CN105267275B - A kind of extraction method of flavonoids in chrysanthemum - Google Patents
A kind of extraction method of flavonoids in chrysanthemum Download PDFInfo
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- CN105267275B CN105267275B CN201510664230.2A CN201510664230A CN105267275B CN 105267275 B CN105267275 B CN 105267275B CN 201510664230 A CN201510664230 A CN 201510664230A CN 105267275 B CN105267275 B CN 105267275B
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- 244000189548 Chrysanthemum x morifolium Species 0.000 title claims description 137
- 238000000605 extraction Methods 0.000 title abstract description 15
- 229930003935 flavonoid Natural products 0.000 title abstract description 8
- 150000002215 flavonoids Chemical class 0.000 title abstract description 8
- 235000017173 flavonoids Nutrition 0.000 title abstract description 8
- 239000000284 extract Substances 0.000 claims abstract description 57
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- 238000000034 method Methods 0.000 claims abstract description 35
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Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
本发明属于食品与医药技术领域，具体涉及一种菊花中黄酮的提取方法。本发明的提取黄酮的步骤如下：取干燥均匀的菊花粉碎过筛后得到菊花粉末，采用乙醇与水的混合物加热回流进行提取，加水浓缩后即为菊花的提取液；继续加入丙酮提取，超声波处理，回收溶剂，剩余溶液通过大孔吸附树脂后，收集洗脱液并进行浓缩干燥，得到菊花的黄酮提取物。本发明提取菊花中黄酮的方法结合回流、超声、大孔吸附树脂辅助手段，控制简单，方便操作，提高了提取效率，有效去除杂质成分，为开发品质优良的抗氧化、延衰老、防癌的食品和药品奠定基础。The invention belongs to the technical field of food and medicine, and particularly relates to a method for extracting flavonoids from chrysanthemums. The steps of extracting flavonoids of the present invention are as follows: take dry and uniform chrysanthemum flowers, crush and sieve them to obtain chrysanthemum flower powder, use a mixture of ethanol and water to heat and reflux for extraction, add water and concentrate to obtain the chrysanthemum flower extract; continue to add acetone for extraction, and ultrasonically treat , the solvent is recovered, and after the remaining solution passes through the macroporous adsorption resin, the eluate is collected and concentrated and dried to obtain the flavonoid extract of chrysanthemum. The method for extracting flavonoids from chrysanthemum in the present invention combines reflux, ultrasonic and macroporous adsorption resin auxiliary means, has simple control and convenient operation, improves the extraction efficiency, effectively removes impurity components, and is for the development of high-quality anti-oxidation, anti-aging and anti-cancer drugs. Food and medicine lay the foundation.
Description
Technical Field
The invention belongs to the technical field of food and medicine, and particularly relates to a method for extracting flavone from chrysanthemum.
Background
Chrysanthemum is the capitate inflorescence of perennial herb of Compositae, is mostly used as tea, and can also be used as medicine or food additive. The most abundant and main bioactive component in chrysanthemum is flavonoid, which is a general name of derivatives taking 2-phenyl chromone as a basic component. The flavonoids separated from flos Chrysanthemi include luteolin, apigenin, quercetin, hesperetin, myricetin, etc. Toxicity tests show that the chrysanthemum and the extract thereof are safe and nontoxic, and the flavone compounds have wide biological activity and pharmacological actions, such as antioxidation, anti-aging, cancer prevention, blood fat reduction, cholesterol reduction, cardiovascular and cerebrovascular protection, pain relief, immunity regulation and the like.
Hangzhou white chrysanthemum (Hangzhou white chrysanthemum)Chrysanthemum Morifolium Ramat.) The chrysanthemum or chrysanthemum has white flower color, faint fragrance, clear soup color and slightly bitter taste, and is worthy of being named as 'West lake Longjing, Hangzhou tribute chrysanthemum'. Modern scientific research proves that the chrysanthemum morifolium ramat has wide biological activity in the aspects of oxidation resistance, virus resistance, tumor inhibition and the like.
With the social progress and the improvement of the living standard of people, the safety of food and medicine is more and more concerned. The substitution of harmful synthetic substances by natural active ingredients with certain biological functions extracted from plants has become a research hotspot in the food and medicine world, for example, large-area planting of marigold (with flavonoids as the main ingredient) in the united states has been carried out instead of antibiotics.
Chinese patent No. CN201310025359.X adopts water extraction method to extract various water-soluble components in chrysanthemum such as chlorogenic acid, flavone, volatile oil, amino acid, polysaccharide, trace elements, etc., and although the used extraction solvent has low cost and does not cause organic solvent residue, the obtained extract has complex components and low yield.
