CN107550964B - Optimized extraction process and application of ageratum thistle flavone by response surface method - Google Patents
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Abstract
The invention discloses a response surface method optimized ageratum thistle flavone extraction process and application thereof, wherein according to the Box-Behnken test Design principle, Design-Expert software is utilized to Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction times of ageratum thistle flavone extraction, ultrasonic wave is adopted to assist in extracting ageratum thistle flavone, and the specific steps are as follows: drying and crushing ageratum conyzoides into powder, putting the ageratum conyzoides powder into an extraction tank, mixing the powder with an ethanol solution for ultrasonic extraction, putting an extracting solution into a rotary evaporator for reduced pressure distillation, ventilating and volatilizing a solvent, and evaporating by using a water bath to dryness to obtain an ageratum conyzoides flavone product. The process has high extraction rate, and the extracted ageratum thistle flavone has strong oxidation resistance and strong application effect in antioxidant drugs and food antioxidants.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of extraction of active ingredients of medicinal plants and food additives, and particularly relates to a response surface method optimized extraction process of ageratum thistle flavone and application thereof.
[ background of the invention ]
Ageratum Conyzoides L, also known as Ageratum Conyzoides, Bischofia scholaris, Lonicera japonica, Oldenlandia diffusa, etc., is an annual herb plant of Ageratum of Compositae
The ageratum thistle has the effects of clearing heat and removing toxicity, stopping bleeding and relieving pain, is a traditional folk medicinal plant in all countries in the world, has traditional medicinal history in Asia, Africa, south America and the like, and is mainly used for treating headache, dyspnea, skin diseases, vaginitis, pneumonia, asthma, spasm and itching, itching relieving, insect killing and the like. In southern China, the traditional Chinese medicine is mainly used for treating symptoms such as cold and fever, sore throat, carbuncle, deep-rooted carbuncle, sore and furuncle, traumatic hemorrhage and the like; the traditional Chinese medicine composition is mainly used for treating diseases such as pelvic inflammation, tonsillitis and pharyngitis in clinic and has better curative effect.
Modern pharmacological studies show that ageratum conyzoides has high biological activity in the aspects of anti-inflammation, pain relieving, fever relieving, radiation resisting, stomach protecting and the like. In order to reveal the pharmacodynamic components of the pharmacological action of ageratum conyzoides, various scholars have also studied the chemical components of ageratum conyzoides, and as a result, the chemical components of ageratum conyzoides are found to be various, and volatile oil, flavone, terpenoid, sterol, alkaloid, amino acid and the like are reported at present. The ageratum thistle volatile oil mainly contains monoterpene and sesquiterpene compounds, and has different producing areas and certain difference in the components and content of the volatile oil. 20 flavonoid compounds are separated from the flavonoid compounds, 14 flavonoid compounds are polymethoxylated flavonoid compounds, and researches of national scholars such as Hefei find that the ageratum flavonoid compounds have a strong inhibiting effect on main pathogenic bacteria in the citrus orchard, and especially the bacteriostatic activity of flavonoid molecules accumulated in the soil of the citrus orchard exceeds that of commercial bactericides. There are mainly 4 kinds of alkaloid compounds. There are also 4 kinds of triterpenes and sterols. In addition, other ingredients include sesamin (Z-sesamin), amide acetate (aurantiamide acetate), fumaric acid (fumaric acid), caffeic acid (caffeic acid), fatty acids, amino acids, vitamins A and C, etc.
The ageratum conyzoides chemical component analysis literature shows that the ageratum conyzoides contains abundant flavonoid and terpene compounds, which are the most effective components for the antioxidation of the traditional Chinese medicine, but the extraction process of ageratum conyzoides flavone and the research on the antioxidation thereof are not reported in the literature at home and abroad at present. Particularly, ageratum thistle is always treated as weed in China, and the research on ageratum thistle is only limited in the aspect of agricultural allelopathy, but the research on the efficacy of ageratum thistle is rarely related.
Ageratum has a large wild resource in the Guangxi region and is generally regarded as weed treatment at the present stage. In order to fully exploit the medicinal value of ageratum conyzoides, the extraction of ageratum conyzoides flavone and the analysis of antioxidant capacity of ageratum conyzoides are researched, and theoretical basis is provided for developing ageratum conyzoides into natural antioxidants.
