CN111187244A - Novel method for extracting apigenin from celery - Google Patents
Novel method for extracting apigenin from celery Download PDFInfo
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- CN111187244A CN111187244A CN202010058121.7A CN202010058121A CN111187244A CN 111187244 A CN111187244 A CN 111187244A CN 202010058121 A CN202010058121 A CN 202010058121A CN 111187244 A CN111187244 A CN 111187244A
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- XADJWCRESPGUTB-UHFFFAOYSA-N apigenin Natural products C1=CC(O)=CC=C1C1=CC(=O)C2=CC(O)=C(O)C=C2O1 XADJWCRESPGUTB-UHFFFAOYSA-N 0.000 title claims abstract description 76
- KZNIFHPLKGYRTM-UHFFFAOYSA-N apigenin Chemical compound C1=CC(O)=CC=C1C1=CC(=O)C2=C(O)C=C(O)C=C2O1 KZNIFHPLKGYRTM-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229940117893 apigenin Drugs 0.000 title claims abstract description 76
- 235000008714 apigenin Nutrition 0.000 title claims abstract description 76
- 235000015849 Apium graveolens Dulce Group Nutrition 0.000 title claims abstract description 36
- 235000010591 Appio Nutrition 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 34
- 244000101724 Apium graveolens Dulce Group Species 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 238000000605 extraction Methods 0.000 claims abstract description 43
- 240000007087 Apium graveolens Species 0.000 claims abstract description 35
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000004262 preparative liquid chromatography Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 34
- 239000012530 fluid Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 18
- URQMEZRQHLCJKR-UHFFFAOYSA-N 3-Methyl-5-propyl-2-cyclohexen-1-one Chemical compound CCCC1CC(C)=CC(=O)C1 URQMEZRQHLCJKR-UHFFFAOYSA-N 0.000 claims description 16
- 238000004811 liquid chromatography Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 3
- 240000008881 Oenanthe javanica Species 0.000 description 2
- 235000000365 Oenanthe javanica Nutrition 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 206010047073 Vascular fragility Diseases 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000033115 angiogenesis Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- -1 flavonoid compound Chemical class 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of food and medicine, and particularly relates to a novel method for extracting apigenin from celery. The invention takes celery/celery leaves as raw materials, and firstly supercritical CO is used2Extracting with ethanol as auxiliary solvent, and separating by preparative liquid chromatography to obtain apigenin. The invention adopts and utilizes supercritical CO for the first time2The extraction method is simple and easy, the purity of the apigenin is high, the yield is high, toxic solvents are not involved in the whole extraction process, and the method is safe and non-toxic and is suitable for the fields of food and drug production.
Description
Technical Field
The invention belongs to the technical field of food and medicine, and particularly relates to a novel method for extracting apigenin from celery.
Background
Apigenin, also called apigenin, is a flavonoid compound widely distributed in nature, wherein celery is the highest in content, and the molecular formula is C15H10O5The molecular structure of the antioxidant contains three hydroxyl groups, so that the antioxidant has very good antioxidant effect. In addition to this, the present invention is,through a large number of researches at home and abroad, apigenin can also reduce vascular fragility and abnormal permeability, reduce blood fat, has the functions of relaxing blood vessels and reducing blood pressure, and is beneficial to inducing angiogenesis.
At present, the methods for extracting apigenin at home and abroad generally comprise the following steps:
a. solvent extraction method. The method has the widest application range, but the obtained apigenin has low purity and large solvent consumption, sometimes even needs a toxic solvent, and is not suitable for food and medicine production;
b. macroporous resin purification method. The method can effectively improve the purity of the apigenin, but has low yield and is not suitable for large-scale industrial production.
Disclosure of Invention
Aiming at the problems, the invention provides a novel method for extracting apigenin from celery, which takes celery/celery leaves as raw materials and firstly adopts supercritical CO2Fluid is used as a main solvent, ethanol is used as an auxiliary solvent for extraction, and then the apigenin is obtained through preparative liquid chromatography separation, so that the yield of the apigenin can be improved, and the purity of the apigenin can be improved.
The ethanol of the invention preferably has a volume fraction of 95%, namely the volume ratio of ethanol to water is 95: 5. The invention relates to a novel method for extracting apigenin from celery, which comprises the following specific steps:
a. drying and crushing the raw materials, and sieving the crushed raw materials with a 40-mesh sieve to obtain celery powder;
b. collecting the above herba Apii Graveolentis powder X1g, placing the mixture into a supercritical extraction kettle, wherein the extraction temperature is 25-40 ℃, the extraction pressure is 25-40 MPa, and the extraction time is 2.5 hours;
c. collecting extractive solution from a separation tank of a supercritical extraction kettle, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution mainly containing flavonoids;
d. separating, purifying and collecting the concentrated extract by preparative liquid chromatography;
e. and (4) freeze-drying the collected substances to obtain light green powder, namely apigenin.
In the invention, celery leaves are preferably selected as raw materials, so that waste utilization can be realized to a certain extent.
