CN113648371A - Extraction and clarification process of medicinal and edible radix astragali extract medicinal tea - Google Patents
Extraction and clarification process of medicinal and edible radix astragali extract medicinal tea Download PDFInfo
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Abstract
The invention discloses an extraction and clarification process of medicinal and edible mountain astragalus essence medicinal tea, which specifically comprises the following steps: (1) weighing radix astragali, rhizoma Polygonati, Corni fructus, rhizoma Dioscoreae and rhizoma Polygonati Odorati in equal amount, and mixing well to obtain radix astragali extract medicinal tea; (2) adding water with the mass being 12 times that of the radix astragali fine medicinal tea, decocting for three times, and combining the three decoctions; (3) concentrating to obtain radix astragali extract medicinal tea extractive solution; (4) adding 10 times of water, placing into a water bath kettle, adding chitosan solution, stirring, standing, centrifuging, and collecting filtrate to obtain the final product. The method has good extraction and clarification effects and stable and feasible process, can ensure that the liquid medicine becomes transparent and bright, retains the effective components to the maximum extent, and provides experimental basis for the later extraction and clarification of the radix astragali extract medicinal tea.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, in particular to an extraction and clarification process of a medicine and food dual-purpose radix astragali extract medicinal tea.
Background
The radix astragali fine medicinal tea consists of five medicines of radix astragali, Chinese yam, dogwood, rhizoma polygonati and radix polygonati officinalis, and is an empirical prescription for clinical health care and health preservation of project teams. Wherein, the astragalus root has the functions of tonifying qi and invigorating yang, and reinforcing the defensive system and consolidating the exterior, and can be used for treating all deficiency and deficiency as a long tonic; the Chinese yam has the effects of tonifying qi and yin and tonifying spleen, lung and kidney; corni fructus has effects of invigorating liver and kidney, astringing, relieving depletion, warming middle warmer, expelling cold, and eliminating turbid pathogen, and can be used for treating diabetes; both Huang Jing and Yu Zhu are yin-nourishing herbs, so they can nourish yin and resist aging after long-term administration. The components supplement each other, so that the radix astragali extract medicinal tea has the effects of reducing blood sugar and improving diabetic complications.
However, no relevant report is found in the prior art on how to extract and clarify the radix astragali extract medicinal tea.
Disclosure of Invention
In view of the above, the invention aims to provide an extraction and clarification process of a medicinal and edible radix astragali extract medicinal tea, so as to solve the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an extraction and clarification process of medicinal and edible mountain astragalus extract medicinal tea specifically comprises the following steps:
(1) weighing radix astragali, rhizoma Polygonati, Corni fructus, rhizoma Dioscoreae and rhizoma Polygonati Odorati in equal amount, and mixing well to obtain radix astragali extract medicinal tea;
(2) adding water with the mass being 12 times of that of the radix astragali fine medicinal tea, decocting for three times, and combining the three decoctions to obtain radix astragali fine medicinal tea decoction;
(3) concentrating the decoction of the radix astragali fine herbal tea to obtain an radix astragali fine herbal tea extract, namely completing the extraction process of the radix astragali fine herbal tea;
(4) adding 10 times of water into the extract of the radix astragali fine medicinal tea, putting into a water bath kettle, adding the chitosan solution, stirring, standing, centrifuging, and collecting the filtrate to obtain the radix astragali fine medicinal tea clear liquid, thus finishing the clarification process of the radix astragali fine medicinal tea.
Further, in the step (2), the decoction time for three times of decoction is 1h, 40min and 40min respectively.
Further, in the above step (3), the mixture was concentrated to a concentration of 2.22 g/mL.
Further, in the step (4), the temperature of the water bath is 80 ℃.
Further, in the step (4), the chitosan solution has a mass concentration of 1% and is added in an amount of 0.2 g/L.
Further, in the step (4), the stirring time is 5 min.
Further, in the step (4), the time for standing was 0.5 hour.
Further, in the step (4), the rotation speed of the centrifugation is 4000r/min, and the time is 15 min.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a heating reflux method to extract the effective components in the radix astragali extract medicinal tea, uses water as a solvent for extraction, and has the advantages of low price, easy obtaining, safety, no toxicity and extraction of most of medicinal material effective components; in addition, the polysaccharide as a polar chemical component has the characteristics of being easily soluble in water and insoluble in alcohol, so that the polysaccharide structure is not easily changed and the environment is not polluted by using water as an extraction solvent.
2. According to verification, under the extraction process, the total polysaccharide content is 79.99mg/g on average, the total saponin content is 2.93mg/g on average, the dry paste yield is 51.25% on average, the water extraction effect is good, the process is stable and feasible, and an experimental basis is provided for the extraction of the radix astragali extract medicinal tea.
3. After the radix astragali fine medicinal tea is extracted, the liquid is turbid, and in consideration of the characteristics of no toxicity, effectiveness, convenience, low cost and good stability of a finished product of a flocculating agent method, a chitosan solution is selectively added to clarify an extracting solution.
4. According to verification, under the clarification process, the light transmittance is 80.60% on average, the saponin content is 1.27mg/10g on average, the solid removal rate is 13.15% on average, the clarification effect is good, the process is stable and feasible, the liquid medicine can be transparent, the effective components are retained to the maximum extent, and an experimental basis is provided for clarification of the radix astragali refined medicinal tea.
Drawings
FIG. 1 is a glucose standard curve diagram in the process of extracting radix astragali extract medicinal tea; FIG. 2 is a standard curve diagram of ursolic acid in the process of extracting radix astragali extract medicinal tea; FIG. 3 is a glucose standard curve diagram in a process of clarifying SHANQIJINGYAOCHA; FIG. 4 is a standard curve diagram of ursolic acid in the process of clarifying SHANQIJING medicated tea; FIG. 5 shows the effect of chitosan addition on the clarification effect of SHANQIJINGYAO tea extract; FIG. 6 shows the effect of the liquid medicine on the clarification effect of the extract of SHANQIJINGYAO tea; FIG. 7 is a graph showing the effect of stirring time on the clarification effect of the extract of the radix astragali extract herbal tea; FIG. 8 shows the effect of flocculation temperature on clarification effect of SHANQIJINGYAO tea extract; FIG. 9 shows the effect of standing time on the clarification effect of the extract of radix astragali extract herbal tea.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The extraction and clarification process of the medicinal and edible mountain astragalus extract medicinal tea specifically comprises the following steps:
(1) weighing 2kg of radix astragali, rhizoma polygonati, dogwood, Chinese yam and radix polygonati officinalis respectively, and uniformly mixing to obtain the radix astragali extract medicinal tea;
(2) adding 12 times of water into the radix astragali fine medicinal tea, decocting for three times (1h, 40min and 40min respectively), and mixing the three decoctions to obtain radix astragali fine medicinal tea decoction;
(3) concentrating the decoction of the radix astragali fine herbal tea to the concentration of 2.22g/mL to obtain the radix astragali fine herbal tea extract, namely completing the extraction process of the radix astragali fine herbal tea;
(4) adding 10 times of water by mass into the extract of the radix astragali fine medicinal tea, putting into a water bath kettle at 80 ℃, adding 0.2g/L of chitosan solution with the mass concentration of 1%, stirring for 5min, standing for 0.5h, centrifuging at 4000r/min for 15min, collecting the filtrate to obtain the radix astragali fine medicinal tea clear liquid, and finishing the clarification process of the radix astragali fine medicinal tea.