[ summary of the invention ]
The invention provides a response surface method optimized extraction process and application of ageratum thistle flavone, and the specific technical scheme is as follows:
a response surface method optimizes the extraction process of ageratum conyzoides flavone, according to Box-Behnken test Design principle, Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum conyzoides flavone by using Design-Expert software, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, comprising the following process steps:
s1: drying the whole plant of ageratum conyzoides, crushing, sieving with a 20-60 mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 30-50% ethanol solution, wherein the material-liquid ratio is 1: (20-40), and carrying out cold soaking for 24 h;
s3: ultrasonic extracting cold soaked herba Agastaches powder for 20-40min for 1-3 times, filtering, and mixing extractive solutions;
s4: and (3) distilling the extracting solution in a rotary evaporator under reduced pressure, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a water bath to obtain the ageratum thistle flavone product.
Preferably, the response surface method optimizes the extraction process of ageratum conyzoides flavone, and utilizes Design-Expert software to Design and optimize the process conditions of ethanol concentration, extraction time, material-liquid ratio and extraction times of ageratum conyzoides flavone according to the Box-Behnken test Design principle, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, and the method comprises the following process steps:
s1: drying the whole ageratum conyzoides, crushing, sieving by a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours;
s3: ultrasonic extracting cold soaked herba Agastaches powder for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) distilling the extracting solution in a rotary evaporator under reduced pressure, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a water bath to obtain the ageratum thistle flavone product.
Preferably, the ageratum powder in step S2 should be shaken up every 2h during the cold soaking process.
Preferably, the temperature of the liquid during the ultrasonic extraction in step S3 is controlled to 50 to 60 ℃.
Preferably, in step S4, the rotary evaporator has a rotation speed of 120r/min, a pressure of 0.06-0.08MPa and a temperature of 70-75 ℃.
Preferably, the water bath is evaporated to dryness in step S4 to 70 ℃ water bath constant temperature.
The invention also aims to provide the application of the ageratum thistle flavone prepared by the extraction process in preparing antioxidant drugs and food antioxidants.
The antioxidant capacity of the antioxidant medicine and food antioxidant is enhanced along with the increase of the content of ageratum thistle flavone.
The antioxidant medicine and food antioxidant have scavenging ability for free radicals.
In one embodiment, the radicals include DPPH radicals and ABTS ·+A free radical.
The invention has the following beneficial effects:
(1) the pharmacological action and clinical application of ageratum conyzoides, and the research on the chemical components of ageratum conyzoides volatile oil are many, but the research on the antioxidant capacity of ageratum conyzoides is not reported. The invention takes ageratum thistle as a raw material, utilizes 30-50% ethanol solution and is assisted with ultrasonic waves to extract ageratum thistle flavone by adopting a DPPH method and ABTS+Evaluation of ageratum thistle flavone extract by phosphomolybdate methodThe antioxidant capacity of the extract provides scientific basis for the utilization of ageratum thistle resources;
(2) according to the invention, based on the Box-Behnken test Design principle, Design-Expert software is utilized to Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum thistle flavone, ultrasonic-assisted extraction of ageratum thistle flavone is adopted, the purification difficulty is low, the yield is high, the cost is low, the free radical scavenging and antioxidant capacity is high, and the application effect in antioxidant drugs and food antioxidants is strong.
[ description of the drawings ]
FIG. 1 is a graph of the effect of time gradient on flavone extraction;
FIG. 2 is a graph of the effect of ethanol concentration on flavone extraction;
FIG. 3 is a graph showing the effect of feed liquid ratio on flavone extraction;
FIGS. 4Y-f (X)1,X2) Response surface and contour plot of);
fig. 5Y ═ f (X)1,X3) The response surface and contour plot of (a);
fig. 6Y ═ f (X)1,X4) The response surface and contour plot of (a);
fig. 7Y ═ f (X)2,X3)The response surface and contour plot of (a);
fig. 8Y ═ f (X)2,X4) The response surface and contour plot of (a);
fig. 9Y ═ f (X)3,X4) The response surface and contour plot of (a);
FIG. 10 is a graph of total antioxidant capacity of ageratum thistle flavonoids;
FIG. 11 is a graph of the scavenging ability of Agastache rugosa flavone on DPPH free radicals;
FIG. 12 Agastache Rugosa thistle flavone pairs ABTS+Free radical scavenging ability.
[ detailed description ] embodiments
The following is a detailed description of specific embodiments.
