CN102727566B - Microwave-assisted extraction process for mongolian milkvetch root saponin and mongolian milkvetch root polysaccharide - Google Patents

Abstract

The present invention discloses a microwave-assisted extraction process for mongolian milkvetch root saponin and mongolian milkvetch root polysaccharide. The process comprises the following steps: a, weighing a mongolian milkvetch root drug material; b, placing the material in a microwave extraction device, and carrying out extraction three times at a temperature of 70 DEG C, wherein the microwave power is 500-900 W, 50-90% ethanol is added in the first extraction, the first extraction time is 10-30 minutes, 50-90% ethanol is added in the second extraction, the second extraction time is 10-30 minutes, distilled water is added in the third extraction, and the third extraction time is 20-40 minutes; c, concentrating the first extracting solution and the second extracting solution, removing the ethanol from the resulting mixture, then adding the third extracting solution to the ethanol-removed mixture, mixing and concentrating to obtain the extract of mongolian milkvetch root saponin and mongolian milkvetch root polysaccharide. With the extraction process of the present invention, utilization rate of active ingredients in the mongolian milkvetch root drug material is improved, yields of he mongolian milkvetch root saponin and the mongolian milkvetch root polysaccharide in the mongolian milkvetch root drug material are improved, the extraction time is shortened, and the extraction process steps are simplified.

Description

A microwave-assisted extraction process of astragalus saponins and astragalus polysaccharides

technical field

The invention provides a process for microwave-assisted extraction of astragalus saponin and astragalus polysaccharide.

Background technique

Astragalus membranaceus (Fisch.) Bge.var.mongholicus (Bge.) Hsiao or Astragalus membranaceus (Fisch.) is a perennial herb of the leguminous family. After reviewing the relevant literature, until now, the research on the extraction process of Astragalus has mainly focused on the single extraction of astragalus saponins or astragalus polysaccharides, which has caused a great waste of rational utilization of medicinal materials.

Currently retrieved patent literature and non-patent literature have reported that microwaves alone extract astragalus polysaccharides or astragalosides, and the solvents and parameters selected are different, such as Hu Rugui et al. Traditional Chinese Medicine, 2007, 18 (5): 1074-1075), using microwave-assisted extraction technology to extract astragalus saponins from Astragalus membranaceus, using water as solvent, the best extraction process obtained is: Astragalus membranaceus 60 mesh, microwave power 800W, 20 times the amount of water extraction 2 times, 15min/time, the content of astragaloside obtained: 3.497mg/g; Gong Shengzhao et al. 889-891), using microwave-assisted extraction technology to extract astragaloside IV from astragalus, using 95% ethanol as solvent, the best extraction process obtained is: take 50g of astragalus powder, add 350mL 95% ethanol, and use microwave radiation 30s, after an interval of 1min, then irradiate for 30s, repeat the interval radiation until the total radiation time is 4min, and filter. Repeat the extraction once under the same conditions. Yield 2.42%. Xu Haiyan et al. (Research on Microwave Extraction of Polysaccharides in Astragalus [J], Chinese Herbal Medicine, 2008.39 (10): 1496-1499), for the extraction of Astragalus polysaccharides in Astragalus, using water as the extraction solvent, the best extraction conditions obtained are: Control the temperature at 70°C, extract 3 times, 10 minutes each time, the extraction rate of astragalus polysaccharide is 9.44%. Gong Shengzhao et al. (Study on Microwave Assisted Extraction of Astragalus Polysaccharides [J], Journal of South China University of Technology (Natural Science Edition), 2004, 32 (8): 93-96), for the extraction of Astragalus polysaccharides in Astragalus, pH=9 The alkaline water is used as the extraction solvent, and the mass ratio of the liquid to the material is 12:1; the pH is adjusted to 9 with saturated lime water; the microwave power is 300W, and the extraction is performed twice, each time for 10 minutes, and the extract is concentrated in vacuum, and ethanol is added to precipitate the polysaccharide. After filtration, the precipitate was washed several times with ethanol and vacuum dried to obtain the crude polysaccharide of Astragalus with a yield of 14.6%.

The currently retrieved literatures are all extracting astragalus saponins or astragalus polysaccharides separately, and there is no literature report on extracting these two types of active ingredients at the same time.

Contents of the invention

The technical solution of the invention is to provide a process for microwave-assisted extraction of astragalus saponin and astragalus polysaccharide.

