A device for purifying cryptochlorogenic acid

Abstract

The utility model discloses a kind of purification devices of cryptogreen acid, including dissolving tank, reaction tank, buffer tank, chromatographic column, first drying tank, crystallization tank, first plate and frame filter, refining tank, second plate and frame filter, second drying tank, cryptogreen acid storage tank;Dissolving tank is communicated with purified water storage tank and first pH regulator storage tank;Reaction tank is communicated with vacuum pump, nitrogen storage tank;Buffer tank is communicated with second pH regulator storage tank;Chromatographic column is respectively communicated with first eluent storage tank, second eluent storage tank, third eluent storage tank;First drying tank is communicated third pH regulator storage tank, crystallization tank is communicated with water-saturated ethyl acetate storage tank;Refining tank is communicated with methyl alcohol solution storage tank and fourth pH regulator storage tank.This device is combined by isomerization reaction, chromatographic separation, fractional crystallization, greatly improve the yield of target product, and recover stevia polyphenols as byproduct, waste liquid in purification process is all recycled, resource utilization is high, economic and environmental protection.

Description

Technical Field

[0001] This utility model relates to a purification device for natural extracts, specifically a purification device for cryptochlorogenic acid. Background Technology

[0002] Cryptochlorogenic acid is an important isomer of chlorogenic acid, widely found in various plants such as stevia, honeysuckle, and coffee beans. Studies have shown that cryptochlorogenic acid possesses excellent antioxidant, anti-inflammatory, antiviral, and α-glucosidase-inhibiting biological activities, demonstrating great application potential in the food, health product, and pharmaceutical fields. However, the efficient and high-purity extraction and separation of cryptochlorogenic acid from plant raw materials has always faced significant challenges. This is because plant extracts are extremely complex, and cryptochlorogenic acid often coexists with various structurally similar isomers, as well as other impurities such as phenolic acids, pigments, and sugars. These impurities with similar physicochemical properties make the separation and purification of cryptochlorogenic acid exceptionally difficult.

[0003] Currently, conventional methods for the industrial production of cryptochlorogenic acid mostly rely on repeated extraction and precipitation using macroporous adsorption resins combined with organic solvents. These traditional methods have the following drawbacks: 1. Low separation efficiency and limited product purity: Macroporous resins have poor selectivity, making it difficult to effectively separate cryptochlorogenic acid from its isomers, resulting in low purity of the final product. 2. Long purification cycle and significant product yield loss: Multiple steps of liquid-liquid extraction, transfer, and precipitation not only increase the production cycle but also cause loss of the target product during purification, leading to a low overall yield. 3. High solvent consumption and severe environmental pollution: The purification process uses large amounts of organic solvents for extraction and washing, and the solvents are difficult to recover efficiently, increasing production costs and placing significant pressure on the environment. 4. Insufficient resource utilization: During the separation of cryptochlorogenic acid, other valuable components in the extract are often not effectively separated and recovered, and are lost with the waste liquid, resulting in resource waste.

[0004] In summary, providing a purification device for cryptochlorogenic acid to solve the above problems is of great significance. Utility Model Content

[0005] The technical problem to be solved by this utility model is to provide a purification device for cryptochlorogenic acid, which greatly improves the yield of the target product by combining isomerization reaction, chromatographic separation and stepwise crystallization, and recovers stevia polyphenols as a by-product. The waste liquid in the purification process is recycled and reused, which has high resource utilization rate and is economical and environmentally friendly.

[0006] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0007] A purification apparatus for cryptochlorogenic acid includes a dissolving tank, a reaction tank, a buffer tank, a chromatographic column, a first drying tank, a crystallizing tank, a first plate and frame filter, a purification tank, a second plate and frame filter, a second drying tank, and a cryptochlorogenic acid storage tank.

[0008] The dissolving tank is connected to a purified water storage tank and a first pH adjuster storage tank; the reaction tank is connected to a vacuum pump and a nitrogen storage tank; the buffer tank is connected to a second pH adjuster storage tank; the chromatographic column is connected to a first eluent storage tank, a second eluent storage tank, and a third eluent storage tank; the first drying tank is connected to a third pH adjuster storage tank; the crystallization tank is connected to a water-saturated ethyl acetate storage tank; and the purification tank is connected to a methanol solution storage tank and a fourth pH adjuster storage tank.

[0009] Preferably, the chromatographic column is filled with reversed-phase chromatographic packing material.

[0010] Preferably, the first eluent outlet of the chromatographic column is connected to the dissolving vessel.

[0011] Preferably, the second eluent outlet of the chromatographic column is connected to the first drying tank.

