CN113616564B - Method for extracting water-soluble flavone from lotus - Google Patents
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- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 41
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 41
- 235000006510 Nelumbo pentapetala Nutrition 0.000 title claims abstract description 41
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
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- 235000011949 flavones Nutrition 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 24
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- 239000000284 extract Substances 0.000 claims abstract description 19
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- 229930003935 flavonoid Natural products 0.000 claims description 12
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- 238000000605 extraction Methods 0.000 description 7
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- 238000010828 elution Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
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- JPUKWEQWGBDDQB-QSOFNFLRSA-N kaempferol 3-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=CC(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O JPUKWEQWGBDDQB-QSOFNFLRSA-N 0.000 description 2
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- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
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- MQVRGDZCYDEQML-UHFFFAOYSA-N Astragalin Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(CO)O2)O)C(=O)C2=C(O)C=C(O)C=C2O1 MQVRGDZCYDEQML-UHFFFAOYSA-N 0.000 description 1
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- DUBCCGAQYVUYEU-UHFFFAOYSA-N Querciturone Natural products O1C(C(O)=O)C(O)C(O)C(O)C1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O DUBCCGAQYVUYEU-UHFFFAOYSA-N 0.000 description 1
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- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
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- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- LOJXBHNAFUDMIQ-UHFFFAOYSA-N quercetin-3-alpha-glucuronide Natural products OC1OC(C(O)C(O)C1O)C(=O)Oc1c(oc2cc(O)cc(O)c2c1=O)-c1ccc(O)c(O)c1 LOJXBHNAFUDMIQ-UHFFFAOYSA-N 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/522—Antioxidants; Radical scavengers
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Mycology (AREA)
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- Public Health (AREA)
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- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Dermatology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Nutrition Science (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Birds (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention discloses a method for extracting water-soluble flavone from lotus, which comprises the following steps: s1, taking fresh lotus, freeze-drying, crushing, sieving, extracting, mixing the extracting solutions, and drying under reduced pressure to obtain an extract; s2, dissolving the extract, standing, filtering, and sequentially eluting the filtrate with water, 30% ethanol, 50% ethanol and 70% ethanol which are 4-10 times of the column volume through D101 macroporous resin; s3, combining the 50% ethanol eluent and the 70% ethanol eluent, and concentrating to obtain an intermediate 1; s4, adsorbing the intermediate 1 by polyamide resin with 100-200 meshes, collecting 30% ethanol eluent, and drying under reduced pressure to obtain an intermediate 2; s5, dissolving the intermediate 2, filtering, and drying the filtrate under reduced pressure to obtain a finished product. The invention can extract water-soluble flavone with antioxidant activity from lotus flower in short time and high efficiency, and the obtained product has high purity of active ingredient, strong activity and stable quality.
Description
Technical Field
The invention relates to a method for extracting water-soluble flavone, in particular to a method for extracting water-soluble flavone from lotus flowers.
Background
Lotus flower is flower of perennial herb lotus of lotus genus of Nymphaeaceae, has abundant resource, is medicinal and edible aquatic plant, has a bitter taste of Wen Wei, can treat traumatic injury, hemorrhage, etc., can be taken orally and applied externally, contains abundant amino acid, mineral composition and flavonoid compounds, and has remarkable oxidation resistance. The toxicology experiment proves that the lotus is a safe and reliable food resource and has good processing application prospect, but the lotus has more active ingredients and lower content, and the research on the active ingredients and the functionality of the lotus is less at present.
The existing extraction method for flavonoid substances in lotus flower comprises the steps of separating and extracting by adopting silica gel column chromatography combined with high-speed countercurrent chromatography, extracting by using petroleum ether and ethyl acetate, eluting by using methanol and chloroform, and obtaining 3 high-purity flavonoid compounds: quercetin-3-O-beta-D-glucuronide (I), myricetin-3-O-beta-D-glucoside (II) and astragalin (III); and the other is to adopt acetone with the volume percentage concentration of 50% as a solvent to ultrasonically extract the lotus crude extract.