The invention provides a process for microwave-assisted extraction of astragalus saponin and astragalus polysaccharide, which comprises the following steps:

a, take the Radix Astragali medicinal material;

b. Put the medicinal material in a microwave extraction device, microwave power 500W-900W, temperature 70°C, extract 3 times in total, add 50%-90% ethanol for the first time, extract for 10min-30min; add 50%-90% for the second time % ethanol, extract for 10min-30min; add distilled water for the third time, extract for 20min-40min;

c. Concentrate the 1st and 2nd ethanol extracts, remove the ethanol, then add the 3rd water extracts, mix and concentrate to obtain astragaloside and astragalus polysaccharide extracts of the present invention.

Wherein, the astragalus medicinal material is medicinal herb decoction pieces or soybean grain-sized decoction pieces, or medicinal powder passed through a No. 1-3 sieve.

Wherein, the medicinal material Radix Astragali described in step a is pulverized to a size below 24 mesh.

Wherein, the consumption of ethanol or water described in step b is 10-14 times of the weight of medicinal material.

Wherein, the ethanol described in step b is 70% ethanol.

Wherein, the microwave power described in step b is 500-700W.

The concrete advantage of extraction technique of the present invention is as follows:

1. The effective substance utilization rate of Astragalus is greatly improved. Through a set of test schemes, the present invention simultaneously extracts effective substances in Astragalus medicinal materials: astragalus saponins and astragalus polysaccharides, which greatly improves the utilization rate of effective substances in Astragalus medicinal materials, and the extraction rates of astragalus saponins and astragalus polysaccharides obtained by this method are both high. stable above 90%.

2. The extraction rate and yield of astragalus polysaccharide are greatly improved. The content of the astragalus polysaccharide obtained by the method of the invention can be stabilized at about 260 mg/g. Yang Yifang et al. (Application No.: 200510026889.1, Invention Name: Method for Extracting Astragalus Polysaccharides by Microwave) obtained the yield of Astragalus polysaccharides in Example 2 at 20.4%, and the yield of Astragalus polysaccharides obtained by the method of the present invention was about 26%. The content of astragalus polysaccharides for five times is 100%, and it is measured that the extraction rate of astragalus polysaccharides obtained by the method of the present invention can be stable at about 91%.

3. The extraction rate of astragaloside is greatly improved, and the yield is relatively improved. The content of astragaloside obtained by the method of the invention can be stabilized at about 11 mg/g, and the extraction rate of astragaloside can be stabilized at about 95%. Wang Xin et al. (Study on the Extraction Technology of Astragalus [J], Chinese Experimental Formula, 2010, 16 (9): 17-18), extracted with the traditional method of ethanol reflux, and only took the yield of Astragalus saponin as the index component, and obtained The content of astragaloside is: 1.342mg/g. However, Hu Rugui et al. (Study on the process of extracting astragalosides with microwave water [J]. Shizhen Guoyi Guoyao, 2007, 18 (5): 1074-1075) used microwave-assisted methods for extraction, and only the yield of astragalosides was used as an index component , the obtained astragaloside content is: 3.497mg/g. Gong Shengzhao et al. (Study on Microwave Extraction of Astragaloside IV [J], Chinese Patent Medicine, 2005, 28 (8): 889-891), used microwave-assisted extraction technology to extract astragaloside IV from Astragalus membranaceus, and measured the yield, In terms of astragaloside IV, it is 2.42%. Although the yield of astragaloside reported in this literature is relatively high, the extraction rate of active ingredients of medicinal materials has not been investigated.

4. The extraction time of Astragalus medicinal materials is shortened. The optimal extraction scheme of the present invention is: without soaking, extracting 3 times altogether, each time extracting 30min, the 4th time 40min, the content of obtained astragaloside is about 11mg/g, and the extraction rate is about 95%, while Chen Tao et al. Research on Microwave Extraction Technology of [J]. Shizhen Guoyi Guoyao, 2009, 20 (2): 349-350), using microwave-assisted extraction technology, only for the extraction of astragaloside IV in Astragalus membranaceus, using water as the solvent, the most obtained The best extraction process is as follows: Astragalus membranaceus is first soaked for 6 hours, then extracted 3 times, each time with 10 times the amount of water, 90 minutes.

