CN1876018A - A herbal extract, its preparation method and use - Google Patents

Abstract

A plant extract and its preparation method and use belong to the field of medicine. The present invention is the extract solution obtained by the unique water extraction ethanol precipitation method or ethanol extraction water precipitation method or ethanol percolation extraction method of Labiatae plants, and the crude extract obtained after separation by macroporous resin adsorption column chromatography, and then through The polyamide column or/and silica gel column chromatography separates and purifies the extract, and the extract contains 22-90% by weight of the active ingredient of phenylpropanoid glycosides in terms of dry product. It can be made into any kind of oral preparation, which can be used as an analgesic and hemostatic drug. The invention has the advantages of clear medicinal active ingredients, high controllability of product quality, high performance liquid chromatography can be used to determine the content of phenylpropanoid glycosides in the extract, and is suitable for industrial batch production.

Description

A kind of plant extract and its preparation method and application

technical field

The invention belongs to the field of medicine, and in particular relates to an extract which is extracted from a single plant and contains phenylpropanoid glycosides as main active ingredients. The invention also relates to the preparation method and application of the active extract.

Background technique

Unique flavor is the dry whole herb of Lamiophlomis rotata (Benth.) Kudo, the unique flavor of Lamiophlomis rotata (Benth.) Kudo. Can promote blood circulation and stop bleeding, dispel wind and relieve pain. For bruises, traumatic bleeding. It has the function of promoting blood circulation to relieve pain, removing blood stasis and stopping bleeding, and is used for incision pain after various surgical operations. Bleeding, surgical fractures, sprains, rheumatic arthralgia, metrorrhagia, dysmenorrhea, gingival swelling, bleeding, etc. The usual dose is 2-3g of crude drug, see the item under Duyiwei on page 184 of the 2005 edition of Chinese Pharmacopoeia.

The existing preparations include Duyiwei tablets and Duyiwei capsules, both of which belong to traditional Chinese patent medicines. It is directly processed from the whole herb or root of a single plant Duyiwei. It is recorded in the Chinese Pharmacopoeia, and the Chinese patent application number is 02134169.9. A dispersible tablet of unique taste is disclosed, but these three preparations are all made by using the water extract of unique taste, which has the disadvantage of large dosage. Generally, 3 capsules need to be taken orally once, each 300mg, a day Three times, equivalent to 9g crude drug.

Chinese Patent Application No. 200410022734.6 patent discloses that the extract obtained from the unique plant is extracted with water or ethanol, and an extract obtained by separating through macroporous resin is used for pain relief and blood circulation. The main components contained in its extract are total glycosides and total flavonoids, the total content of which is 50%. But in fact, our research found that the content of flavonoids in Duyiwei is relatively low, and in fact it is mainly composed of glycosides. Most substances with flavonoid structure exist in the form of flavonoid glycosides. However, after separation with macroporous resin, luteolin, which has the highest content among flavonoid glycosides, only accounts for about 5% in the extract, while the content of luteolin, a flavonoid component, is about 1/20 of that of luteolin.

In addition, the determination method of total glycosides and total flavonoids is too general, which is prone to large measurement deviations. As long as it contains substances with similar structures, it will be mistaken for total glycosides or total flavonoids. That is to say, this patent application did not make specific confirmation of the active ingredients of its extract, and did not specify which ingredients play the key active ingredients for therapeutic effects. Therefore, it is necessary to further separate the unique extract.

Contents of the invention

The purpose of the present invention is to provide a relatively pure and unique active ingredient to prepare analgesic and hemostatic drugs, so as to better control product quality. Another object is to provide a method for the preparation of this extract.

The technical scheme of the present invention is: the extract solution obtained by extracting the unique medicinal material of Labiatae plant with water extraction ethanol precipitation method or ethanol extraction water precipitation method or ethanol percolation extraction method is obtained after separation by macroporous resin adsorption column chromatography The extract is separated and purified by polyamide column and/or silica gel column chromatography, and the extract contains 22-90% by weight of the active ingredient of phenylpropanoid glycosides in terms of dry product.

Phenylpropanoid glycosides have anti-tumor (Chinese Journal of Pharmaceutical Sciences, 1995, 30(5): 269) and anti-platelet aggregation (Journal of Second Military Medical University, 2004, 25(8): 920). The present invention extracts and separates the substance containing phenylpropanoid glycosides from the plant, and finds that it has analgesic and hemostatic effects, and can be used to prepare analgesic and hemostatic medicines.

