CN110548053A - a method for preparing fructus Hippophae extract rich in total flavonoids and natural vitamin C - Google Patents
a method for preparing fructus Hippophae extract rich in total flavonoids and natural vitamin C Download PDFInfo
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention belongs to the field of natural organic chemistry, and relates to a preparation method of a sea buckthorn extract rich in total flavonoids and natural VC. The method comprises the steps of firstly extracting the seabuckthorn fruits by using an ultrahigh pressure technology, then treating an extracting solution by using a centrifugal machine and a ceramic membrane, and then carrying out molecular distillation on a treating solution to obtain a concentrate. Separating and purifying with macroporous adsorbent resin, respectively collecting water washing part and alcohol washing part, treating the water washing part with nanofiltration membrane, and concentrating by molecular distillation to obtain VC-containing extract (A); directly concentrating the alcohol-washed part to obtain fluid extract (B) containing total flavonoids of fructus Hippophae; and (3) uniformly mixing the fluid extract (A) and the fluid extract (B), and freeze-drying to obtain the seabuckthorn extract containing the total flavonoids and the natural vitamin C. The advantages are that: 1. the ultrahigh pressure can enable the extraction solvent to better enter the interior of plant cells, so that the high-efficiency extraction of the total flavonoids and VC is realized; 2. the extraction time is short, the temperature is low, and the energy consumption is low; 3. the molecular distillation technology can effectively reduce the content loss of VC in the concentration process.
Description
Technical Field
The invention belongs to the field of natural organic chemistry, and relates to a preparation method of a sea buckthorn extract rich in total flavonoids and natural vitamin C.
background
Seabuckthorn is a deciduous shrub which is drought-resistant and sand-resistant and can survive in saline-alkali lands, so that seabuckthorn is widely used for water and soil conservation. Sea buckthorn is planted in great amount in northwest China for desert greening. The sea buckthorn fruit has high vitamin C content, and the vitamin is the name of vitamin C king. Sea buckthorn is a generic term for plants and their fruits. The plant Hippophae rhamnoides is Hippophae of Elaeagnaceae, and is deciduous shrub. The fructus Hippophae is a medicinal and edible plant. The roots, stems, leaves, flowers and fruits of the sea-buckthorn, especially the fruits of the sea-buckthorn contain rich nutrient substances and bioactive substances, and can be widely applied to a plurality of fields of national economy such as food, medicine, light industry, spaceflight, farming and animal husbandry fish industry and the like.
the fructus Hippophae has effects of relieving cough, eliminating phlegm, invigorating stomach, resolving food stagnation, promoting blood circulation and removing blood stasis. Modern medical research shows that seabuckthorn can reduce cholesterol, relieve angina attack and prevent and treat coronary atherosclerotic heart disease.
The application of fructus Hippophae is as fruit and fruit juice, and part of fructus Hippophae is used as raw material of plant extract to produce fructus Hippophae extract. However, the current domestic patents are that either vitamin C is extracted from the vitamin C or total flavonoids are extracted from the vitamin C, and patents of extracting both are rarely seen. For example, Chinese patent CN 106343427A, which describes a method for extracting Vc from sea buckthorn fruits, is a patent for independently extracting vitamin C from sea buckthorn fruits. Also, as shown in chinese patent CN 1451658A, a method for extracting total flavonoids from hippophae rhamnoides fruits by using a three-solvent system is disclosed, which is a patent for extracting total flavonoids from hippophae rhamnoides fruits individually.
Disclosure of Invention
The invention aims to provide a method for preparing a seabuckthorn extract rich in total flavonoids and natural vitamin C, and provides a new preparation route for producing the seabuckthorn extract rich in the total flavonoids and the natural vitamin C.
The invention has the advantages that the extract product not only retains the total flavone, but also retains the vitamin C, thereby providing high-quality raw materials for further processing and utilizing the seabuckthorn extract.
