CN109293509B - Method for preparing high-purity chlorogenic acid from bamboo leaf extract - Google Patents
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Abstract
A method for preparing high-purity chlorogenic acid from bamboo leaf extract belongs to the technical field of natural product extraction. The method comprises the following process steps: 1) separating by macroporous resin: loading bamboo leaf extract as raw material onto macroporous adsorbent resin, sequentially eluting with distilled water, 60% ethanol and 95% ethanol, collecting unadsorbed part and water eluted part respectively, and concentrating to obtain concentrate A and concentrate B; 2) high-speed countercurrent chromatographic separation: separating and purifying the concentrate A and the concentrate B in an HSCCC chromatograph by taking an ethyl acetate-methanol or acetonitrile-acetic acid-water two-phase solvent system to obtain a chlorogenic acid monomer. The method can simply, conveniently and efficiently obtain the chlorogenic acid compound from the bamboo leaf extract, realizes effective separation of the chlorogenic acid compound from the bamboo leaf flavone component of the bamboo leaf extract, is suitable for small-scale or industrial application in the production and preparation processes of the chlorogenic acid compound and the bamboo leaf flavone component, and is beneficial to improving the additional value of production.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and particularly relates to a method for preparing high-purity chlorogenic acid from a bamboo leaf extract by combining macroporous resin column chromatography with a high-speed countercurrent chromatography (HSCCC) technology.
Background
Bamboo is a perennial plant of the subfamily bambusoideae of the family gramineae and has a long history of eating and medicinal use in China. Researches show that the bamboo leaves contain a plurality of rich chemical components, including flavonoid, phenolic acids, polysaccharide, coumarin lactone, anthraquinone, amino acids, aromatic substances and trace elements such as manganese, zinc, selenium and the like. The bamboo leaf flavonoid mainly comprises orientin, isoorientin, vitexin, isovitexin, etc., and has antibacterial, antiinflammatory, repercussive, blood lipid reducing, and oxygen free radical scavenging effects. Chlorogenic acid is a main phenolic acid component of bamboo leaves, is also one of important active ingredients of traditional Chinese medicines such as honeysuckle, eucommia leaves and the like, has wide biological activity, and has the effects of resisting bacteria and viruses, increasing leucocytes, protecting liver and gallbladder, resisting tumors, reducing blood pressure, reducing blood fat, removing free radicals, exciting the central nervous system and the like; the research and application of the modern science on the biological activity of the chlorogenic acid are deeply carried out in a plurality of fields of food, health care, medicine, daily chemical industry and the like. Therefore, the development of the method for separating and purifying the chlorogenic acid in the bamboo leaf extract has great practical value.
The macroporous adsorption resin is a common natural product separation material and has the advantages of good adsorption selection, low cost, simple and convenient operation and the like. The invention patent of Chinese patent application No. 200910223926.6 discloses a method for preparing bamboo leaf flavone by using HP-20 macroporous adsorption resin.
High-speed counter-current chromatography (HSCCC) is a novel chromatographic separation and purification technology based on a liquid-liquid distribution mechanism, and has the advantages of high sample recovery rate, few operation steps and the like because no solid supports or carriers are used, and is particularly suitable for separation of natural active monomer components. Related researches on separation of chlorogenic acid by using HSCCC have been reported previously. Chinese patent application No. 201010542548.0 discloses a method for obtaining chlorogenic acid from folium Eucommiae extract by HSCCC using ethyl acetate-n-butanol-water system. The invention with Chinese patent application number of 201510316229.0 discloses a method for obtaining chlorogenic acid from a mahonia leaf extract by HSCCC (high speed charge control chromatography) by using an n-hexane-ethyl acetate-methanol-water system. The invention with Chinese patent application number of 201710120670.0 discloses a method for obtaining chlorogenic acid from burdock extract by HSCCC (high speed current chromatography) by using an ethyl acetate-methanol-water system.
