the overall pretreatment conditions for the coarse particles of rhubarb, in order to further improve the leaching efficiency of the effective components, the water addition amount of the primary leaching is 10-13 times of the weight of the solid phase, and the decoction time is 1-2 h; the water adding amount of the secondary leaching is 7-10 times of the weight of the solid phase, and the decocting time is 0.5-1 h; the water adding amount of the three times of leaching is 5-8 times of the weight of the solid phase, and the decocting time is 0.5-1 h.

Specifically, in the leaching in the step 3, the specific operation steps are as follows: leaching for the first time, adding water according to the weight ratio for soaking, adding ethanol while soaking, and gradually adding ethanol according to batches to ensure that the ethanol content is gradually increased according to a set proportion; heating to 45-60 ℃ after the first addition of ethanol, maintaining the temperature unchanged, and shaking and stirring after the second addition of ethanol; secondary leaching, namely adding water for soaking according to the weight ratio, and adding a proper amount of ethanol to ensure that the content of the ethanol in the solution is 40-60% of the highest content of the primary leaching; leaching for three times, stirring at high speed by a machine, and raising the temperature of the solution to 70-80 ℃.

Specifically, in the process of secondary leaching, the leaching liquor is sufficiently vibrated by microwave vibration, and the interface air pressure is reduced during secondary leaching.

In the process, the organic substances are added, so that the rapid diffusion of the internal organic components can be promoted, and the ethanol is adopted for extraction, so that the high-temperature impurity removal at the later stage is facilitated. In the embodiment, the content of the ethanol is controlled to avoid that the ethanol is greatly volatilized due to the temperature in the extraction process on one hand, and the total content of the ethanol is reasonably controlled to avoid that the ethanol with high concentration absorbs other impurities and the ethanol with high concentration poisons the effective components. In order to obtain better concentration effect in the step 3, the concentration in the step 3 adopts reduced pressure concentration or film concentration.

Likewise, in a further preferred embodiment, the drying in step 4 is carried out by drying under reduced pressure or by spray drying.

Of course, in order to improve the stability of the finally obtained licorice, the drying and granulating in step 4 includes the following steps: a. adding dextrin into the extract, and mixing by adopting a trough type mixing machine to obtain a mixture; b. and (3) placing the mixture into a swing granulator for granulation and molding, drying at the temperature of 60-70 ℃, and finishing granules to prepare the liquorice formula granules.

In conclusion, the pretreatment method adopted in the invention can effectively improve the content of the active ingredients of the finally obtained liquorice. On the premise that the used pretreatment methods are completely consistent, the content of effective components such as glycyrrhizic acid, glycyrrhetinic acid and the like in the extract can be further improved by enhancing the extraction time. In the pretreatment method, the adjustment of the halving rate, the temperature, and the like may also affect the extraction rate of the entire effective components to some extent. Meanwhile, the finer the particle size is, the better the extraction of the effective components in the later period is not necessarily improved to some extent, and the condition in the most preferable range can improve the extraction of the effective components better. In the embodiment of the invention, other solvents which need further treatment are not introduced, and compared with the prior art, the effective substances in the medicine are better preserved, and the quality of the liquorice formula granules is greatly improved.

The above is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make several variations and modifications without departing from the concept of the present invention, and these should be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the utility of the patent.

Claims

1. The preparation method of the liquorice formula granules is characterized by comprising the following steps:

2. The method for preparing licorice root dispensing granule according to claim 1, wherein in step 1, the particle size of the coarse particles is 20-40 mesh, and the specific steps of soaking in water under high pressure and swelling are as follows: a. directly soaking the crushed coarse particles in water for more than 2 hours; b. sealing the soaked coarse particles, introducing carbon dioxide after sealing, and introducing sufficient carbon dioxide to maintain the pressure of the soaking solution at more than 2 MPa; c. carbon dioxide was continuously introduced to maintain the above pressure.

3. The method of claim 1, wherein the licorice formulation granule comprises: and 2, rapidly freezing the suspension under a high-pressure condition, and gradually releasing the expansion pressure to normal pressure after the suspension is completely frozen.

4. The method for preparing licorice formulation granule according to claim 3, wherein the frozen suspension after microwave disruption is thawed by a specific method comprising: mechanically crushing the frozen suspension after microwave crushing again, and uniformly spreading the crushed frozen suspension on a low-temperature heating flat plate; melting of the frozen suspension is facilitated by low temperature heating.

5. The method of claim 4, wherein the licorice formulation granule comprises: the melting temperature of the low-temperature heating flat plate is 15-20 ℃.

6. The method of claim 5, wherein the licorice formulation granule comprises: in the step 3, the leaching comprises primary leaching, secondary leaching and tertiary leaching which are sequentially carried out; primary leaching, secondary leaching and tertiary leaching; the water adding amount of the primary leaching is 10-13 times of the weight of the solid phase, and the decocting time is 1-2 hours; the water adding amount of the secondary leaching is 7-10 times of the weight of the solid phase, and the decocting time is 0.5-1 h; the water adding amount of the three times of leaching is 5-8 times of the weight of the solid phase, and the decocting time is 0.5-1 h.

7. The method of claim 6, wherein in step 3, the licorice granule is extracted once, water is added for soaking according to a weight ratio, ethanol is added while soaking, and ethanol is gradually added in batches so that the ethanol content is gradually increased according to a set ratio; heating to 45-60 ℃ after the first addition of ethanol, maintaining the temperature unchanged, and shaking and stirring after the second addition of ethanol; secondary leaching, namely adding water for soaking according to the weight ratio, and adding a proper amount of ethanol to ensure that the content of the ethanol in the solution is 40-60% of the highest content of the primary leaching; leaching for three times, stirring at high speed by a machine, and raising the temperature of the solution to 70-80 ℃.

8. The method of claim 7, wherein the licorice formulation granule comprises: in the secondary leaching process, the leaching liquor is fully vibrated by microwave vibration, and the interfacial air pressure is reduced during the secondary leaching.

9. The method of claim 1, wherein the licorice formulation granule comprises: in the step 4, reduced pressure drying or spray drying is adopted for drying.

10. The method of claim 9, wherein the licorice formulation granule comprises: in step 4, the drying and granulation comprises the following steps: a. adding dextrin into the extract, and mixing by adopting a trough type mixing machine to obtain a mixture; b. and (3) placing the mixture into a swing granulator for granulation and molding, drying at the temperature of 60-70 ℃, and finishing granules to prepare the liquorice formula granules.