The technical scheme of the invention is realized in such a way that the method comprises the following steps:
(1) Extracting fructus Hippophae with ethanol as extraction solvent in ultrahigh pressure extraction tank, starting high pressure pump, discharging air in container, rapidly increasing pressure to process parameter range in short time, maintaining for a certain time in the pressure range, rapidly opening valve for controlling pressure, removing pressure, and discharging extractive solution;
(2) Centrifuging the extracting solution collected in the step (1) by using a centrifugal machine, then treating by using a ceramic membrane, and collecting a permeate;
(3) carrying out molecular distillation on the permeate collected in the step (2), and recovering an ethanol solution to obtain a concentrate;
(4) preliminarily separating the concentrate obtained in the step (3) by using macroporous adsorption resin, eluting by using purified water and ethanol respectively, and collecting a water washing part (I) and an alcohol washing part (II);
(5) treating the water washing part (I) obtained in the step (4) with a nanofiltration membrane to remove polysaccharide and part of disaccharide, and collecting nanofiltration membrane permeate (III);
(6) Concentrating the nanofiltration membrane permeate (III) obtained in the step (5) by adopting molecular distillation to obtain a fluid extract (A) containing vitamin C;
(7) Concentrating the alcohol washing part (II) obtained in the step (4) to obtain a fluid extract (B) containing the seabuckthorn general flavone;
(8) And (3) uniformly mixing the fluid extract (A) and the fluid extract (B), and then freeze-drying to obtain the seabuckthorn extract rich in total flavonoids and natural vitamin C.
the better technical scheme of the invention is as follows: in the step (1), the seabuckthorn fruits are extracted by adopting ultrahigh pressure extraction equipment, ethanol with volume percentage of 71% -80% is adopted for extraction, the ratio of extraction materials to liquid is 1: 8-10 (m/v), the extraction pressure is 100-120 Mpa, the extraction temperature is 40-50 ℃, the extraction time is 31-40 min, the pressure rise time is 2-3 min, and the pressure relief time is 3-5 s.
The better technical scheme of the invention is as follows: in the step (2), a tubular centrifuge is adopted to process the extracting solution, the rotating speed of the centrifuge is more than 16000r/min, the centrifugate is processed by a ceramic membrane, a membrane element with the aperture of 200nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane processing solution is 20-25 ℃, the pressure is 0.2-0.5 MPa, and the membrane flux is 60-120L/m 2 x h.
The better technical scheme of the invention is as follows: in the step (3), the pressure of molecular distillation is 50-60 Pa, the evaporation temperature is 30-40 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 2.0-3.0L/min.
The better technical scheme of the invention is as follows: in the step (4), macroporous absorption resin with AB-8, D101 and other types is adopted to treat the molecular distillate. And (3) washing the distillate with deionized water after entering the resin column, keeping the flow rate at 1.5-2.5 BV/h, stopping washing after washing for 1.5-2 h, and collecting a washing part (I). Then washing with 10-20% ethanol at a washing speed of 1.0-2.0 BV/h and with an ethanol solution amount of 2-4 BV. Finally, washing with 70-90% ethanol at a washing speed of 1.5-2.5 BV/h and an ethanol solution dosage of 6-8 BV, and collecting an ethanol washing part (II).
The better technical scheme of the invention is as follows: in the step (5), the cut-off molecular weight of the nanofiltration membrane is 200-400 Dal, the temperature of the nanofiltration membrane treatment liquid is 20-25 ℃, the pressure is 0.3-0.5 MPa, and the membrane flux is 8-12L/m 2 × h.
The better technical scheme of the invention is as follows: in the step (6), the pressure of molecular distillation is 20-30 Pa, the evaporation temperature is 30-40 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 1.0-2.0L/min.
the better technical scheme of the invention is as follows: in the step (8), the vacuum degree is controlled to be 10-13 Pa during freezing, the temperature is controlled to be-50 to-40 ℃, and the freezing and drying are carried out until the moisture content is below 5 percent.
Detailed Description
Example 1
Weighing 100 kg of seabuckthorn fruits, putting the seabuckthorn fruits into an ultrahigh pressure extraction tank, and taking 1000L of 71% ethanol in volume percentage as an extraction solvent. After the sea buckthorn berries and the ethanol solution are put into the ultrahigh pressure extraction tank, starting the high pressure pump, discharging air in the container, rapidly increasing the pressure to 100Mpa within 2-3 minutes, then increasing the temperature to 40 ℃, and extracting for 40min at the pressure and the temperature. And after extraction is finished, a valve for controlling high pressure is quickly opened to relieve pressure, and the pressure relief time is 3 seconds. The extraction solvent was removed to yield 1033L of extract.
