CN113616564A - Method for extracting water-soluble flavone from lotus - Google Patents
Method for extracting water-soluble flavone from lotus Download PDFInfo
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- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 46
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 46
- 235000006510 Nelumbo pentapetala Nutrition 0.000 title claims abstract description 46
- 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 40
- 238000000034 method Methods 0.000 title claims abstract description 39
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 38
- 229930003944 flavone Natural products 0.000 title claims abstract description 38
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 38
- 235000011949 flavones Nutrition 0.000 title claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 152
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000000047 product Substances 0.000 claims abstract description 26
- 239000003480 eluent Substances 0.000 claims abstract description 22
- 239000000284 extract Substances 0.000 claims abstract description 20
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000010828 elution Methods 0.000 claims description 20
- 238000002137 ultrasound extraction Methods 0.000 claims description 13
- 230000003078 antioxidant effect Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000004480 active ingredient Substances 0.000 abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 238000000605 extraction Methods 0.000 description 9
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229930003935 flavonoid Natural products 0.000 description 6
- 235000017173 flavonoids Nutrition 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 150000002215 flavonoids Chemical class 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000007760 free radical scavenging Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- -1 flavonoid compounds Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 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
- 230000031700 light absorption Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- FOHXFLPXBUAOJM-LIBJPBHASA-N myricetin 3-O-beta-D-glucopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=C(O)C=2)OC2=CC(O)=CC(O)=C2C1=O FOHXFLPXBUAOJM-LIBJPBHASA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 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
- 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
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- FOHXFLPXBUAOJM-UHFFFAOYSA-N Isomyricitrin Natural products OC1C(O)C(O)C(CO)OC1OC1=C(C=2C=C(O)C(O)=C(O)C=2)OC2=CC(O)=CC(O)=C2C1=O FOHXFLPXBUAOJM-UHFFFAOYSA-N 0.000 description 1
- DUBCCGAQYVUYEU-VFKUPZNOSA-N Miquelianin Natural products O=C(O)[C@@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@H](OC2=C(c3cc(O)c(O)cc3)Oc3c(c(O)cc(O)c3)C2=O)O1 DUBCCGAQYVUYEU-VFKUPZNOSA-N 0.000 description 1
- 241000209477 Nymphaeaceae Species 0.000 description 1
- 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
- 206010053476 Traumatic haemorrhage Diseases 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Inorganic materials [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 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
- 238000002474 experimental method Methods 0.000 description 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- DUBCCGAQYVUYEU-ZUGPOPFOSA-N miquelianin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O DUBCCGAQYVUYEU-ZUGPOPFOSA-N 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 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
- 150000003254 radicals 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
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a method for extracting water-soluble flavone from lotus flowers, which comprises the following steps: s1, taking fresh lotus flowers, freeze-drying, crushing, sieving, extracting, combining extracting solutions, and drying under reduced pressure to obtain an extract; s2, dissolving the extract, standing, filtering, passing the filtrate through D101 macroporous resin, and sequentially eluting with 4-10 column volumes of water, 30% ethanol, 50% ethanol and 70% ethanol; s3, mixing the 50% ethanol eluate and the 70% ethanol eluate, and concentrating to obtain an intermediate 1; s4, adsorbing the intermediate 1 by polyamide resin of 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 the finished product. The method can be used for extracting the water-soluble flavone with the antioxidant activity from the lotus flower in a short time and high efficiency, and the obtained product has high purity of active ingredients, 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
The lotus flower is a flower of a perennial aquatic herb lotus of the genus lotus of the family Nymphaeaceae, has rich resources, is an aquatic plant with dual purposes of medicine and food, has warm and bitter taste, can treat traumatic injury, bleeding and other diseases, can be orally taken and externally used, contains rich amino acid, mineral substance components and flavonoid compounds, and has remarkable oxidation resistance. Toxicological experiments prove that the lotus is a safe and reliable food resource and has good processing and application prospects, 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.