Although the above method can obtain bamboo leaf flavone or chlorogenic acid component respectively, it does not aim at the characteristics of bamboo leaf extract, and develops a method which can not only effectively separate chlorogenic acid and bamboo leaf flavone by using macroporous resin, but also can efficiently remove bamboo leaf pigment and impurities by using HSCCC to obtain high-purity chlorogenic acid.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a method for preparing high-purity chlorogenic acid from a bamboo leaf extract. The method comprises the steps of firstly, separating and purifying through optimized macroporous resin, and effectively separating to obtain chlorogenic acid; then, HSCCC separation is carried out by adopting an ethyl acetate-methanol (or acetonitrile) -acetic acid-water solvent system, and the chlorogenic acid with medium and high purity is obtained from the chlorogenic acid concentrate. The method can effectively obtain chlorogenic acid, and simultaneously realize effective separation of the chlorogenic acid and bamboo leaf flavone components of the bamboo leaf extract.
The method for preparing the high-purity chlorogenic acid from the bamboo leaf extract is characterized by comprising the following process steps:
1) separating by macroporous resin: loading bamboo leaf extract as raw material onto macroporous adsorbent resin, sequentially eluting with distilled water, 60% ethanol and 95% ethanol, collecting unadsorbed part and water eluted part respectively, and concentrating to obtain concentrate A and concentrate B; through analysis, the concentrate A and the concentrate B both contain a large amount of chlorogenic acid components (the total recovery rate is more than or equal to 90 percent) and only contain a small amount of bamboo leaf total flavone components (the total recovery rate is less than or equal to 10 percent). Collecting the 60% ethanol eluate (fraction C), concentrating to obtain concentrate C, and analyzing the concentrate to obtain a large amount of bamboo leaf total flavone (total recovery rate greater than or equal to 80%) and only a small amount of chlorogenic acid (total recovery rate less than or equal to 5%);
2) high-speed countercurrent chromatographic separation: separating and purifying the concentrate A and the concentrate B in an HSCCC chromatograph by using an ethyl acetate-methanol or acetonitrile-acetic acid-water two-phase solvent system, automatically collecting effluent at an outlet according to the running time of the HSCCC chromatograph, performing HPLC (high performance liquid chromatography) detection on the effluent, respectively combining the collected liquids with the chlorogenic acid purity of more than 90%, and recovering the solvent by using a rotary evaporator to obtain a chlorogenic acid monomer;
the two-phase solvent system comprises 30-45 volume percent of ethyl acetate, 5-15 volume percent of methanol, 5-15 volume percent of acetic acid and 30-50 volume percent of water, or 30-45 volume percent of ethyl acetate, 5-15 volume percent of acetonitrile, 5-15 volume percent of acetic acid and 30-50 volume percent of water, wherein the upper phase is a stationary phase, and the lower phase is a mobile phase.
The method for preparing high-purity chlorogenic acid from the bamboo leaf extract is characterized in that the concentration of the bamboo leaf extract in the step 1) is as follows: 5-100 mg/mL of aqueous solution based on dry weight of the extract.
The method for preparing high-purity chlorogenic acid from the bamboo leaf extract is characterized in that the type of the macroporous adsorption resin in the step 1) is D101 or XAD-7 HP.
The method for preparing high-purity chlorogenic acid from the bamboo leaf extract is characterized in that in the step 1), the sampling flow rate is 1-4 BV/h, the quality of the sampled extract is less than or equal to 1 g/g of resin, the elution volume of water is 3-6 BV, the elution volume of 60% ethanol is greater than or equal to 4BV, and the elution flow rate is 1-4 BV/h.