5. The extraction process operation is greatly simplified. At the same time, to use the astragalus saponin and astragalus polysaccharide traditional Chinese medicine compound, it is necessary to extract the astragalus saponin and astragalus polysaccharide respectively, and the method of the invention does not need to carry out pH treatment on the extraction solvent. For example, Gong Shengzhao et al. (Study on Microwave Assisted Extraction of Astragalus Polysaccharides [J], Journal of South China University of Technology (Natural Science Edition), 2004, 32 (8): 93-96), for the extraction of Astragalus polysaccharides in Astragalus, the pH = The alkaline water of 9 is the extraction solvent, and the yield is only 14.6%.

The extraction process of the present invention greatly improves the utilization rate of active ingredients in Astragalus medicinal materials (using this test scheme, astragalus saponin and astragalus polysaccharide in Astragalus can be extracted at one time, and the extraction rate of the two active ingredients can be stabilized at more than 90% ), improve the yield of Astragalus polysaccharide in Astragalus medicinal material (the existing yield is about 20%, the yield of Astragalus polysaccharide by the extraction method of the present invention can be stabilized at 24%-26%, and the extraction rate of Astragalus polysaccharide can be stabilized at about 91%); Ensure the stable yield of Astragalus saponin in Astragalus medicinal materials (the current yield is 0.13%-2.42%, the yield of Astragaloside extracted through the optimal process of this test can be stabilized at 1%-1.1%, and the extraction rate of Astragaloside can be stabilized at 95% or so); Relatively shorten the test time and simplify the extraction process steps.

Description of drawings

Figure 1 The effect of the particle size of Astragalus medicinal materials on the extraction process (among them, the particle sizes of medicinal materials 1-5 are: astragalus decoction pieces, the size of soybean grains, passing through No. 1 sieve, passing through No. 2 sieve, and passing through No. 3 sieve).

Detailed ways

Embodiment 1 Extraction process parameter screening test of the present invention

1 Instruments and reagents

1.1 Instrument

HWC-3 microwave extraction experimental equipment (Tianshui Huayuan Medical Equipment Co., Ltd.); UV-6000 ultraviolet-visible spectrophotometer (Shanghai Meipuda Instrument Co., Ltd.); swinging high-speed universal pulverizer (DFY-300, Wenling City Linda Machinery Co., Ltd.); rotary evaporator (RE52CS-1 type, Shanghai Yarong Biochemical Instrument Factory); vacuum drying oven (DZG-6020 type, Shanghai Senxin Experimental Instrument Co., Ltd.); BP61 electronic balance (ten thousandth 1, Germany Satorius); electronic balance (BP211D type, one hundred thousandth, Germany Satorius); UPT-I-10T ultra-pure water device (Chengdu Ultra Pure Technology Co., Ltd.); constant temperature water bath (Jintan City Hongke instrument factory); pipette guns of various models.

1.2 Reagent

Astragalus medicinal material (purchased from Chengdu Hehuachi Traditional Chinese Medicinal Materials Market, identified as authentic by the teachers of the Chinese Medicine Identification Department of Chengdu University of Traditional Chinese Medicine); company); D-anhydrous glucose reference substance (batch number l 10833-200302, for content determination, provided by China Institute for the Control of Pharmaceutical and Biological Products). 5% phenol solution; 5% vanillin-glacial acetic acid solution; concentrated sulfuric acid, perchloric acid, ammonia water, phenol, vanillin, etc. are all analytically pure.

2 Methods and results

2.1 Determination of the content of total saponins of astragalus

2.1.1 Preparation of astragaloside standard curve

Accurately weigh a certain amount of astragaloside IV reference substance, put it in a 10mL measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and obtain astragaloside IV reference substance solution. Take 0.0, 0.4, 0.8, 1.2, 1.6mL of the reference substance solution respectively and place them in a 10mL graduated test tube with stopper, evaporate to dryness in a water bath, cool, add 0.2mL of 5% vanillin-glacial acetic acid solution and 0.8mL of perchloric acid, and mix well , heated in a water bath at 60°C for 15 minutes, took it out, and immediately cooled it in an ice bath for 5 minutes, then added 5 mL of glacial acetic acid, mixed thoroughly, and measured its absorbance at 561 nm with the solution in a "0 mL" stoppered graduated test tube as a blank. Taking the mass concentration m of the astragaloside IV reference substance as the abscissa and the absorbance A as the ordinate, a regression equation C=0.0010+0.0474A (r=0.9997) was established. Astragaloside IV has a good linear relationship in the absorbance of 0.0816-0.3254mg.

