CN110684063A

CN110684063A - Method for preparing naringin

Info

Publication number: CN110684063A
Application number: CN201911028816.4A
Authority: CN
Inventors: 刘应建; 韩峰; 李正帮
Original assignee: Chengdu Shuxi Pharmaceutical Co Ltd
Current assignee: Chengdu Shuxi Pharmaceutical Co Ltd
Priority date: 2019-10-28
Filing date: 2019-10-28
Publication date: 2020-01-14

Abstract

The invention discloses a method for preparing naringin, which comprises the steps of crushing pomelo fruits, extracting naringin in the crushed particles of the pomelo fruits by countercurrent heating, filtering the filtrate after dregs are cooled and crystallized, dissolving crystals in hot water, filtering again, and cooling and crystallizing again. The solvent adopted in the preparation process of the naringin is water, organic solvent or acid-base components are not involved, the risks or hazards such as fire, explosion or high salt solution and the like are avoided, the operation is simple, the practicability is high, the safety and the environmental protection are realized, and the preparation method is suitable for industrial production.

Description

Method for preparing naringin

Technical Field

The invention relates to the technical field of comprehensive utilization and deep processing of agricultural and sideline products, in particular to a method for preparing naringin.

Background

Most of the existing industrialized naringin production methods adopt organic solvents, acid and alkali and other raw materials for extraction and preparation, have safety risks, cause great pollution to the society, are not in line with future development of the industry, and are of great importance in finding a more green and environment-friendly industrialized preparation method under the condition of ensuring similar extraction rate and cost.

Disclosure of Invention

The invention aims to: aiming at the existing problems, the invention provides the method for preparing the naringin, the adopted solvents are all water, organic solvents or acid-base components are not involved, the risks or hazards such as fire, explosion or high salt solution and the like can not be caused, the operation is simple, the practicability is strong, the safety and the environmental protection are realized, and the method is suitable for industrial production.

The technical scheme adopted by the invention is as follows:

the method for preparing the naringin comprises the following steps:

(1) crushing the pomelo fruits;

(2) extracting, namely heating and extracting naringin in the crushed particles of the pomelo fruits in a countercurrent manner to obtain a solid-liquid mixture containing the naringin;

(3) filtering, and cooling and crystallizing the filtered filtrate;

(4) dissolving the crystal in hot water, filtering, and cooling for crystallization to obtain naringin crystal.

In the method, the extraction steps of the naringin are simple, the operation is simple, the equipment used in the preparation method is conventional, the method is very economical and practical, the method is suitable for industrial production, and the naringin in the crushed particles of the pomelo fruits is extracted by adopting a countercurrent heating mode due to the maximum average temperature difference of countercurrent heat transfer and good heat transfer driving force, so that the extraction yield of the naringin can be obviously improved; meanwhile, through twice cooling crystallization, impurities in the components can be fully removed, and the purity of the naringin is improved.

Further, the filtering mode in the step (3) comprises primary filtering and refined filtering, the primary filtering filters out the dregs of a decoction mixed liquor, and the refined filtering filters the filtrate after the primary filtering for purification again.

Further, the preliminary filtration mode is the reciprocating sieve filtration, the refined filtration mode is plate filtration or centrifugal filtration.

Further, the refiltering mode in the step (4) is centrifugal filtration.

Further, the particle size of the crushed pomelo fruit particles in the step (1) is 3-5 mm.

Further, the countercurrent heating temperature in the step (2) is 90-100 ℃, and the heating time is 2-3 h.

Further, the cooling crystallization mode in the step (3) and the step (4) is natural cooling.

Further, the pomelo fruit is pomelo peel and/or dried fruit containing naringin.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. the method for preparing the naringin fully removes impurities in the extracted components by two crystallization processes by utilizing the principle that the naringin is soluble in hot water but not in cold water, and has the advantages of simple and easy operation, strong practicability, safety, environmental protection and less wastewater treatment amount.

2. The equipment used in the method for preparing the naringin is more conventional, the investment of industrial enterprises is reduced, and meanwhile, in the preparation process, no organic solvent, acid-base and other substances are involved, so that the method is efficient, environment-friendly and suitable for industrial large-scale production.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the following examples further illustrate the present invention in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Example 1

The method for preparing naringin sequentially comprises the following steps: crushing pomelo fruits, carrying out countercurrent heating extraction, filtering medicine residues by using a vibrating screen, carrying out plate-frame filtration or centrifugal filtration on filtrate, naturally cooling and crystallizing the filtrate, dissolving the filtrate in hot water, carrying out centrifugal filtration, and cooling and crystallizing the filtrate. Wherein the pomelo fruit is pomelo pericarp and/or dried fruit containing naringin.

In the method for preparing the naringin, hot water is adopted for extraction in the whole process, conventional equipment such as a vibrating screen, a plate-and-frame filtering device and a centrifugal filtering device is adopted, the naringin in the pomelo fruits can be fully extracted only through simple combined treatment of steps of countercurrent heating extraction, filtering and repeated cooling crystallization, and meanwhile, substances such as organic solvents, acid and alkali are not involved, so that the method is efficient and environment-friendly, and the extraction cost is reduced.