[0012] Preferably, the third eluent outlet of the chromatographic column is sequentially connected to a third drying tank and a stevia polyphenol storage tank.

[0013] Preferably, the crystallization tank is provided with a cryptochlorogenic acid seed crystal addition port.

[0014] Preferably, the filtrate outlet of the first plate and frame filter is connected to the buffer tank via a concentration tank.

[0015] Preferably, both the reaction vessel and the crystallization vessel are equipped with a stirring device, which includes a stirring shaft, a stirring motor for driving the stirring shaft to rotate, and multiple stirring blades disposed on the stirring shaft.

[0016] Preferably, the filtrate outlet of the second plate and frame filter is connected to the first drying tank.

[0017] By adopting the above technical solution, this utility model has at least the following beneficial effects:

[0018] This invention provides a purification device for cryptochlorogenic acid, which integrates isomerization reaction, chromatographic separation, and stepwise crystallization into one unit, improving product production efficiency and minimizing the introduction of impurities and product degradation, thereby ensuring high purity and high yield of cryptochlorogenic acid product.

[0019] In chromatographic separation, this device employs gradient elution with a first eluent, a second eluent, and a third eluent. The collected eluent containing the target product is then subjected to further crystallization treatment, and stevia polyphenols are recovered. A portion of the eluent is recycled to a dissolving tank for further processing, thereby improving resource utilization and avoiding wastewater discharge that could pollute the environment.

[0020] This device regulates the pH of key purification steps through multiple pH adjuster tanks, ensuring the smooth progress of cryptochlorogenic acid purification and thus improving product yield and purity. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0023] In the diagram, 1. Dissolving tank; 2. Reaction tank; 3. Buffer tank; 4. Chromatographic column; 5. First drying tank; 6. Crystallization tank; 7. First plate and frame filter; 8. Purification tank; 9. Second plate and frame filter; 10. Second drying tank; 11. Cryptochlorogenic acid storage tank; 12. Purified water storage tank; 13. First pH adjuster storage tank; 14. Vacuum pump; 15. Nitrogen storage tank; 16. Second pH adjuster storage tank; 17. First eluent storage tank; 18. Second eluent storage tank; 19. Third eluent storage tank; 20. Reversed-phase chromatography packing material; 21. Third pH adjuster storage tank; 22. Water-saturated ethyl acetate storage tank; 23. Cryptochlorogenic acid seed crystal addition port; 24. Methanol solution storage tank; 25. Fourth pH adjuster storage tank; 26. Third drying tank; 27. Stevia polyphenol storage tank; 28. Stirring shaft; 29. ​​Stirring motor; 30. Stirring blades; 31. Concentrator. Detailed Implementation

[0024] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.

[0025] Example 1

[0026] like Figure 1As shown, a purification apparatus for cryptochlorogenic acid includes a dissolving tank 1, a reaction tank 2, a buffer tank 3, a chromatographic column 4, a first drying tank 5, a crystallizing tank 6, a first plate and frame filter 7, a purification tank 8, a second plate and frame filter 9, a second drying tank 10, and a cryptochlorogenic acid storage tank 11, all connected together.

[0027] The dissolving tank 1 is connected to a purified water storage tank 12 and a first pH adjuster storage tank 13; the reaction tank 2 is connected to a vacuum pump 14 and a nitrogen storage tank 15; the buffer tank 3 is connected to a second pH adjuster storage tank 16; the chromatographic column 4 is connected to a first eluent storage tank 17, a second eluent storage tank 18, and a third eluent storage tank 19, respectively, and the chromatographic column 4 is filled with reversed-phase chromatographic packing material 20, and the second eluent outlet of the chromatographic column 4 is connected to the first drying tank 5; the first drying tank 5 is connected to a third pH adjuster storage tank 21; the crystallization tank 6 is connected to a water-saturated ethyl acetate storage tank 22, and the crystallization tank 6 is provided with a cryptochlorogenic acid seed crystal addition port 23; the purification tank 8 is connected to a methanol solution storage tank 24 and a fourth pH adjuster storage tank 25.

[0028] This device recovers high-purity cryptochlorogenic acid through multiple operations, including dissolving crude stevia chlorogenic acid, isomerization reaction, chromatographic separation, gradient elution, crystallization, purification, and drying, making it suitable for large-scale industrial production.

[0029] In this embodiment, the first eluent outlet of the chromatographic column 4 is connected to the dissolving tank 1. The first eluent is recycled back to the dissolving tank 1 for the next batch of purification and separation, which improves the product yield and avoids resource waste.

[0030] In this embodiment, the third eluent outlet of the chromatographic column 4 is sequentially connected to the third drying tank 26 and the stevia polyphenol storage tank 27.