The phenylpropanoid glycosides obtained in the present invention specifically refer to pedicularioside A and lamiophlomioside A. Thereby these two kinds of substances can be used as reference substances for qualitative and quantitative control of product quality. Reference substance pedicularioside A, and the preparation method of lamiophlomioside A are summarized as follows:

The extract containing the active ingredient of phenylpropanoid glycoside obtained from the following Example 6 was repeatedly applied to the column on the C18 preparative high performance liquid phase, eluted with 30% methanol aqueous solution, and the two substances with the highest content were collected sequentially. Measure the spectral data of the two substances to determine their structures, and their structural formulas are shown in the accompanying drawings.

The spectral data of substance 1 is completely consistent with the spectral data of pedicularioside A in the Phytochemistry, 1991, 30: 3745-3747 literature, and the structure can be confirmed. The structural formula is shown in Figure 1, which is used as reference substance 1 below. The spectral data of substance 2 is completely consistent with the spectral data of lamiophlomioside A in the literature data of Acta Pharmaceutica Sinica, 1995, 30 (3): 206-210, and the structure can be confirmed. The structural formula is shown in accompanying drawing 2, which is used as reference substance 2 below.

The method of its qualitative and quantitative control product adopts high performance liquid chromatography: make working curve with reference substance, test substance and reference substance go out peak at same retention time, record its peak area, calculate content by working curve, thus phenylpropanoid Glycoside components were qualitatively and quantitatively determined.

Determination of pedicularioside A content:

Preparation of Reference Substance Solution Take an appropriate amount of pedicularioside A reference substance dried overnight with phosphorus pentoxide, weigh it accurately, add methanol to make a solution containing 10 μg per 1 ml, and obtain it.

Preparation of the test solution Take 150 mg of the test sample, weigh it accurately, put it in a 25ml measuring bottle, shake it up, filter it, transfer it to a 25ml measuring bottle, add methanol to the mark, shake it up, and you get it.

Determination method: Precisely draw 5 μl each of the reference substance solution and the test solution, inject it into a liquid chromatograph, and measure it according to the HPLC method in the appendix of the Chinese Pharmacopoeia.

Determination of lamiophlomioside A content:

Preparation of Reference Substance Solution Take an appropriate amount of lamiophlomioside A reference substance dried overnight with phosphorus pentoxide, weigh it accurately, add methanol to make a solution containing 10 μg per 1 ml, and obtain it.

Preparation of the test solution Take 150mg of the content of this product, weigh it accurately, put it in a 25ml measuring bottle, shake well, filter, transfer to a 25ml measuring bottle, add methanol to the mark, shake well, and you get it.

Determination method: Precisely draw 5 μl each of the reference substance solution and the test solution, inject it into a liquid chromatograph, and measure it according to the HPLC method in the appendix of the Chinese Pharmacopoeia.

The sum of the contents of pedicularioside A and lamiophlomioside A is the content of phenylpropanoid glycosides in the test sample.

The preparation method of plant extract provided by the present invention is to adopt the following steps to carry out:

(1) Extraction: using the unique plant of Labiatae as raw material, the extract obtained by water extraction ethanol precipitation method or ethanol extraction water precipitation method or ethanol percolation extraction method commonly used in pharmaceutical technology;

(2) Separation: the extract obtained in step (1) is absorbed by a macroporous resin, and after the extract passes through the resin column, rinse the resin column with water or an ethanol solution lower than 20%, until the eluent is nearly colorless , continue to elute with 30-80% ethanol solution, collect the ethanol eluate,

a. The solution after recovering ethanol is absorbed by a polyamide column with a particle size of 80-200 meshes, eluted with a gradient of 10-95% ethanol solution, and the eluate of 30-95% ethanol solution is collected, and dried after recovering the solvent. Extracts of active ingredients of phenylpropanoid glycosides;

Or b. the solution after recovering ethanol is adsorbed by a silica gel column with a particle size of 80 to 200 meshes, eluted with a gradient of methanol solution of 10 to 95% ethyl acetate, and the eluent of methanol solution of 10 to 80% ethyl acetate is collected , recovering the solvent and then drying to obtain the extract of the active ingredient of phenylpropanoid glycosides;

or c. the eluate of the 30-95% ethanol solution obtained in a, and the solution after recovering the ethanol is then processed according to step b to obtain an extract containing phenylpropanoid glycosides active ingredients.