2.1.2 Preparation of Astragalus total saponins test solution

Precisely draw 40mL of Astragalus extract (equivalent to 4g of the original medicinal material), put it in an evaporating dish, evaporate to dryness in a water bath, add 10mL of water to the residue, dissolve it with slight heat, shake and extract 4 times with n-butanol saturated with water, 40mL each time, combine Wash the n-butanol extract twice with ammonia test solution, 40mL each time, discard the ammonia solution, evaporate the n-butanol to dryness, dissolve the residue in methanol and transfer it to a 10mL measuring bottle, add methanol to the mark, shake well, and use as The test solution.

2.1.3 Precision test

Take the same test solution, prepare the test solution according to 2.1.2, repeat the measurement 5 times, and get an RSD of 0.52%.

2.1.4 Stability test

After developing the color of the same reference substance solution, time scanning for 1 hour, Abs changed between 0.8031-0.8033, indicating that the test solution was stable within 1 hour after color development.

2.1.5 Repeatability test

Take 5 parts of the same sample solution, 0.2 mL each, prepare the test product according to item 2.1.2, and measure the total saponin content of Astragalus membranaceus. The measured RSD is 1.30%, which shows that the repeatability of the method is good.

2.2 Astragalus polysaccharide content determination

2.2.1 Preparation of Astragalus polysaccharide standard curve

Accurately weigh a number of D-glucose anhydrous reference substances dried at 105°C to constant weight, put them into a 50mL volumetric flask, add deionized water to the mark, and shake well to obtain the standard solution. Pipette 0.0, 0.2, 0.4, 0.8, 1.2, 1.6, 2.0 mL of prepared glucose standard solutions into 10 mL graduated test tubes with stoppers, add deionized water to 2 mL, add 1 mL of 5% phenol solution, shake well, add 5 mL concentrated Shake with sulfuric acid for 5 minutes, heat in a boiling water bath for 15 minutes, cool in a cold water bath for 30 minutes, and measure the absorbance at 490 with a blank solvent as a reference. With the mass concentration m of the D-anhydrous glucose reference substance as the abscissa and the absorbance A as the ordinate, a regression equation C=0.0001+0.0141A (r=0.9995) was established. D-glucose anhydrous reference substance has a good linear relationship in the absorbance of 0.0025～0.0250mg·mL ^-1 .

2.2.2 Preparation of astragalus polysaccharide test solution

This experiment uses the phenol-sulfuric acid method to determine the content of astragalus polysaccharides. The specific preparation process is: take 0.2mL of astragalus extract into a 100mL volumetric flask, shake well, take 1mL of the solution in a 10mL stoppered test tube, and follow the steps in item 2.2.1 Prepared by the following preparation process.

2.2.3 Precision test

Take the same test solution, prepare the test solution according to 2.2.2, repeat the measurement 5 times, and get an RSD of 0.49%.

2.2.4 Stability test

After developing the color of the same reference substance solution, time scanning for 1 hour, Abs changed between 0.6151-0.6154, indicating that the test solution was stable within 1 hour after color development.

2.2.5 Repeatability test

Take 5 parts of the same sample solution, 0.2 mL each, prepare the test product according to 2.1.2, and measure the total saponin content of Astragalus membranaceus. The RSD of the determination is 1.17%, which shows that the repeatability of the method is good.

2.3 Single factor test

In this test plan, the particle size of Astragalus membranaceus and the soaking time were firstly investigated by single factor; after consulting the relevant literature, the particle size mainly affects the total saponins of Astragalus, so in the single factor test, only the total saponins of Astragalus were used as the index component. filter.

2.3.1 Effect of particle size of Astragalus membranaceus on extraction process

A total of 5 kinds of particle sizes were examined in this single factor test, namely: astragalus decoction pieces, soybean grain size, passing through No. 1 sieve, passing through No. 2 sieve, and passing through No. 3 sieve. The specific results are shown in Figure 1.

It can be seen from the above figure that with the decrease of the particle size of medicinal materials, the extraction amount of total saponins of Astragalus gradually increases, and when the particle size is 4, the extraction amount of total saponins basically tends to be stable. The requirements for the extraction process are higher, so this test selects the particle size of medicinal materials that pass the No. 2 sieve.

