CN104840501A - Preparation method for total flavonoids of chrysanthemum - Google Patents

Preparation method for total flavonoids of chrysanthemum Download PDF

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CN104840501A
CN104840501A CN201510261737.3A CN201510261737A CN104840501A CN 104840501 A CN104840501 A CN 104840501A CN 201510261737 A CN201510261737 A CN 201510261737A CN 104840501 A CN104840501 A CN 104840501A
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flos chrysanthemi
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CN104840501B (en
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苏少中
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Shaanxi Ke Hong health industry Co., Ltd.
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Ningbo Good Taste Food Co Ltd
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Abstract

The invention relates to a preparation method for total flavonoids of chrysanthemum. By the combination of ultrahigh pressure extraction and ultrasonic extraction, the extraction sufficiency is ensured; after the chrysanthemum is subjected to ultrahigh pressure treatment and ultrasonic treatment, cells of the chrysanthemum are broken due to the collapse of cavitation bubbles instantaneously generated in a solvent under special actions such as an ultrahigh pressure extrusion action and ultrasonic cavitation and crushing actions, so that the solvent permeates into the cells, flavone components in the cells are dissolved in the solvent to accelerate mutual permeation and dissolution. Compared with a common extraction method, the preparation method for the total flavonoids of the chrysanthemum has the advantages that the yield of the total flavonoids is greatly improved, the extraction time is shortened, and the industrial production efficiency is improved.