Concrete preferred extraction process is:

Step (1) Extraction a. Water extraction and ethanol precipitation method: Weigh the coarse powder of medicinal materials, add water to decoct 1 to 3 times, combine each decoction, concentrate to a relative density of about 1.02 to 1.12 (24°C), add ethanol to adjust When the alcohol concentration reaches 30-70%, let it stand still. After the precipitation is complete, pour out the supernatant, filter, and concentrate the medicinal solution until the relative density is 1.02-1.12 at 24°C, and set aside;

b. The ethanol extraction water precipitation method: take the coarse powder of medicinal materials, add 40-90% ethanol solution to reflux extraction, reclaim the ethanol, concentrate the medicinal solution to a relative density of about 1.02-1.12 (24 ° C), add 2-4 times Measure water, mix and stir evenly, let it stand still, after the precipitation is complete, pour out the supernatant, concentrate the liquid until the relative density is 1.02-1.12 at 24°C, and set aside;

c. The so-called ethanol percolation extraction method: Weigh the coarse powder of the unique medicinal material, add 40-90% ethanol to soak, then carry out percolation, collect the percolation liquid, recycle ethanol, and concentrate the medicinal solution to a relative density of about 1.02-1.12 (24°C), add 2 to 4 times the amount of water, mix and stir evenly, let stand, after the precipitation is complete, pour out the supernatant, concentrate the liquid until the relative density measured at 24°C is 1.02 to 1.12, and set aside.

The macroporous resin used during step (2) separation is preferably non-polar or weakly polar macroporous resin.

The use of the plant extract provided by the invention is to prepare medicines for relieving pain and stopping bleeding. In particular, it is used to prepare medicines for treating various pain and bleeding diseases such as incision pain and bleeding after surgical operations, traumatic fractures and the like. The drug is made from a unique plant extract containing phenylpropanoid glycoside active ingredients in a conventional traditional Chinese medicine preparation method, and is added with pharmaceutically acceptable excipients to make any kind of oral preparations, such as tablets, dispersible tablets, granules formulations, capsules, mixtures, oral liquids, syrups, pills, dripping pills. In order to reduce the production cost, the extract used to make the oral preparation should contain 22-55% of the active ingredients of phenylpropanoid glycosides.

The plant extract provided by the present invention proves that it can be used for the preparation of analgesic and hemostatic medicines through pharmacodynamic tests, especially suitable for the preparation of various pains and bleedings such as incision pain and bleeding after surgical operations, traumatic fractures, etc. sick medicine.

1. Analgesic experiment:

1 material

1.1 Animals: Kunming white mice, weighing 18-22g, half male and half male for acetic acid writhing method, all females for hot plate method.

1.2 Main medicines and reagents: Demerol is used in hospitals.

"Duyiwei water extract" is self-made: it adopts the method described in the first part of the Chinese Pharmacopoeia, decocts the unique medicinal material with 8 times the amount of water for three times, each time for 1.5 hours, and the obtained solution is concentrated to a concentration of 1.2g/ml. of extracts.

Test samples: take the extracts of the following examples 2, 4, and 6 respectively, containing 22%, 52% and 90% of the active ingredients of phenylpropanoid glycosides as test groups 1, 2, and 3, respectively.

2 Experimental methods

2.1 Mouse acetic acid writhing method:

Animals were randomly divided into normal control, pethidine, Duyiwei water extract, test group 1, 2, 3, a total of six groups. The normal control group was administered with normal saline; the Duyiwei water extract group was administered with a dose of 1.2g/kg (extract/body weight), and the dosage of the test group was the same, both 0.06g/kg (extract/body weight) . Continuous intragastric administration for 3 days, 30 minutes after the last administration, intraperitoneal injection of 0.6% acetic acid 0.1ml/rat, observe the number of writhing caused within 10 minutes. The data of each group was processed using the t-test for the comparison of the means of two samples, and the calculation was carried out under the SPSS statistical software.

2.2 Hot plate method:

Animals were randomly divided into normal control, pethidine, Duyiwei water extract, test group 1, 2, 3, a total of six groups. Each group was administered orally for 7 days according to the dosage, and the pain threshold of the mice at the last administration was measured by using the hot plate method. The data of each group was processed using the t-test for the comparison of the means of two samples, and the calculation was carried out under the SPSS statistical software.