In order to maximally realize the sufficient extraction of the active ingredients such as apigenin and the like, in the step b, ethanol and supercritical CO are used2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. In this application, supercritical CO2The fluid and the ethanol are pumped in real time for extraction, and the fresh solvent can obviously improve the extraction capacity. Supercritical CO2Fluid with X2Pumping into extraction kettle at a flow rate of g/min, and adding ethanol at X3Pumping into the extraction kettle at a speed of ml/min, wherein X1/X2＝5，X1/X3＝78-79。
Extracting and concentrating to obtain concentrated extract. In the step d, the liquid chromatography conditions are as follows: analytical column Kromasil100-5-C18250mm multiplied by 4.6mm, 5 μm, the analysis wavelength is set to 343nm, and the flow rate is 1 mL/min; methanol is used as a mobile phase A, 1 percent (mass fraction) acetic acid aqueous solution is used as a mobile phase B, and gradient elution is adopted.
TABLE 1 elution gradient for HPLC analysis
The invention adopts and utilizes supercritical CO for the first time2The extraction method is simple and easy to implement, the apigenin purity is high, the yield is high, toxic solvents are not involved in the whole extraction process, and the method is safe and non-toxic and is suitable for the fields of food and drug production.
Drawings
FIG. 1 is an HPLC chromatogram of apigenin standard;
FIG. 2 is an HPLC chromatogram of the concentrated extract obtained in comparative example 3;
FIG. 3 is an HPLC chromatogram of the concentrated extract obtained in comparative example 2;
FIG. 4 is an HPLC chromatogram of the concentrated extract obtained in example 1.
Detailed Description
Example 1
A method for extracting apigenin from herba Apii graveolentis comprises extracting herba Apii graveolentis/folium Apii graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
taking fresh Majiagou celery, drying and crushing the celery, and sieving the celery with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at the temperature of 30 ℃ and under the extraction pressure of 30MPa, and extracting apigenin for 2.5 hours by using the supercritical extraction device; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; freeze drying the collected matter to obtain light green powder apigenin with yield of 53.36 μ g/g and purity of 97.5%.
The ethanol is 95% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In step d, the liquid chromatography condition is that Kromasil100-5-C is used18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Example 2
A method for extracting apigenin from herba Apii graveolentis comprises extracting herba Apii graveolentis/folium Apii graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
drying and crushing celery from fresh celery, and sieving the celery with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at the temperature of 25 ℃ and under the extraction pressure of 25MPa, and extracting apigenin for 2.5 hours by using the supercritical extraction device; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; and freeze-drying the collected substances to obtain light green powder, namely apigenin, wherein the yield of the apigenin is 52.49 mu g/g, and the purity of the apigenin is 95.3%.
The ethanol is 95% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In the step d, the liquid chromatography conditions are as follows: using Kromasil100-5-C18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Example 3
A method for extracting apigenin from herba Apii graveolentis comprises extracting herba Apii graveolentis/folium Apii graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
taking fresh Oenanthe Javanica, drying and pulverizing the celery leaves, and sieving with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at 40 ℃ under the extraction pressure of 35MPa, and extracting apigenin for 2.5 hours by using the supercritical extraction device; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; freeze drying the collected matter to obtain light green powder apigenin with apigenin yield of 52.35 μ g/g and purity of 95.7%.
The ethanol is 95% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In the step d, the liquid chromatography conditions are as follows: using Kromasil100-5-C18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Example 4
A method for extracting apigenin from herba Apii graveolentis comprises extracting herba Apii graveolentis/folium Apii graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
taking fresh Oenanthe Javanica, drying and pulverizing the celery leaves, and sieving with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at 35 ℃ under 40MPa for 2.5 hours by using the supercritical extraction device to extract apigenin; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; freeze drying the collected matter to obtain light green powder apigenin with yield of 53.32 μ g/g and purity of 97.5%.
The ethanol is 95% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In the step d, the liquid chromatography conditions are as follows: using Kromasil100-5-C18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Example 5
A method for extracting apigenin from herba Apii graveolentis comprises extracting herba Apii graveolentis/folium Apii graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
taking fresh Majiagou celery, drying and crushing celery leaves, and sieving by a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at 40 ℃ under 25MPa for 2.5 hours by using the supercritical extraction device to extract apigenin; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; freeze drying the collected matter to obtain light green powder apigenin with apigenin yield of 53.25 μ g/g and purity of 97.3%.
The ethanol is 95% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In the step d, the liquid chromatography conditions are as follows: using Kromasil100-5-C18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Comparative example 1
A method for extracting apigenin from herba Apii Graveolentis comprises extracting herba Apii Graveolentis/folium Apii Graveolentis with supercritical CO2Extracting with ethanol as auxiliary solvent, and separating by liquid chromatography to obtain celeryA vegetable element.
