CN104840501B - A kind of preparation method of chrysanthemum total flavone - Google Patents

A kind of preparation method of chrysanthemum total flavone Download PDF

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CN104840501B
CN104840501B CN201510261737.3A CN201510261737A CN104840501B CN 104840501 B CN104840501 B CN 104840501B CN 201510261737 A CN201510261737 A CN 201510261737A CN 104840501 B CN104840501 B CN 104840501B
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chrysanthemum
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extracting solution
extraction
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苏少中
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Shaanxi Ke Hong health industry Co., Ltd.
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Abstract

The present invention relates to a kind of preparation methods of chrysanthemum total flavone.It is combined using ultra high pressure extraction and ultrasonic extraction, the combination of the two ensure that the adequacy of extraction, chrysanthemum is after super-pressure, ultrasonication, due to super-pressure squeezing action and ultrasonic wave cavitation, crush the special effects such as, make the collapse for the cavitation bubble that the cell of chrysanthemum instantaneously generates in a solvent and ruptures, so as to solvent penetration to cell interior, among so that the flavone component in cell is dissolved in solvent, to accelerate to interpenetrate, dissolve.It compares common extracting method, and general flavone yield has larger promotion, and extraction time also shortens, and improves industrial production efficiency.

Description

A kind of preparation method of chrysanthemum total flavone
Technical field
The invention belongs to food, health food and the field of Chinese medicines, are related to a kind of preparation method of chrysanthemum total flavone.
Background technology
Chrysanthemum(Chrysanthemum morifolium Ramat), in Plant Taxonomy be composite family, Chrysanthemum for many years Raw persistent root herbs, in China, plantation is extensive, drinks with a long history, is medicine food and excellent representative plant.China chrysanthemum master There are 8 kinds, respectively Hang Ju, milli chrysanthemum, Chen Ju, tribute chrysanthemum, Qi Ju, bosom chrysanthemum, Ji chrysanthemum, Huang Ju.Chrysanthemum is conventional Chinese medicine, with flower It is used as medicine, is partly commonly the dry capitulum of feverfew chrysanthemum, it is nature and flavor sweetness and bitterness, cool, there is dispelling wind improving eyesight, heat-clearing solution The effect of poison, soothing the liver cool courage, the diseases such as primary treatment headache, dizziness, hot eyes, ambition dysphoria with smothery sensation, treatment sore, pyogenic infections.Modern pharmacological research Show that the principle active component of chrysanthemum is flavone compound, triterpene compound and volatile oil etc., chrysanthemum total flavone is chrysanthemum Main pharmacodynamics active constituent, have the function of good action, with inhibiting a variety of physiology such as cholinesterase to cardiovascular system Activity, clinical test show it with blood pressure lowering, and coronary artery dilator prevents coronary atherosclerosis, treatment coronary heart disease, drop Low blood pressure prevents a variety of effects such as hyperlipidemia, antibacterial, antiviral, anti-inflammatory, anti-aging.
The traditional extraction technique of chrysanthemum total flavone includes cold-maceration, Suo Tifa, circumfluence method, ultrasonic method etc., from Extraction solvent On from the point of view of, common Extraction solvent includes methanol, ethyl alcohol, acetone, petroleum ether etc., such as certain patent of invention 2013104510XX.X A kind of extracting method of chrysanthemum total flavone is disclosed, is that chrysanthemum is smashed it through into 20 mesh sieve, petroleum ether is added and is uniformly mixed, It is fully filtered through filter paper after decoloration, takes filter residue to volatilize spare, then accurately weigh the material pre-processed, by solid-liquid ratio (g/mL) 1 :The ethanol solution of 40-70% is added in 10-30, is impregnated 1 hour after fully shaking up, at 20-50 DEG C of temperature, supersonic frequency 40KHz extracts 20-35min, obtains chrysanthemum total flavone extract.However, conventional extracting method exist extraction organic efficiency it is low or The problem of person's organic solvent residual, ultimately limits the application of chrysanthemum total flavone extract.The present invention extracts chrysanthemum total flavone Technique is studied, it is desirable to obtain optimum extraction process.
Invention content
In order to solve the problems, such as prepared by existing chrysanthemum total flavone, the present invention is intended to provide a kind of chrysanthemum total flavone Preparation method need not use harmful, easily remaining organic solvent to remain to obtain very high extraction efficiency, meet modern pharmaceutical The development trend of technique also complies with people's health pursuit.