Performance testing
A process for extracting radix astragali extract medicinal tea
1 laboratory apparatus and device
1.1 the specific instruments, models and manufacturers of the experiments are shown in Table 1.
TABLE 1 Instrument usage record
Instrument for measuring the position of a moving object | Model number | Manufacturer of the product |
Digital display constant temperature electric heating jacket | HWM-1000 | Jie Rui Electrical appliances Co., Ltd, King Tan City |
Digital display constant temperature water bath | HH-2 | Jie Rui Electrical appliances Co., Ltd, King Tan City |
Ultrasonic cleaning machine | SB-800DTD | NINGBO SCIENTZ BIOTECHNOLOGY Co.,Ltd. |
Ultraviolet visible spectrophotometer | UV-6100S | SHANGHAI METASH INSTRUMENTS Co.,Ltd. |
Electric heating constant temperature blast air drying box | DHG-9075 type A | SHANGHAI YIHENG INSTR Co.,Ltd. |
Analytical balance | AB135-5 type | Tianjin Hui Ke instruments and Equipment Co Ltd |
Analytical balance | FA2104 | Shanghai sperm balance |
Mini centrifuge of trace | FC5306 | OHAUS INSTRUMENT (CHANGZHOU) Co.,Ltd. |
Vortex oscillator | MX-5 | Shanghai Bajiu industries Ltd |
Low-speed centrifuge | LC-4012 | ANHUI USTC ZONKIA SCIENTIFIC INSTRUMENTS Co.,Ltd. |
Freeze dryer | SCIENTZ-12N | NINGBO SCIENTZ BIOTECHNOLOGY Co.,Ltd. |
1.2 the specific reagents, grades and manufacturers of the experiments are shown in Table 2.
TABLE 2 reagent usage records
Reagent | Manufacturer of the product |
95% ethanol | Tianjin City Suzuki-Kogyo Tech Co Ltd |
Methanol | Tianjin chemical reagent Co Ltd |
N-butanol | Kaiton chemical reagent Co., Ltd, Tianjin City |
Sulfuric acid | TIANJIN KERMEL CHEMICAL REAGENT Co.,Ltd. |
Glacial acetic acid | Tianjin chemical reagent Co Ltd |
Vanillin | TIANJIN KWANGFU FINE CHEMICAL INDUSTRY Research Institute |
Anthracene ketones | Jiangsu Shipu auxiliary agent factory |
Sodium hydroxide | Sengchang reagent factory of Sengchang Industrial and trade Co Ltd, Tianjin City |
Perchloric acid | Tianjin Xin Yuan chemical Co., Ltd |
Ursolic acid (110742 baking 201622) | China Institute for food and drug control |
Anhydrous glucose | Tianjin City of TianjinWind vessel chemical reagent science and technology Limited |
1.3 Experimental drugs
Sealwort (produced in Hunan), pulp of dogwood fruit (produced in Shanxi), rhizoma dioscoreae (produced in Henan), polygonatum odoratum (produced in Hunan) and astragalus root (produced in Gansu) are all purchased from drug sources and trade company Limited in Anguo city.
2 methods and results
2.1 preparation of test articles
Weighing 3g of each of radix astragali, rhizoma polygonati, radix polygonati officinalis, Chinese yam and dogwood, adding a proper amount of water into a round-bottom flask, heating, refluxing and extracting, concentrating and drying an extracting solution, and grinding into powder.
2.2 ultraviolet-visible spectrophotometry for determining total polysaccharide content in extract
2.2.1 preparation of test solutions
Precisely weighing 0.1g of powder under the item of 2.1, adding 0.5mL of water to dissolve the powder, uniformly swirling on a vortex oscillator, adding 5mL of 95% ethanol, uniformly shaking and centrifuging (the rotating speed is 3500, the centrifuging time is 3min), discarding supernatant, dissolving the precipitate into a 25mL measuring flask by using distilled water, and continuously adding the solution to a scale mark to obtain the product.
2.2.2 preparation of control solutions
Weighing 20mg of glucose powder in a 100mL volumetric flask by using an analytical balance, adding distilled water to dissolve the glucose powder and fixing the volume to a scale mark to obtain a reference substance solution with the concentration of 0.205 mg/mL.
2.2.3 selection of the wavelength of maximum absorption
Sucking the test solution and the reference solution by a pipette with 0.15mL respectively into 10mL of dry and clean test tubes with stoppers, adding distilled water to complement to 1mL, slowly adding 0.2% anthrone-sulfuric acid solution with 2mL in an ice water bath, keeping the temperature of a water bath kettle at 100 ℃ for 10min, cooling in the ice water bath for 10min, using the distilled water as a blank, carrying out full-wavelength scanning by an instrument, and setting the scanning range to be 200-700 nm.
The results showed that the sample solution and the glucose-free control solution both had maximum absorption at 628nm, so that 628nm was used as the absorption wavelength for absorbance measurement.
2.2.4 methodology investigation
2.2.4.1 standard curve drawing
0.1mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL, and 0.9mL of the control solutions were pipetted into 10mL of dry and clean test tubes with stoppers, 1mL of the control solutions was made up with distilled water, and 0.2% anthrone-sulfuric acid solution was added to develop color in accordance with the method under "2.2.3" with distilled water as a blank, and the absorbance value was measured at 628 nm. A standard curve (ordinate: absorbance A, abscissa: concentration C) was plotted, as shown in FIG. 1.
FIG. 1 is a glucose standard curve diagram in the process of extracting radix astragali extract medicinal tea. As can be seen from FIG. 1, the standard curve equation for glucose is: a 22.76C-0.0144(r 0.9949) indicating that glucose is in a good linear relationship with absorbance a in the range of 0.0068-0.0615 mg/mL.
2.2.4.2 examination of precision
0.5mL of the control solution was pipetted into a dry clean stoppered tube, developed with 0.2% anthrone-sulfuric acid solution by the method under "2.2.3" and then absorbance was measured, and the measurement was repeated 6 times to calculate the relative standard deviation (RSD value). The results are shown in Table 3.