Example 1:
a response surface method optimizes the extraction process of ageratum conyzoides flavone, according to Box-Behnken test Design principle, Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum conyzoides flavone by using Design-Expert software, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, comprising the following process steps:
s1: naturally drying the complete plant of ageratum conyzoides in the shade, crushing, sieving with a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours, and shaking up once every 2 hours;
s3: ultrasonic extracting cold-soaked herba Agastaches powder at 50 deg.C for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) putting the extracting solution into a rotary evaporator with the rotation speed of 120r/min, the pressure of 0.06MPa and the temperature of 70 ℃ for reduced pressure distillation, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a water bath at the constant temperature of 70 ℃ to obtain the ageratum thistle flavone product of 396 mg.
Example 2:
a response surface method optimizes the extraction process of ageratum conyzoides flavone, according to Box-Behnken test Design principle, Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum conyzoides flavone by using Design-Expert software, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, comprising the following process steps:
s1: naturally drying the complete plant of ageratum conyzoides in the shade, crushing, sieving with a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours, and shaking up once every 2 hours;
s3: ultrasonic extracting cold soaked herba Agastaches powder at 55 deg.C for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) putting the extracting solution into a rotary evaporator with the rotation speed of 120r/min, the pressure of 0.07MPa and the temperature of 72 ℃, carrying out reduced pressure distillation, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a 70 ℃ water bath at constant temperature to obtain 407mg of ageratum thistle flavone product.
Example 3:
a response surface method optimizes the extraction process of ageratum conyzoides flavone, according to Box-Behnken test Design principle, Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum conyzoides flavone by using Design-Expert software, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, comprising the following process steps:
s1: naturally drying the complete plant of ageratum conyzoides in the shade, crushing, sieving with a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours, and shaking up once every 2 hours;
s3: ultrasonic extracting cold-soaked herba Agastaches powder at 60 deg.C for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) putting the extracting solution into a rotary evaporator with the rotation speed of 120r/min, the pressure of 0.08MPa and the temperature of 75 ℃, carrying out reduced pressure distillation, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness by using a 70 ℃ water bath at constant temperature to obtain the ageratum thistle flavone product 383 mg.
Example 4:
a response surface method optimizes the extraction process of ageratum conyzoides flavone, according to Box-Behnken test Design principle, Design and optimize the process conditions of ethanol concentration, extraction time, feed-liquid ratio and extraction frequency of ageratum conyzoides flavone by using Design-Expert software, and adopts ultrasonic wave to assist in extracting ageratum conyzoides flavone, comprising the following process steps:
s1: naturally drying the complete plant of ageratum conyzoides in the shade, crushing, sieving with a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours, and shaking up once every 2 hours;
s3: ultrasonic extracting cold-soaked herba Agastaches powder at 58 deg.C for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) putting the extracting solution into a rotary evaporator with the rotation speed of 120r/min, the pressure of 0.078MPa and the temperature of 75 ℃, carrying out reduced pressure distillation, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a 70 ℃ water bath at constant temperature to obtain 415mg of ageratum thistle flavone products.
Example 5: in order to discuss the influence of single-factor extraction on the content of ageratum conyzoides flavone, and simultaneously carry out Box-Behnken test design and response surface analysis and evaluate the antioxidant capacity of ageratum conyzoides flavone, the following experiments are carried out.
Influence of single-factor extraction on content of ageratum thistle flavone
1. Effect of time on flavone content
Taking 2.0g of ageratum conyzoides powder which is sieved by a 60-mesh sieve as a raw material, adding 40% ethanol extractant according to the liquid-material ratio of 1:40, and setting different extraction time: 20. 30, 40, 50, 60 and 90 min. The flavone content was determined after extraction, and the results are shown in FIG. 1.
Before the extraction time is 30min, the flavone content in the extractive solution increases with the increase of the extraction time, and at 30min, the content is highest, and the flavone content is 46.931mg, and the yield is reduced. This is because the flavone structure is destroyed or oxidized and polymerized to be lost due to the prolonged extraction time. Therefore, the examination was continued with the extraction time of 30min as a subsequent test.
2. Effect of ethanol volume fraction on flavone content
Extracting with 30, 40, 50, 60, 70, 80, and 95% ethanol respectively for 30 min. The flavone content was measured after extraction, and the results are shown in FIG. 2.
As can be seen from FIG. 2, the highest content of 65.485mg is obtained when the ethanol concentration is 40%, and the content is reduced with the increase of the concentration, so that herba Agastaches powder sieved with 60 mesh sieve is used as raw material, and different ethanol concentrations are added according to the ratio of 1: 40. In order to reduce the cost and the difficulty of subsequent concentration and purification, the ethanol concentration is selected to be 40%.