One of the existing extraction methods for flavonoid substances in lotus flowers is to adopt silica gel column chromatography combined with high-speed counter-current chromatography for separation and extraction, extract with petroleum ether and ethyl acetate, and elute with methanol and chloroform to obtain 3 high-purity flavonoid compounds: quercetin-3-O-beta-D-glucuronide (I), myricetin-3-O-beta-D-glucoside (II) and astragalin (III); the other method is to adopt acetone with the volume percentage concentration of 50 percent as a solvent to perform ultrasonic extraction on the lotus crude extract.
However, the extraction method of the former extraction method is long in time consumption and high in extraction preparation cost, and organic solvents such as acetone, chloroform, methanol, ethyl acetate and the like are adopted, so that the method is not environment-friendly, has harm to human health and is low in use safety; the flavonoid extracted by the latter extraction method has poor water solubility and low antioxidant activity, and the application of the flavonoid in the fields of cosmetics and foods is limited. In the prior art, no report related to the preparation of water-soluble flavone with antioxidant activity from lotus flowers is found.
Disclosure of Invention
The invention aims to provide a method for extracting water-soluble flavone from lotus flowers. The method can be used for extracting the water-soluble flavone with the antioxidant activity from the lotus flower in a short time and high efficiency, and the obtained product has high purity of active ingredients, strong activity and stable quality.
The technical scheme of the invention is as follows: a method for extracting water-soluble flavone from lotus flowers comprises the following steps:
s1, taking fresh lotus flowers, freeze-drying, crushing, sieving, extracting, combining 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, and sequentially eluting with 4-10 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol;
s3, mixing 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 components in the intermediate 1 by polyamide resin of 100-200 meshes, eluting by using 30% ethanol, collecting 30% ethanol eluent, and drying under reduced pressure to obtain an intermediate 2;
and 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 water-soluble flavone from lotus flowers, step S1 is specifically that fresh lotus flowers are taken, freeze-dried, crushed and sieved by a 40-80 mesh sieve, 5-10 times of water is added at normal temperature, ultrasonic extraction is carried out for 2-5 times, each time lasts for 0.5-2 hours, extracting solutions are combined, and drying under reduced pressure is carried out to obtain an extract.
In the method for extracting water-soluble flavone from lotus flowers, 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 flowers, the temperature of the reduced pressure drying in the step S1 and the step S3 is 60-80 ℃, and the vacuum degree is-0.1-0.08 MPa.
In the method for extracting water-soluble flavone from lotus flowers, in the step S2, the elution flow rate of water and ethanol 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 flowers, in step S4, the elution flow rate of ethanol is 0.5-0.8 BV/h, and the elution amount of ethanol is 3-5 times of the column volume.
The method for extracting the water-soluble flavone from the lotus flowers comprises the following steps:
s1, taking fresh lotus flowers, 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, and sequentially eluting with 8 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol;
s3, mixing 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 components in the intermediate 1 by polyamide resin of 100-200 meshes, eluting by using 30% ethanol, collecting 30% ethanol eluent, 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 extraction of water-soluble components is facilitated by the normal-temperature water + ultrasonic extraction mode, the dissolution of polar substances is reduced, the interference of low-polarity components on the preparation of water-soluble flavone is avoided, the damage of high temperature on antioxidant substances is reduced, the purity and the antioxidant performance of the water-soluble flavone are improved, and no toxic chemical solvent is used in the extraction and purification process, so that the method is healthy, safe and environment-friendly;
the D101 macroporous resin has a styrene-divinylbenzene porous skeleton structure, and separation and purification of the compound are realized by the principle of combining adsorption and screening. Polyamide resins are high molecular compounds obtained by polymerizing amide groups, and are adsorbed by forming hydrogen bonds with phenols, quinones, nitro compounds, and the like, and separated from compounds incapable of forming hydrogen bonds. Performing column chromatography treatment by combining D101 macroporous resin and polyamide resin, collecting 50% and 70% ethanol eluate from D101 macroporous resin, removing impurities such as saccharides and pigments, avoiding adverse effect on quality of finished product, and enriching total flavone part with best activity to obtain intermediate 1; and (3) a polyamide resin adsorption method, namely collecting 30% ethanol eluent, 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 a finished product.