TABLE 3 results of the precision test
Number of |
1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD(%) |
A | 0.709 | 0.708 | 0.709 | 0.708 | 0.708 | 0.708 | 0.7083 | 0.072 |
As is clear from Table 3, the absorbance values did not change much, indicating that the precision of the instrument used was good.
2.2.4.3 stability examination
0.1mL of the test solution under the term "2.2.1" was pipetted, and then the absorbance was measured after coloring by adding 0.2% anthrone-sulfuric acid solution according to the method under the term "2.2.3" and 1 time per 2 hours, and the RSD value was calculated. The results are shown in Table 4.
TABLE 4 stability test results
Time (h) | 0 | 2 | 4 | 6 | 8 | 10 | 12 | Mean value | RSD(%) |
A | 0.618 | 0.619 | 0.594 | 0.612 | 0.595 | 0.587 | 0.600 | 0.603 | 2.106 |
As can be seen from Table 4, the change in the absorbance value was small, indicating that the stability of the sample solution was good within 12 hours.
2.2.4.4 repeatability test
6 parts of the sample solution was prepared by the method under "2.2.1", 0.1mL of each sample solution was pipetted into a dry tube with a stopper, and 0.2% anthrone-sulfuric acid solution was added to the sample solution to develop color and measure absorbance by the method under "2.2.3", and the RSD value was calculated. The results are shown in Table 5.
TABLE 5 results of the repeatability tests
As can be seen from Table 5, the absorbance values did not change much, indicating that the reproducibility of the method of the present invention was good.
2.2.4.5 investigation of sample recovery
6 parts of dry paste powder of the shanqi extract medicinal tea with known total polysaccharide content are weighed by an analytical balance, each part is about 0.1g, a glucose reference substance (the preparation concentration is 25mL of solution containing 0.205mg of glucose per milliliter, each part is 2.7mL) is added according to the content of a sample and the amount of a standard substance (1:1), a test sample solution is prepared according to the item of '2.2.1', the absorbance is measured according to the item of '2.2.3', and the recovery rate and the RSD value are calculated. The results are shown in Table 6.
Table 6 sample recovery rate test results (n ═ 6)
As can be seen from Table 6, the average recovery rate was 99.70%, indicating that the method of the present invention is excellent in accuracy.
2.2.5 determination of samples
Precisely transferring 0.1mL of the test solution, adding distilled water to complement to 0.6mL, slowly adding 1.2mL of newly-prepared 0.2% anthrone-sulfuric acid solution into a beaker filled with ice water, shaking up, keeping the temperature in a water bath kettle at 100 ℃ for 10min, carrying out ice water bath for 10min, taking distilled water as a blank, and measuring the absorbance value at 628 nm.
2.3 ultraviolet-visible spectrophotometry for determining total saponin content in extract
2.3.1 preparation of test solutions
Taking 0.5g of powder under the item of 2.1, precisely weighing, adding 10mL of distilled water for dissolving, extracting 30mL of water saturated n-butyl alcohol for three times, combining n-butyl alcohol layers, eluting the n-butyl alcohol layer with 1% sodium hydroxide solution for 2 times, taking the n-butyl alcohol layer, evaporating the n-butyl alcohol layer on a water bath kettle to dryness, adding methanol for dissolving, and fixing the volume to a 2mL measuring flask to obtain the product.
2.3.2 preparation of control solutions
Weighing 2mg of ursolic acid by using an analytical balance, adding methanol into a 5mL volumetric flask for dissolving, and fixing the volume to a scale mark to obtain a reference substance solution with the concentration of 0.4 mg/mL.
2.3.3 selection of the wavelength of maximum absorption
Sucking 0.25mL of the test solution and 0.25mL of the reference solution by a pipette, respectively putting the test solution and the reference solution into a dry test tube with a plug, heating in a water bath to volatilize methanol, adding 0.1mL of newly-configured 5% vanillin-glacial acetic acid solution and 0.4mL of perchloric acid, shaking up, keeping the temperature in the water bath at 60 ℃ for 40min, putting the test solution and the reference solution into a beaker filled with ice water, cooling to room temperature, adding 2.5mL glacial acetic acid, shaking up, taking a corresponding reagent as a blank, and scanning with the instrument at the full wavelength, wherein the range is set to 200-700 nm.
The results show that the test solution and the ursolic acid control solution have maximum absorption at 538nm, so 538nm is used as the absorption wavelength of the absorbance.
2.3.4 methodology investigation
2.3.4.1 standard curve drawing
0.2mL, 0.4mL, 0.6mL, 0.8mL, 1.0mL, 1.2mL of the control solution was pipetted into a 10mL dry clean stoppered tube, heated in a water bath to evaporate the methanol, developed with vanillin-perchloric acid according to the procedure under "2.3.3" using the corresponding reagent blank as a reference, and measured for absorbance at 538 nm. A standard curve (ordinate: absorbance A, abscissa: concentration C) was plotted, as shown in FIG. 2.
Fig. 2 is a standard curve diagram of ursolic acid in the process of extracting the radix astragali extract medicinal tea. As can be seen from FIG. 2, the standard curve equation of ursolic acid is: a-7.0786C +0.0538 (r-0.9995), indicating a good linear relationship of ursolic acid to absorbance a in the range of 0.0281-0.1688 mg/mL.
2.3.4.2 examination of precision
0.25mL of the control solution was pipetted into a dry clean stoppered tube, developed by adding vanillin-perchloric acid according to the method of "2.3.3" and measured for absorbance, and the RSD value was calculated by conducting parallel measurements 6 times. The results are shown in Table 7.
TABLE 7 results of the precision test
Number of |
1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD(%) |
A | 0.977 | 0.977 | 0.974 | 0.973 | 0.974 | 0.974 | 0.9748 | 0.1613 |
As is clear from Table 7, the absorbance values did not change much, indicating that the precision of the instrument used was good.
2.3.4.3 stability examination
0.25mL of the test solution was pipetted into a dry clean stoppered tube, stained with vanillin-perchloric acid in the method of "2.3.3" and absorbance was measured, and the RSD value was calculated every 2 hours. The results are shown in Table 8.
TABLE 8 stability test results
Time (h) | 0 | 2 | 4 | 6 | 8 | 10 | 12 | Mean value | RSD(%) |
A | 0.533 | 0.530 | 0.526 | 0.526 | 0.530 | 0.528 | 0.531 | 0.529 | 0.493 |
As can be seen from Table 8, the change in the absorbance value was small, indicating that the stability of the sample solution was good within 12 hours.