3. Influence of feed liquid ratio on flavone content
2.0g of ageratum powder which is sieved by a 60-mesh sieve is taken as a raw material, 40% ethanol is used according to different material-liquid ratios: extracting at 1:10, 1:15, 1:20, 1:30, 1:40, and 1:50 for 30min, and measuring flavone content after extraction, with the result shown in FIG. 3.
As can be seen from FIG. 3, before the feed-liquid ratio is 1:30, the flavone content increases with the increase of the feed-liquid ratio, and the highest content is 75.857mg at 1: 30; while the trend of the flavone content rising after 1:30 is not obvious. Therefore, in combination with the influence of other single factors, the feed-liquid ratio is selected to be 1:30 in order to reduce the cost and the difficulty of subsequent concentration and purification.
4. Influence of extraction times on flavone content
Taking 2.0g of ageratum conyzoides powder which is sieved by a 60-mesh sieve as a raw material, fixing the material-liquid ratio of 1:40, controlling the ethanol concentration to be 40%, controlling the extraction time to be 30min, and investigating the influence of the extraction frequency on the flavone content, wherein the result is shown in table 1, and the flavone content is slightly increased after 2-time extraction, so that the extraction frequency is selected to be 3 times for reducing the cost and the difficulty of subsequent concentration and purification.
Table 1: influence of extraction frequency on flavone extraction
| Number of extractions/n | 1 | 2 | 3 |
| Flavone content/mg | 43.110 | 84.571 | 87.118 |
Second, Box-Behnken test design and response surface analysis
In order to optimize the technological conditions for extracting the flavone from the ageratum thistle, the extraction conditions are optimized by adopting a four-factor three-level response surface analysis method on the basis of a single-factor test according to the Box-Behnken test design principle: precisely weighing 2.0g of ageratum thistle sample in a triangular flask, and selecting ethanol concentration (X)1) Extraction time (X)2) Ratio of material to liquid (X)3) Number of times of extraction (X)4) Four factors which have great influence on the extraction rate of the effective components of ageratum conyzoides, and response surface analysis is carried out on the extraction process, and specific test schemes and results are shown in tables 2 and 3.
Table 2: response surface test design factor level gauge
Table 3: response surface test design and results
1. Model establishment and significance test thereof
According to the data in the table 3, a Design Expert 7.0 software is used for carrying out multiple regression fitting analysis to obtain the predicted value (Y) of the yohimbine extraction amount extracted by ultrasonic assistance to the independent variable ethanol volume fraction (X)1) Extraction time (X)2) Ratio of material to liquid (X)3) Number of times of extraction (X)4) The quadratic multiple regression equation of (1) is as follows:
Y＝155.649-4.0597·X1-0.96123·X2-4.34823·X3-11.2577·X4+0.0556·X1·X2+0.01542·X1·X3+0.60842·X1·X4-0.0429·X2·X3+0.11893·X2·X4+0.0133·X1 2+0.1006·X3 2-2.5156·X4 2
the results of regression model equation coefficients, analysis of variance, and significance testing of factors according to the test results of table 3 are shown in table 4.
Table 4: regression model significance test
Note: very significant differences, p < 0.01; the difference is significant, p is less than 0.05
From the results of ANOVA, Table 4 shows that F is 3.24 and p is 0.0177 (p) in the mathematical model of regression equation for the extraction of ageratum thistle flavone<0.05), indicating that the fit of the regression model equation is significant. Coefficient of determination R of regression model equation2Adjusting the correlation coefficient R as 0.90132 Adj0.8018, which indicates that the fitting degree of the model equation and the test data is high, the error of the test group is small, so the model equation can be completely used for the analysis and prediction guidance of the ageratum thistle flavone ultrasonic-assisted extraction result.
Meanwhile, as can be seen from the results of the anova in Table 4, the feed-liquid ratio and the number of extraction times have a significant influence on the extraction amount of flavone in the first term (p)<0.01 or p<0.05), other factors have no significant influence; in the second order, the ratio of liquid to feed (C)2) Reach a very significant level (p)<0.01); in interactive items, the effect is not significant (p)>0.05), suggesting that the interaction between the factors is not significant. According to the F value, the influence of all factors on the extraction amount of the flavone is sequentially C (material-liquid ratio) > D (extraction times) > A (ethanol concentration) > B (extraction time).