However, the extraction method of the former extraction method has long time consumption and high extraction and preparation cost, and adopts organic solvents such as acetone, chloroform, methanol, ethyl acetate and the like, which is not friendly to the environment, has harm to the health of human body and has low use safety; the flavonoid extracted by the extraction method has poor water solubility and low antioxidant activity, and limits the application of the flavonoid in the fields of cosmetics and foods. No report on the preparation of water-soluble flavonoids with antioxidant activity from lotus flowers is found in the prior art.
Disclosure of Invention
The invention aims to provide a method for extracting water-soluble flavone from lotus. The invention can extract water-soluble flavone with antioxidant activity from lotus flower in short time and high efficiency, and the obtained product has high purity of active ingredient, strong activity and stable quality.
The technical scheme of the invention is as follows: a method for extracting water-soluble flavone from lotus flower comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving, extracting, mixing the extracting solutions, and drying under reduced pressure to obtain extractum;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with water with 4-10 times of column volume, ethanol with 30% volume concentration, ethanol with 50% volume concentration and ethanol with 70% volume concentration in sequence;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the components of the intermediate 1 through 100-200 meshes of polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, and drying under reduced pressure to obtain an intermediate 2;
s5, dissolving the intermediate 2 with 8-15 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product.
In the method for extracting the water-soluble flavone from the lotus flower, the step S1 is specifically that fresh lotus flower is taken, freeze-dried, crushed, sieved by a 40-80-mesh sieve, added with 5-10 times of water at normal temperature, ultrasonically extracted for 2-5 times for 0.5-2 hours each time, and the extracting solutions are combined and dried under reduced pressure to obtain the extract.
In the method for extracting the water-soluble flavone from the lotus flower, the power of ultrasonic extraction in the step S1 is 300-800W, and the frequency of ultrasonic extraction is 20-40 KHz.
In the method for extracting the water-soluble flavone from the lotus flower, the temperature of the decompression drying in the step S1 and the step S3 is 60-80 ℃, and the vacuum degree is minus 0.1-minus 0.08MPa.
In the method for extracting the water-soluble flavone from the lotus flower, the elution flow rate of water and ethanol in the step S2 is 0.5-1BV/h, and the elution amount of water and ethanol is 3-5 times of the column volume.
In the method for extracting water-soluble flavone from lotus flower, in the step S4, the eluting flow rate of the ethanol is 0.5-0.8 BV/h, and the eluting amount of the ethanol is 3-5 times of the column volume.
The method for extracting the water-soluble flavone from the lotus flower comprises the following steps of:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 40-mesh sieve, adding 8 times of water at normal temperature, ultrasonically extracting for 3 times each time for 1 hour, combining the extracting solutions, and drying under reduced pressure to obtain an extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with 8 times of water, 30% ethanol, 50% ethanol and 70% ethanol in sequence;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the components of the intermediate 1 through 100-200 meshes of polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, and drying under reduced pressure to obtain an intermediate 2;
s5, dissolving the intermediate 2 with 10 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product, wherein the total flavone content in the finished product is 70-80%.
Compared with the prior art, the method is beneficial to extracting water-soluble components by means of low-temperature water and ultrasonic extraction, reduces the dissolution of polar substances, avoids the interference of low-polarity components on the preparation of water-soluble flavonoids, reduces the damage of high-temperature oxidation resistant substances, improves the purity and oxidation resistance of the water-soluble flavonoids, does not use toxic chemical solvents in the extraction and purification processes, and is healthy, safe and environment-friendly;
d101 macroporous resin has a porous skeleton structure of styrene-divinylbenzene, and realizes the separation and purification of compounds by the principle of combination of adsorption and screening. Polyamide resins are a type of polymer compound polymerized by amide groups, and can be adsorbed by forming hydrogen bonds with phenols, quinones, nitro compounds, and the like, and separated from compounds that cannot form hydrogen bonds. Column chromatography is carried out by combining D101 macroporous resin and polyamide resin, 50% and 70% ethanol eluent is collected by the D101 macroporous resin, and impurities such as saccharides, pigments and the like are removed, so that adverse effects on the quality of finished products are avoided, and the total flavone part with the best activity is enriched to be intermediate 1; and (3) collecting 30% ethanol eluent by a polyamide resin adsorption method, further purifying and enriching the intermediate 1 to obtain a total flavone part with high water solubility and antioxidant activity, and improving the purity and activity of the total flavone in the finished product.