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, relate to a kind of preparation method of chrysanthemum total flavone.
Background technology
Flos Chrysanthemi ( chrysanthemum morifolium Ramat), being the perennial root herbaceous plant of Compositae, Chrysanthemum in Plant Taxonomy, in China's plantation extensively, drinking with a long history, is that excellent representative plant of holding concurrently eaten by medicine.China's Flos Chrysanthemi mainly contains 8 kinds, is respectively Flos Chrysanthemi, milli chrysanthemum, Chen Ju, Flos Chrysanthemi, Flos Chrysanthemi, Flos Chrysanthemi, Flos Chrysanthemi, Herba Tagetis Patulae.Flos Chrysanthemi is conventional Chinese medicine, be used as medicine with flower, conventional part is the dry capitulum of feverfew Flos Chrysanthemi, nature and flavor sweetness and bitterness, cool, there is effect of dispelling wind improving eyesight, heat-clearing and toxic substances removing, the cool gallbladder of suppressing the hyperactive liver, the disease such as primary treatment headache, dizzy, conjunctival congestion, irritable feverish sensation of chest and heart, treatment skin ulcer, toxic swelling.Modern pharmacological research shows, the principle active component of Flos Chrysanthemi is flavone compound, triterpenoid compound and volatilization wet goods, chrysanthemum total flavone is the main pharmacodynamics active component of Flos Chrysanthemi, to cardiovascular system, there is good action, there is the multiple physiologically actives such as the effect of suppression cholinesterase, clinical trial shows that it has blood pressure lowering, coronary artery dilator, prevents coronary atherosclerosis, treatment coronary heart disease, reduces blood pressure, prevents hyperlipidemia, antibacterial, antiviral, antiinflammatory, anti-ageing multiple effect of waiting for a long time.
The traditional extraction technique of chrysanthemum total flavone comprises cold-maceration, Suo Tifa, circumfluence method, ultrasonic method etc., from Extraction solvent, conventional Extraction solvent comprises methanol, ethanol, acetone, petroleum ether etc., such as certain patent of invention 2013104510XX.X discloses a kind of extracting method of chrysanthemum total flavone, it crosses 20 mesh sieves after being pulverized by Flos Chrysanthemi, add petroleum ether mix homogeneously, through filter paper filtering after abundant decolouring, getting filtering residue volatilizes for subsequent use, accurately take the good material of pretreatment again, the alcoholic solution of 40-70% is added by solid-liquid ratio (g/mL) 1: 10-30, fully shake up rear immersion 1 hour, under temperature 20-50 0C, supersonic frequency 40KHz extracts 20-35min, obtain the total yellow intoxicated extract of Flos Chrysanthemi.But there is the problem extracting the low or organic solvent residual of organic efficiency in conventional extracting method, ultimately limit the application of chrysanthemum total flavone extract.The present invention is studied chrysanthemum total flavone extraction process, ites is desirable to obtain optimum extraction process.
Summary of the invention
In order to solve Problems existing in the preparation of existing chrysanthemum total flavone, the present invention aims to provide a kind of preparation method of chrysanthemum total flavone, it does not need to adopt harmful, easily residual organic solvent still can obtain very high extraction efficiency, meet the development trend of modern pharmaceutical technique, the health also meeting people is pursued.
A preparation method for chrysanthemum total flavone, is characterized in that, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 20-25 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 40-45 DEG C is mixed according to the ratio of mass ratio 1:1.8-2.2, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 40-45 DEG C, be forced into 15-20MPa, after maintaining 20-25min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 60-65U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2-2.5 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 70-75 DEG C, pressure is 20-25MPa, HIGH PRESSURE TREATMENT 5-10min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 62-65 DEG C, time 5-10min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum.
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 30-35 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
Method tool of the present invention has the following advantages and beneficial effect:
First, the present invention only selects alcoholic solution as Extraction solvent in the process extracting chrysanthemum total flavone, it is all reclaimed in follow-up rotary evaporation process, and it is as a kind of Extraction solvent of food stage, there is not residual and safety issue, meet the growth requirement of modern food and medicine trade.
The second, present invention employs supertension ferment treatment, in the process, by the pressure of supertension and the effect of enzyme, cellularity is sufficiently damaged before extraction, be conducive to the release of Flavonoid substances and fully carrying out of extraction.
3rd, the present invention adopts hyperpressure extraction and supersound extraction to combine, both combinations ensure that the adequacy of extraction, Flos Chrysanthemi is after supertension, ultrasonic Treatment, due to the special role such as squeezing action and hyperacoustic cavitation, pulverizing of supertension, make the cell of Flos Chrysanthemi in a solvent the cavitation bubble of instantaneous generation collapse and break, so that solvent penetration is to cell interior, thus make the flavone component in cell be dissolved among solvent, to accelerate to interpenetrate, dissolve.It compares common extracting method, and total flavones yield has had larger lifting, and extraction time also shortens, and improves industrial production efficiency.
In a word, the multiple advanced technology of methods combining of the present invention, production efficiency and the extraction ratio of chrysanthemum total flavone is drastically increased by the adjustment of processing step and the optimization of technological parameter, and obtained product also meets the growth requirement of modern food, health product and medicine trade, there is wide market prospect.
Detailed description of the invention
embodiment 1: a kind of preparation method of chrysanthemum total flavone, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 22 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 42 DEG C is mixed according to the ratio of mass ratio 1:1.9, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 42 DEG C, be forced into 18MPa, after maintaining 22min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 63U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 70 DEG C, pressure is 22.5MPa, HIGH PRESSURE TREATMENT 8min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 62 DEG C, time 5min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum.
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 32 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
embodiment 2: a kind of preparation method of chrysanthemum total flavone, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 25 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 40 DEG C is mixed according to the ratio of mass ratio 1:2.2, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 40 DEG C, be forced into 20MPa, after maintaining 20min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 60U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 75 DEG C, pressure is 20MPa, HIGH PRESSURE TREATMENT 10min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 65 DEG C, time 8min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum.
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 35 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
embodiment 3: a kind of preparation method of chrysanthemum total flavone, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 20 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 45 DEG C is mixed according to the ratio of mass ratio 1:1.8, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 45 DEG C, be forced into 15MPa, after maintaining 25min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 65U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2.5 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 72 DEG C, pressure is 20MPa, HIGH PRESSURE TREATMENT 10min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 62 DEG C, time 10min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum.
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 35 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
embodiment 4: with comparing of traditional method
comparative example 1: certain method described in patent of invention 2013104510XX.X embodiment 1; namely Flos Chrysanthemi herb crosses 20 mesh sieves after pulverizing; add oil by solid-liquid ratio (g/mL) 1:8 to wake up mix homogeneously; after abundant decolouring; through filter paper sucking filtration, filtering residue adds solid-liquid ratio (g/mL) 1: 8 again and adds oil enzyme mix homogeneously, fully after decolouring; through filter paper sucking filtration, get filtering residue and volatilize for subsequent use; The material that accurately competent pretreatment is good, adds the alcoholic solution of 70%, fully shakes up rear immersion 1 hour, at temperature 20 0C, extract 30min under supersonic frequency 40KHz, obtain chrysanthemum total flavone extract by solid-liquid ratio (g/mL) 1 15.Put in baking oven again and carry out cold drying, control temperature is 32 DEG C, is dried to water content lower than 5%.
comparative example 2: traditional cold-maceration: take Flos Chrysanthemi part 100g, use 2000ml 70%(V/V respectively) ethanol, 95%(V/V) ethanol, methanol soak, after 24h, immersion is filtered, collect filtrate, use Rotary Evaporators vacuum distillation recovered solvent, obtain concentrated solution, the extractum namely extracted.Cream liquid puts oven drying at low temperature in baking oven, and weigh (put in baking oven and carry out cold drying, control temperature is 32 DEG C, is dried to water content lower than 5%).
With 100g Flos Chrysanthemi for test material, compare the output of the extractive of general flavone of embodiment 1,2,3 and comparative example 1,2 and recorded the purity of each extract ZHONGJUHUA total flavones by HPLC method, concrete outcome is: embodiment 1 obtains Flos Chrysanthemi flavone extract 4.79g, and purity is 65.2%; It is 4.91g that embodiment 2 obtains chrysanthemum total flavone extract, and purity is 62.1%; It is 4.56g that embodiment 3 obtains chrysanthemum total flavone extract, and purity is 69.3%; Comparative example 1 obtains chrysanthemum total flavone 3.24g, and purity is 43.5%; Comparative example 2 obtains chrysanthemum total flavone extract 2.07g, and purity is 45.1%.From above result of the test relatively, method of the present invention is combined by supertension enzymolysis and supersound extraction and drastically increases the yield of chrysanthemum total flavone extraction and the purity of extract, it can make limited Flos Chrysanthemi raw material prepare more Flavonoid substances on the one hand, has saved production cost; The purity of its obtained extract is higher on the other hand, and follow-up purifying process more simply, is easily realized.