2.3.2 The effect of soaking time of Astragalus membranaceus on the extraction process

In this test, three gradients of soaking time of 0, 30, and 60 min were selected for investigation, and astragaloside was still selected as the index component. The results are shown in Table 1.

It can be seen that the soaking time basically has no significant effect on the extraction of total astragalus saponins, so this experiment chooses not to soak.

In addition, the experiment also examined the effect of extraction temperature on the extraction process of Astragalus membranaceus, and learned that the extraction temperature had no significant impact on the extraction process. Considering comprehensively, the extraction temperature was selected to be 70°C.

2.4 Orthogonal experimental design

On the basis of the pre-test and single-factor experiment, three times of extraction are planned, the first two times are ethanol extraction of corresponding concentration, and the third time is water extraction of corresponding multiple. Select microwave power, extraction time, solvent dosage, and solvent concentration to conduct an orthogonal experiment design with 4 factors and 3 levels, and use Orthogonal Experiment Assistant II to conduct statistical analysis. The specific factor levels are shown in Table 2. The corresponding orthogonal experiment design is shown in Table 3. The analysis of variance is shown in Table 4.

Table 2 Factor level table

Note: This test is extracted 3 times, the first 2 times are the ethanol solution extraction of the corresponding concentration, and the third time is the water extraction of the corresponding multiple.

Table 3 Orthogonal test table

Note: Y ₁ : Extraction of Astragalus saponin Y ₂ : Extraction of Astragalus polysaccharide Y ₃ : Yield of extract

Y _{comprehensive score} = (0.5Y ₁ /Ymax ₁ +0.3Y ₂ /Ymax ₂ +0.2Y ₃ /Ymax ₃ )×100%

Table 4 variance analysis table

Note: F _0.05 (2.2)=19.000; *significant

It can be known from Table 3 that the effect of the four factors on the extraction process is: B>A>D>C. Combined with Table 4, considering various factors, the optimal process conditions for extracting total saponins and polysaccharides of astragalus are: A ₁ B ₃ C ₃ D ₂ , that is: without soaking the medicinal materials, the medicinal powder is passed through a No. 2 sieve, the microwave power is 500W, and the extraction is performed 3 times. The first 2 extractions are 14 times the amount of 70% ethanol, and the third extraction is the corresponding amount of water extraction 40min.

2.5 Confirmatory experiments

According to the above-mentioned process conditions that have been examined, the examination is repeated three times, and the experimental results are shown in Table 5.

Extraction rate of astragalus saponin (%)=(volume of extract x saponin concentration measured in extract)/(mass of medicinal material x saponin content measured in medicinal material) x 100%

Astragalus polysaccharide extraction rate (%) = (extract volume × polysaccharide concentration measured in the extract) / (5 extract volume × concentration of astragalus polysaccharide in 5 extracts) × 100%

Table 5 verification test

3 Discussion

On the basis of the confirmatory experiment, an enlarged experiment was done again, that is, the amount of the medicinal material was enlarged by 10 times. The experimental results showed that the repeatability was good. The best extraction process of the present invention was: the medicinal material was not soaked, the medicinal powder was passed through a No. 2 sieve, and microwave Power 500W, extraction 3 times, first 2 times with 14 times the amount of 70% ethanol, the third time with the corresponding amount of water extraction for 40 minutes.

Example 2 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Precisely weigh 10 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 900W, keep the temperature at 70°C, extract 3 times in total, add 158mL of 50% ethanol for the first time, and extract for 10 minutes; the second time Add 140mL of 50% ethanol solution and extract for 10min; add 140mL of distilled water for the third time and extract for 20min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 60mL, add distilled water to a 100mL volumetric flask, and use phenol-sulfuric acid method The content of astragalus polysaccharide in the extract was determined to be 1.720g, the yield was 18.49%, and the extraction rate was 65.32%; the content of total astragalus saponins was 0.053g, the yield was 0.57%, and the extraction rate was 49.72%.