2.3.4.4 repeatability test
6 parts of the test solution was prepared by the method of "2.3.1", 0.25mL of the test solution was pipetted into a dry and clean test tube with a stopper, and the solution was colored with vanillin-perchloric acid by the method of "2.3.3" and then absorbance was measured to calculate the RSD value. The results are shown in Table 9.
TABLE 9 results of the repeatability tests
As can be seen from Table 9, the change in absorbance was not large, indicating that the reproducibility of the method of the present invention was good.
2.3.4.5 investigation of sample recovery
6 parts of dry paste powder of the shanqi extract medicinal tea with known total saponin content are weighed by an analytical balance, each part is about 1g, an ursolic acid reference substance (the preparation concentration is 10mL of a solution containing 0.4mg of ursolic acid per milliliter and 1mL of each part is added) is added according to the content and the standard quantity (1:1) in a sample, a test sample solution is prepared according to the item '2.3.1', the absorbance is measured according to the method under the item '2.3.3', and the recovery rate and the RSD are calculated, and the result is shown in a table 10.
TABLE 10 recovery rate of sample application test results (n ═ 6)
As can be seen from Table 10, the average recovery rate was 100.1%, indicating that the method of the present invention is excellent in accuracy.
2.3.5 determination of samples
Sucking 0.25mL of sample solution into a dry and clean test tube with a plug by using a pipette, heating in a water bath to volatilize methanol, adding 0.1mL of newly-prepared 5% vanillin-glacial acetic acid solution and 0.4mL of perchloric acid solution, uniformly mixing, keeping the temperature of a water bath kettle at 60 ℃ for 40min, putting the mixture into a small beaker with ice water, cooling the temperature to room temperature, adding 2.5mL of glacial acetic acid, shaking uniformly, taking a corresponding reagent as a blank, and measuring the absorbance at 538 nm.
2.4 study of extraction Process of Shanqi extract medicinal tea
The extraction rate of Chinese medicinal materials is affected by the ratio of materials to liquids, soaking time, decocting time and decocting times. The invention aims to determine the optimal extraction process of the radix astragali extract medicinal tea, and determine the suitable extraction process parameters of the radix astragali extract medicinal tea through single factor and orthogonal test design. The influence of the water addition amount, the decoction time and the decoction times on the extraction of the radix astragali extract medicinal tea is examined by taking water as a solvent, and the examination indexes are respectively the dry extract yield, the total polysaccharide content and the total saponin content.
2.4.1 Single factor investigation
2.4.1.1 Effect of water addition on Dry extract yield, Total polysaccharide content and Total Saponin content
4 parts of astragalus, rhizoma polygonati, dogwood, Chinese yam and polygonatum which form the radix astragali fine medicinal tea are weighed and respectively added with 6 times, 8 times, 10 times and 12 times of water to be decocted for 1 hour and 1 time. The results are shown in Table 11.
TABLE 11 influence of water addition on dry extract yield, total polysaccharide content and total saponin content
Adding water (times) | Dry extract yield (%) | Total polysaccharide content (mg) | Total saponins content (mg) |
6 | 30.39 | 39.61 | 2.094 |
8 | 33.79 | 45.39 | 1.980 |
10 | 36.99 | 49.48 | 2.359 |
12 | 38.53 | 52.78 | 2.462 |
As can be seen from Table 11, the yield of dry extract and the total polysaccharide content increased with the increase of water addition, the total saponin content increased in the case of 8-10 times the water addition amount, and tended to be gentle in the case of 10-12 times the water addition amount. Thus, 12 times of water is the optimal water adding amount.
2.4.1.2 influence of decoction times on dry extract yield, total polysaccharide content and total saponin content
4 parts of astragalus, rhizoma polygonati, dogwood, Chinese yam and polygonatum which form the radix astragali fine medicinal tea are weighed and respectively decocted for 1 time, 2 times, 3 times and 4 times with 10 times of water, and each time lasts for 1 hour. The results are shown in Table 12.
TABLE 12 influence of the number of decocts on the yield of dry extract, the content of total polysaccharides and the content of total saponins
As can be seen from table 12, the total polysaccharide content and the total saponin content increased with the increase of the number of times of decoction, and the rising trend was significant 1-3 times, the rising trend was slow after three times, and the total saponin content in the extract decreased after three times of decoction. The change of the yield of the total polysaccharide and the yield of the total saponin is not obvious along with the increase of the decocting times. The yield of the dry paste can also be obtained by decocting for three times, and the yield of the paste is not changed greatly. Thus, the optimal number of times of decoction is three times.
2.4.1.3 influence of decoction time on dry extract yield, total polysaccharide content and total saponin content
4 parts of astragalus, rhizoma polygonati, dogwood, Chinese yam and radix polygonati officinalis which form the radix astragali fine medicinal tea are weighed and added with 10 times of water to be respectively decocted for 0.5, 1, 1.5 and 2 hours, and the decoction is respectively decocted for 1 time. The results are shown in Table 13.
TABLE 13 influence of decoction time on dry extract yield, total polysaccharide content and total saponin content
Time of decoction (h) | Dry extract yield (%) | Total polysaccharide content (mg) | Total saponins content (mg) |
0.5 | 25.55 | 33.33 | 1.392 |
1 | 29.32 | 41.03 | 1.791 |
1.5 | 30.36 | 41.88 | 1.978 |
2 | 31.91 | 40.09 | 1.977 |
As can be seen from Table 13, the rising trend between 0.5 and 1 hour was large; after 1h, the trend of rising is very slow, probably because the balance among the dry extract yield, the total polysaccharide content and the total saponin content is reached in 1 h. Thus, 1h is the optimal decoction time.
2.4.2 orthogonal design experiments
The optimal extraction process of the radix astragali fine medicinal tea is obtained by screening four-factor three-level orthogonal experiments including water addition amount, decoction times, blank and decoction time by taking water as an extraction solvent.
The orthogonal design experiments are shown in table 14.
TABLE 14 orthogonal test factor level table
The orthogonal experimental design is examined by looking at factor A, B, C, D. The results of the visual analysis of the orthogonal experiments are shown in Table 15.
TABLE 15 visual analysis results of orthogonal experiments
As is clear from Table 15, test group 6A3B3D2Is the best process combination for extracting the radix astragali extract medicinal tea. The different levels of the factors have the sequence of A3>A2>A1,B3>B2>B1,D2>D3>D1I.e. A3B3D2Is the best combination.
Results of the analysis of variance in the orthogonal experiments are shown in tables 16-18.