[0031] In this embodiment, the filtrate outlet of the first plate and frame filter 7 is connected to the buffer tank 3 through the concentration tank 31, and the filtrate is recovered for the next batch of chromatographic separation.

[0032] In this embodiment, both the reaction tank 2 and the crystallization tank 6 are equipped with a stirring device. The stirring device includes a stirring shaft 28, a stirring motor 29 that drives the stirring shaft 28 to rotate, and a plurality of stirring blades 30 provided on the stirring shaft 28.

[0033] In this embodiment, the filtrate outlet of the second plate and frame filter 9 is connected to the first drying tank 5, and the filtrate is recovered for the next batch of crystallization treatment.

[0034] The working principle of this device is as follows:

[0035] Crude stevia chlorogenic acid and purified water were added to dissolving tank 1 and stirred until dissolved. The pH of the solution was adjusted using the first pH adjuster tank 13. The solution was then transferred to reaction tank 2. After sealing reaction tank 2, a vacuum was drawn, and nitrogen was added to reaction tank 2 through nitrogen tank 15 until atmospheric pressure was reached. This process was repeated 3-5 times. The temperature was then increased to allow the reaction to proceed. After the reaction, the solution was transferred to buffer tank 3, cooled to room temperature, and the pH was adjusted using the second pH adjuster tank 16. The solution then entered the chromatographic column 4 for separation, followed by separation through the first eluent tank 17, the second eluent tank 18, and the third eluent tank 19. The three eluent storage tanks 19 contain eluents of different polarities that perform gradient elution on the chromatographic column 4. The first impurities eluted are those containing small amounts of active ingredients, which are returned to the dissolving tank 1 through the first eluent outlet for the next batch of purification. Cryptochlorogenic acid, due to its specific polarity, is eluted under specific eluent conditions and is collected through the second eluent outlet and enters the first drying tank 5 for further processing. The eluent containing stevia polyphenols enters the third drying tank 26 through the third eluent outlet for drying and is then recovered into the stevia polyphenol storage tank 27, thus realizing the high-value utilization of resources.

[0036] The eluent containing cryptochlorogenic acid, which enters the first drying tank 5, is dried after the pH is adjusted by the third pH adjuster storage tank 21. It then enters the crystallization tank 6, where water-saturated ethyl acetate is used as the crystallization solvent, and cryptochlorogenic acid seed crystals are added for crystallization. The crystallized liquid is filtered by the first plate and frame filter press 7. The filtrate is desolventized by the concentration tank 31 and then recycled to the buffer tank 3 for the next batch of chromatographic separation. The filter cake enters the purification tank 8, where it is purified again using methanol solution as the purification solvent. The liquid is filtered by the second plate and frame filter press 9, and the filtrate is recycled to the first drying tank 5 for the next batch of crystallization. The filter cake is dried by the second drying tank 10 and recycled to the cryptochlorogenic acid storage tank 11.

[0037] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A purification apparatus for cryptochlorogenic acid, characterized in that: It includes a connected dissolving tank, reaction tank, buffer tank, chromatographic column, first drying tank, crystallizing tank, first plate and frame filter, purification tank, second plate and frame filter, second drying tank, and cryptochlorogenic acid storage tank; The dissolving tank is connected to a purified water storage tank and a first pH adjuster storage tank; the reaction tank is connected to a vacuum pump and a nitrogen storage tank; the buffer tank is connected to a second pH adjuster storage tank; the chromatographic column is connected to a first eluent storage tank, a second eluent storage tank, and a third eluent storage tank; the first drying tank is connected to a third pH adjuster storage tank; the crystallization tank is connected to a water-saturated ethyl acetate storage tank; and the purification tank is connected to a methanol solution storage tank and a fourth pH adjuster storage tank.

2. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The chromatographic column is filled with reversed-phase chromatographic packing material.

3. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The first eluent outlet of the chromatographic column is connected to the dissolving tank.

4. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The second eluent outlet of the chromatographic column is connected to the first drying tank.

5. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The third eluent outlet of the chromatographic column is sequentially connected to the third drying tank and the stevia polyphenol storage tank.

6. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The crystallization tank is equipped with a cryptochlorogenic acid seed crystal addition port.

7. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The filtrate outlet of the first plate and frame filter is connected to the buffer tank via a concentration tank.

8. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: Both the reaction vessel and the crystallization vessel are equipped with a stirring device, which includes a stirring shaft, a stirring motor that drives the stirring shaft to rotate, and multiple stirring blades mounted on the stirring shaft.

9. The purification apparatus for cryptochlorogenic acid according to claim 1, characterized in that: The filtrate outlet of the second plate and frame filter is connected to the first drying tank.

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