As a preferred embodiment, in this embodiment, the decoction dregs filtrate is dissolved in hot water after being subjected to plate-frame filtration or centrifugal filtration, cooling crystallization, and the centrifugal filtration and cooling crystallization steps are repeated, preferably two crystallization processes, so that impurities in the extracted components can be sufficiently removed on the basis of saving procedures, and the purity of naringin can be improved.

As a preferred example, in order to improve the extraction yield of naringin, in the step of pulverizing pomelo fruit, the particle size of the particles of the pulverized pomelo fruit is preferably 3mm to 5 mm; and during the countercurrent heating, the heating temperature is 90-100 ℃, the boiling time is 2-3 h based on boiling; the natural cooling crystallization time depends on the ambient temperature and is generally 4h-5 h.

In the embodiment, by the process flow method, a final naringin crystal finished product is tested by using a high performance liquid chromatography detector, the naringin extraction yield can reach 25%, the purity can reach 98%, and compared with the existing extraction mode of organic solvent extraction or alkali-soluble acid-precipitated extraction, the yield and the purity are basically consistent.

Example 2

Based on example 1 above, this example gives the total specific gravity consumed by the grapefruit and water, and the optional amount of hot water consumed during a single step.

In the embodiment, in order to extract naringin to the maximum extent, improve the utilization rate of hot water and save water resources, the total consumption of the hot water is preferably 8-10 times of the weight of the pomelo fruit, and the sewage treatment capacity is also the least when the naringin is produced in the specific gravity range.

As a preferred example, in the countercurrent heating extraction step, the consumption of hot water may be selected to be 5 times the weight of the pomelo fruit, and in the hot water dissolution step, the consumption of hot water may be selected to be 3 times the weight of the pomelo fruit, so that the total amount of hot water consumption is 8 times the weight of the pomelo fruit; alternatively, the hot water consumption may be 6 times the weight of the pomelo fruit, and in the hot water dissolution step, the hot water consumption may be 3 times the weight of the pomelo fruit, so that the total amount of the hot water consumption is 9 times the weight of the pomelo fruit. In this embodiment, the water consumption of each stage is not limited to the specific times listed in the embodiments, as long as the total consumption of hot water is in the range of 8-10 times of the weight of the pomelo fruit.

Example 3

Based on the above embodiment 1, the embodiment can appropriately repeat the countercurrent heating extraction step, that is, after the dregs are filtered by the vibrating screen, the dregs can be subjected to countercurrent heating again to further extract naringin in the pomelo fruit, so as to avoid excessive naringin remaining in the dregs, thereby improving the extraction yield of naringin. In order to save the preparation process of naringin, the dregs of a decoction can be repeatedly extracted for 2-3 times, then the filtrates obtained after filtering the dregs of a decoction are mixed, and the naringin is further prepared by the steps of plate-and-frame filtration or centrifugal filtration, cooling crystallization and the like.

As a preferred example, when the extraction of the dregs is repeated 2 or 3 times, in view of the overall hot water consumption in the whole preparation process, in order to keep the minimum sewage treatment amount, the specific gravity of the hot water consumption in each stage can be properly adjusted, and the overall hot water consumption is properly enlarged to 8-12 times of the weight of the pomelo fruit.

In this example, after the dregs are extracted by repeated countercurrent heating, compared with example 1, the yield of naringin extraction is higher than 25%, the purity is higher than 98%, and both are higher than the existing organic solvent extraction or alkali-soluble acid-precipitated extraction method.

In the method for preparing naringin in the embodiment, the solvents adopted in the whole process are all water, the characteristic that naringin is soluble in hot water but not in cold water is utilized, the problems that the impurities are more and the extraction yield is not high when the naringin is extracted by hot water are solved, the conventional equipment is adopted in the whole process, and only the simple combined treatment of the steps of continuous countercurrent heating extraction and repeated cooling crystallization is adopted, so that the naringin in pomelo fruits can be extracted to the maximum extent, the extraction yield and the purity of the naringin are ensured, meanwhile, organic solvents, acid-base substances and the like are not involved, the method is efficient and environment-friendly, the investment of industrial enterprises is reduced, and the method is suitable for industrial large-.

The principle and embodiments of the present invention are illustrated herein by using specific examples, and the above description of the examples is only for the purpose of helping understanding the method for preparing naringin and the core concept thereof. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims

1. A method for preparing naringin is characterized by comprising the following steps:

(1) crushing the pomelo fruits;

(3) filtering, and cooling and crystallizing the filtered filtrate;

2. The method for preparing naringin according to claim 1, wherein the filtering manner in the step (3) comprises primary filtering for filtering the dregs of the dregs mixture and refined filtering for filtering and purifying the filtrate after the primary filtering again.

3. The method for preparing naringin according to claim 2, wherein the primary filtration mode is vibrating screen filtration, and the fine filtration mode is plate-frame filtration or centrifugal filtration.

4. The method for preparing naringin according to claim 1, wherein the refiltering manner in the step (4) is centrifugal filtration.

5. The method for preparing naringin according to claim 1, wherein the particle size of the crushed pomelo fruit particles in the step (1) is 3mm to 5 mm.

6. The method for preparing naringin according to claim 1, wherein the counter-current heating temperature in step (2) is 90-100 ℃ and the heating time is 2-3 h.

7. The method for preparing naringin according to claim 1, wherein the cooling crystallization in the steps (3) and (4) is natural cooling.

8. The method of claim 1, wherein the pomelo fruit is a pomelo peel and/or a dried fruit containing naringin.