Rutin is used as standard substance, and NaNO is adopted2-Al(NO3)3And (3) performing color analysis on the finished product by using a NaOH color development system, and calculating the content of the total flavone in the finished product to obtain the final finished product with high purity of active ingredients, strong activity, stable quality and good water solubility, wherein the content of the total flavone in the finished product can reach 80%.
1mL of lotus flavonoid acetone solution (concentrations of 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL, 40. mu.g/mL, and 80. mu.g/mL, respectively) was added to 4mL of DPPH (0.04mg/mL) acetone solution, shaken well, kept in a 30 ℃ water bath under shade for 30min, and the absorbance was measured at 517 nm. Taking 1mL of lotus flavone solution and 4mL of DPPH as an experimental group, and measuring the light absorption value AtMeanwhile, 1mL of acetone +4mLDPPH is used as a control group to determine the light absorption value A0. The clearance (%) was calculated as (A)0-At)/A0X 100%. The concentration of compound EC50 that reduced the absorbance of DPPH solution by 50% was calculated.
The experimental EC50 for eliminating DPPH free radicals of the product is 30-40 mu g. 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, mass production and large-scale popularization and use.
Therefore, the method can extract the water-soluble flavone with antioxidant activity from the lotus flower in a short time and high efficiency, and the obtained product has high purity of active ingredients, strong activity and stable quality.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1:
a method for extracting water-soluble flavone from lotus flowers comprises the following steps:
s1, taking fresh lotus flowers, freeze-drying, crushing, sieving with a 80-mesh sieve, adding 5 times of water at normal temperature, ultrasonically extracting for 5 times, each time for 0.5 hour, wherein the power of ultrasonic extraction is 300W, the frequency of ultrasonic extraction is 20KHz, combining the extracting solutions, and drying under reduced pressure at the temperature of 60 ℃ and the vacuum degree of-0.08 MPa to obtain an extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, and sequentially eluting with 4 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol; the elution flow rate of water and ethanol is 0.5BV/h, and the elution amount of water and ethanol is 3 times of the column volume;
s3, mixing 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 components in the intermediate 1 by polyamide resin of 100 meshes, eluting by using 30% ethanol in volume concentration, collecting 30% ethanol eluent in volume concentration, wherein the elution flow rate of the ethanol is 0.5BV/h, and the elution amount of the ethanol is 3 times of the column volume; drying under reduced pressure at 60 deg.C under-0.08 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 in 8 times of water, filtering, and drying the filtrate under reduced pressure to obtain the finished product.
The detection shows that the total flavone content in the finished product is 70%.
The finished product was tested for DPPH free radical scavenging EC50 of 30 μ g.
Example 2:
a method for extracting water-soluble flavone from lotus flowers comprises the following steps:
s1, taking fresh lotus flowers, freeze-drying, crushing, sieving with a 60-mesh sieve, adding 10 times of water at normal temperature, ultrasonically extracting for 2 times (2 hours each time) with the ultrasonic extraction power of 800W and the ultrasonic extraction frequency of 40KHz, combining the extracting solutions, drying under reduced pressure at the temperature of 80 ℃ and the vacuum degree of-0.1 MPa to obtain an extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, and sequentially eluting with 10 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol; the elution flow rate of water and ethanol is 1BV/h, and the elution amount of water and ethanol is 5 times of the column volume;
s3, mixing 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, subjecting the intermediate 1 to 200-mesh polyamide resin enrichment, eluting with 30% ethanol, collecting 30% ethanol eluate, wherein the ethanol eluate has an elution flow rate of 0.8BV/h and an elution amount of 5 times of column volume; drying under reduced pressure at 80 deg.C under-0.1 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 in 15 times of water, filtering, and drying the filtrate under reduced pressure to obtain the finished product.
The detection shows that the content of the total flavone in the finished product is 75%.
The finished product was tested for DPPH free radical scavenging EC50 of 35 μ g.