3 results

Table 1 Writhing test to determine the analgesic effect of different extracts on mice (X±SD) group Dose (g/kg) number of animals Number of twists P blank control 12 42.33±9.3 Demerol 0.05 12 10.5±3.8 <0.01 unique water extract 1.2 12 29.8±8.8 >0.05 Test group 1 0.06 12 23.08±7.3 <0.01 Test group 2 0.06 12 17.24±6.8 <0.01 Test group 3 0.06 12 10.58±3.8 <0.01

Table 2 hot plate method to determine the analgesic effect of different extracts on mice (X±SD) group Dose (g/kg) number of animals Additional time (S) P blank control 12 15.4±8.6 Demerol 0.05 12 35.9±15.2 <0.01 unique water extract 1.2 12 21.8±12.9 <0.01 Test group 1 0.06 12 25.8±6.30 <0.05 Test group 2 0.06 12 26.6±19.8 <0.05 Test group 3 0.06 12 33.2±18.6 <0.05

The results showed that the active ingredients of phenylpropanoid glycosides can reduce the number of writhing reactions in mice, and have analgesic effect, which is significantly different from normal, and the analgesic effect is obvious.

2. Hemostasis experiment

1.1 Animals: Kunming white mice, weighing 18-22g, half male and half male.

1.2 Main drugs and reagents: the same as the analgesic experiment.

2 Experimental methods

2.1 tail cutting method:

Animals were randomly divided into normal control group, test group 1, 2, 3, a total of five groups. The normal control group was administered with normal saline; the Duyiwei water extract group was administered with a dose of 1.2 g/kg, and the doses of the three test groups were the same, all 0.06 g/kg. Continuous intragastric administration for 7 days, fixed after the last administration, measured the length of the tail of the mouse and marked it, and cut the tail tip of the mouse at 3 mm after 30-40 minutes, and started timing when the blood overflowed by itself, and sucked the blood with filter paper every 30 seconds Drop until the blood stops naturally, and calculate the coagulation time. The data of each group was processed using the t-test for the comparison of the means of two samples, and the calculation was carried out under the SPSS statistical software.

2.2 slide method

The animals were randomly divided into five groups: normal control, water extract of Duyiwei, and test groups 1, 2, and 3. Intragastric administration for 3 days, 30 minutes after the last administration, drop a drop of mouse eyeball blood on each end of the glass slide, immediately count with a stopwatch, observe whether there are blood streaks every 30 seconds, record the coagulation time, and take the average value. The data of each group was processed using the t-test for the comparison of the means of two samples, and the calculation was carried out under the SPSS statistical software.

3 results

Table 3 Effects of different extracts on bleeding time in normal mice (X ± SD) group Dose (g/kg) number of animals Coagulation time (S) P blank control 12 135.83±19.77 unique water extract 1.2 12 85.6±20.8 <0.01 Test group 1 0.06 12 80.4±18.4 <0.01 Test group 2 0.06 12 74.61±12.3 <0.01 Test group 3 0.06 12 62.6.2±18.6 <0.01

Table 4 is the same as the impact of the extract on the coagulation time of normal mice (X ± SD) group Dose (g/kg) number of animals Coagulation time (S) P blank control 12 135.83±19.77 unique water extract 1.2 12 102.50±8.29 <0.01 Test group 1 0.06 12 95.8±6.30 <0.01 Test group 2 0.06 12 89.42±14.13 <0.01 Test group 3 0.06 12 75.42±24.19 <0.01

in conclusion:

From the above experimental results, it can be seen that:

1. The crude extract of medicinal materials is further separated and purified to the effective parts, which improves the curative effect of the drug and can significantly reduce the dosage of the patient. The unit dose is equivalent to a high amount of crude drug, which improves the curative effect.

2. The characteristics of this drug are: it can both relieve pain and stop bleeding. Therefore, it is especially suitable for incision pain and bleeding after surgical operations, as well as traumatic fractures and other pains accompanied by bleeding embolism.

The beneficial effects of the present invention are: 1. The medicinal active ingredient of the unique extract is clear. 2. The controllability of product quality is high, and the content of phenylpropanoid glycosides in the extract can be determined by high performance liquid chromatography. 3. The preparation method is suitable for industrial batch production.

Description of drawings:

Figure 1 is a chemical structure diagram of the reference substance pedicularioside A.

Figure 2 is a chemical structure diagram of the reference substance lamiophlomioside A.

Fig. 3 is the HPLC spectrogram of the extract obtained in Example 3 of the present invention, in which A is the peak of the pedicularioside A compound, B is the peak of the lamiophlomioside A compound, and C is the peak of luteolin.