Treating the extract with a tubular centrifuge at 16000r/min to remove large particulate impurities and pectin, fine-filtering the centrifugate with a ceramic membrane at 20 deg.C under 0.5MPa and a membrane flux of 60L/m 2h, and collecting 929L ceramic membrane permeate.
And (3) concentrating the ceramic membrane permeate by adopting a molecular distillation mode, wherein the pressure of the molecular distillation is 50Pa, the evaporation temperature is 30 ℃, the condensation temperature is 0 ℃, and the material flow rate is 2.0L/min, so that 20.86kg of the molecular distillation concentrate is obtained.
Separating chemical components in the molecular distillation concentrated solution by adopting macroporous adsorption resin with the model number of AB-8, washing the distillate with deionized water after entering a resin column at the flow rate of 1.5BV/h for 2h, stopping washing, and collecting about 152L of a washing part (I). Then washing with 10% ethanol at a speed of 1.0BV/h, wherein the amount of 10% ethanol solution is 4 BV. Finally, the mixture is washed by 70 percent ethanol with the washing speed of 1.5BV/h and the using amount of 70 percent ethanol solution of 8BV, and about 400L of the alcohol washing part (II) is collected.
And (3) treating the collected 152L solution of the water washing part (I) by using a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is 200Dal, the temperature of the nanofiltration membrane treatment solution is 20 ℃, the pressure is 0.5MPa, the membrane flux is 8L/m2 xh, and 132L of nanofiltration membrane permeate is collected.
Concentrating the nanofiltration membrane permeate by molecular distillation at 20Pa, 30 deg.C for evaporation, 0 deg.C for condensation, and 2.0L/min for material flow rate to obtain 3.63kg of fluid extract (A). Concentrating the collected alcohol washing part (II) by adopting a conventional reduced pressure concentration mode to obtain 3.22kg of fluid extract (B).
Mixing the fluid extract (A) and the fluid extract (B), and drying in a vacuum freeze-drying machine at-50 deg.C under 10Pa until the water content is 4.29%. The weight of the obtained fructus Hippophae extract is 2.025kg, wherein the purity of vitamin C is 40.74% and the purity of total flavonoids is 30.86%.
example 2
Weighing 100 kg of seabuckthorn fruits, putting the seabuckthorn fruits into an ultrahigh pressure extraction tank, and taking 800L of ethanol with volume percentage of 80% as an extraction solvent. After the sea buckthorn berries and the ethanol solution are put into the ultrahigh pressure extraction tank, starting the high pressure pump, discharging air in the container, rapidly increasing the pressure to 120Mpa within 2-3 minutes, then increasing the temperature to 50 ℃, and extracting for 31min at the pressure and the temperature. And after extraction is finished, a valve for controlling high pressure is quickly opened to relieve pressure, and the pressure relief time is 5 seconds. The extraction solvent was removed to obtain 829L of an extract.
Treating the extract with a tubular centrifuge at 17000r/min to remove large particulate impurities and pectin, fine-filtering the centrifugate with a ceramic membrane with 200nm membrane element as pore diameter, treating at 25 deg.C under 0.2MPa and membrane flux of 100L/m2 × h, and collecting 752L ceramic membrane permeate.
and (3) concentrating the ceramic membrane permeate by adopting a molecular distillation mode, wherein the pressure of the molecular distillation is 60Pa, the evaporation temperature is 40 ℃, the condensation temperature is 5 ℃, and the material flow rate is 3.0L/min, so that 21.44kg of molecular distillation concentrate is obtained.
