阅读说明：本技术 一种富含总黄酮和天然维生素c的沙棘提取物的制备方法 (a method for preparing fructus Hippophae extract rich in total flavonoids and natural vitamin C ) 是由 刘巍 石华强 吕传智 于 2018-06-04 设计创作，主要内容包括：本发明属天然有机化学领域,涉及富含总黄酮和天然VC的沙棘提取物的制备方法。本法先是将沙棘果利用超高压技术进行提取,后将提取液用离心机和陶瓷膜进行处理,再将处理液进行分子蒸馏,得到浓缩物。后用大孔吸附树脂进行分离纯化,分别收集水洗和醇洗部分,纳滤膜处理水洗部分,后用分子蒸馏进行浓缩,得含有VC浸膏(A)；醇洗部分直接浓缩,得含有沙棘总黄酮的流浸膏(B)；将流浸膏(A)和流浸膏(B)混合均匀,后冻干,得含总黄酮和天然维生素C的沙棘提取物。优点：1、超高压可使提取溶剂更好的进入植物细胞内部,实现总黄酮和VC高效提取；2、提取时间短、温度低、能耗低；3、分子蒸馏技术可有效降低VC在浓缩过程中含量损失。(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.)

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.

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