The technical solutions of the present invention will be further described below in conjunction with the examples.

Detailed ways:

Example 1:

Weigh 100 kg of the unique herb powder, add 800 kg of water and decoct for 1.5 hours, add 1000 kg of water to the dregs and decoct for 1.5 hours, combine the decoction, concentrate to a relative density of about 1.02, add ethanol to adjust the alcohol concentration to 30%, and let it stand. After the precipitation was complete, the supernatant was filtered and concentrated to a relative density of about 1.05. Pass the concentrated solution through the WLD macroporous resin. After the concentrated solution passes through the resin column, rinse the resin column with water until the water eluent is nearly colorless, and continue to elute the adsorbed substances on the resin column with 30% ethanol. Collect the ethanol eluate. The recovered solvent is concentrated, dried, and measured by the aforementioned HPLC analysis method, containing 10% of the active ingredient of phenylpropanoid glycosides. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 80-200 mesh, and eluted with a gradient of 30% ethanol to 95%, collecting the eluate of 50-85% ethanol, recovering the solvent and concentrating to a relative density 1.12, drying to obtain 6kg of extract. Measured by the aforementioned HPLC analysis method, it contains 40% of the active ingredient of phenylpropanoid glycosides (based on the weight of the dry product, the same below).

Example 2:

Weigh 100kg of the unique medicinal herb coarse powder, add 900kg of water to decoct for 2 hours, add 900kg of water to the dregs and decoct for 2 hours, combine the decoction, concentrate to a relative density of about 1.05, add ethanol to adjust the alcohol concentration to 50%, and let it stand. After the precipitation was complete, the supernatant was filtered and concentrated to a relative density of about 1.07. Pass this concentrated solution through ZTC-5 macroporous resin. After all the concentrated solution passes through the resin column, rinse the resin column with water until the water eluent is nearly colorless, and continue to wash the adsorbed substances on the resin column with 50% ethanol. Remove and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a silica gel column with a particle size of 100-200 mesh, and eluted with a gradient of 30% ethyl acetate methanol solution to 85%, and the elution of 30-85% ethyl acetate methanol solution is collected. After recovering the solvent, it was concentrated to a relative density of 1.25, and dried under reduced pressure to obtain 8 kg of extract. The measured content of phenylpropanoid glycosides was 22%.

Example 3:

Weigh 100kg of the unique herb powder, add 1000kg of water and decoct for 2 hours, add 1000kg of water to the dregs and decoct for 2 hours, combine the decoction, concentrate to a relative density of about 1.09, add ethanol to adjust the alcohol concentration to 70%, and let it stand. After the precipitation was complete, the supernatant was filtered and concentrated to a relative density of about 1.08. Pass this concentrated solution through HPD-100 macroporous resin. After the concentrated solution has passed through the resin column, rinse the resin column with 20% ethanol until the eluate is nearly colorless, and then use 80% ethanol to remove the adsorbed substances on the resin column. Perform elution and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 120-200 mesh, eluted with a gradient of 30% ethanol to 85%, and the eluate of 40-80% ethanol is collected. The solution after recovering ethanol under reduced pressure is then adsorbed by a silica gel column with a particle size of 80-100 mesh, and eluted with a gradient of 30% ethyl acetate methanol solution to 85%, collecting 40-80% ethyl acetate methanol solution. dehydration. The solvent was recovered, concentrated to a relative density of 1.06, and spray-dried to obtain 4.5 kg of the extract. The measured content of phenylpropanoid glycosides is 60%.

Example 4:

Weigh 100kg of the coarse powder of the unique medicinal material, add 800kg of 40% ethanol to reflux extraction for 3 times, combine the ethanol extracts, recover the ethanol, concentrate the medicinal solution to a relative density of 1.02, add an appropriate amount of water to mix evenly, and let stand. After the precipitation is complete, pour out the supernatant, filter, and concentrate the medicinal solution to a relative density of about 1.04. Pass the concentrated solution through HPD-450 macroporous resin. After the concentrated solution passes through the resin column, rinse the resin column with water until the eluent is nearly colorless, and continue to elute the adsorbed substances on the resin column with 40% ethanol. , and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 80-200 mesh, and eluted with a gradient of 30% ethanol to 85%, collecting the eluate of 40-85% ethanol, recovering the solvent and concentrating to a relative density 1.06, spray drying promptly obtains extract 4.9kg. The measured content of phenylpropanoid glycosides was 52%.