Separating chemical components in the molecular distillation concentrated solution by adopting macroporous adsorption resin with the model number of D101, washing the distillate with deionized water after entering a resin column at the flow rate of 2.5BV/h for 1.5h, stopping washing, and collecting about 189L of a washing part (I). Then washing with 20% ethanol at a speed of 2.0BV/h, wherein the amount of 20% ethanol solution is 2 BV. Finally, 90% ethanol is used for washing, the washing speed is 2.5BV/h, the using amount of 90% ethanol solution is 6BV, and about 300L of the alcohol washing part (II) is collected.
and (3) treating the collected 189L solution of the water washing part (I) with a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is 400Dal, the temperature of the nanofiltration membrane treatment solution is 25 ℃, the pressure is 0.3MPa, the membrane flux is 10L/m2 xh, and the nanofiltration membrane permeate is collected 159L.
concentrating the nanofiltration membrane permeate by molecular distillation at 30Pa, 40 deg.C for evaporation, 5 deg.C for condensation, and 1.0L/min for material flow rate to obtain 3.37kg of fluid extract (A). The collected alcohol-washed part (II) was concentrated by conventional concentration under reduced pressure to obtain 3.53kg of fluid extract (B).
Mixing the fluid extract (A) and the fluid extract (B), and drying in a vacuum freeze-drying machine at-40 deg.C under 13Pa until the water content is 4.47%. The weight of the obtained fructus Hippophae extract is 2.241kg, wherein the purity of vitamin C is 38.81%, and the purity of total flavone is 28.42%.
Example 3
Weighing 100 kg of seabuckthorn fruits, putting the seabuckthorn fruits into an ultrahigh pressure extraction tank, and taking 900L of 75% ethanol by volume percentage as an extraction solvent. After the sea buckthorn berries and the ethanol solution are put into the ultrahigh pressure extraction tank, starting the high pressure pump, discharging air in the container, rapidly increasing the pressure to 110Mpa within 2-3 minutes, then increasing the temperature to 45 ℃, and extracting for 35min at the pressure and the temperature. And after extraction is finished, a valve for controlling high pressure is quickly opened to relieve pressure, and the pressure relief time is 2 seconds. The extraction solvent was discharged to obtain an extract 931L.
Treating the extract with a tubular centrifuge at 18000r/min to remove large-particle impurities and pectin, fine-filtering the centrifugate with a ceramic membrane at 23 deg.C and 0.4MPa, wherein the diameter of the membrane is 200nm, the membrane flux is 120L/m2 × h, and collecting the ceramic membrane filtrate 838L.
And (3) concentrating the ceramic membrane permeate by adopting a molecular distillation mode, wherein the pressure of the molecular distillation is 55Pa, the evaporation temperature is 35 ℃, the condensation temperature is 10 ℃, and the material flow rate is 2.5L/min, so that 21.12kg of the molecular distillation concentrate is obtained.
Separating chemical components in the molecular distillation concentrated solution by adopting macroporous adsorption resin with the model number of AB-8, washing the distillate with deionized water after entering a resin column at the flow rate of 2.0BV/h, stopping washing after washing for 2h, and collecting about 203L of a washing part (I). Then washing with 15% ethanol at a speed of 1.5BV/h, wherein the 15% ethanol solution is used at a dosage of 3 BV. Finally, the mixture is washed by 80 percent ethanol with the washing speed of 2.0BV/h and the using amount of 80 percent ethanol solution of 7BV, and the alcohol washing part (II) is collected for about 356L.
And (3) treating the collected 203L solution of the water washing part (I) by using a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is 300Dal, the temperature of the nanofiltration membrane treatment solution is 23 ℃, the pressure is 0.4MPa, the membrane flux is 12L/m2 xh, and the nanofiltration membrane permeate is collected to 176L.
Concentrating the nanofiltration membrane permeate by molecular distillation at 25Pa, 35 deg.C for evaporation, 10 deg.C for condensation, and 1.5L/min for material flow rate to obtain 3.49kg of fluid extract (A). The collected alcohol-washed part (II) was concentrated by conventional vacuum concentration to obtain 3.36kg of fluid extract (B).
mixing the fluid extract (A) and the fluid extract (B), and drying in a vacuum freeze-drying machine at-50 deg.C under 10Pa until the water content is 4.68%. The weight of the obtained fructus Hippophae extract is 2.136kg, wherein the purity of vitamin C is 40.08%, and the purity of total flavone is 29.38%.
