CN108096455B - Preparation method of radix adenophorae and radix ophiopogonis granules - Google Patents

Abstract

The invention discloses a preparation method of radix glehniae and radix ophiopogonis granules, which comprises the steps of crushing radix glehniae, radix ophiopogonis, polygonatum odoratum, radix trichosanthis, mulberry leaves, white hyacinth beans and liquorice into certain granularity, adding a solvent for soaking for a period of time, then carrying out ultrahigh pressure extraction, finally concentrating an extracting solution into thick paste, adding auxiliary materials for granulation. Compared with the existing extraction method, the method of the invention can improve the content of active ingredients in the extract and reduce impurities; meanwhile, the transfer rate of active ingredients can be improved, so that the extraction is more sufficient, and the radix adenophorae and radix ophiopogonis particles prepared by the method have better pharmacodynamic activity.

Description

Preparation method of radix adenophorae and radix ophiopogonis granules

Technical Field

The invention belongs to the field of pharmacy, and particularly relates to a preparation method of radix adenophorae and radix ophiopogonis granules.

Background

The Chinese medicine for curing cough is made up by using 7 Chinese medicinal materials of adenophora root, polygonatum root, raw licorice, winter mulberry leaf, ophiopogon tuber, raw hyacinth bean and trichosanthes root, in which the adenophora root and ophiopogon root can be used for clearing lung and stomach, polygonatum root and pollen can produce saliva and relieve thirst, and the raw hyacinth bean and raw licorice can be used for supplementing qi and nourishing stomach, and can be matched with mulberry leaf, and can be combined into a prescription with the functions of clearing lung and stomach and moistening dryness.

CN 103432386A discloses a Chinese medicinal preparation for treating cough, which is prepared by extracting seven medicinal materials with water or ethanol on the basis of adenophora stricta and ophiopogon japonicus decoction, refining the extract by a macroporous adsorption resin column, and adding auxiliary materials. The method can enrich effective components in SHASHEN radix Ophiopogonis decoction, and reduce ineffective components, thereby improving curative effect, reducing side effect and dosage, and improving compliance. However, the invention adopts the macroporous resin adsorption process in the extraction process, so that the production period of the product is too long, the cost is too high, a large amount of effective components are lost in the refining and impurity removal process, and the transfer rate is low although the content of the effective components in the extract is high, so that the waste of raw materials is further increased, and the cost is further increased.

With the continuous progress of the extraction technology of traditional Chinese medicines, more and more new methods such as supercritical carbon dioxide extraction, ultrasonic-assisted extraction, microwave extraction, ultrasonic-microwave synergistic extraction, ultrahigh pressure extraction and the like are used for extracting active ingredients of traditional Chinese medicines. However, no report of extracting the adenophora stricta and ophiopogon japonicus decoction by an ultrahigh pressure method is found up to now.

The ultrahigh pressure extraction is also called ultrahigh cold isostatic pressure extraction, which is characterized in that 100-1000MPa ultrahigh hydrostatic pressure is applied to a mixed solution of an extraction solvent and Chinese medicinal materials, and the mixed solution is kept for a period of time under preset pressure, so that the pressure inside and outside plant cells is quickly released within a very short time after the pressure inside and outside the plant cells is balanced. Under the action of reverse pressure, the volume of the medicinal material matrix is exploded and expanded, the osmotic pressure inside and outside the plant cell is suddenly increased, and the structure of the cell membrane is changed, so that the effective components in the cell can rapidly pass through the cell membrane and are transferred to an extraction solvent outside the cell, and the purpose of extracting the effective components of the traditional Chinese medicine is achieved. Compared with other extraction modes, the ultrahigh pressure extraction has the advantages of low temperature, short time, high efficiency and the like.

Disclosure of Invention

The invention aims to provide a preparation method of radix adenophorae and radix ophiopogonis particles, which adopts ultrahigh pressure to extract active ingredients in medicinal materials and has the advantages of high extraction efficiency, less impurities and the like.

The method provided by the invention comprises the following steps:

1) taking 15-30 parts of radix glehniae, 10-20 parts of radix ophiopogonis, 3-15 parts of radix polygonati officinalis, 5-20 parts of trichosanthes root, 15-30 parts of folium mori, 5-20 parts of white hyacinth bean and 5-25 parts of liquorice, crushing the medicinal materials together into powder with the granularity of 20-80 meshes, adding a solvent 5-20 times of the total weight of the medicinal materials, soaking for 0.5-3 hours, filling the medicinal materials and the solvent together into a plastic bag, sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and performing ultrahigh pressure extraction at normal temperature;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding adjuvants into the soft extract, and making into clinically acceptable dosage forms.

The medicinal material is crushed to 20-80 meshes before extraction, because the particle size is too large, the solvent is not easy to permeate the medicinal material to permeate into tissue cells under ultrahigh pressure, and the contact between the active ingredients and the solvent is reduced, so that the extraction efficiency is reduced; on the other hand, if the particle size is too small, the dissolution of the active ingredient increases, and the dissolution of impurity components such as medicinal tissue, starch, and tannin also increases, which in turn leads to a decrease in the content of the active ingredient in the extract.