TABLE 16 results of analysis of variance of orthogonal experiments (Total polysaccharide)
Sources of variance | Sum of squares of deviation | Degree of freedom | F ratio | Critical value of F | Significance of |
A | 135.142 | 2 | 75.71 | 19 | * |
B | 1937.162 | 2 | 1085.245 | 19 | * |
C | 1.785 | 2 | 1 | 19 | |
D | 105.637 | 2 | 59.18 | 19 | * |
Error of the measurement | 1.78 | 2 |
TABLE 17 results of analysis of variance in orthogonal experiments (Total saponins)
Sources of variance | Sum of squares of deviation | Degree of freedom | F ratio | Critical value of F | Significance of |
A | 0.908 | 2 | 1.348 | 6.94 | |
B | 1.262 | 2 | 1.874 | 6.94 | |
C | 0.712 | 2 | 1.057 | 6.94 | |
D | 0.635 | 2 | 0.943 | 6.94 | |
Error of the measurement | 1.35 | 4 |
TABLE 18 results of analysis of variance in orthogonal experiments (dry extract yield)
Sources of variance | Sum of squares of deviation | Degree of freedom | F ratio | Critical value of F | Significance of |
A | 55.935 | 2 | 2.469 | 6.94 | |
B | 290.218 | 2 | 12.813 | 6.94 | * |
C | 29.785 | 2 | 1.315 | 6.94 | |
D | 15.517 | 2 | 0.685 | 6.94 | |
Error of the measurement | 45.3 | 4 |
From tables 16-18, it can be seen that factor B (number of times of decoction) is the main factor affecting the extraction rate of the radix astragali extract tea, factor a (amount of water added) is the number of times of decoction, and factor D (time of decoction) has little effect. In visual analysis, both theoretical combination and actual measurement show that3B3The extraction is best at the horizontal level. Comprehensively considering the extraction rate of the radix astragali extract medicinal tea, the material-liquid ratio is 112(12mL water/1 g crude drug), and decocting in water for three times (1h, 40min, 40min) to obtain the best extraction process combination of the radix astragali extract medicinal tea.
2.4.3 validation experiments
According to the preparation method of the radix astragali extract medicinal tea, the astragalus, the rhizoma polygonati, the dogwood, the Chinese yam and the polygonatum are weighed by an analytical balance, 12 times of water is added, the mixture is decocted for three times (1h, 40min and 40min), an extracting solution is concentrated and dried to obtain the weight of dry paste, the dry paste is ground into fine powder at low temperature, the absorbance values are measured according to the methods of 2.2.3 and 2.3.3, and the total polysaccharide content and the total saponin content are calculated. The results are shown in Table 19.
Table 19 verifies the results of the experiments
Numbering | Dry extract yield (%) | Total polysaccharide content (mg/g) | Total saponins content (mg/g) |
1 | 51.4 | 80.12 | 2.97 |
2 | 51.1 | 79.86 | 2.88 |
Mean value of | 51.25 | 79.99 | 2.93 |
As shown in Table 19, the total polysaccharide content, total saponin content and dry extract yield averaged 79.99mg/g, 2.93mg/g and 51.25%, respectively.
Second, clarification process research of radix astragali extract medicinal tea
1 laboratory apparatus and device
1.1 the specific instruments, models and manufacturers of the experiments are shown in Table 20.
TABLE 20 Instrument usage records
Instrument for measuring the position of a moving object | Manufacturer of the product |
UV-6100S ultraviolet visible spectrophotometer | METASH Shanghai Meta analytical instruments Ltd |
HH-2 digital display constant temperature water bath | Jie Rui Electrical appliances Co., Ltd, King Tan City |
DHG-9075A type electric heating constant-temperature air-blast drying oven | SHANGHAI YIHENG INSTR Co.,Ltd. |
Model AB135-5 analytical balance | Tianjin Hui Ke instruments and Equipment Co Ltd |
LC-4012 low-speed centrifuge | ANHUI USTC ZONKIA SCIENTIFIC INSTRUMENTS Co.,Ltd. |
MX-5 vortex oscillator | Shanghai Bajiu industries Ltd |
SB-800DTD ultrasonic cleaning machine | NINGBO SCIENTZ BIOTECHNOLOGY Co.,Ltd. |
1.2 the specific reagents, grades and manufacturers of the experiments are shown in Table 21.
TABLE 21 record of reagent use
1.3 Experimental drugs
Sealwort (produced in Hunan), pulp of dogwood fruit (produced in Shanxi), rhizoma dioscoreae (produced in Henan), polygonatum odoratum (produced in Hunan) and astragalus root (produced in Gansu) are all purchased from drug sources and trade company Limited in Anguo city.
2. Method and results
2.1. Preparation of extractive solution of radix astragali extract medicinal tea
About 4500mL of the radix astragali extract herbal tea extract prepared in the step (3) of the embodiment 1 is taken for standby.
2.2 preparation of Chitosan solution
100mL of 1% acetic acid solution is mixed with 1g of chitosan powder which is precisely weighed to obtain 1% chitosan acetic acid solution.
2.3 clarity determination
Taking one part of the liquid before and after the extract of the radix astragali extract medicinal tea is clarified, and scanning the liquid with a UV-6100S ultraviolet-visible spectrophotometer at full wavelength, wherein the range is set to be 200-800nm, the absorbance is smaller and the absorption curve is gentle in the range of the wavelength above 600nm, and therefore, the detection wavelength of the light transmittance of the extract of the radix astragali extract medicinal tea is determined to be 670 nm.
Using water as blank, taking appropriate sample solution to measure absorbance value A at 670nm, and using T% for light transmittance (T%: 10)-A) And (4) showing. Higher values of T% indicate better clarification results.
2.4 determination of polysaccharide content
2.4.1 preparation of the solution
0.5mL of the extract of the radix astragali extract medicinal tea is sucked by a pipette, 5mL of 95% ethanol is added, centrifugation is carried out, the precipitate is dissolved in 5mL volumetric flask with water, and water is sucked by a rubber-tipped dropper to a scale mark, thus obtaining a test solution.
Weighing glucose (40785) and 20.5mg powder with an analytical balance, dissolving in 100mL volumetric flask with water, and sucking water with rubber-tipped dropper to scale line to obtain control solution (0.205mg/mL) to obtain control solution.
500mL of sulfuric acid was added to 1.0g of anthrone (40785powder) weighed out on an analytical balance, and a 0.2% sulfuric acid-anthrone solution was obtained after standing, followed by preparation.
2.4.2 selection of the wavelength of maximum absorption
0.1mL of each of the test solution and the reference solution is sucked by a pipette, distilled water is added to a constant volume of 0.6mL, 1.2 mL0.2% sulfuric acid-anthrone solution is dripped into a beaker filled with ice blocks, the mixture is uniformly shaken and placed into a 100 ℃ water bath kettle for 10min, the mixture is taken out, the temperature is reduced for 10min, the distilled water is used as a blank, full-wavelength scanning is carried out at 200-700nm, the absorption curve of the polysaccharide is obtained, and the detection wavelength of the polysaccharide is determined to be 628 nm.