The method comprises the following specific steps:
taking fresh Majiagou celery, drying and crushing the celery, and sieving the celery with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at the temperature of 30 ℃ and under the extraction pressure of 30MPa, and extracting apigenin for 2.5 hours by using the supercritical extraction device; collecting extractive solution from the separation tank, and rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; and freeze-drying the collected substances to obtain light green powder, namely apigenin, wherein the yield of the apigenin is 41.96 mu g/g, and the purity of the apigenin is 95.4%.
The ethanol is 99% ethanol by volume fraction.
In step b, ethanol and supercritical CO2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin. Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50g/min and ethanol was pumped into the extraction vessel at a flow rate of 3.2 ml/min.
In the step d, the liquid chromatography conditions are as follows: using Kromasil100-5-C18(250 mm. times.4.6 mm, 5 μm) as an analytical column, the analytical wavelength was 343nm, the flow rate was 1mL/min, the mobile phase was flushed with the gradient shown in Table 1, and the retention time of the standard was 95 min.
Comparative example 2
A method for extracting apigenin from herba Apii Graveolentis comprises extracting herba Apii Graveolentis/folium Apii Graveolentis with supercritical CO2Extracting the fluid with solvent, and separating by liquid chromatography to obtain apigenin.
The method comprises the following specific steps:
taking fresh Majiagou celery, drying and crushing the celery, and sieving the celery with a 40-mesh sieve to obtain celery powder; putting 250g of celery powder into an extraction kettle of a supercritical extraction device, extracting at the temperature of 30 ℃ and under the extraction pressure of 30MPa, and extracting apigenin for 2.5 hours by using the supercritical extraction device; collecting extractive solution from the separation tank, and treating to obtain concentrated extractive solution; separating, purifying and collecting the concentrated extract by preparative liquid chromatography; freeze drying the collected matter to obtain light green powder apigenin with apigenin yield of 5.86 μ g/g and purity of 96.4%.
Supercritical CO2The fluid was pumped into the extraction vessel at a flow rate of 50 g/min.
Comparative example 3
Extracting with solvent commonly used in the prior art, wherein the solvent is methanol
According to the comparison between the example 1 and the comparative examples 1, 2 and 3, the comparative example 3 only adopts 95% ethanol for extraction, and the extracted components are complex and have low apigenin content; comparative example 2 supercritical CO2The fluid is extracted by a solvent, and the extracted components are relatively simple, but the apigenin content is low; comparative example 1 Using 99% ethanol and supercritical CO2The yield and purity of the fluid and the apigenin are improved; example 1 supercritical CO2The fluid and 95% ethanol are extracted together, the extracted components are relatively simple, the apigenin content is high, the liquid phase condition can realize the complete separation of various components, and finally the apigenin yield is high and the purity is high.
Claims (6)
1. A new method for extracting apigenin from celery is characterized in that celery/celery leaves are used as raw materials, and supercritical CO is firstly used2Extracting with ethanol as auxiliary solvent, and separating by preparative liquid chromatography to obtain apigenin.
2. The new method for extracting apigenin from celery, as claimed in claim 1, wherein the ethanol is 95% ethanol by volume fraction.
3. The new method for extracting apigenin from celery as claimed in claim 1, wherein the method comprises the following steps:
a. drying and crushing the raw materials, and sieving the crushed raw materials with a 40-mesh sieve to obtain celery powder;
b. collecting the above herba Apii Graveolentis powder X1g, placing the mixture in a supercritical extraction kettle for extractionThe temperature is 25-40 ℃, the extraction pressure is 25-40 MPa, and the extraction time is 2.5 hours;
c. collecting extractive solution from the separation tank of supercritical extraction kettle, rotary evaporating until no alcohol smell exists to obtain concentrated extractive solution;
d. separating, purifying and collecting the concentrated extract by preparative liquid chromatography;
e. and (4) freeze-drying the collected substances to obtain light green powder, namely apigenin.
4. The new method for extracting apigenin from celery as claimed in claim 3, wherein in the step b, ethanol and supercritical CO are used2The fluid is pre-mixed before the inlet end of the supercritical extraction kettle, and then enters the supercritical extraction kettle together to extract the apigenin.
5. The new method for extracting apigenin from celery as claimed in claim 3, wherein supercritical CO2Fluid with X2Pumping into extraction kettle at a flow rate of g/min, and adding ethanol at X3Pumping into the extraction kettle at a speed of ml/min, wherein X1/X2＝5，X1/X3＝78-79。
6. The novel method for extracting apigenin from celery as claimed in claim 3, wherein in the step d, the liquid chromatography conditions are as follows: analytical column Kromasil100-5-C18250mm multiplied by 4.6mm, 5 μm, the analysis wavelength is set to 343nm, and the flow rate is 1 mL/min; taking methanol as a mobile phase A and 1% acetic acid aqueous solution as a mobile phase B, and performing gradient elution;
elution gradient for HPLC analysis
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| 王正云 等: "超临界CO2法萃取芹菜叶黄酮", 《食品与发酵工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484473A (en) * | 2020-06-16 | 2020-08-04 | 青岛科技大学 | Apigenin extraction method and apigenin buccal tablet |
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