Rutin is used as a standard substance, and NaNO is adopted 2 -Al(NO3) 3 And (3) performing color development analysis on the finished product by using a NaOH color development system, and calculating the content of total flavonoids in the finished product to obtain the final finished product, wherein the purity of the active ingredients in the finished product is high, the activity is strong, the quality is stable, the water solubility is good, and the content of the total flavonoids in the finished product can reach 80%.
1mL of lotus flavone acetone solution (the concentration is 5 mug/mL, 10 mug/mL, 20 mug/mL, 40 mug/mL, 80 mug/mL respectively) is added into 4mL of DPPH (0.04 mg/mL) acetone solution, shaking and shaking are carried out, shading is carried out for 30min in a water bath kettle at 30 ℃, and the absorbance is measured at 517 nm. 1mL lotus flavone solution and 4mL DPPH are taken as experimental group, and the absorbance A is measured t At the same time, 1mL of acetone+4mLDPPH is used as a control group to determine the absorbance A 0 . Calculate clearance (%) = (a) 0 -A t )/A 0 X 100%. The EC50 of the compound concentration that reduced the absorbance of DPPH solution by 50% was calculated.
The EC50 of the DPPH free radical scavenging experiment of the product is measured to be 30-40 mug. Can be effectively used in the fields of cosmetics and foods.
The process has the advantages of low cost, little environmental pollution, strong production operability, short time, high extraction efficiency, and mass production and wide popularization and application.
Therefore, the invention can extract the water-soluble flavone with antioxidant activity from lotus flower in short time and high efficiency, and the obtained product has high purity of active ingredients, strong activity and stable quality.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1:
a method for extracting water-soluble flavone from lotus flower comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 80-mesh sieve, adding 5 times of water at normal temperature, carrying out ultrasonic extraction for 5 times, wherein the power of ultrasonic extraction is 300W, the frequency of ultrasonic extraction is 20KHz, merging extracting solutions, drying under reduced pressure, and the temperature of drying under reduced pressure is 60 ℃ and the vacuum degree is-0.08 MPa, thus obtaining extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with water with the volume of 4 times of column volume, ethanol with the volume concentration of 30%, ethanol with the volume concentration of 50% and ethanol with the volume concentration of 70% in sequence; the eluting flow rate of water and ethanol is 0.5BV/h, and the eluting amount of water and ethanol is 3 times of the column volume;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the intermediate 1 with 100-mesh polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, wherein the elution flow rate of ethanol is 0.5BV/h, and the elution amount of ethanol is 3 times of the column volume; drying under reduced pressure at 60deg.C and vacuum degree of-0.08 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 with 8 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product.
The detection shows that the total flavone content in the finished product is 70%.
The test shows that the EC50 of the DPPH free radical scavenging experiment of the finished product is 30 mug.
Example 2:
a method for extracting water-soluble flavone from lotus flower comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 60-mesh sieve, adding 10 times of water at normal temperature, carrying out ultrasonic extraction for 2 times, wherein the power of ultrasonic extraction is 800W, the frequency of ultrasonic extraction is 40KHz, mixing the extracting solutions, drying under reduced pressure, and the temperature of drying under reduced pressure is 80 ℃ and the vacuum degree is-0.1 MPa, thus obtaining extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with 10 times of water, 30% ethanol, 50% ethanol and 70% ethanol in sequence; the eluting flow rate of water and ethanol is 1BV/h, and the eluting amount of water and ethanol is 5 times of the column volume;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the intermediate 1 with 200-mesh polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, wherein the elution flow rate of ethanol is 0.8BV/h, and the elution amount of ethanol is 5 times of the column volume; drying under reduced pressure at 80deg.C and vacuum degree of-0.1 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 with 15 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product.
The detection shows that the total flavone content in the finished product is 75%.
The test shows that the EC50 of the DPPH free radical scavenging experiment of the finished product is 35 mug.