Among them, the description of the conversion rate of astragalus saponins and astragalus polysaccharides is as follows:

After reviewing relevant literature, the yield of astragaloside in Astragalus membranaceus ranges from 0.13% to 2.42%, and the yield varies greatly, which may be caused by the quality of medicinal materials. The yield of astragaloside extracted by the optimal process in this test can be stabilized at 1%-1.1%. Yield: It is the percentage of active ingredients contained in the unit medicinal material mass, and the corresponding formula is:

Astragalus saponin yield (%)=(volume of extract x saponin concentration measured in extract)/mass of medicinal material x 100%

Astragalus polysaccharide yield (%) = (volume of extract x polysaccharide concentration in the extract)/mass of medicinal material x 100%

Existing data show that the indicator components to measure the pros and cons of Astragalus extracting technology are mainly based on the yield, and the inventor thinks that the measurement index is open to question. Therefore, the most convincing indicator for evaluating the quality of the extraction process should be the "extraction rate of active ingredients of medicinal materials".

The extraction rate formula is as follows:

Extraction rate of astragalus saponin (%)=(volume of extract x saponin concentration measured in extract)/(mass of medicinal material x saponin content measured in medicinal material) x 100%

Astragalus polysaccharide extraction rate (%) = (extract volume × polysaccharide concentration measured in the extract) / (5 extract volume × concentration of astragalus polysaccharide in 5 extracts) × 100%

It was measured that the extraction rates of astragalus saponins and astragalus polysaccharides were stable above 90%.

Explanation on the transfer rate of astragalus polysaccharide:

Because the previous editions of the Pharmacopoeia have not stipulated the content standard of Astragalus polysaccharide in Astragalus medicinal materials. Therefore, the inventor only took astragalus polysaccharide as the content index, and extracted the same medicinal material 5 times. The first 2 times were extracted with 14 times the amount of 70% ethanol for 30 minutes, and the last 3 times were extracted with the same times the amount of distilled water for 40 minutes. The content of astragalus polysaccharide in the extract, the obtained data are as follows:

sequence Mass percentage of astragalus polysaccharide in each extract (%) 1 and 2 18.92 3 4.61 4 2.56 5 2.21

As can be seen from the figure, from the 3rd time, the mass percent increase of astragalus polysaccharide gradually weakened, and the mass percentage of astragalus polysaccharide in the 4th and 5th extracts was very close. Therefore, the inventor extracted five times The sum of astragalus polysaccharides is set at 100%.

Example 3 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Precisely weigh 10 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 500W, keep the temperature at 70°C, extract 3 times in total, add 118mL of 50% ethanol for the first time, and extract for 10 minutes; the second time Add 100mL of 50% ethanol solution and extract for 10min; add 100mL of distilled water for the third time and extract for 20min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 60mL, add distilled water to a 100mL volumetric flask, and use phenol-sulfuric acid method The content of astragalus polysaccharide in the extract was determined to be 1.772g, the yield was 19.05%, and the extraction rate was 67.30%; the content of total astragalus saponins was 0.067g, the yield was 0.72%, and the extraction rate was 62.88%.

Example 4 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Precisely weigh 10 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 500W, keep the temperature at 70°C, extract 3 times in total, add 138mL of 70% ethanol for the first time, and extract for 10 minutes; the second time Add 120mL of 70% ethanol solution and extract for 10min; add 120mL distilled water for the third time and extract for 20min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 60mL, add distilled water to a 100mL volumetric flask, and use phenol-sulfuric acid method The content of astragalus polysaccharide in the extract was determined to be 1.764g, the yield was 18.97%, and the extraction rate was 67.01%; the content of total astragalus saponins was 0.088g, the yield was 0.95%, and the extraction rate was 82.67%.

Example 5 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Precisely weigh 20 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 700W, keep the temperature at 70°C, extract 3 times in total, add 276mL of 70% ethanol for the first time, and extract for 20 minutes; the second time Add 240mL of 70% ethanol solution and extract for 20min; add 240mL distilled water for the third time and extract for 30min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 150mL, add distilled water to a 200mL volumetric flask, and use phenol-sulfuric acid The content of astragalus polysaccharide in the extract was determined to be 4.240g, the yield was 22.80%, and the extraction rate was 80.53%; the content of total astragalus saponins was 0.193g, the yield was 1.04%, and the extraction rate was 90.68%.

Example 6 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Accurately weigh 50 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 900W, keep the temperature at 70°C, extract 3 times in total, add 790mL of 90% ethanol for the first time, and extract for 30 minutes; the second time Add 700mL of 90% ethanol solution, extract for 30min; add 700mL of distilled water for the third time, extract for 40min, and filter the extract with a suction filter, transfer the extract for the first two times to a rotary evaporator, concentrate to a certain volume, and add the extract for the third time , concentrated to about 450mL, added distilled water and fixedly dissolved to a 500mL volumetric flask, the content of astragalus polysaccharides in the extract was measured by the phenol-sulfuric acid method to be 9.631g, the productive rate was 20.71%, and the extraction rate was 73.16%; the content of total astragalus saponins was 0.480g, the yield is 1.03%, and the extraction rate is 90.07%.