2. Response surface analysis and optimization
And (3) performing quadratic multivariate fitting by using Design Expert 7.0 software to obtain a response surface curve of a quadratic regression equation, and investigating the influence of interaction of other two factors on the extraction amount (Y) of the ageratum thistle flavone under the condition that the level values of the other two factors are fixed to be zero, wherein the obtained response surface is shown in figures 4-9. If the gradient of one response curved surface is relatively flat, the response curved surface shows that the change of the response curved surface is relatively small along with the change of the processing conditions; whereas a steeper slope of a response surface indicates a greater change in response value with changing process conditions.
As can be seen from FIG. 5, FIG. 7 and FIG. 9, the slope of the response surface is steeper, indicating that the interaction between the feed-liquid ratio and the ethanol concentration, the feed-liquid ratio and the extraction time, and the feed-liquid ratio and the extraction frequency has a greater influence on the flavone yield; the density of the contour lines can be judged, and the influence of the feed liquid on the response value is larger than that of ethanol concentration, extraction time and extraction times; as can be seen from fig. 4, 6 and 8, the slope of the response surface is gentle, the interaction between the ethanol concentration and the extraction time, and the interaction between the ethanol concentration and the extraction frequency have little influence on the flavone yield, and it can be determined from the density of the contour lines that the influence of the extraction frequency on the response value is greater than the ethanol concentration, and the influence of the ethanol concentration on the response value is greater than the extraction time. In summary, the influence of the feed liquid ratio on the flavone yield is the largest, the extraction times are the lowest, and the influence of the extraction time is the smallest; and the flavone content is increased along with the increase of the feed-liquid ratio and the extraction times.
3. Determination of optimal conditions and validation of models
Optimizing optimal conditions in an experimental range by using the established mathematical model, wherein the ethanol concentration is 48.04%, the extraction time is 23.9min, and the material-liquid ratio is 1: 40; the extraction times are 3; under the condition, the extraction amount of flavone from ageratum thistle by ultrasonic assistance is 427.03 mg. Considering actual operation conditions, correcting the conditions to 48% ethanol concentration, 24min extraction time and 1:40 feed-liquid ratio; the number of extractions was 3. The conditions are used for carrying out a verification test, 3 times of parallel tests are carried out, and the test result shows that the average value of the flavone is 415mg by using 2g of ageratum thistle, compared with the theoretical predicted value, the relative error is about 2.81 percent, and the optimization result is reliable.
And thirdly, evaluating the oxidation resistance of ageratum thistle flavone.
1. Determination of total antioxidant capacity of ageratum thistle flavone
The optimal extraction conditions obtained by response surface analysis are utilized to extract ageratum conyzoides flavone, and the obtained ageratum conyzoides flavone product is prepared into the following series of solutions: 5mg/ml, 10mg/ml, 15mg/ml, 20mg/ml, 25mg/ml, 30mg/ml, 35mg/ml, etc., and the above-mentioned series of solutions were subjected to tests for the antioxidant ability of ageratum conyzoides flavone, and the results are shown in FIG. 10.
As can be seen from FIG. 10, the total antioxidant capacity of ageratum conyzoides flavone is strong, and the total antioxidant capacity is increased with the increase of the concentration of ageratum conyzoides flavone.
2. Clearance rate of ageratum thistle flavone on DPPH free radical
The optimal extraction conditions obtained by response surface analysis are utilized to extract ageratum conyzoides flavone, and the obtained ageratum conyzoides flavone product is prepared into the following series of solutions: 5mg/ml, 10mg/ml, 15mg/ml, 20mg/ml, 25mg/ml, 30mg/ml, 35mg/ml, and the above-mentioned series of solutions were subjected to DPPH radical scavenging ability test, and the results are shown in FIG. 11.
As can be seen from FIG. 11, the Agastache rugosa flavone has strong DPPH clearance, half clearance is 22.78mg/ml, and the clearance (clearance) increases with the concentration of Agastache rugosa flavone.
3. Agastache rugosus flavone pairs ABTS+Clearance rate of free radical
The optimal extraction conditions obtained by response surface analysis are utilized to extract ageratum conyzoides flavone, and the obtained ageratum conyzoides flavone product is prepared into the following series of solutions: 5mg/ml, 10mg/ml, 15mg/ml, 20mg/ml, 25mg/ml, 30mg/ml, 35mg/ml, and processing the above series of solutions into ABTS ·+The results of the radical scavenging ability test are shown in FIG. 12.
