CN106916065B - Method for preparing high-purity chlorogenic acid from burdock roots - Google Patents
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Abstract
A method for separating and purifying chlorogenic acid from burdock roots is characterized by comprising the following steps: (1) preparing a burdock root extracting solution; pulverizing dried radix Arctii, soaking in alkaline water for 30min, extracting with ultrasound or microwave, and adjusting pH of the extractive solution to 11-12; (2) purifying and enriching; loading the extracting solution obtained in the step (1) to an anion exchange column, wherein the column filler in the anion exchange column is weakly alkaline anion resin, sequentially eluting with distilled water to remove impurities such as saccharides and the like, eluting with alkali liquor, adjusting the pH of the eluent with acid water to 2-5, extracting with ethyl acetate with the same volume for three times, combining ethyl acetate phases, concentrating under reduced pressure and drying to obtain a burdock root extract; (3) the method for separating and purifying the chlorogenic acid by adopting the high-speed counter-current chromatography takes the alkaline water as the extraction solvent, greatly improves the solubility of the chlorogenic acid, does not need organic solvent extraction and enrichment, does not need a fixed carrier in the separation process, does not have dead adsorption, and has the advantages of simple process, high speed and high efficiency, good repeatability and high purity of the obtained target compound.
Description
Technical Field
The invention relates to a method for extracting, enriching and separating effective components from food, in particular to an extraction method for preparing high-purity chlorogenic acid from burdock roots.
Background
Great burdock achene (A. B.)ArctiumlappaL.) is a two-year-old herbaceous plant of the Compositae, can be used as both medicine and food, is imported from China into Japan and is improved into high-quality vegetables, and is planted in large quantities in Feng county, Pei county and cang mountain of Shandong province in China. The burdock root is the main edible part of the burdock and has excellent health care value, and the record of the compendium of materia medica records that the burdock root can ' dredge the twelve main channels, remove the bad breath of the five internal organs ' and lighten the body and resist the aging after long-time taking '. The medical research proves that the burdock root has the effects of strengthening the spleen and stomach, clearing away heat and toxic materials, protecting blood vessels and the like, and has the treatment effect on diseases such as hypertension, diabetes, arteriosclerosis and the like.
The burdock root is rich in components such as inulin, organic acid, sterol and the like, wherein chlorogenic acid is a main component of an organic acid compound and is often used as an important index component in the burdock root for quality evaluation at present. Chlorogenic acid has wide bioactivity, has the functions of resisting bacteria, viruses, tumors, blood pressure, blood fat, free radicals, exciting central nervous system and the like, and the research on the biological activity of the chlorogenic acid by modern science is deeply carried out in various fields of food, health care, medicine, daily chemical industry and the like.
The literature search of the prior art finds that:
chinese patent application No. 200510000484.0 discloses a process for extracting chlorogenic acid from burdock leaves, which requires degreasing with chloroform, extracting and enriching the degreased sample with acid water with ethyl acetate, eluting, concentrating and recrystallizing with AB-8 resin column twice to obtain chlorogenic acid, the operation steps of early enrichment and later two-step enrichment are complicated, the energy consumption is large, and a large amount of organic chemical reagents are consumed.
Chinese patent application No. CN03111946.8 also discloses a process for extracting chlorogenic acid from burdock leaves, the extraction solvent used is an acidic organic solvent, the obtained burdock leaf crude extract passes through a polyamide column, is eluted by water and methanol, and the eluent is concentrated and refined to obtain the pure chlorogenic acid.
The invention of Chinese patent application number 201310726468.4 discloses a method for extracting eucommia chlorogenic acid by cell wall breaking at low temperature, which comprises the steps of soaking and destroying the cuticle on a leaf by alkaline water with pH of 9, then dynamically extracting for 2 hours at normal temperature by pure water with pH of 2 which is 7 times of that, repeatedly extracting by acid water, and then preparing eucommia chlorogenic acid by membrane treatment, reverse osmosis, resin elution and other processes.
The invention with Chinese patent application number of 201010542548.0 discloses a method for separating and purifying chlorogenic acid from eucommia ulmoides leaves, which is to separate and purify high-purity chlorogenic acid by high-speed counter-current chromatography for 200min by taking ethyl acetate/n-butanol/water as a solvent system from the eucommia ulmoides leaves.
The invention of Chinese patent application No. 201510316229.0 discloses a method for separating and purifying monomeric compounds in mahonia leaves by using high-speed counter-current chromatography, which uses n-hexane-ethyl acetate-methanol-water as a solvent system, and purifies for 100min by using high-speed counter-current chromatography, so that 18.32mg of high-purity chlorogenic acid can be obtained from an ethyl acetate phase of an ethanol extract of mahonia leaves.