Example 5:

Weigh 100kg of the coarse powder of the unique medicinal material, add 60% ethanol and 900kg of reflux to extract 3 times, combine the ethanol extracts, recover ethanol, concentrate the medicinal solution to a relative density of 1.05, add an appropriate amount of water to mix and stir evenly, and let stand. After the precipitation is complete, pour out the supernatant, filter, and concentrate the medicinal solution to a relative density of about 1.04. Pass this concentrated solution through AB-8 macroporous resin. After all the concentrated solution passes through the resin column, rinse the resin column with 10% ethanol until the eluate is nearly colorless, and then use 60% ethanol to remove the adsorbed substances on the resin column Perform elution and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a silica gel column with a particle size of 100-200 mesh, and eluted with a gradient of 30% ethyl acetate methanol solution to 85%, and the elution of 40-90% ethyl acetate methanol solution is collected. After recovering the solvent, it was concentrated to a relative density of 1.07, and spray-dried to obtain 5.8 kg of the extract. The measured content of phenylpropanoid glycosides was 63%.

Embodiment 6:

Weigh 100kg of the coarse powder of the unique medicinal material, add 1000kg of 80% ethanol to reflux extraction for 3 times, combine the alcohol extracts, recover the ethanol, concentrate the medicinal solution to a relative density of 1.08, add an appropriate amount of water to mix and stir evenly, and let stand. After the precipitation is complete, pour out the supernatant, filter, and concentrate the medicinal solution to a relative density of about 1.08. Pass this concentrated solution through HPD-100 macroporous resin. After the concentrated solution has passed through the resin column, rinse the resin column with 20% ethanol until the eluate is nearly colorless, and then use 80% ethanol to remove the adsorbed substances on the resin column. Perform elution and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 120-200 mesh, eluted with a gradient of 30% ethanol to 95%, and the eluate of 40-80% ethanol is collected. The solution after recovering ethanol under reduced pressure is then adsorbed by a silica gel column with a particle size of 120-200 mesh, and eluted with a gradient of 30% ethyl acetate in methanol solution to 95%, collecting 40-80% ethyl acetate in methanol solution for washing. dehydration. After the solvent is recovered, it is concentrated to a relative density of 1.08, spray-dried to obtain 3.8 kg of an extract, and the measured content of phenylpropanoid glycosides is 90%.

Embodiment 7:

Weigh 10kg of the coarse powder of the unique medicinal material, add 50% ethanol to soak, then percolate at a speed of 3ml/min, collect the percolation liquid, recover ethanol, concentrate the medicinal liquid to a relative density of 1.1, add an appropriate amount of water to mix and stir evenly, stand still. After the precipitation is complete, pour out the supernatant, filter, and concentrate the drug solution to a relative density of 1.06. Pass this concentrated solution through HPD-100 macroporous resin. After all the concentrated solution passes through the resin column, rinse the resin column with water until the eluent is nearly colorless, and continue to elute the adsorbed substances on the resin column with 40% ethanol. , and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 80-200 mesh, and eluted with a gradient of 30% ethanol to 95%, collecting the eluate of 40-85% ethanol, recovering the solvent and concentrating to a relative density 1.05, spray drying promptly obtains extract 0.58kg. The measured content of phenylpropanoid glycosides was 45%.

Embodiment 8:

Weigh 10kg of the coarse powder of the unique medicinal material, add 70% ethanol to soak, then percolate at a speed of 5ml/min, collect the percolation liquid, recover ethanol, concentrate the medicinal liquid to a relative density of 1.08, add an appropriate amount of water to mix and stir evenly, stand still. After the precipitation is complete, pour out the supernatant, filter, and concentrate the medicinal solution to a relative density of 1.08. Pass this concentrated solution through AB-8 macroporous resin. After the concentrated solution has passed through the resin column, rinse the resin column with 20% ethanol until the eluate is nearly colorless, and then use 70% ethanol to remove the adsorbed substances on the resin column. Perform elution and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a silica gel column with a particle size of 100-200 mesh, and eluted with a gradient of 30% ethyl acetate methanol solution to 95%, and the elution of 40-80% ethyl acetate methanol solution is collected. After recovering the solvent, it was concentrated to a relative density of 1.06, and spray-dried to obtain 0.6 kg of the extract. The measured content of phenylpropanoid glycosides was 43%.