A kind of preparation method of chrysanthemum total flavone, which is characterized in that include the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into 20- 25 mesh powders;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 40-45 DEG C of warm water according to mass ratio 1:The ratio of 1.8-2.2 Mixing is then added cellulase and mixes thoroughly, is placed in high-pressure-resistant vessel, maintains the temperature at 40-45 DEG C, be forced into 15-20MPa, Pressure release obtains enzymolysis liquid after maintaining 20-25min, and the dosage of cellulase is 60-65U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethyl alcohol are added into the enzymolysis liquid of step 2 The addition of solution is 2-2.5 times of chrysanthemum powder quality, continues to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, protect Hold temperature be 70-75 DEG C, pressure 20-25MPa, HIGH PRESSURE TREATMENT 5-10min filters after pressure release, detaches filter residue and filtrate, filtrate As extracting solution A;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, into Row ultrasonic wave extraction, ultrasound condition are frequency 40kHz, 62-65 DEG C of temperature, and time 5-10min is filtered after supersound process and received Collect filtrate, as extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, with rotation Evaporation under reduced pressure is distilled to recover solvent, obtains concentrate, as medicinal extract.
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 30-35 DEG C, It is dry to water content less than 5% to get to chrysanthemum total flavone.
The method of the present invention has the following advantages that and advantageous effect:
First, the present invention only selects ethanol solution as Extraction solvent during extracting chrysanthemum total flavone, rear It is all recycled during continuous rotary evaporation, and it as a kind of Extraction solvent of food-grade, there is no residual and safeties Problem meets the growth requirement of modern food and medicine trade.
Second, present invention employs super-pressure enzymatic treatments, in the process, by the pressure of super-pressure and the effect of enzyme, So that eucaryotic cell structure is sufficiently damaged before extraction, be conducive to the abundant progress of release and the extraction of Flavonoid substances.
Third, the present invention are combined using ultra high pressure extraction and ultrasonic extraction, and the combination of the two ensure that the abundant of extraction Property, chrysanthemum is after super-pressure, ultrasonication, due to the squeezing action of super-pressure and the special work such as cavitation, crushing of ultrasonic wave With, make the collapse for the cavitation bubble that the cell of chrysanthemum instantaneously generates in a solvent and ruptures, so as to solvent penetration to cell interior, from And the flavone component in cell is made to be dissolved among solvent, to accelerate to interpenetrate, dissolve.It compares common extracting method, always Flavones yield has larger promotion, and extraction time also shortens, and improves industrial production efficiency.
In short, the method for the present invention combines a variety of advanced technologies, pass through the excellent of the adjustment of processing step and technological parameter Change the production efficiency and recovery rate for greatly improving chrysanthemum total flavone, and obtained product also complies with modern food, health care The growth requirement of product and medicine trade, has a vast market foreground.
Specific implementation mode
Embodiment 1:A kind of preparation method of chrysanthemum total flavone, includes the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into 22 mesh Powder;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 42 DEG C of warm water according to mass ratio 1:1.9 ratio mixing, and Cellulase is added afterwards to mix thoroughly, is placed in high-pressure-resistant vessel, maintains the temperature at 42 DEG C, is forced into 18MPa, let out after maintaining 22min Pressure obtains enzymolysis liquid, and the dosage of cellulase is 63U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethyl alcohol are added into the enzymolysis liquid of step 2 The addition of solution is 2 times of chrysanthemum powder quality, continues to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keeps temperature Degree is 70 DEG C, pressure 22.5MPa, and HIGH PRESSURE TREATMENT 8min is filtered after pressure release, and it is extracting solution to detach filter residue and filtrate, filtrate A;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, into Row ultrasonic wave extraction, ultrasound condition are frequency 40kHz, and filter is collected by filtration after supersound process in 62 DEG C, time 5min of temperature Liquid, as extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, with rotation Evaporation under reduced pressure is distilled to recover solvent, obtains concentrate, as medicinal extract.
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 32 DEG C, is done It is dry to water content less than 5% to get to chrysanthemum total flavone.