At present, the process for extracting the flavone from the chrysanthemum morifolium ramat has a certain research foundation in China, but is limited to one to two conventional extraction processes, such as common extraction solvents used in an aqueous extraction method, low cost, little pollution and low flavone yield; the organic solvent extraction method has the disadvantages of high cost of solvents such as methanol, acetonitrile, ethyl acetate and the like, toxicity of most organic solvents, environmental pollution, solvent residue in the obtained product and hidden danger of utilization of the product in food and medicines.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method for extracting flavone from chrysanthemum, which has the advantages of safe and simple process, high yield, low cost and capability of effectively removing impurity components, aiming at the defects of the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: pulverizing and sieving dried flos Chrysanthemi to obtain flos Chrysanthemi powder;
2) solvent extraction: weighing flos Chrysanthemi powder, adding extractant I, heating and reflux extracting for 2 times, each for 3 hr, mixing 2 times of extractive solutions, filtering, concentrating the filtrate in 75 deg.C water bath by rotary evaporation, adding distilled water, and concentrating to obtain concentrated solution I;
3) ultrasonic extraction: adding an extracting agent II into the chrysanthemum extracting solution I, carrying out ultrasonic treatment for 10min, extracting for 3 times, combining the extracting solutions, and recovering the solvent, wherein the residual solution is the chrysanthemum extracting solution II;
4) and (3) purification: after the chrysanthemum extracting solution II passes through macroporous adsorption resin at the flow rate of 1-10 mL/min, eluting by using an eluent, and collecting the eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying under vacuum to obtain flos Chrysanthemi flavone extract.
The flos Chrysanthemi is flos Chrysanthemi.
The granularity of the chrysanthemum powder in the step 1 is 20-300 meshes.
In the step 2, the extracting agent I is a mixture of ethanol and water. The volume of the ethanol in the mixture of the ethanol and the water is 50-99% of the mixing volume of the ethanol and the water.
In the step 3, the extractant II is petroleum ether. The boiling point of the petroleum ether is 30-60 ℃.
The ultrasonic treatment in the step 3 is carried out under the conditions that the ultrasonic power is 200-800W and the ultrasonic frequency is 20-40 kHz.
The macroporous adsorption resin is an organic polymer adsorbent with good adsorption performance and no ionic group, has a good macroporous network structure and a large specific surface area, can selectively adsorb organic matters from a solution through physical adsorption, and has different adsorption performance and adsorption condition parameters due to different physicochemical properties of compounds. The macroporous adsorption resin can be divided into three types of non-polarity, medium polarity and polarity according to the difference of polarity and the molecular structure of the selected monomer. The macroporous adsorption resin in the step 4 is a spherical nonpolar adsorbent, and the macroporous adsorption resin is styrene type macroporous adsorption resin.
The eluent in the step 4 is pure ethanol.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention combines reflux, ultrasonic and macroporous adsorption resin auxiliary means through twice extraction, and has simple extraction mode control and convenient operation.
2. The extraction method of the invention has the flavone yield of more than 8 percent, solves the problems of low flavone yield, large reagent dosage, high cost, large pollution and the like when the conventional single method is used for extraction, improves the extraction efficiency and effectively removes impurity components.
3. The invention lays a foundation for developing antioxidant, anti-aging and cancer-preventing foods and medicines with excellent quality by starting with the natural plant resource chrysanthemum morifolium ramat.
Detailed Description
In order to better understand the present invention, the following examples are further provided to clearly illustrate the contents of the present invention, but the contents of the present invention are not limited to the following examples.
Example 1
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 95% ethanol, heating and refluxing for extraction for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 2
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 3
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 50% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 4
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 1mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 5
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 10mL/min, ethanol is adopted for elution, and an eluent is collected;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 6
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through AB-8 macroporous adsorption resin at the flow rate of 5mL/min, ethanol is adopted for elution, and eluent is collected;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 7
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through DM-130 macroporous adsorption resin at the flow rate of 5mL/min, ethanol is adopted for elution, and eluent is collected;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 8
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, treating for 10min by adopting ultrasonic waves with power of 480W and frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through DM-130 macroporous adsorption resin at the flow rate of 5mL/min, ethanol is adopted for elution, and eluent is collected;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Example 9
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 100g of chrysanthemum morifolium ramat powder, adding 1000mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, performing rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 1200mL of water, and continuously concentrating to 600mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 600mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through DM-130 macroporous adsorption resin at the flow rate of 5mL/min, ethanol is adopted for elution, and eluent is collected;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
Comparative example 1
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of acetone, heating and refluxing for 2 times (each time for 3 hours), mixing the extracting solutions for 2 times, filtering, performing rotary evaporation concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying under vacuum to obtain flos Chrysanthemi flavone extract.