Example 3:
a method for extracting water-soluble flavone from lotus flower comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 40-mesh sieve, adding 8 times of water at normal temperature, carrying out ultrasonic extraction for 3 times, wherein the power of ultrasonic extraction is 500W, the frequency of ultrasonic extraction is 30KHz, mixing the extracting solutions, drying under reduced pressure, and the temperature of drying under reduced pressure is 70 ℃ and the vacuum degree is-0.1 MPa, thus obtaining extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with 8 times of water, 30% ethanol, 50% ethanol and 70% ethanol in sequence; the eluting flow rate of water and ethanol is 0.8BV/h, and the eluting amount of water and ethanol is 4 times of the column volume;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the intermediate 1 with 150-mesh polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, wherein the eluting flow rate of water and ethanol is 0.8BV/h, and the eluting amount of water and ethanol is 4 times of the column volume; drying under reduced pressure at 70deg.C and vacuum degree of-0.1 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 with 10 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product. The detection shows that the total flavone content in the finished product is 80%.
The test shows that the EC50 of the DPPH free radical scavenging experiment of the finished product is 40 mug.
Claims (3)
1. A method for extracting water-soluble flavone from lotus flower is characterized in that: the method comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 40-80 mesh sieve, adding 5-10 times of water at normal temperature, performing ultrasonic extraction for 2-5 times, wherein the power of ultrasonic extraction is 300-800W, the frequency of ultrasonic extraction is 20-40 KHz, each time is 0.5-2 hours, combining the extracting solutions, and performing reduced pressure drying to obtain an extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with water with 4-10 times of column volume, ethanol with 30% volume concentration, ethanol with 50% volume concentration and ethanol with 70% volume concentration in sequence; the eluting flow rate of water and ethanol is 0.5-1BV/h, and the eluting amount of water and ethanol is 3-5 times of the column volume;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the intermediate 1 with 100-200 meshes of polyamide resin, eluting with 30% ethanol, wherein the eluting flow rate of the ethanol is 0.5-0.8 BV/h, and the eluting amount of the ethanol is 3-5 times of the column volume; collecting ethanol eluent with volume concentration of 30%, and drying under reduced pressure to obtain intermediate 2;
s5, dissolving the intermediate 2 with 8-15 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product.
2. The method for extracting water-soluble flavonoids from lotus according to claim 1, wherein: the temperature of the decompression drying in the step S1 is 60-80 ℃, and the vacuum degree is minus 0.1-minus 0.08MPa.
3. A method for extracting water-soluble flavonoids from lotus according to any one of claims 1 to 2, wherein: the method comprises the following steps:
s1, taking fresh lotus, freeze-drying, crushing, sieving with a 40-mesh sieve, adding 8 times of water at normal temperature, ultrasonically extracting for 3 times each time for 1 hour, combining the extracting solutions, and drying under reduced pressure to obtain extractum;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, eluting with 8 times of water, 30% ethanol, 50% ethanol and 70% ethanol in sequence;
s3, combining the ethanol eluent with the volume concentration of 50% and the ethanol eluent with the volume concentration of 70%, and concentrating to obtain an intermediate 1;
s4, enriching the components of the intermediate 1 through 100-200 meshes of polyamide resin, eluting with ethanol with the volume concentration of 30%, collecting ethanol eluent with the volume concentration of 30%, and drying under reduced pressure to obtain an intermediate 2;
s5, dissolving the intermediate 2 with 10 times of water, filtering, and drying the filtrate under reduced pressure to obtain a finished product, wherein the total flavone content in the finished product is 70-80%.
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| CN106038713A (en) * | 2016-08-02 | 2016-10-26 | 新疆维吾尔自治区药物研究所 | Nymphaea candida presl total flavonoid extract as well as preparation method and application thereof |
| CN111110726A (en) * | 2020-02-25 | 2020-05-08 | 福建中医药大学 | Preparation method of lotus seed pot total flavonoids |
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| CN102031013A (en) * | 2010-11-12 | 2011-04-27 | 合肥工业大学 | Method for extracting brown pigment from lotus receptacle |
| CN106038713A (en) * | 2016-08-02 | 2016-10-26 | 新疆维吾尔自治区药物研究所 | Nymphaea candida presl total flavonoid extract as well as preparation method and application thereof |
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