As can be seen from FIG. 12, ageratum conyzoides flavone has stronger ABTS+The free radical scavenging ability, and the scavenging ability (clearance rate) is enhanced with the increase of the concentration of ageratum conyzoides flavone.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A response surface method optimizes the extraction process of ageratum thistle flavone, which is characterized in that: according to the Box-Behnken test Design principle, Design and optimization of technological conditions of ethanol concentration, extraction time, material-liquid ratio and extraction times of ageratum thistle flavone extraction by using Design-Expert software and ultrasonic-assisted extraction of ageratum thistle flavone are adopted, and the method comprises the following technological steps:
s1: drying the whole plant of ageratum conyzoides, crushing, sieving with a 20-60 mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 30-50% ethanol solution, wherein the material-liquid ratio is 1: (20-40), and carrying out cold soaking for 24 h;
s3: ultrasonic extracting cold soaked herba Agastaches powder for 20-40min for 1-3 times, filtering, and mixing extractive solutions;
s4: and (3) distilling the extracting solution in a rotary evaporator under reduced pressure, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a water bath to obtain the ageratum thistle flavone product.
2. The response surface method for optimizing the extraction process of ageratum thistle flavonoids according to claim 1, wherein the response surface method comprises the following steps: according to the Box-Behnken test Design principle, Design and optimization of technological conditions of ethanol concentration, extraction time, material-liquid ratio and extraction times of ageratum thistle flavone extraction by using Design-Expert software and ultrasonic-assisted extraction of ageratum thistle flavone are adopted, and the method comprises the following technological steps:
s1: drying the whole ageratum conyzoides, crushing, sieving by a 60-mesh sieve, and weighing 2.0g of ageratum conyzoides powder for later use;
s2: placing ageratum thistle powder into an extraction tank, adding 48% ethanol solution, wherein the material-liquid ratio is 1:40, cold soaking for 24 hours;
s3: ultrasonic extracting cold soaked herba Agastaches powder for 24min for 3 times, filtering, and mixing extractive solutions;
s4: and (3) distilling the extracting solution in a rotary evaporator under reduced pressure, recovering the solvent, volatilizing the solvent in a fume hood, and evaporating to dryness in a water bath to obtain the ageratum thistle flavone product.
3. The response surface method for optimizing the extraction process of ageratum thistle flavonoids according to claim 1 or 2, wherein the response surface method comprises the following steps: in the cold soaking process of the ageratum conyzoides powder in the step S2, the ageratum conyzoides powder should be uniformly shaken every 2 h.
4. The response surface method for optimizing the extraction process of ageratum thistle flavonoids according to claim 1 or 2, wherein the response surface method comprises the following steps: the temperature of the feed liquid during the ultrasonic extraction in step S3 is controlled to 50 to 60 ℃.
5. The response surface method for optimizing the extraction process of ageratum thistle flavonoids according to claim 1 or 2, wherein the response surface method comprises the following steps: in step S4, the rotation speed of the rotary evaporator is 120r/min, the pressure is 0.06-0.08MPa, and the temperature is 70-75 ℃.
6. The response surface method for optimizing the extraction process of ageratum thistle flavonoids according to claim 1 or 2, wherein the response surface method comprises the following steps: and in the step S4, the water bath is evaporated to dryness at the constant temperature of 70 ℃.
7. Use of ageratum conyzoides flavone prepared by the extraction process according to any one of claims 1-6 in the preparation of antioxidant drugs and food antioxidants.
8. Use according to claim 7, characterized in that: the antioxidant capacity of the antioxidant drugs and food antioxidants is enhanced with the increase of the content of ageratum conyzoides flavone prepared by the extraction process of any one of claims 1 to 6.
9. Use according to claim 7, characterized in that: the antioxidant medicine and food antioxidant have scavenging ability for free radicals.
10. Use according to claim 9, characterized in that: the radicals include DPPH radical and ABTS ·+A free radical.
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| CN109771460B (en) * | 2019-03-27 | 2021-07-27 | 安徽中医药大学 | Method for optimizing and extracting total flavonoids in fresh cotton flowers by response surface method |
| CN110037203B (en) * | 2019-05-17 | 2022-10-14 | 内江师范学院 | Agastache rugosus extract, application of ageratum conyzoides extract in fish feed, fish feed and preparation method of fish feed |
| CN114555104A (en) * | 2019-08-14 | 2022-05-27 | Ge营养有限公司 | Herbal preparation for stimulating hair growth, controlling hair loss, dandruff and infections thereof using ageratum species |
| CN112251044B (en) * | 2020-11-13 | 2021-11-16 | 安顺职业技术学院 | Response surface method optimized hotbed chives pigment extraction process and application thereof |
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