2.4.3 methodology investigation
2.4.3.1 drawing of Standard Curve
0.1mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL, 0.9mL to 6mL of the control solution in a clean test tube, supplementing 1mL with distilled water, dropping 2mL of 0.2% sulfuric acid-anthrone solution in ice water, shaking uniformly, placing in a 100 ℃ water bath for 10min, taking out, cooling for 10min, using distilled water as a blank, and measuring the absorbance value at 628 nm. The concentrations and absorbances of the controls are shown in Table 22.
TABLE 22 Absorbance against glucose control concentration
Group of | 1 | 2 | 3 | 4 | 5 | 6 |
Concentration (mg/mL) | 0.0068 | 0.0136 | 0.0273 | 0.041 | 0.0547 | 0.0615 |
A | 0.194 | 0.243 | 0.606 | 0.919 | 1.17 | 1.445 |
The absorbance of the control solution was set as the ordinate and the concentration was set as the abscissa to draw a standard curve, as shown in FIG. 3.
FIG. 3 is a glucose standard curve diagram in the process of clarifying SHANQIJINGYAO tea. As can be seen from FIG. 3, the standard curve equation for glucose is: y 22.76 x-0.0144.
2.4.3.2 precision investigation
0.5mL of the control solution under the term "2.4.1" was pipetted, the absorbance was measured in the manner under the term "2.4.2", and the RSD value was calculated after repeating the measurement 6 times. The results are shown in Table 23.
TABLE 23 results of the precision experiments
Serial number | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Mean value | RSD(%) |
A | 0.709 | 0.708 | 0.709 | 0.708 | 0.708 | 0.708 | 0.708 | 0.072 |
As is clear from Table 23, the absorbance values did not change much, indicating that the precision of the instrument used was good.
2.4.3.3 stability examination
0.1mL of the test solution under the item "2.4.1" was pipetted, and the absorbance was measured in the manner under the item "2.4.2" every 2 hours to calculate the RSD value. The results are shown in Table 24.
TABLE 24 stability test results
Time (h) | 0 | 2 | 4 | 6 | 8 | 10 | 12 | Mean value | RSD(%) |
A | 0.612 | 0.600 | 0.595 | 0.587 | 0.618 | 0.594 | 0.619 | 0.603 | 2.106 |
As can be seen from Table 24, the change in the absorbance value was small, indicating that the stability of the sample solution was good within 12 hours.
2.4.3.4 repeatability test
0.1mL of 6 test solutions under the term "2.4.1" was pipetted, and the absorbance was measured in the manner under the term "2.4.2" to calculate RSD, and the results are shown in Table 25.
TABLE 25 results of the repeatability tests
As can be seen from Table 25, the absorbance values did not vary much, indicating that the reproducibility of the method of the invention was good.
2.4.3.5 sample recovery test
6 parts of the extract of the mountain astragalus root extract tea with known polysaccharide content, each part of which is 0.5mL, are pipetted by a pipette, glucose reference substances (50 mL of glucose reference substance solution with the preparation concentration equal to about 0.205mg/mL and 5mL of glucose reference substance solution for each part) are added according to the amount that the sample content is 1:1, the sample solution is prepared according to the method under the item '2.4.1', and the absorbance, the recovery rate and the RSD are measured according to the method under the item '2.4.2', and the results are shown in a table 26.
Table 26 sample recovery rate experimental results (n ═ 6)
As can be seen from Table 26, the average recovery rate was 100.05%, indicating that the method of the present invention is excellent in accuracy.
2.4.4 sample determination
Taking 0.5mL of the radix astragali extract medicinal tea extract before and after clarification, adding 5mL of 95% ethanol, centrifuging, dissolving the precipitate in a 5mL volumetric flask with water, and sucking water to the scale mark by using a rubber-tipped dropper. 0.1mL of each sample solution is sucked by a pipette, distilled water is added to the volume of 0.6mL, 1.2mL of 0.2% sulfuric acid-anthrone solution is dropwise added into a beaker filled with ice blocks, the mixture is uniformly shaken and placed into a 100 ℃ water bath kettle for 10min, the mixture is taken out, the temperature is reduced for 10min, then distilled water is used as a blank, and the absorbance value is measured at 628 nm.
2.5 determination of the Saponin content
2.5.1 preparation of the solution
Adding 10mL of distilled water into the dry extract powder of 0.5g of the extracting solution weighed by an analytical balance, extracting with 30mL of water saturated n-butanol for three times, eluting the n-butanol layer with 20mL of 1% sodium hydroxide solution for 2 times, evaporating the n-butanol layer to dryness on a boiling water bath, dissolving with methanol and supplementing 2mL to obtain a sample solution.
Weighing 1mg ursolic acid with an analytical balance, dissolving into a 1mL volumetric flask with methanol, and sucking methanol to scale marks with a rubber head dropper to obtain a control solution.
Weighing 1.0g vanillin \40785powderwith analytical balance, dissolving with 20mL glacial acetic acid to obtain 5% vanillin-glacial acetic acid solution, and making into final product.
2.5.2 selection of the wavelength of maximum absorption
Sucking 0.25mL of the reference solution and the sample solution into a clean test tube by a pipette respectively, evaporating to dryness in a boiling water bath, dripping 0.1mL of 5% vanillin-glacial acetic acid solution and 0.4mL of perchloric acid, placing in a water bath kettle at 60 ℃ for 40min, placing in ice water for returning to the temperature, adding 2.5mL of glacial acetic acid, shaking uniformly, and scanning at 200-700nm with a corresponding reagent as a blank at full wavelength to obtain an absorption curve of the saponin, thereby finding out the maximum absorption wavelength of the saponin as 538 nm.
2.5.3 methodology investigation
2.5.3.1 preparation of Standard Curve
Dissolving 2mg ursolic acid weighed by an analytical balance with methanol, fixing the volume to a 5mL volumetric flask, sucking 0.2mL, 0.4mL, 0.6mL, 0.8mL and 1.0mL into a clean test tube by a pipette, evaporating to dryness on a boiling water bath, dripping 0.1mL 5% vanillin-glacial acetic acid solution and 0.4mL perchloric acid, placing in a 60 ℃ water bath for 40min, then placing ice cubes in water for returning to the temperature, adding 2.5mL glacial acetic acid, shaking uniformly, and measuring the absorbance value by taking a corresponding reagent as a blank at 538 nm. The concentrations and absorbances of the controls are shown in Table 27.
TABLE 27 Absorbance corresponding to Ursolic acid control concentration
Group of | 1 | 2 | 3 | 4 | 5 | 6 |
Concentration (mg/mL) | 0.0281 | 0.0563 | 0.0844 | 0.1125 | 0.1407 | 0.1688 |
A | 0.252 | 0.457 | 0.661 | 0.832 | 1.042 | 1.261 |
The absorbance of the control solution was set as the ordinate and the concentration was set as the abscissa to draw a standard curve, as shown in FIG. 4.