Example 7 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Precisely weigh 20 grams of astragalus powder (passed through a No. 2 sieve), put it in a microwave extraction device, microwave power 500W, keep the temperature at 70°C, extract 3 times in total, add 276mL of 70% ethanol for the first time, and extract for 20min; the second time Add 240mL of 70% ethanol solution and extract for 20min; add 240mL distilled water for the third time and extract for 30min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 150mL, add distilled water to a 200mL volumetric flask, and use phenol-sulfuric acid The content of astragalus polysaccharide in the extract was determined to be 4.550g, the yield was 24.46%, and the extraction rate was 86.41%; the content of astragalus total saponins was 0.176g, the yield was 0.94%, and the extraction rate was 82.45%.

Example 8 Extraction process of astragalus saponins and astragalus polysaccharides of the present invention

Accurately weigh 20 grams of the raw medicinal material of Astragalus membranaceus, put it in a microwave extraction device, microwave power 500W, keep the temperature at 70°C, extract 3 times in total, add 316mL of 70% ethanol for the first time, extract for 30min; add 70% ethanol solution for the second time 280mL, extract for 30min; add 280mL distilled water for the third time, extract for 40min. Put the extraction solution in a suction filtration device for suction filtration, transfer the first two extractions to a rotary evaporator, concentrate to a certain volume, add the third extraction, concentrate to about 150mL, add distilled water to a 200mL volumetric flask, and use phenol-sulfuric acid The content of astragalus polysaccharides in the extract was determined to be 4.812g, the yield was 25.87%, and the extraction rate was 91.40%; the content of astragalus total saponins was 0.204g, the yield was 1.10%, and the extraction rate was 95.65%.

By comparing and analyzing the test results of extracting astragalus polysaccharides and astragalus total saponins with different quality astragalus medicinal materials in Examples 2 to 8:

Among them, the content, yield and extraction rate of astragalus polysaccharides and total astragalus saponins in Example 8 are higher than those in other examples. Therefore, the process described in Example 8 is the best process of the present invention.

The above test proves that the extraction process of the present invention greatly improves the utilization rate of the active ingredients in the Astragalus medicinal material, increases the yield of Astragalus polysaccharide and Astragalus saponin in the Astragalus medicinal material, shortens the test time, and simplifies the extraction process steps.

Claims (6)

1. microwave-assisted extracts a technique for Radix Astragali saponin and astragalus polysaccharides, and it comprises the steps:

A, take Milkvetch Root;

B, medical material is put in microwave extraction device, microwave power 500W-900W, temperature 70 C, extracts 3 times altogether, adds the ethanol of 50%-90% the 1st time, extracts 10min-30min; Add 50%-90% ethanol the 2nd time, extract 10min-30min; The 3rd adding distil water, extracts 20min-40min;

C, the ethanol extract of the 1st, 2 times is concentrated, removes ethanol, then adds the aqueous extract of the 3rd time, mixes, concentrated, obtains Radix Astragali saponin and astragalus polysaccharide extract.

2. microwave-assisted according to claim 1 extracts the technique of Radix Astragali saponin and astragalus polysaccharides, it is characterized in that: described Milkvetch Root is the decoction pieces of pharmaceutical decocting piece or soybean grain size, or crosses the medicated powder of No. 1-3 sieve.

3. microwave-assisted according to claim 2 extracts the technique of Radix Astragali saponin and astragalus polysaccharides, it is characterized in that: the Milkvetch Root described in a step is crushed to below 24 orders.

4. microwave-assisted according to claim 1 extracts the technique of Radix Astragali saponin and astragalus polysaccharides, it is characterized in that: the ethanol described in b step or the consumption of water are 10-14 times of medical material weight.

5. microwave-assisted according to claim 1 extracts the technique of Radix Astragali saponin and astragalus polysaccharides, it is characterized in that: the ethanol that the ethanol described in b step is 70%.

6. microwave-assisted according to claim 1 extracts the technique of Radix Astragali saponin and astragalus polysaccharides, it is characterized in that: the microwave power 500-700W described in b step.