Example 3:
a method for extracting water-soluble flavone from lotus flowers comprises the following steps:
s1, taking fresh lotus flowers, freeze-drying, crushing, sieving with a 40-mesh sieve, adding 8 times of water at normal temperature, ultrasonically extracting for 3 times (1 hour each time) with the ultrasonic extraction power of 500W and the ultrasonic extraction frequency of 30KHz, combining the extracting solutions, drying under reduced pressure at the temperature of 70 ℃ and the vacuum degree of-0.1 MPa to obtain an extract;
s2, dissolving the extract with water, standing, filtering, passing the filtrate through D101 macroporous resin, and sequentially eluting with 8 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol; the elution flow rate of water and ethanol is 0.8BV/h, and the elution amount of water and ethanol is 4 times of the column volume;
s3, mixing 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 components in the intermediate 1 by using 150-mesh polyamide resin, eluting by using 30% ethanol in volume concentration, collecting 30% ethanol eluent in volume concentration, wherein the elution flow rate of water and ethanol is 0.8BV/h, and the elution amount of the water and the ethanol is 4 times of the column volume; drying under reduced pressure at 70 deg.C under-0.1 MPa to obtain intermediate 2;
s5, dissolving the intermediate 2 in 10 times of water, filtering, and drying the filtrate under reduced pressure to obtain the finished product. The detection shows that the content of the total flavone in the finished product is 80%.
The finished product was tested for DPPH free radical scavenging EC50 of 40 μ g.
Claims (7)
1. A method for extracting water-soluble flavone from lotus flowers is characterized by comprising the following steps: the method comprises the following steps:
s1, taking fresh lotus flowers, freeze-drying, crushing, sieving, extracting, combining 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, and sequentially eluting with 4-10 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol;
s3, mixing 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 components in the intermediate 1 by polyamide resin of 100-200 meshes, eluting by using 30% ethanol, collecting 30% ethanol eluent, and drying under reduced pressure to obtain an intermediate 2;
and 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 flavone from lotus flowers as claimed in claim 1, wherein the method comprises the following steps: and S1, specifically, taking fresh lotus flowers, freeze-drying, crushing, sieving with a 40-80-mesh sieve, adding 5-10 times of water at normal temperature, ultrasonically extracting for 2-5 times for 0.5-2 hours each time, combining the extracting solutions, and drying under reduced pressure to obtain an extract.
3. The method for extracting water-soluble flavone from lotus flowers as claimed in claim 1, wherein the method comprises the following steps: in the step S1, the power of ultrasonic extraction is 300-800W, and the frequency of ultrasonic extraction is 20-40 KHz.
4. The method for extracting water-soluble flavone from lotus flowers as claimed in claim 1, wherein the method comprises the following steps: the temperature of the reduced pressure drying in the step S1 and the step S3 is 60-80 ℃, and the vacuum degree is-0.1 to-0.08 MPa.
5. The method for extracting water-soluble flavone from lotus flowers as claimed in claim 1, wherein the method comprises the following steps: and in the step S2, the elution flow rate of the water and the ethanol is 0.5-1BV/h, and the elution amount of the water and the ethanol is 3-5 times of the column volume.
6. The method for extracting water-soluble flavone from lotus flowers as claimed in claim 1, wherein the method comprises the following steps: in the step S4, the elution flow rate of the ethanol is 0.5-0.8 BV/h, and the elution amount of the ethanol is 3-5 times of the column volume.
7. The method for extracting water-soluble flavone from lotus flowers according to any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
s1, taking fresh lotus flowers, 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, and sequentially eluting with 8 times of column volume of water, 30% ethanol, 50% ethanol and 70% ethanol;
s3, mixing 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 components in the intermediate 1 by polyamide resin of 100-200 meshes, eluting by using 30% ethanol, collecting 30% ethanol eluent, 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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| CN117442534A (en) * | 2023-12-14 | 2024-01-26 | 广州嘉瑜生物科技有限公司 | Abelmoschus manihot extract, preparation method thereof and application thereof in preparing skin care product |
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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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117442534A (en) * | 2023-12-14 | 2024-01-26 | 广州嘉瑜生物科技有限公司 | Abelmoschus manihot extract, preparation method thereof and application thereof in preparing skin care product |
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