Embodiment 9:

Weigh 10kg of the coarse powder of the unique medicinal material, add 50% ethanol to soak, then percolate at a speed of 3ml/min, collect the percolation liquid, recover ethanol, concentrate the medicinal liquid to a relative density of 1.1, add an appropriate amount of water to mix and stir evenly, stand still. After the precipitation is complete, pour out the supernatant, filter, and concentrate the drug solution to a relative density of 1.06. Pass this concentrated solution through HPD-100 macroporous resin. After all the concentrated solution passes through the resin column, rinse the resin column with water until the eluent is nearly colorless, and continue to elute the adsorbed substances on the resin column with 40% ethanol. , and collect the ethanol eluate. The solution after recovering ethanol under reduced pressure is adsorbed by a polyamide column with a particle size of 80-200 mesh, and eluted with a gradient of 30% ethyl acetate in methanol solution to 95%, collecting 40-85% ethyl acetate in methanol solution for washing. dehydration. The solution after recovering ethanol under reduced pressure is then adsorbed by a silica gel column with a particle size of 80-200 mesh, and eluted with a gradient of 30% ethanol to 95%, and the eluate of 40-85% ethanol is collected. After recovering the solvent, it was concentrated to a relative density of 1.05, and spray-dried to obtain 0.45 kg of the extract. The measured content of phenylpropanoid glycosides was 84%.

Prepare various oral dosage forms below with the active extract that above-mentioned embodiment 4 makes:

Embodiment A, tablet:

Take about 150 grams of dry powder of the extract containing phenylpropanoid glycosides, add sugar powder and dextrin in an appropriate amount, mix with 6% sodium carboxymethyl starch, pass through a 100 mesh sieve, and use 70% ethanol to wet process Granules, after drying and granulating, add appropriate amount of magnesium stearate, mix and compress into tablets. Make 1000 tablets, each weighing about 0.3g, which is equivalent to 3g of crude drug. Each tablet contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Take orally, one tablet each time, 3 times a day.

Embodiment B, capsule

Take 150 g of the dry extract powder containing phenylpropanoid glycosides, add appropriate amount of starch, mix with 10% sodium carboxymethyl starch, pass through a 100-mesh sieve, granulate, dry, pour into No. 1 capsule, Make 1000 capsules, each weighing about 0.25g, which is equivalent to 3g crude drug. Each tablet contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. 1 capsule each time, 3 times a day.

Embodiment C, dispersible tablet

Take 150 grams of the dry powder of the extract containing phenylpropanoid glycosides, mix with 16% sodium carboxymethyl starch, pass through a 100 mesh sieve, appropriate amount of low-substituted hydroxypropyl methylcellulose, and use polyethylene Pyrrolidone ethanol liquid soft material, wet granulation, after drying and granulation, add appropriate amount of magnesium stearate, mix and compress into tablets. Make 1000 tablets, each weighing about 0.3g, which is equivalent to 3g of crude drug. Each tablet contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Take orally, one tablet each time, 3 times a day. According to the disintegration time limit method of the Chinese Pharmacopoeia, the sample should disintegrate within 3 minutes.

Embodiment D, oral liquid

Take about 150g of the dry powder of the extract containing phenylpropanoid glycosides, add a small amount of hot water to dissolve, stir well, add an appropriate amount of simple syrup, add water to 1000ml, adjust the pH to 6-7, filter, and pot , sterilized, and obtained. Specifications: 10ml/bottle, equivalent to 3g crude drug. Each tube contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Take orally, one tablet each time, 3 times a day.

Embodiment E, dropping pill

Get 150g of the extract dry powder containing phenylpropanoid glycosides, pass through a 120 mesh sieve, add to the mixed solution of about 250g of molten polyethylene glycol 6000 and 4000, fully mix, and put it on the dropping pill machine with 70 10,000 drop pills were dripped at the temperature of the liquid medicine, each weighing about 50 mg. Each 10 capsules is equivalent to 3g of crude drug. Each 10 capsules contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Oral, 6 capsules each time, 3 times a day.

Embodiment F, syrup

Take about 150g of the dry powder of the extract containing phenylpropanoid glycosides, add a small amount of hot water to dissolve, stir well, add an appropriate amount of simple syrup, add water to 1000ml, adjust the pH value to 6-7, filter, and pot , sterilized, and obtained. Specifications: 100ml/bottle, equivalent to 30g crude drug. Each 10ml contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Orally, 10ml each time, 3 times a day.