Fig. 4 is a standard curve diagram of ursolic acid in the process of clarifying the radix astragali extract medicinal tea. As can be seen from FIG. 4, the standard curve equation of ursolic acid is: 7.0786 x-0.0538.
2.5.3.2 examination of precision
0.25mL of the control solution was pipetted under the term "2.5.1", and the absorbance was measured by the method under the term "2.5.2" for 6 times to calculate the RSD value. The results are shown in Table 28.
TABLE 28 precision results
Serial number | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Mean value | RSD(%) |
A | 0.977 | 0.977 | 0.974 | 0.973 | 0.974 | 0.974 | 0.975 | 0.161 |
As is clear from Table 28, the absorbance values did not change much, indicating that the precision of the instrument used was good.
2.5.3.3 stability examination
0.25mL of the test solution under the term "2.5.1" was pipetted, and the absorbance was measured in the same manner as under the term "2.5.2" every 2 hours to calculate RSD, and the results are shown in Table 29.
TABLE 29 stability test results
Time (h) | 0 | 2 | 4 | 6 | 8 | 10 | 12 | Mean value | RSD(%) |
A | 0.528 | 0.530 | 0.530 | 0.526 | 0.531 | 0.533 | 0.526 | 0.529 | 0.493 |
As can be seen from Table 29, the change in the absorbance value was small, indicating that the stability of the sample solution was good within 12 hours.
2.5.3.4 repeatability test
0.25mL of 6 test solutions under the term "2.5.1" was pipetted, and the absorbance was measured in the manner under the term "2.5.2" to calculate RSD, and the results are shown in Table 30.
TABLE 30 results of the repeatability tests
As can be seen from Table 30, the absorbance values did not change much, indicating that the reproducibility of the method of the present invention was good.
2.5.3.5 sample recovery test
6 parts of the radix astragali extract medicinal tea extract dry paste powder with known saponin content are weighed by an analytical balance, each part is 1g, the content of a standard sample is 1:1, an ursolic acid reference substance (25 mL of solution with the concentration being equal to 0.4mg/mL is added, 3.3mL is added for each part) is added, a test sample solution is prepared according to the method under the item '2.5.1', the absorbance, the recovery rate and the RSD are measured according to the method under the item '2.5.2', and the result is shown in a table 31.
TABLE 31 sample recovery test results (n ═ 6)
As can be seen from Table 31, the average recovery rate was 99.86%, indicating that the method of the present invention is excellent in accuracy.
2.5.4 sample determination
Sucking 0.25mL of a test sample solution into a clean test tube by a pipette, evaporating to dryness on a boiling water bath, dripping 0.1mL of 5% vanillin-glacial acetic acid solution and 0.4mL of perchloric acid, placing in a water bath kettle at 60 ℃ for 40min, placing ice cubes in the water for returning to the temperature, adding 2.5mL of glacial acetic acid, uniformly shaking, taking a corresponding reagent as a blank, and measuring the absorbance value at 538 nm.
2.6 measurement of solid removal Rate
Respectively weighing 20mL of the radix astragali extract medicinal tea extract before and after adding the chitosan solution, placing in a 65 ℃ oven, drying to constant weight, precisely weighing the mass, and calculating the solid content clearance rate.
The solid removal rate (mass of solid before adding chitosan solution-mass of solid after adding chitosan solution)/mass of solid before adding chitosan solution x 100%.
2.7 clarification Process investigation of extractive solution of radix astragali extract medicated tea with chitosan
2.7.1 Single factor test
2.7.1.1 examination of the amount of Chitosan added
Adding 20mL of the radix astragali extract medicinal tea extract and the medicinal liquid with the water ratio of 1:10 into a 50mL beaker, parallelly processing 5 parts, respectively adding 1% chitosan solution according to the amount of 0, 0.2g/L, 0.4g/L, 0.8g/L and 1.2g/L at normal temperature, stirring for 5min, standing at room temperature for 0.5h, centrifuging at the rotating speed of 4000r/min for 15min, packaging the filtrates together, and measuring 4 indexes. The results are shown in FIG. 5.
FIG. 5 shows the effect of chitosan addition on the clarification effect of SHANQIJINGYAO tea extract. As can be seen from FIG. 5, the transmittance and the solid removal rate increased with the increase of the chitosan addition, and the transmittance has a peak value at 0.8 g/L; with the increase of the addition amount of the chitosan, the polysaccharide content and the saponin content are in a descending trend; after 0.4g/L, the decline tends to be gentle. Therefore, the addition amount of chitosan has a great influence on the flocculation clarification effect. Comprehensively, the addition amount of the chitosan is properly selected to be 0.2 g/L.
2.7.1.2 investigation of liquid-drug ratio
Preparing 20mL of 5 liquid medicines with different proportions, namely 1:1, 1:2, 1:5, 1:10 and 1:20(g/mL), respectively putting the liquid medicines into 50mL beakers, adding 1% chitosan solution in an amount of 0.2g/L at indoor temperature, stirring for 5min, putting the liquid medicines indoors for 0.5h, centrifuging for 15min at the rotating speed of 4000r/min, putting the filtrates together, and measuring 4 indexes. The results are shown in FIG. 6.
FIG. 6 shows the effect of the liquid medicine on the clarification effect of the extract of SHANQIJINGYAO tea. As can be seen from FIG. 6, the transmittance is in an increasing trend with the decreasing ratio of the liquid medicine, the increasing trend is obvious between 1:2 and 1:5, and the trend is gradually reduced after 1: 5; the saponin content rises first and then falls, and a peak value exists at a position of 1: 10; along with the reduction of the liquid-medicine ratio, the solid clearance rate is reduced, and the content of polysaccharide is not changed greatly. Therefore, the effect of clarifying the liquid medicine is greatly influenced than that of clarifying the liquid medicine. Comprehensively, the ratio of the liquid medicine to the liquid medicine is more suitable to be selected to be 1: 10.
2.7.1 examination of the stirring time
Taking 20mL of liquid medicine with the liquid medicine ratio of 1:10, putting the liquid medicine into a 50mL beaker, carrying out parallel treatment for 2 parts, adding 1% chitosan solution in an amount of 0.2g/L at indoor temperature, respectively stirring for 1min and 10min, putting the liquid medicine in the chamber for 0.5h, centrifuging the liquid medicine for 15min at the rotating speed of 4000r/min, putting the filtrate together, and measuring 4 indexes. The results are shown in FIG. 7.