Lo in auspicious treatise on functional ingredients of burdock and research on antioxidant and antibacterial activity thereof (Jiangnan university, 2010: 34-36) adopts 70% ethanol solution as an extraction solvent, extracts are concentrated and then are respectively extracted by petroleum ether, ethyl acetate, n-butanol and water to obtain four parts, wherein the ethyl acetate component is subjected to column chromatography pretreatment and then is subjected to high-speed countercurrent chromatography n-butanol-acetic acid-water (4: 1: 5) system to prepare chlorogenic acid with the purity of 98.3% respectively.
Chengdai et al, in food science (2008, 29(11): 298-299) "research on separating and purifying chlorogenic acid by high-speed counter-current chromatography, found that 40mg of chlorogenic acid with purity of 98.1% can be obtained from a honeysuckle extract by using a n-butyl alcohol-glacial acetic acid-water (4: 1: 5, V/V) system for 6 h.
Zhang Xia et al found that 11.2mg of chlorogenic acid with purity of 98.2% was obtained by using n-butanol-acetic acid-water (4: 1: 5) as a solvent system and preparing for 4h in journal of drug analysis (2010, 30 (1): 106-109) 'separating and purifying chlorogenic acid in honeysuckle flower by high-speed counter-current chromatography'.
Shiberyang et al, food science (2013, 34(13): 87-90) "high-speed countercurrent chromatographic separation of chlorogenic acid and isochlorogenic acid in purple sweet potato" found that 28mg of chlorogenic acid with purity of 98.5% was obtained from 200mg of purple sweet potato extract by preparing a separation compound using ethyl acetate-methanol-water (3: 1: 5) as a solvent system over 4 hours.
The solvent used in the above method is neutral or acidic extraction solvent such as water, acid water, water-alcohol, and acidic alcohol solution, and chlorogenic acid in the obtained extractive solution is in molecular state; the obtained extract is subjected to ethyl acetate extraction enrichment or acid-base treatment for preliminary purification, and the pretreatment operation steps are relatively complex. The method for extracting eucommia chlorogenic acid by breaking cell wall and low temperature in the prior patent still belongs to the acid extraction category by using acid water for extraction in the later period and aiming at destroying the cuticle of leaves although the method carries out pretreatment by using alkali water. In addition, the high-speed countercurrent separation process involved in the previous research has the problems of low preparation amount and long preparation time, the preparation amount at one time is up to 40mg, and the required time is basically over 100 min.
Disclosure of Invention
The invention provides a method for quickly and efficiently extracting and separating chlorogenic acid from burdock roots, which is used for extracting and enriching the chlorogenic acid by alkaline water and separating and purifying by high-speed counter-current chromatography, thereby obtaining high-purity chlorogenic acid (the purity is more than 90%). The scheme overcomes the problems of low preparation amount, long preparation time, more types of required system solvents and the like of the conventional purification method, greatly improves the production efficiency and reduces the production cost.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a method for separating and purifying chlorogenic acid from burdock root comprises the following steps:
(1) preparing a burdock root extracting solution;
pulverizing dried radix Arctii, soaking in alkaline water for 30min, extracting with ultrasound or microwave, and adjusting pH of the extractive solution to 11-12;
(2) purifying and enriching;
and (2) loading the extracting solution obtained in the step (1) to an anion exchange column, wherein column packing in the anion exchange column is weak-base anion resin, eluting by using distilled water in sequence to remove impurities such as saccharides and the like, eluting by using alkali liquor, adjusting the pH of the eluent to 2-5 by using acid water, extracting by using ethyl acetate with the same volume for three times, combining ethyl acetate phases, concentrating under reduced pressure and drying to obtain the burdock root extract.
(3) Separating and purifying chlorogenic acid by adopting high-speed counter-current chromatography: ethyl acetate, methanol and water are mixed according to a volume ratio of 4-5: 0.1-1: 4-5, placing the mixed solution in a separating funnel, standing for 30min, taking the upper layer as a stationary phase, and taking the lower layer as a mobile phase; pumping the stationary phase, filling the high-speed counter-current chromatographic column with the stationary phase, starting a rotating speed regulator, pumping the mobile phase, dissolving the burdock root extract obtained in the step (2) in the stationary phase and the mobile phase which are equal in number when the mobile phase flows out and the reading of the ultraviolet detector is stable, carrying out sample injection, observing a chromatogram, collecting fractions when a target peak appears, carrying out rotary concentration to remove an organic solvent, and carrying out freeze drying to obtain the high-purity chlorogenic acid.
The method is characterized in that the alkali in the alkaline water in the step (1) is an alkaline sample such as potassium hydroxide, sodium carbonate, potassium carbonate, sodium methoxide, sodium ethoxide and the like, and the concentration is 0.1-1 mol/L.