Before extraction, the medicinal materials are soaked in 5-20 times of solvent for 0.5-3 hours, so that the active ingredients and the solvent can be better dissolved and balanced during ultrahigh pressure extraction, the dissolution of the active ingredients is promoted, the extraction efficiency is improved, and the cost is increased when too much solvent is used.

Preferably, the pressure of the ultrahigh pressure extraction is 200-700 MPa. The higher the pressure is, the faster the solvent infiltration and the transfer speed of the active ingredients are, and the density, the activity and the structure of the medicinal material basic block can be influenced, so that the dissolution speed of the active ingredients is accelerated, and the dissolution amount is increased; however, if the pressure is too high, the elution of the impurity components is also increased, which is disadvantageous in extraction and increases the cost.

Preferably, the decompression time of the ultrahigh pressure extraction is 10-30 s. The pressure of the medicinal material tissue cells is quickly reduced from ultrahigh pressure of hundreds of megapascals to normal pressure, the explosive expansion of fluid and medicinal material matrix volume is generated under the action of reverse pressure, the medicinal material tissues are strongly impacted to cause deformation, and meanwhile, the cell structures are loosened, perforated and cracked, so that the medicinal material components are fully contacted with the solvent and quickly diffused outwards. Therefore, it is theoretically preferable that the pressure release time is shorter, but if the time is too short, a large amount of ineffective components such as tissue cells of the medicinal material are eluted, which is disadvantageous in extraction.

Preferably, the times of the ultrahigh pressure extraction are 1-5 times, the more the times of extraction, the more sufficient the extracted active ingredients, and the more the times of extraction, the more the impurities can be extracted, and the cost can not be reduced.

The ethanol concentration in the invention is volume concentration, for example, 10-50% ethanol means that 10-50ml ethanol is contained in each 100ml ethanol water solution.

The invention has the beneficial effects that:

1) compared with the decocting method, the radix adenophorae and radix ophiopogonis granules prepared by adopting ultrahigh pressure extraction have higher active ingredient content and lower corresponding impurity content, thereby being beneficial to improving the drug effect and reducing the side effect; meanwhile, the transfer rate of active ingredients is improved, so that the extraction of the active ingredients is more sufficient, and the reasonable utilization of medicinal material resources is facilitated, and the production cost is reduced.

2) Although the macroporous resin adsorption process is more beneficial to improving the content of active ingredients, a large amount of active ingredients are lost in the refining and impurity removing process, so that the utilization rate of medicinal materials is reduced, the production period is overlong, and the production cost is higher.

3) Compared with the conventional extraction methods such as hot reflux, decoction and the like, the method is carried out at a lower temperature (room temperature), so that the energy consumption and the damage of active ingredients are reduced, and the result of a pharmacodynamic test shows that the medicine prepared by the method has better cough relieving and phlegm reducing activities compared with the existing radix adenophorae and radix ophiopogonis granules.

Detailed Description

The present invention will be described in detail below with reference to specific examples.

Example 1

Prescription: 30Kg of radix glehniae, 20Kg of radix ophiopogonis, 10Kg of radix polygonati officinalis, 15Kg of radix trichosanthis, 30Kg of folium mori, 15Kg of white hyacinth bean and 15Kg of liquorice

The preparation method comprises the following steps: 1) weighing the seven medicinal materials according to the proportion, crushing the seven medicinal materials together to powder with the granularity of 50 meshes, then adding 20 percent ethanol for soaking for 1.5 hours according to 15 times of the total weight of the medicinal materials, then putting the medicinal materials and the ethanol into a plastic bag for sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and carrying out ultrahigh pressure extraction at normal temperature, wherein the extraction procedure is as follows:

and A, boosting stage: raising the pressure in the extraction vessel to 500 Mpa;

b, pressure maintaining stage: keeping the pressure for 30 min;

c, pressure relief stage: quickly releasing the pressure to normal pressure for 12 s;

d, repeating A-C2 times;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste with the relative density of 1.35;

3) adding 3 parts of sugar powder and 1 part of dextrin into the thick paste according to the weight of the thick paste, uniformly mixing, granulating, drying, and preparing into granules.

Example 2

Prescription: same as the recipe of example 1.

The preparation method comprises the following steps: 1) weighing the seven medicinal materials according to the proportion, crushing the seven medicinal materials into powder with the granularity of 80 meshes, adding water for soaking for 1 hour according to 10 times of the total weight of the medicinal materials, then putting the medicinal materials and the water into a plastic bag for sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and carrying out ultrahigh pressure extraction at normal temperature, wherein the extraction procedure is as follows:

and A, boosting stage: raising the pressure in the extraction vessel to 300 Mpa;

b, pressure maintaining stage: keeping the pressure for 15 min;

c, pressure relief stage: quickly releasing the pressure to normal pressure, wherein the pressure release time is 15 s;

d, repeating A-C3 times;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding sugar powder and dextrin into the soft extract, mixing, granulating, and making into granule.

Example 3

Prescription: same as the recipe of example 1.