Embodiment 2:A kind of preparation method of chrysanthemum total flavone, includes the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into 25 mesh Powder;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 40 DEG C of warm water according to mass ratio 1:2.2 ratio mixing, and Cellulase is added afterwards to mix thoroughly, is placed in high-pressure-resistant vessel, maintains the temperature at 40 DEG C, is forced into 20MPa, let out after maintaining 20min Pressure obtains enzymolysis liquid, and the dosage of cellulase is 60U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethyl alcohol are added into the enzymolysis liquid of step 2 The addition of solution is 2 times of chrysanthemum powder quality, continues to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keeps temperature Degree is 75 DEG C, pressure 20MPa, and HIGH PRESSURE TREATMENT 10min is filtered after pressure release, and it is extracting solution A to detach filter residue and filtrate, filtrate;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, into Row ultrasonic wave extraction, ultrasound condition are frequency 40kHz, and filter is collected by filtration after supersound process in 65 DEG C, time 8min of temperature Liquid, as extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, with rotation Evaporation under reduced pressure is distilled to recover solvent, obtains concentrate, as medicinal extract.
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 35 DEG C, is done It is dry to water content less than 5% to get to chrysanthemum total flavone.
Embodiment 3:A kind of preparation method of chrysanthemum total flavone, includes the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into 20 mesh Powder;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 45 DEG C of warm water according to mass ratio 1:1.8 ratio mixing, and Cellulase is added afterwards to mix thoroughly, is placed in high-pressure-resistant vessel, maintains the temperature at 45 DEG C, is forced into 15MPa, let out after maintaining 25min Pressure obtains enzymolysis liquid, and the dosage of cellulase is 65U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethyl alcohol are added into the enzymolysis liquid of step 2 The addition of solution is 2.5 times of chrysanthemum powder quality, continues to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keep Temperature is 72 DEG C, pressure 20MPa, and HIGH PRESSURE TREATMENT 10min is filtered after pressure release, and it is extracting solution to detach filter residue and filtrate, filtrate A;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, into Row ultrasonic wave extraction, ultrasound condition are frequency 40kHz, and filter is collected by filtration after supersound process in 62 DEG C, time 10min of temperature Liquid, as extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, with rotation Evaporation under reduced pressure is distilled to recover solvent, obtains concentrate, as medicinal extract.
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 35 DEG C, is done It is dry to water content less than 5% to get to chrysanthemum total flavone.
Embodiment 4:With the comparison of conventional method
Comparative example 1:After method recorded in certain patent of invention 2013104510XX.X embodiments 1, i.e. chrysanthemum herb crush 20 mesh sieve is crossed, by solid-liquid ratio (g/mL) 1:8, which are added petroleum ether, is uniformly mixed, and fully after decoloration, is filtered through filter paper, filter residue adds again Enter solid-liquid ratio (g/mL) 1:8, which are added petroleum ether, is uniformly mixed, and fully after decoloration, is filtered through filter paper, takes filter residue to volatilize spare;It is accurate The material pre-processed really is weighed, by solid-liquid ratio (g/mL) 1:15 are added 70% ethanol solution, impregnate 1 after fully shaking up Hour, 30min is extracted at 20 DEG C of temperature, supersonic frequency 40KHz, obtains chrysanthemum total flavone extract.It sets in baking oven and carries out again Low temperature drying, controlled at 32 DEG C, drying to water content is less than 5%.
Comparative example 2:Traditional cold-maceration:Chrysanthemum powder 100g is weighed, uses 2000ml 70% respectively(V/V)Ethyl alcohol, 95%(V/V) Ethyl alcohol, methanol impregnate, and for 24 hours afterwards filter immersion liquid, collect filtrate and obtain concentrate with Rotary Evaporators vacuum distillation recovered solvent, The medicinal extract extracted.Cream liquid sets low temperature drying in baking oven, and weighs(It sets and carries out low temperature drying in baking oven, controlled at 32 DEG C, Drying to water content is less than 5%).
Using 100g chrysanthemums as test material, the yield of the extractive of general flavone of embodiment 1,2,3 and Comparative Examples 1 and 2 is compared And the purity of chrysanthemum total flavone in each extract has been measured by HPLC methods, concrete outcome is:Chrysan Yellow is made in embodiment 1 Ketone extract 4.79g, purity 65.2%;It is 4.91g, purity 62.1% that chrysanthemum total flavone extract, which is made, in embodiment 2;Implement It is 4.56g, purity 69.3% that chrysanthemum total flavone extract, which is made, in example 3;Chrysanthemum total flavone 3.24g is made in comparative example 1, and purity is 43.5%;Chrysanthemum total flavone extract 2.07g, purity 45.1% is made in comparative example 2.Compared by the above test result it is found that originally The method of invention by super-pressure enzymolysis and ultrasonic extraction be combined greatly improve chrysanthemum total flavone extraction yield and The purity of extract, one side can make limited chrysanthemum raw material prepare more Flavonoid substances, save and be produced into This;On the other hand the purity higher of its extract obtained so that subsequent purifying process is simpler, easy to implement.