The method for preparing high-purity chlorogenic acid from the bamboo leaf extract is characterized in that the high-speed countercurrent chromatographic separation in the step 2) is specifically as follows: preparing a mixed solution from an ethyl acetate-methanol or acetonitrile-acetic acid-water two-phase solvent system in a separating funnel, taking the upper layer as a stationary phase and the lower layer as a mobile phase; pumping a stationary phase into an HSCCC chromatograph at a speed of 10-20 mL/min, rotating a main machine at 600-1000 rpm after a pipeline is completely filled with the stationary phase, simultaneously pumping a mobile phase at a speed of 1-3 mL/min until the mobile phase flows out and an ultraviolet detector monitors that a base line is stable, injecting a proper amount of concentrate A or B dissolved in the mobile phase into the HSCCC chromatograph by using a sample injector, automatically collecting effluent liquid at an outlet according to running time, carrying out HPLC (high performance liquid chromatography) detection on the effluent liquid, respectively combining the collected liquids with the purity of chlorogenic acid of more than 90%, and recovering a solvent by using a rotary evaporator to obtain a chlorogenic acid monomer.
The method can simply, conveniently and efficiently obtain the chlorogenic acid compound from the bamboo leaf extract, realizes effective separation of the chlorogenic acid compound from the bamboo leaf flavone component of the bamboo leaf extract, is suitable for small-scale or industrial application in the production and preparation processes of the chlorogenic acid compound and the bamboo leaf flavone component, and is beneficial to improving the additional value of production.
Drawings
FIG. 1 is HPLC chromatogram of folium Bambusae extract, wherein peaks 1-5 are chlorogenic acid, isoorientin, orientin, vitexin, and isovitexin, respectively;
FIG. 2 is an HPLC chart of fraction A separated by macroporous column of example 1, wherein peaks 1 are chlorogenic acid respectively;
FIG. 3 is an HPLC chart of fraction B separated by macroporous column of example 1, wherein peaks 1 are chlorogenic acid respectively;
FIG. 4 is an HPLC chart of fraction C separated by macroporous columns in example 1, wherein peaks 1-4 are isoorientin, orientin, vitexin, and isovitexin, respectively;
FIG. 5 is HSCCC separation chromatogram of fraction A of macroporous resin in example 1, wherein peaks 1 are the collected chlorogenic acid peaks, respectively;
FIG. 6 is an HPLC chromatogram of a chlorogenic acid standard;
FIG. 7 is an HPLC chromatogram of chlorogenic acid separated from fraction A HSCCC of macroporous resin in example 1.
Detailed Description
The present invention is further illustrated by the following examples.
The folium Bambusae extract in the invention is obtained by extracting folium Bambusae with water and concentrating, and its HPLC chromatogram is shown in figure 1, wherein peaks 1-5 are chlorogenic acid, isoorientin, orientin, vitexin, and isovitexin, respectively.
Example 1
(1) Separation with macroporous resin
Taking 16.8 g of the freeze-dried bamboo leaf extract, diluting with water to obtain 840 mL of the bamboo leaf extract with the concentration of 20 mg/mL, loading the bamboo leaf extract on 50g D101 macroporous adsorption resin (1 BV = 40 mL) at the flow rate of 2BV/h, and then sequentially eluting with 5BV distilled water, 4BV 60% ethanol and 4BV 95% ethanol at the flow rate of 2 BV/h. Collecting the effluent (fraction A) and the water eluate (fraction B) respectively, and concentrating to obtain concentrates A and B; collecting 60% ethanol eluate (fraction C), and concentrating to obtain bamboo leaf flavone concentrate C. FIG. 2 is an HPLC chart of fraction A separated by a large pore, wherein peak 1 is chlorogenic acid; FIG. 3 is an HPLC chart of fraction B separated by a large pore, wherein peaks 1 are chlorogenic acid respectively; FIG. 4 is an HPLC chart of fraction C separated by macroporous columns in example 1, wherein peaks 1-4 are isoorientin, orientin, vitexin, and isovitexin, respectively.