The preparation method comprises the following steps: 1) weighing the seven medicinal materials according to the proportion, crushing the seven medicinal materials together to powder with the granularity of 60 meshes, then adding 10 percent ethanol for soaking for 3 hours according to 6 times of the total weight of the medicinal materials, then putting the medicinal materials and the ethanol into a plastic bag for sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and carrying out ultrahigh pressure extraction at normal temperature, wherein the extraction procedure is as follows:

and A, boosting stage: raising the pressure in the extraction vessel to 600 Mpa;

b, pressure maintaining stage: keeping the pressure for 60 min;

c, pressure relief stage: quickly releasing the pressure to normal pressure for 10 s;

d, repeating A-C4 times;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding sugar powder and dextrin into the soft extract, mixing, granulating, and making into granule.

Example 4

Prescription: same as the recipe of example 1.

The preparation method comprises the following steps: 1) weighing the seven medicinal materials according to the proportion, crushing the seven medicinal materials together to powder with the granularity of 30 meshes, then adding 50 percent ethanol for soaking for 0.5 hour according to 20 times of the total weight of the medicinal materials, then putting the medicinal materials and the ethanol into a plastic bag for sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and carrying out ultrahigh pressure extraction at normal temperature, wherein the extraction procedure is as follows:

and A, boosting stage: raising the pressure in the extraction vessel to 200 Mpa;

b, pressure maintaining stage: keeping the pressure for 40 min;

c, pressure relief stage: rapidly releasing the pressure to normal pressure for 20 s;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding sugar powder and dextrin into the soft extract, mixing, granulating, and drying.

Example 5

Prescription: same as the recipe of example 1.

The preparation method comprises the following steps: 1) weighing the seven medicinal materials according to the proportion, crushing the seven medicinal materials together to powder with the granularity of 20 meshes, then adding 30 percent ethanol for soaking for 2 hours according to 12 times of the total weight of the medicinal materials, then putting the medicinal materials and the ethanol into a plastic bag for sealing, putting the plastic bag into an extraction container of an ultrahigh pressure extraction device, and carrying out ultrahigh pressure extraction at normal temperature, wherein the extraction procedure is as follows:

and A, boosting stage: raising the pressure in the extraction vessel to 400 Mpa;

b, pressure maintaining stage: keeping the pressure for 20 min;

c, pressure relief stage: quickly releasing the pressure to normal pressure for 30 s;

d, repeating A-C1 times;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding sugar powder and dextrin into the soft extract, mixing, granulating, and drying.

Test example 1

Taking part of the thick paste obtained in the step 2) in the embodiment 1-5, drying to constant weight, weighing, and converting the total amount of the thick paste obtained in the step 2) into the total amount of the extracted dry paste; detecting the contents of active ingredients, namely ophiopogonin D, chlorogenic acid and glycyrrhizic acid in the dry paste by adopting an HPLC method, and calculating the transfer rate of the active ingredients according to the total amount of the dry paste and the contents of medicinal materials, wherein the calculation formula is as follows:

wherein, the content of ophiopogonin D in the radix ophiopogonis medicinal material is 0.024%, the content of chlorogenic acid in the folium mori medicinal material is 0.80%, and the content of glycyrrhizic acid in the liquorice medicinal material is 0.88%.

Meanwhile, according to the prescription of the embodiment 1, the conventional method of adding water for decoction and extraction is adopted, and the extracting solution is concentrated and dried to be used as a comparative example 1; the extract was extracted by the method of example 2 of CN 103432386A according to the recipe of example 1, and the extract was concentrated and dried to give comparative example 2.

TABLE 1 amount of dry extract and active ingredient content

TABLE 2 transfer rates of active ingredients extracted

From the results, compared with the conventional water decoction extraction, the ultrahigh pressure extraction can greatly improve the content of active ingredients and the transfer rates of ophiopogonin D and glycyrrhizic acid, which indicates that the extraction is more sufficient and the impurities are less; compared with the macroporous resin adsorption process, the invention can greatly improve the transfer rate of the active ingredients, thereby fully utilizing the medicinal material resources and reducing the production cost.

Claims (1)

1. A preparation method of radix adenophorae and radix ophiopogonis granules is characterized by comprising the following steps:

1) taking 15-30 parts of radix glehniae, 10-20 parts of radix ophiopogonis, 3-15 parts of radix polygonati officinalis, 5-20 parts of trichosanthes root, 15-30 parts of folium mori, 5-20 parts of white hyacinth bean and 5-25 parts of liquorice, crushing the medicinal materials together into powder with the granularity of 50 meshes, adding 20% ethanol according to 15 times of the total weight of the medicinal materials, soaking for 1.5 hours, filling the medicinal materials and a solvent together into a plastic bag, sealing, putting into an extraction container of an ultrahigh-pressure extraction device, and performing ultrahigh-pressure extraction at normal temperature;

2) taking out the plastic bag from the extraction container, pouring out the materials, filtering, centrifuging, and concentrating the extracting solution into thick paste;

3) adding adjuvants into the soft extract, granulating, and drying,

the pressure of the ultrahigh pressure extraction is 500Mpa,

the decompression time of the ultrahigh pressure extraction is 12s,

the times of ultrahigh pressure extraction are 3 times.