阅读说明：本技术 一种从蓝靛果中制备花青素的方法 (Method for preparing anthocyanin from indigo fruit ) 是由 刘巍 于 2019-10-07 设计创作，主要内容包括：本发明属于天然有机化学领域,公开了一种从蓝靛果中制备花青素的方法,该方法先将蓝靛果鲜果采用胶体磨破碎打浆后在抗氧化剂的存在下利用亚临界水提取技术对其进行提取,然后离心并将离心液放置至室温分层,收集下层水层并过滤,然后冬化并过滤,滤液再先后采用陶瓷膜和纳滤膜进行处理,最后再采用分子蒸馏和真空冷冻干燥技术得到花青素成品。采用本发明制备的花青素产品具有无溶剂残留、成本低、环境无污染、使用和食用安全性高等优点。(The invention belongs to the field of natural organic chemistry, and discloses a method for preparing anthocyanin from lonicera edulis. The anthocyanin product prepared by the invention has the advantages of no solvent residue, low cost, no environmental pollution, high use and edible safety and the like.)

1. A method for preparing anthocyanin from indigo fruit is characterized by comprising the following steps:

(1) crushing and pulping fresh indigo honeysuckle fruits by adopting a colloid mill to obtain fruit pulp;

(2) extracting the fruit pulp obtained in the step (1) by using a subcritical water extraction technology in the presence of an antioxidant, centrifuging, and collecting a centrifugate;

(3) standing the centrifugate obtained in the step (2) to room temperature for layering, collecting a lower water layer and filtering to obtain a filtrate A;

(4) winterizing the filtrate A in the step (3), and then filtering again to obtain a filtrate B;

(5) treating the filtrate B in the step (4) by adopting a ceramic membrane and a nanofiltration membrane in sequence to obtain a concentrated solution A;

(6) concentrating the concentrated solution A in the step (5) by adopting molecular distillation to obtain a concentrated solution B;

(7) and (4) carrying out vacuum freeze drying on the concentrated solution B in the step (6) to obtain the finished anthocyanin.

2. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (2), the indigo fruit pulp is extracted by adopting a subcritical water extraction technology, the pressure range is 16-20 MPa, the extraction temperature is 300-340 ℃, and the fruit pulp: water =1: 1-3 (m/m), extraction time is 10-30 min, and extraction is performed for 2 times.

3. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (2), the added antioxidant is EGCG, and the addition amount of the 2 times of extraction is 0.01-0.05% of the weight of the lonicera edulis.

4. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (4), the winterization temperature is 1-5 ℃, and the winterization time is 5-10 h.

5. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (5), a membrane element with the aperture of 100nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane treatment solution is 21-25 ℃, and the pressure is 0.2-0.4 MPa; the molecular weight cut-off of the nanofiltration membrane is 200Da, the temperature of the nanofiltration membrane treatment liquid is 23-28 ℃, and the pressure is 0.3-0.5 MPa.

6. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (6), the pressure of molecular distillation is 20-30 Pa, the evaporation temperature is 30-35 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 1.0-2.0L/min.

7. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (7), 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 method for preparing anthocyanin by taking lonicera edulis as a raw material. In particular to a method for preparing anthocyanin by utilizing subcritical water technology extraction, winterization and membrane technology purification.

Background

Anthocyanidin is a water-soluble pigment, and can change color with acid and alkali of cell sap. The acid cell sap is reddish, the alkaline cell sap is blue, and anthocyanin is one of the main pigments forming the colors of petals and fruits. The anthocyanin is a plant secondary metabolite and plays an important role in physiology, is a pure natural anti-aging nutritional supplement, is one of the most effective plant antioxidants found by human beings at present, has the biological effectiveness of 100 percent on a human body, can be detected in blood twenty minutes after being taken, has obvious effects of enhancing eyesight, eliminating eye fatigue and delaying cranial nerve aging, has a better treatment effect on capillary diseases caused by diabetes, and also can enhance the functions of heart and lung and prevent senile dementia and other diseases.

The lonicera edulis is a fruit of lonicera japonica of the genus lonicera of the family loniceraceae, is an oval bluish purple berry, contains a large amount of anthocyanin, mainly contains anthocyanin substances taking cyanidin as a main component and anthocyanin substances taking cyanidin as an aglycon, and is one of the plant sources containing much anthocyanin at present.