Embodiment G, granules

Take 150 g of dry powder of the extract containing phenylpropanoid glycosides, add appropriate amount of lactose and dextrin, mix evenly, wet granulate, dry and granulate, and pack separately. Made into 1000g, 2g per pack. Equivalent to 3g crude drug. Each contains about 45mg of pedicularioside A and about 33mg of lamiophlomioside A. Take orally, one pack each time, 3 times a day.

Claims (7)

1. A plant extract, the extract obtained by the unique water extraction ethanol precipitation method or ethanol extraction water precipitation method or ethanol percolation extraction method obtained by Labiatae plant, the crude product obtained after separation by macroporous resin adsorption column chromatography The extract is characterized in that the crude extract obtained after separation by macroporous resin adsorption column chromatography is separated and purified by polyamide column or/and silica gel column chromatography, and the extract contains styrene-acrylic acid in dry form. The percentage by weight of the vegetarian glycoside active ingredient is 22-90%. 2. the preparation method of said plant extract according to claim 1, is characterized in that, comprises the following steps: (1) Extraction: using the unique plant of Labiatae as a raw material, the extract is obtained through the common water extraction ethanol precipitation method or ethanol extraction water precipitation method or ethanol percolation extraction method in the pharmaceutical process; (2) Separation: the extract obtained in step (1) is absorbed by a macroporous resin, and after the extract passes through the resin column, rinse the resin column with water or an ethanol solution lower than 20%, until the eluent is nearly colorless , continue to elute with 30-80% ethanol solution, collect the ethanol eluate, a. recover the solution after ethanol, absorb it on a polyamide column with a particle size of 80-200 mesh, and elute with a gradient of 10-95% ethanol solution, Collect the eluate of 30-95% ethanol solution, recover the solvent and dry to obtain the extract of the active ingredient of phenylpropanoid glycosides; or b. The solution after recovering ethanol is adsorbed by a silica gel column with a particle size of 80-200 mesh to obtain Gradient elution of 10-95% ethyl acetate in methanol solution, collecting the eluate of 10-80% ethyl acetate in methanol solution, recovering the solvent and drying to obtain the extract of the active ingredient of phenylpropanoid glycosides; or c. From the eluate of 30-95% ethanol solution obtained in a, the solution after recovering ethanol is then processed according to step b to obtain the extract containing phenylpropanoid glycosides active ingredients. 3. The preparation method of the plant extract according to claim 2, characterized in that, step (1) extraction: said water extraction ethanol precipitation method is to weigh the unique medicinal material, decoct it with water for 2 to 3 times, Combine each water decoction, concentrate until the relative density measured at 24°C is 1.02-1.12, add ethanol to adjust the alcohol concentration to 30-70%, let it stand, and after the precipitation is complete, pour out the supernatant, filter, and the liquid Concentrate until the relative density measured at 24°C is 1.02-1.12, set aside; The said ethanol extraction water precipitation method is to weigh the unique medicinal material, add 40-90% ethanol solution to reflux extraction, recycle the ethanol, concentrate the medicinal solution until the relative density is 1.02-1.12 at 24°C, add 2-4 times the amount Mix with water and stir evenly, let it stand still, after the precipitation is complete, pour out the supernatant, concentrate the liquid until the relative density is 1.02-1.12 at 24°C, and set aside; The so-called ethanol percolation extraction method is to weigh the unique medicinal material, add 40-90% ethanol to soak, then carry out diafiltration, collect the percolation liquid, recycle the ethanol, and concentrate the medicinal solution until the relative density is measured as 1.02-1.02 at 24°C. 1.12, add 2 to 4 times the amount of water to mix and stir evenly, let it stand still, after the precipitation is complete, pour out the supernatant, concentrate the liquid to a relative density of 1.02 to 1.12 at 24°C, and set aside. 4. The preparation method of the plant extract according to claim 2, characterized in that, said macroporous resin is non-polar or weakly polar macroporous resin. 5. according to the purposes of the said plant extract of claim 1, it is characterized in that the medicine of preparing analgesic, hemostasis. 6. The use of the plant extract according to claim 5, characterized in that it is for the preparation of medicines for treating incision pain and bleeding after surgical operations, traumatic fracture pain and bleeding. 7. according to the purposes of the said plant extract of claim 5, it is characterized in that said medicine is to use conventional Chinese medicine preparation method, get the extract containing phenylpropanoid glycosides active ingredient, add the adjuvant that is allowed on pharmacy, Make any medicine of oral preparation, said oral preparation has tablet, dispersible tablet, granule, capsule, mixture, oral liquid, syrup, pill, drop pill.

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