Claims (3)

1. a preparation method for chrysanthemum total flavone, is characterized in that, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 20-25 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 40-45 DEG C is mixed according to the ratio of mass ratio 1:1.8-2.2, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 40-45 DEG C, be forced into 15-20MPa, after maintaining 20-25min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 60-65U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2-2.5 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 70-75 DEG C, pressure is 20-25MPa, HIGH PRESSURE TREATMENT 5-10min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 62-65 DEG C, time 5-10min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum;
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 30-35 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
2. the preparation method of chrysanthemum total flavone according to claim 1, is characterized in that, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 22 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 42 DEG C is mixed according to the ratio of mass ratio 1:1.9, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 42 DEG C, be forced into 18MPa, after maintaining 22min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 63U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 70 DEG C, pressure is 22.5MPa, HIGH PRESSURE TREATMENT 8min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 62 DEG C, time 5min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum;
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 32 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
3. the preparation method of chrysanthemum total flavone according to claim 1, is characterized in that, comprises the steps:
Step one, pulverizes: drying in oven Flos Chrysanthemi being placed in 60 DEG C lower than 5%, is then ground into 25 object powder to moisture;
Step 2, supertension enzymolysis: the warm water of Flos Chrysanthemi powder with 40 DEG C is mixed according to the ratio of mass ratio 1:2.2, then add cellulase to mix thoroughly, be placed in high-pressure-resistant vessel, maintain the temperature at 40 DEG C, be forced into 20MPa, after maintaining 20min, pressure release obtains enzymolysis solution, and the consumption of its cellulase is 60U/g Flos Chrysanthemi;
Step 3, hyperpressure extraction: add the alcoholic solution that volumetric concentration is 85% in the enzymolysis solution of step 2, the addition of alcoholic solution is 2 times of Flos Chrysanthemi powder quality, mix rear continuation thoroughly and carry out ultra high pressure treatment in high-pressure-resistant vessel, maintenance temperature is 75 DEG C, pressure is 20MPa, HIGH PRESSURE TREATMENT 10min, filters after pressure release, be separated filtering residue and filtrate, filtrate is extracting solution A;
Step 4, ultrasound assisted extraction: the ethanol adding 75% of filtering residue quality 2 times in the filtering residue that step 3 obtains, carries out ultrasonic extraction, ultrasound condition is frequency 40kHz, temperature 65 DEG C, time 8min, supersound process terminates rear collecting by filtration filtrate, is extracting solution B;
Step 5, concentrated: the extracting solution B that extracting solution A step 3 obtained, step 4 obtain merges, and uses Rotary Evaporators vacuum distillation recovered solvent, obtains concentrated solution, be extractum;
Step 6, dry: put in baking oven by the extractum that step 5 is obtained and carry out cold drying, control temperature is 35 DEG C, is dried to water content lower than 5%, namely obtains chrysanthemum total flavone.
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CN106860502A (en) * 2017-03-09 2017-06-20 桂林融通科技有限公司 The preparation method of bitter melon seed flavones
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
CN108530432A (en) * 2017-03-01 2018-09-14 南京泽朗生物科技有限公司 A kind of preparation method of Puerarin
CN108684909A (en) * 2018-06-28 2018-10-23 广西昭平县凝香翠茶厂 Green tea super-pressure method for increasing aroma
CN110237143A (en) * 2019-06-14 2019-09-17 铜仁职业技术学院 A method of enzymatic hydrolysis auxiliary reflux extracts Chinese lizardtail flavone
CN112159316A (en) * 2020-10-28 2021-01-01 深圳市萱嘉生物科技有限公司 Method for extracting gingerol by using ultrahigh pressure combined ultrasonic technology

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105087201A (en) * 2015-08-26 2015-11-25 甘肃省轻工研究院 Method for manufacturing maca beer
CN105326876A (en) * 2015-11-11 2016-02-17 南阳师范学院 Method for extracting total flavonoids of chrysanthemum
CN108530432A (en) * 2017-03-01 2018-09-14 南京泽朗生物科技有限公司 A kind of preparation method of Puerarin
CN106860502A (en) * 2017-03-09 2017-06-20 桂林融通科技有限公司 The preparation method of bitter melon seed flavones
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
CN108684909A (en) * 2018-06-28 2018-10-23 广西昭平县凝香翠茶厂 Green tea super-pressure method for increasing aroma
CN110237143A (en) * 2019-06-14 2019-09-17 铜仁职业技术学院 A method of enzymatic hydrolysis auxiliary reflux extracts Chinese lizardtail flavone
CN112159316A (en) * 2020-10-28 2021-01-01 深圳市萱嘉生物科技有限公司 Method for extracting gingerol by using ultrahigh pressure combined ultrasonic technology

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