The current common extraction methods for preparing anthocyanin are as follows: organic solvent extraction, supercritical extraction, microwave extraction and ultrasonic extraction. Organic solvent extraction is a common method for extracting anthocyanin, and after extraction with a solvent, some organic solvents such as petroleum ether, n-hexylen, diethyl ether and the like are required for extraction to remove fat-soluble substances in a crude extract. The organic solvent extraction method has the advantages of simple extraction equipment and simple and convenient operation; the disadvantages are that the organic solvent is easy to consume, takes time, easily causes high solvent residue in the product, and also causes pollution to the environment. The microwave method and the ultrasonic method may cause great harm to the health of operators due to equipment factors. The supercritical extraction method can realize industrialization at present, but as the technology is to convert gaseous carbon dioxide into liquid carbon dioxide, and the liquid carbon dioxide has stronger extraction capability on fat-soluble substances, the proportion of fat-soluble impurities in the product is higher, thereby greatly increasing the cost for producing the anthocyanin.

The prior common purification method is mainly carried out by adopting macroporous adsorption resin, and the macroporous adsorption resin has the advantages of large adsorption capacity and repeated utilization; the disadvantages are that a large amount of ethanol is needed for elution in the purification process, the loss amount of the solvent is large, and the production cost is increased.

Disclosure of Invention

The invention aims to provide a preparation method of anthocyanin in lonicera edulis. The method comprises the steps of pulping lonicera edulis, extracting by using subcritical water, enriching by using winterization and membrane technology, and finally obtaining the anthocyanin product by using molecular distillation and freeze drying.

The technical scheme of the invention is realized in such a way that the method comprises the following steps:

(1) crushing and pulping fresh indigo honeysuckle fruits by adopting a colloid mill to obtain fruit pulp;

(2) extracting the fruit pulp obtained in the step (1) by using a subcritical water extraction technology in the presence of an antioxidant, centrifuging, and collecting a centrifugate;

(3) standing the centrifugate obtained in the step (2) to room temperature for layering, collecting a lower water layer and filtering to obtain a filtrate A;

(4) winterizing the filtrate A in the step (3), and then filtering again to obtain a filtrate B;

(5) treating the filtrate B in the step (4) by adopting a ceramic membrane and a nanofiltration membrane in sequence to obtain a concentrated solution A;

(6) concentrating the concentrated solution A in the step (5) by adopting molecular distillation to obtain a concentrated solution B;

(7) and (4) carrying out vacuum freeze drying on the concentrated solution B in the step (6) to obtain the finished anthocyanin.

The better technical scheme of the invention is as follows: in the step (2), the indigo fruit pulp is extracted by adopting a subcritical water extraction technology, the pressure range is 16-20 MPa, the extraction temperature is 300-340 ℃, and the fruit pulp: water =1: 1-3 (m/m), extraction time is 10-30 min, and extraction is performed for 2 times.

The better technical scheme of the invention is as follows: : in the step (2), the added antioxidant is EGCG, and the addition amount of the 2 times of extraction is 0.01-0.05% of the weight of the lonicera edulis.

The better technical scheme of the invention is as follows: in the step (4), the winterization temperature is 1-5 ℃, and the winterization time is 5-10 h.

The better technical scheme of the invention is as follows: in the step (5), a membrane element with the aperture of 100nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane treatment solution is 21-25 ℃, and the pressure is 0.2-0.4 MPa; the molecular weight cut-off of the nanofiltration membrane is 200Da, the temperature of the nanofiltration membrane treatment liquid is 23-28 ℃, and the pressure is 0.3-0.5 MPa.

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 30-35 ℃, 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 (7), 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.

The invention has the following advantages: 1) according to the method, the lonicera edulis is pulped by adopting a colloid mill, so that the contact area of the raw materials and water in the extraction process can be effectively increased, and the extraction yield is improved; 2) the method adopts a subcritical water extraction technology, adopts water in a subcritical state as an extraction solvent instead of other organic solvents and acidic aqueous solutions, can improve the extraction efficiency, avoids resource waste, does not pollute the environment, does not have solvent residues in products, and greatly improves the use and edible safety of anthocyanin; 3) in the subcritical water extraction process, the antioxidant is added, so that the influence of the extraction temperature on the anthocyanin can be effectively reduced, and the loss of the anthocyanin is reduced; 4) compared with other purification processes requiring organic solvents, the method for enriching anthocyanin by adopting winterization and membrane technology has the advantages of simple operation, resource saving, no environmental pollution, no introduction of organic solvents into products and the like.

Detailed description of the preferred embodiments