The liquid chromatography (HPLC) conditions for analyzing chlorogenic acid and 4 flavones in the bamboo leaf extract are as follows: shimadzu C18 column (4.6 mm. times.250 mm, 5 μm) as a packing material, acetonitrile A as a mobile phase, 0.1% formic acid solution as a mobile phase B, gradient elution time program: 15% of mobile phase A in 0-10 min, and 15 → 30% of mobile phase A in 10-30 min. The detection wavelength is 325nm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the sample injection amount is 20 mu l.
(2) High-speed countercurrent chromatography separation and purification
The mixture is fully shaken in a separating funnel by taking ethyl acetate, acetonitrile, acetic acid and water (the volume ratio is 35:10:5: 50) as an HSCCC solvent system, and then is placed for half an hour for fully layering. The phases were then separated, with the upper phase as the stationary phase and the lower phase as the mobile phase, and degassed ultrasonically for 30 min. The concentrate A510 mg was taken, dissolved in 10 mL of a mobile phase, and filtered to obtain a sample to be separated. Pumping the stationary phase into an HSCCC chromatograph at a speed of 20mL/min, rotating a main machine at 850rpm after a pipeline is fully filled with the stationary phase, simultaneously pumping a mobile phase at 2 mL/min, setting the detection wavelength to be 325nm, and injecting a sample by using a sample injector after the two phases reach equilibrium and the base line is stable; the effluent was automatically collected from the outlet, analyzed by HPLC detection and combined in 160min fractions at 140-. Dissolving the concentrate B634 mg in 10 mL of mobile phase, collecting 140-160min fractions under the same HSCCC condition, concentrating and drying to obtain chlorogenic acid 24 mg with the purity of 92.1%.
The liquid chromatography (HPLC) conditions for analyzing the purity of chlorogenic acid in the bamboo leaf extracting solution are adopted in the experiment as follows: shimadzu C18 column (4.6 mm. times.250 mm, 5 μm) was used as a packing material, and acetonitrile-0.1% formic acid solution (15: 85) was used as a mobile phase. The detection wavelength is 325nm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the sample injection amount is 20 mu l. FIG. 5 is HSCCC separation chromatogram of fraction A of macroporous resin in example 1, wherein peaks 1 are the collected chlorogenic acid peaks respectively. FIG. 6 is an HPLC chromatogram of a chlorogenic acid standard. FIG. 7 is an HPLC chromatogram of chlorogenic acid separated from fraction A HSCCC of macroporous resin in example 1.
Example 2
(1) Separation with macroporous resin
Taking 16.1 g of the freeze-dried bamboo leaf extract, diluting with water to obtain 805 mL of 20 mg/mL bamboo leaf extract, loading onto 50g XAD-7HP macroporous adsorption resin (1 BV = 35 mL) at the flow rate of 2BV/h, and then sequentially eluting with 5BV distilled water, 6BV 60% ethanol and 4BV mL 95% ethanol at the flow rate of 2 BV/h. Collecting the effluent (fraction A) and the water eluate (fraction B) respectively, and concentrating to obtain concentrates A and B; collecting 60% ethanol eluate (fraction C), and concentrating to obtain bamboo leaf flavone concentrate C. The liquid chromatography (HPLC) conditions for analyzing chlorogenic acid and 4 flavones in the bamboo leaf extract are the same as above.