FIG. 7 shows the effect of stirring time on the clarification effect of the extract of SHANQIJINGYAO tea. As can be seen from fig. 7, the solid removal rate decreased with the increase of the stirring time, and the light transmittance, polysaccharide content and saponin content did not change much. Therefore, the stirring time has little influence on the flocculation clarification effect. Comprehensively considering, the stirring time is suitably selected to be 5 min.
2.7.1.4 investigation of flocculation temperature
Taking 20mL of liquid medicine with the liquid medicine ratio of 1:10, putting the liquid medicine into a 50mL beaker, parallelly processing 4 parts, respectively adding 0.2g/L of chitosan solution into a water bath kettle with the temperature of 20 ℃, 40 ℃, 60 ℃ and 80 ℃, stirring for 5min, placing the mixture indoors for 0.5h, centrifuging the mixture for 15min at the rotating speed of 4000r/min, putting the filtrate together, and measuring 4 indexes. The results are shown in FIG. 8.
FIG. 8 shows the effect of flocculation temperature on clarification effect of SHANQIJINGYAO tea extract. As can be seen from fig. 8, as the flocculation temperature increases, the light transmittance and the solid removal rate decrease, the polysaccharide content and the saponin content increase, and the saponin content increases significantly at a flocculation temperature of 80 ℃. Therefore, the flocculation temperature has a great influence on the flocculation clarification effect. In comprehensive consideration, the flocculation temperature is suitably selected to be 80 ℃.
2.7.1.5 examination of standing time
Taking 20mL of liquid medicine with the liquid medicine ratio of 1:10, putting the liquid medicine into a 50mL beaker, parallelly processing 2 parts, adding 1% chitosan solution in an amount of 0.2g/L at indoor temperature, stirring for 5min, respectively putting the liquid medicine in the chamber for 0.5h and 1h, centrifuging for 15min at the rotating speed of 4000r/min, putting the filtrates together, and measuring 4 indexes. The results are shown in FIG. 9.
FIG. 9 shows the effect of standing time on the clarification effect of the extract of radix astragali extract herbal tea. As can be seen from fig. 9, as the standing time is prolonged, the light transmittance, the polysaccharide content, the saponin content, and the solid removal rate are not significantly changed, so the standing time has little influence on the flocculation clarification effect. Comprehensively considering, the standing time is properly selected to be 0.5 h.
2.7.2 Cross-testing preferred Chitosan clarification Process
Analyzing the result of single-factor investigation, designing four-factor three-level orthogonal test including chitosan addition, liquid medicine ratio, blank and water bath temperature, and screening to obtain the optimal clarification process of the radix astragali extract medicinal tea extract.
The factors and levels of the orthogonality test are shown in Table 32.
TABLE 32 orthogonal test factors and horizon table
The detailed operation and visual analysis results of the orthogonal test are shown in Table 33.
TABLE 33 orthogonal test arrangement and results
As can be seen from table 33, the influence degree of each factor on the experimental results is: b > A > D, wherein A1>A2>A3、B3>B2>B1、D3>D2>D1。
The results of the anova are shown in table 34.
TABLE 34 results of ANOVA
From table 34, it can be seen that factor B (drug-to-liquid ratio) is the main factor affecting the clarification effect of the extract of the radix astragali extract herbal tea, and factor a (chitosan addition) is inferior, and factor D (flocculation temperature) is less affected. As described above, test group 3A1B3D3The method is an optimal clarification process combination of the radix astragali extract medicinal tea extract, namely the chitosan addition amount is 0.2g/L, the medicinal liquid ratio is 1:10, and the flocculation temperature is 80 ℃.
2.7.3 verification experiment
Taking 20mL of liquid medicine with the liquid medicine ratio of 1:10, putting the liquid medicine into a 50mL beaker, parallelly processing 3 parts, adding 1% chitosan solution according to the amount of 0.2g/L into a water bath kettle at the temperature of 80 ℃, stirring for 5min, standing at the indoor temperature for 0.5h, centrifuging at the rotating speed of 4000r/min for 15min, putting the filtrate together, and measuring 4 indexes. The results are shown in Table 35.
Table 35 verifies the results of the experiments
As can be seen from Table 35, the average light transmittance was 80.60%, the average saponin content was 1.27mg/10g, and the average solid removal rate was 13.15% in the clarification process.
Claims (10)
1. An extraction and clarification process of medicinal and edible mountain astragalus extract medicinal tea is characterized by comprising the following steps:
(1) weighing radix astragali, rhizoma Polygonati, Corni fructus, rhizoma Dioscoreae and rhizoma Polygonati Odorati in equal amount, and mixing well to obtain radix astragali extract medicinal tea;
(2) adding water with the mass being 12 times of that of the radix astragali fine medicinal tea, decocting for three times, and combining the three decoctions to obtain radix astragali fine medicinal tea decoction;
(3) concentrating the decoction of the radix astragali fine herbal tea to obtain an radix astragali fine herbal tea extract, namely completing the extraction process of the radix astragali fine herbal tea;
(4) adding 10 times of water into the extract of the radix astragali fine medicinal tea, putting into a water bath kettle, adding the chitosan solution, stirring, standing, centrifuging, and collecting the filtrate to obtain the radix astragali fine medicinal tea clear liquid, thus finishing the clarification process of the radix astragali fine medicinal tea.
2. The extraction and clarification process of radix astragali refined herb tea as both medicine and food according to claim 1, wherein in the step (2), the decoction time for three times of decoction is 1h, 40min and 40min respectively.
3. The extraction and clarification process of radix astragali extract medicinal tea as claimed in claim 1, wherein in step (3), the concentration is 2.22 g/mL.
4. The extraction and clarification process of the medicinal and edible radix astragali extract medicinal tea as claimed in claim 1, wherein in step (4), the temperature of the water bath kettle is 80 ℃.
5. The extraction and clarification process of radix astragali extract medicinal tea as both medicine and food according to claim 1, wherein in step (4), the mass concentration of the chitosan solution is 1%.
6. The extraction and clarification process of radix astragali extract medicinal tea as both medicine and food according to claim 5, wherein in step (4), the addition amount of the chitosan solution is 0.2 g/L.
7. The extraction and clarification process of the radix astragali extract medicinal tea used as both medicine and food according to claim 1, wherein in the step (4), the stirring time is 5 min.
8. The extraction and clarification process of the medicinal and edible radix astragali extract medicinal tea as claimed in claim 1, wherein in the step (4), the standing time is 0.5 h.
9. The extraction and clarification process of the medicinal and edible radix astragali extract medicinal tea as claimed in claim 1, wherein in step (4), the rotation speed of the centrifugation is 4000 r/min.
10. The extraction and clarification process of radix astragali extract medicinal tea as claimed in claim 9, wherein in step (4), the centrifugation time is 15 min.
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