Novel method for adsorption separation of high purity chlorogenic acid

A technology of adsorption separation and chlorogenic acid, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of low utilization rate and discontinuity of upper column liquid and eluent, and achieve No environmental pollution, easy to transport, good separation effect

Inactive Publication Date: 2008-12-03
NANJING UNIV OF TECH
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Problems solved by technology

Patent CN1974527A discloses a method for separating chlorogenic acid by using macroporous resin. In this method, Eucommia ulmoides leaves are extracted with alcohol solution, and the extract is absorbed and desorbed by macroporous resin to obtain chlorogenic acid. However, this method adopts single-stage separation and alcohol The method of extracting chlorogenic acid; patent CN1730015 discloses a method for separating chlorogenic acid from honeysuckle, the method extracts honeysuckle with water, adjusts the pH of the extract, separates chlorogenic acid on a macroporous adsorption column, and finally extracts it with ethyl acetate Refining, but the method still adopts a single-stage separation method, and reducing the residue of ethyl acetate in chlorogenic acid will bring additional operating costs
[0005] A more efficient and continuous separation can be achieved by using a multi-stage separation system. For example, Ramamurthy et al. reported a method for separating aromatic compounds by connecting multi-stage columns in parallel (Parallel column liquid chromatography with asingle multi-wavelength absorbance detector for enhanced selectivity using chemometric analysis[ J]. Analytica Chimica Acta, 2003, 490 (1~2): 197~210); German patent DE883806372 discloses a method for removing caffeine and chlorogenic acid in coffee bean extract, which will be heated with 80 ℃ The coffee bean extract after mixing and shaking with water for 3 hours passes through the gel chromatographic columns packed with Sephadex G-15 and Sephadex G-10 respectively in the secondary connection, and 56% of caffeine can be retained in the Sephadex G-15 gel chromatographic column , and 73.4% of chlorogenic acid can be retained in the Sephadex G-10 gel chromatography column, but the method is essentially a single-stage separation of a single substance
[0006] In short, the existing methods all have the disadvantages of intermittent and discontinuous operation, low utilization rate of the upper column liquid and eluent, etc., which hinders the application of resin separation technology in industrial production. Advantages, optimizing the separation process will greatly reduce production costs, improve production efficiency, non-toxic and environmentally friendly, and open up a new industrial pattern for chlorogenic acid technology

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  • Novel method for adsorption separation of high purity chlorogenic acid

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Embodiment 1

[0038] In this embodiment, the honeysuckle water extraction stock solution with a pH value of 6 and a concentration of 5.0 mg / mL is used. The series of adsorption columns is three stages, and the adsorption columns at each level are glass columns with a height-to-diameter ratio of 1:10 (Φ15×150mm). Pack non-polar macroporous adsorption resin XDA-1 (Xi'an Electronic Resin Factory).

[0039] The original solution passes through the first-level adsorption column 10BV, the second-level adsorption column 8BV, and the third-level adsorption column 10BV in sequence, so that each column reaches the breakthrough point, and the flow rate of the solution is controlled to be 12BV / h. The first-level adsorption column, the second-level adsorption column, The column temperature of the tertiary adsorption column is 25°C. Choose water as the washing liquid, wash the primary adsorption column 4BV, the secondary adsorption column 2BV, and the tertiary adsorption column 4BV in sequence, and the e...

Embodiment 2

[0041]In this example, the tobacco water extraction stock solution with a pH value of 7 and a concentration of 4.0 mg / mL is used. The series of adsorption columns is three stages, and the adsorption columns at each level are resistant to organic solvents with a height-to-diameter ratio of 1:4 (Φ15×60mm). The column was filled with medium polar macroporous adsorption resin HZ-806 (Shanghai Huazhen Technology Co., Ltd.).

[0042] The original solution passes through the primary adsorption column 2BV, the secondary adsorption column 1BV, and the tertiary adsorption column 2BV in sequence, so that each column reaches the breakthrough point, the flow rate of the solution is controlled to be 5BV / h, and the primary adsorption column, the secondary adsorption column, The column temperature of the tertiary adsorption column is 25°C. Choose 50% ethanol aqueous solution as the washing liquid, wash the primary adsorption column 0.5BV, the secondary adsorption column 0.5BV, and the tertiar...

Embodiment 3

[0044] In this example, Eucommia ulmoides water extraction stock solution with a pH value of 6 and a concentration of 2.0 mg / mL was used. Stainless steel column, filled with weak polar macroporous adsorption resin XDA-5 (Xi'an Electronic Resin Factory).

[0045] The original solution passes through the primary adsorption column 7BV and the secondary adsorption column 4BV in sequence, so that each column reaches the breakthrough point, the flow rate of the solution is controlled to 15BV / h, and the column temperature of the primary adsorption column and the secondary adsorption column is controlled at 25°C. Choose 1M hydrochloric acid aqueous solution as the washing liquid, wash the primary adsorption column 2BV, and the secondary adsorption column 1BV in sequence, and the elution flow rate is 15BV / h, until the effluent is sugar-free and protein-free. Then use acetone with a pH value of 5 to dynamically elute the primary adsorption column 5BV and the secondary adsorption column ...

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Abstract

The invention provides a novel method for absorption and separation of high-purity chlorogenic acid, comprising an absorption process, an impurity cleaning process and an elution process. The method is characterized in that: after chlorogenic acid stock solution is dynamically absorbed by at least dual tandem absorption column which is filled with macroporous resins until penetration, impurity removal solution is added for impurity removal; and finally eluent is used for elution until no chlorogenic acid flows out, and effluent is collected. The purity of the pure chlorogenic acid solution obtained by the method can reach over 92 percent as shown by HPLC detection, and the concentration can reach between 0.1 and 0.8 milligram per milliliter; and the pure chlorogenic acid solution can be widely applied in the fields such as foodstuff, medicines, cosmetics and so on. Solid, namely dried chlorogenic acid powder, obtained after direct drying of the pure chlorogenic acid solution prepared by the method, does not require reprocessing, can be directly applied, and is convenient for conveying.

Description

technical field [0001] The invention relates to a new method for adsorption and separation of high-purity chlorogenic acid, which belongs to the natural product extraction technology in the field of biochemical industry. Background technique [0002] Chlorogenic acid is a kind of depsipphenolic acid, which belongs to phenolic compound, and is a kind of phenylpropanoid compound formed by shikimic acid pathway in the process of plant aerobic respiration. Chlorogenic acid is an important physiologically active substance, which has the functions of antibacterial, antiviral, increasing white blood cells, protecting liver and gallbladder, antitumor, lowering blood pressure, lowering blood fat, and scavenging free radicals. It is one of the main active ingredients of many medicinal materials and Chinese patent medicines; at the same time, the content of chlorogenic acid is the quality index of some patent medicines, and it is also one of the nutritional components of many fruit jui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/56
Inventor 卢定强洪声王俊梁铭鑫张淑敏凌岫泉
Owner NANJING UNIV OF TECH
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