(2) High-speed countercurrent chromatography separation and purification
The mixture is fully shaken in a separating funnel by taking ethyl acetate, methanol, acetic acid and water (the volume ratio is 40:10:5: 45) as an HSCCC solvent system, and then is placed for half an hour for fully layering. The phases were then separated, with the upper phase as the stationary phase and the lower phase as the mobile phase, and degassed ultrasonically for 30 min. 523 mg of the concentrate A was dissolved in 10 mL of a mobile phase and filtered to obtain a sample to be separated. Pumping the stationary phase into an HSCCC chromatograph at a speed of 20mL/min, rotating a main machine at 850rpm after a pipeline is fully filled with the stationary phase, simultaneously pumping a mobile phase at 2 mL/min, setting the detection wavelength to be 325nm, and injecting a sample by using a sample injector after the two phases reach equilibrium and the base line is stable; the effluent was automatically collected from the outlet, analyzed by HPLC analysis and combined in the 185 min fraction of 165-. Dissolving 634mg of the concentrate B in 10 mL of mobile phase, collecting 165-185 min fractions by adopting the same HSCCC condition, concentrating and drying to obtain 20 mg of chlorogenic acid with the purity of 95.1 percent. The liquid chromatography (HPLC) conditions for analyzing the purity of chlorogenic acid in the bamboo leaf extract are the same as above.
Claims (4)
1. A method for preparing high-purity chlorogenic acid from bamboo leaf extract is characterized by comprising the following process steps:
1) separating by macroporous resin: loading folium Bambusae extract as raw material onto macroporous adsorbent resin, sequentially eluting with distilled water, 60% ethanol and 95% ethanol, collecting eluate and eluate, and concentrating to obtain concentrate A and concentrate B;
2) high-speed countercurrent chromatographic separation: separating and purifying the concentrate A and the concentrate B in an HSCCC chromatograph by taking a two-phase solvent system, preparing a mixed solution in a separating funnel by taking the two-phase solvent system, and taking the upper layer as a stationary phase and the lower layer as a mobile phase; pumping a stationary phase into an HSCCC chromatograph at a speed of 10-20 mL/min, rotating a main machine at 600-1000 rpm after a pipeline is completely filled with the stationary phase, simultaneously pumping a mobile phase at a speed of 1-3 mL/min until the mobile phase flows out and an ultraviolet detector monitors that a base line is stable, injecting a proper amount of concentrate A or B dissolved in the mobile phase into the HSCCC chromatograph by using a sample injector, automatically collecting effluent liquid at an outlet according to running time, carrying out HPLC (high performance liquid chromatography) detection on the effluent liquid, respectively combining the collected liquids with chlorogenic acid purity of more than 90%, and recovering a solvent by using a rotary evaporator to obtain a chlorogenic acid monomer;
the two-phase solvent system comprises 30-45 volume percent of ethyl acetate, 5-15 volume percent of methanol, 5-15 volume percent of acetic acid and 30-50 volume percent of water, or 30-45 volume percent of ethyl acetate, 5-15 volume percent of acetonitrile, 5-15 volume percent of acetic acid and 30-50 volume percent of water, wherein the upper phase is a stationary phase, and the lower phase is a mobile phase.
2. The method for preparing high-purity chlorogenic acid from bamboo leaf extract in the step 1) as claimed in claim 1, wherein the concentration of bamboo leaf extract in the step 1) is as follows: 5-100 mg/mL of aqueous solution based on dry weight of the extract.
3. The method for preparing chlorogenic acid with high purity from bamboo leaf extract of claim 1, wherein the macroporous adsorbent resin type in step 1) is D101 or XAD-7 HP.
4. The method for preparing chlorogenic acid from bamboo leaf extract as claimed in claim 1, wherein the flow rate of sample loading in step 1) is 1-4 BV/h, the quality of the sample loading extract is less than or equal to 1 g/g resin, the elution volume of water is 3-6 BV, the elution volume of 60% ethanol is greater than or equal to 4BV, and the flow rate of elution is 1-4 BV/h.
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| CN109809996B (en) * | 2019-02-19 | 2021-09-24 | 西昌学院 | Method for preparing chlorogenic acid from potato peels |
| CN110015959B (en) * | 2019-03-26 | 2021-09-24 | 北京林业大学 | Method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves |
| CN115433085B (en) * | 2022-10-17 | 2023-05-16 | 南京久安源环保科技有限公司 | Production process for extracting bamboo leaf flavone and/or chlorogenic acid from bamboo leaves |
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