Comparative example 2
A method for extracting flavone from chrysanthemum comprises the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of methanol, heating and refluxing for 2 times (each time for 3 hours), mixing the extracting solutions for 2 times, filtering, performing rotary evaporation concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying under vacuum to obtain flos Chrysanthemi flavone extract.
In order to observe the yield of chrysanthemum morifolium ramat flavone in examples 1-9 and comparative examples 1-2, the following method can be adopted for testing:
the chrysanthemum morifolium ramat flavone extracts in the examples and the comparative examples are accurately weighed, 25mg of each chrysanthemum morifolium ramat flavone extract is placed in a 25ml volumetric flask, 2.5ml of methanol is added for full dissolution, and the volume is determined by using distilled water. Taking 5ml of each sample solution, adding into a 25ml volumetric flask, adding distilled water to 6ml, adding 1ml of 5% sodium nitrite solution, mixing, standing for 7min, adding 1ml of 10% aluminum nitrate solution, mixing, standing for 7min, adding 10ml of 5% sodium hydroxide solution, adding distilled water to a constant volume, mixing, and standing for 20 min. The absorbance A of each sample at a wavelength of 510nm was measured according to an aluminum nitrate-sodium nitrite color development method, and the test was repeated three times to obtain an average value. The concentration of the flavone in each extracted sample of the Hangzhou white chrysanthemum is obtained by a rutin standard curve, and the yield of the flavone is calculated according to the concentration.
Y=[(C*V*F/M*106)×100]%
In the formula: c, the concentration of the flavone in the chrysanthemum morifolium ramat sample solution is mu g/ml;
v, volume of chrysanthemum morifolium sample solution, ml;
f is the dilution multiple;
M-Hangzhou white chrysanthemum sample mass, g;
the yield of Y-chrysanthemum morifolium ramat flavone is percent.
The flavone yields of examples 1 to 9 and comparative examples 1 to 2 are shown in the following table:
| quality of flavone powder (g) | Flavone yield (%) | |
| Example 1 | 6.335 | 12.67±0.12 |
| Example 2 | 6.360 | 12.72±0.23 |
| Example 3 | 4.010 | 8.02±0.24 |
| Example 4 | 4.835 | 9.67±0.12 |
| Example 5 | 6.080 | 12.16±0.31 |
| Example 6 | 5.440 | 10.88±0.36 |
| Example 7 | 5.970 | 11.94±0.25 |
| Example 8 | 4.235 | 8.47±0.30 |
| Example 9 | 12.590 | 12.59±0.14 |
| Comparative example 1 | 6.805 | 13.61±0.19 |
| Comparative example 2 | 6.225 | 12.45±0.24 |
In conclusion, the chrysanthemum morifolium ramat flavone obtained in the embodiments 1-2 has the highest yield, the optimal technological parameter values are achieved, the used reagents are low in cost and low in toxicity, the operation is simple, the whole extraction time is short, and the method lays a foundation for developing antioxidant, anti-aging and cancer-preventing foods and medicines with excellent quality from natural chrysanthemum plant resources.
Claims (1)
1. The method for extracting the flavone from the chrysanthemum is characterized by comprising the following steps:
1) crushing: crushing the uniformly dried chrysanthemum morifolium ramat, and sieving the crushed chrysanthemum morifolium ramat with a sieve of 30-60 meshes to obtain chrysanthemum morifolium ramat powder;
2) solvent extraction: weighing 50g of chrysanthemum morifolium ramat powder, adding 500mL of 70% ethanol, heating, refluxing and extracting for 2 times, each time for 3 hours, combining the extracting solutions for 2 times, filtering, carrying out rotary evaporation and concentration on the obtained filtrate in a water bath at 75 ℃, adding 600mL of water, and continuously concentrating to 300mL to obtain a concentrated solution, namely chrysanthemum morifolium ramat extracting solution I;
3) ultrasonic extraction: adding 300mL of petroleum ether into the chrysanthemum morifolium ramat extract I, performing ultrasonic treatment for 10min at the power of 800W and the frequency of 40kHz, extracting for 3 times, combining the extracts, recovering the solvent, and obtaining a residual solution, namely chrysanthemum morifolium ramat extract II;
4) and (3) purification: after the chrysanthemum morifolium ramat extract II passes through D101 macroporous adsorption resin at the flow rate of 5mL/min, eluting by using ethanol, and collecting eluent;
5) concentrating and drying: concentrating the eluate by rotary evaporation, and drying by vacuum method.
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