Claims (3)

1. a kind of preparation method of chrysanthemum total flavone, which is characterized in that include the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into 20-25 mesh Powder;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 40-45 DEG C of warm water according to mass ratio 1:The ratio of 1.8-2.2 mixes, Cellulase is then added to mix thoroughly, is placed in high-pressure-resistant vessel, maintains the temperature at 40-45 DEG C, is forced into 15-20MPa, maintain Pressure release obtains enzymolysis liquid after 20-25min, and the dosage of cellulase is 60-65U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethanol solution are added into the enzymolysis liquid of step 2 Addition be 2-2.5 times of chrysanthemum powder quality, continue to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keep warm Degree is 70-75 DEG C, pressure 20-25MPa, and HIGH PRESSURE TREATMENT 5-10min is filtered after pressure release, detaches filter residue and filtrate, filtrate are Extracting solution A;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, is surpassed Sound wave extracts, and ultrasound condition is frequency 40kHz, 62-65 DEG C of temperature, and filter is collected by filtration after supersound process in time 5-10min Liquid, as extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, rotary evaporation is used Instrument vacuum distillation recovered solvent obtains concentrate, as medicinal extract;
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, it is dry controlled at 30-35 DEG C To water content less than 5% to get to chrysanthemum total flavone.
2. the preparation method of chrysanthemum total flavone according to claim 1, which is characterized in that include the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into the powder of 22 mesh End;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 42 DEG C of warm water according to mass ratio 1:1.9 ratio mixing, then adds Enter cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 42 DEG C, be forced into 18MPa, maintain 22min after pressure release obtain Dosage to enzymolysis liquid, cellulase is 63U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethanol solution are added into the enzymolysis liquid of step 2 Addition be 2 times of chrysanthemum powder quality, continue to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keep the temperature to be 70 DEG C, pressure 22.5MPa, HIGH PRESSURE TREATMENT 8min are filtered after pressure release, and it is extracting solution A to detach filter residue and filtrate, filtrate;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, is surpassed Sound wave extracts, and ultrasound condition is frequency 40kHz, and filtrate is collected by filtration after supersound process, i.e., in 62 DEG C, time 5min of temperature For extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, rotary evaporation is used Instrument vacuum distillation recovered solvent obtains concentrate, as medicinal extract;
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 32 DEG C, drying is extremely Water content is less than 5% to get to chrysanthemum total flavone.
3. the preparation method of chrysanthemum total flavone according to claim 1, which is characterized in that include the following steps:
Step 1 crushes:Chrysanthemum is placed in 60 DEG C of drying in oven to moisture and is less than 5%, is then ground into the powder of 25 mesh End;
Step 2, super-pressure enzymolysis:By chrysanthemum powder and 40 DEG C of warm water according to mass ratio 1:2.2 ratio mixing, then adds Enter cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 40 DEG C, be forced into 20MPa, maintain 20min after pressure release obtain Dosage to enzymolysis liquid, cellulase is 60U/g chrysanthemums;
Step 3, ultra high pressure extraction:The ethanol solution that volumetric concentration is 85%, ethanol solution are added into the enzymolysis liquid of step 2 Addition be 2 times of chrysanthemum powder quality, continue to carry out ultra high pressure treatment in high-pressure-resistant vessel after mixing thoroughly, keep the temperature to be 75 DEG C, pressure 20MPa, HIGH PRESSURE TREATMENT 10min are filtered after pressure release, and it is extracting solution A to detach filter residue and filtrate, filtrate;
Step 4, ultrasound assisted extraction:75% ethyl alcohol of 2 times of filter residue quality is added in the filter residue obtained to step 3, is surpassed Sound wave extracts, and ultrasound condition is frequency 40kHz, and filtrate is collected by filtration after supersound process, i.e., in 65 DEG C, time 8min of temperature For extracting solution B;
Step 5, concentration:Extracting solution B made from extracting solution A made from step 3, step 4 is merged, rotary evaporation is used Instrument vacuum distillation recovered solvent obtains concentrate, as medicinal extract;
Step 6, it is dry:Medicinal extract made from step 5 is set and carries out low temperature drying in baking oven, controlled at 35 DEG C, drying is extremely Water content is less than 5% to get to chrysanthemum total flavone.
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CN105326876A (en) * 2015-11-11 2016-02-17 南阳师范学院 Method for extracting total flavonoids of chrysanthemum
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CN107468738A (en) * 2017-09-22 2017-12-15 安徽菊泰滁菊草本科技有限公司 A kind of extracting method of chrysanthemum total flavone
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