Claims (11)
1. a preparation method of a sea buckthorn extract rich in total flavonoids and natural vitamin C is characterized by comprising the following steps:
(1) Extracting fructus Hippophae with ethanol as extraction solvent in ultrahigh pressure extraction tank, starting high pressure pump, discharging air in container, rapidly increasing pressure to process parameter range in short time, maintaining for a certain time in the pressure range, rapidly opening valve for controlling pressure, removing pressure, and discharging extractive solution;
(2) Centrifuging the extracting solution collected in the step (1) by using a centrifugal machine, then treating by using a ceramic membrane, and collecting a permeate;
(3) Carrying out molecular distillation on the permeate collected in the step (2), and recovering an ethanol solution to obtain a concentrate;
(4) Preliminarily separating the concentrate obtained in the step (3) by using macroporous adsorption resin, eluting by using purified water and ethanol respectively, and collecting a water washing part (I) and an alcohol washing part (II);
(5) Treating the water washing part (I) obtained in the step (4) with a nanofiltration membrane to remove polysaccharide and part of disaccharide, and collecting nanofiltration membrane permeate (III);
(6) Concentrating the nanofiltration membrane permeate (III) obtained in the step (5) by adopting molecular distillation to obtain a fluid extract (A) containing vitamin C;
(7) Concentrating the alcohol washing part (II) obtained in the step (4) to obtain a fluid extract (B) containing the seabuckthorn general flavone;
(8) And (3) uniformly mixing the fluid extract (A) and the fluid extract (B), and then freeze-drying to obtain the seabuckthorn extract rich in total flavonoids and natural vitamin C.
2. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the seabuckthorn fruits are extracted by adopting ultrahigh pressure extraction equipment, ethanol with volume percentage of 71% -80% is adopted for extraction, the ratio of extraction materials to liquid is 1: 8-10 (m/v), the extraction pressure is 100-120 Mpa, the extraction temperature is 40-50 ℃, the extraction time is 31-40 min, the pressure rise time is 2-3 min, and the pressure relief time is 3-5 s.
3. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (2), a tubular centrifuge is adopted to process the extracting solution, the rotating speed of the centrifuge is more than 16000r/min, the centrifugate is processed by a ceramic membrane, a membrane element with the aperture of 200nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane processing solution is 20-25 ℃, the pressure is 0.2-0.5 MPa, and the membrane flux is 60-120L/m 2 x h.
4. the method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the pressure of molecular distillation is 50-60 Pa, the evaporation temperature is 30-40 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 2.0-3.0L/min.
5. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (4), macroporous absorption resin with AB-8, D101 and other types is adopted to treat the molecular distillate.
6. and (3) washing the distillate with deionized water after entering the resin column, keeping the flow rate at 1.5-2.5 BV/h, stopping washing after washing for 1.5-2 h, and collecting a washing part (I).
7. Then washing with 10-20% ethanol at a washing speed of 1.0-2.0 BV/h and with an ethanol solution amount of 2-4 BV.
8. Finally, washing with 70-90% ethanol at a washing speed of 1.5-2.5 BV/h and an ethanol solution dosage of 6-8 BV, and collecting an ethanol washing part (II).
9. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (5), the cut-off molecular weight of the nanofiltration membrane is 200-400 Dal, the temperature of the nanofiltration membrane treatment liquid is 20-25 ℃, the pressure is 0.3-0.5 MPa, and the membrane flux is 8-12L/m 2 × h.
10. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (6), the pressure of molecular distillation is 20-30 Pa, the evaporation temperature is 30-40 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 1.0-2.0L/min.
11. The method for preparing the seabuckthorn extract rich in total flavonoids and natural vitamin C as claimed in claim 1, wherein the method comprises the following steps: in the step (8), the vacuum degree is controlled to be 10-13 Pa during freezing, the temperature is controlled to be-50 to-40 ℃, and the freezing and drying are carried out until the moisture content is below 5 percent.
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| CN111418842A (en) * | 2020-03-31 | 2020-07-17 | 山西纳安健康科技有限公司 | Oral peony paste with heat clearing and detoxifying functions and preparation method thereof |
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