In the step (2), the weak base anion resin is diethylamine anion exchange resin, macroporous weak base styrene anion exchange resin or weak base anion exchange resin D301.
In the step (2), the acid water for adjusting the pH value of the eluent is hydrochloric acid, sulfuric acid, phosphoric acid and formic acid with the concentration of 1mol/L-5 mol/L.
In the step (3), the high-speed counter-current chromatograph is the same-field TBE-3000C, and the flow rate of the mobile phase is 5-12 mL/min.
The invention has the beneficial effects that: compared with the existing chlorogenic acid extraction technology with neutral and acidic extractants, the method creatively utilizes the alkaline water as the extraction solvent, so that the chlorogenic acid reacts with the alkali to form salt, the solubility of the chlorogenic acid in the extractant can be greatly improved, and compared with the neutral and acidic extractants in the prior literature, the solubility of the chlorogenic acid can be improved by more than 50%; the purity of chlorogenic acid in a sample to be prepared can be greatly improved by enrichment means such as anion exchange resin and ethyl acetate extraction after pH adjustment; the established high-speed counter-current chromatographic separation method has the advantages of high flow rate, short preparation time, preparation efficiency 5-10 times that in the literature and outstanding effect.
Drawings
FIG. 1 is a high-speed countercurrent chromatogram.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
a method for preparing high-purity chlorogenic acid from burdock root comprises the following steps:
(1) preparation of burdock root extract
Pulverizing dry decoction pieces of radix Arctii, sieving with 40 mesh sieve, collecting 100g sample, ultrasonic extracting with 0.1mol/L sodium hydroxide at a material-to-liquid ratio of 1: 10 for three times (1.5 hr, 1 hr and 0.5 hr respectively), and mixing extractive solutions; the pH is adjusted to 11-12 with 0.1mol/L hydrochloric acid.
(2) Purification and enrichment
Loading the burdock root extract into a diethylamine anion exchange resin chromatographic column at a loading rate of 3BV/h, eluting with distilled water at 5BV/h for 2h, then eluting with 0.1mol/L sodium hydroxide solution at 3BV/h for 1h, and receiving 500mL of the solution as a unit, and combining the eluates; adjusting pH to 4-5 with 1mol/L hydrochloric acid, extracting with equal volume of ethyl acetate for three times, mixing ethyl acetate phases, concentrating under reduced pressure, and drying to obtain radix Arctii extract 3.6 g.
(3) Separating and purifying chlorogenic acid by high-speed countercurrent chromatography
Pouring ethyl acetate, methanol and water into a separating funnel according to a volume ratio of 5: 1: 5, namely pouring 1000mL of ethyl acetate, 200mL of methanol and 1000mL of water, shaking uniformly, and standing for 30min for later use. The upper layer is taken as a stationary phase, and the lower layer is taken as a mobile phase. Taking 450mg of the burdock root extract prepared in the step (2), respectively dissolving the extract in a dissolving system consisting of 15mL of upper and lower phases in equal amount, ultrasonically dissolving the extract, and separating the extract by high-speed countercurrent chromatography of Homopodia TBE-3000C. Setting the temperature of the constant temperature circulator at 25 ℃, starting the ultraviolet detector, pumping the stationary phase at 40mL/min, starting the main machine to adjust the rotating speed to 800rpm after the stationary phase is filled in the pipeline, and pumping the mobile phase at the flow rate of 10 mL/min. And when the mobile phase flows out and is stable at the limit, injecting sample by using a sample injection valve, recording a countercurrent chromatogram, collecting a fraction (10 mL/tube), detecting the fraction by using a high performance liquid chromatograph, performing rotary concentration to remove the organic solvent, and performing freeze drying to obtain the high-purity chlorogenic acid.
(4) Purity testing of target Compounds
The HPLC detection conditions were as follows: gemini NX-C18 (250X 4.6 mm, 5 μm), column temperature 25 deg.C; mobile phase: methanol-0.1% formic acid water (27: 73); the flow rate is 1 mL/min; the sample volume is 10 mu L; the detection wavelength was 330 nm.
Collecting the target compound: detecting the collected fractions to find that the target compound (chlorogenic acid) flows out within 23-38 min of the high-speed counter-current chromatography.
And (3) measuring the purity of the target compound, collecting fractions of 26-35 min of high-speed countercurrent chromatography, removing the organic solvent, freeze-drying to obtain 108.3mg of a sample, and measuring the purity to be 93.1% by a high performance liquid chromatography area normalization method.
Example 2:
the same parts of this embodiment as embodiment 1 will not be described again, but the differences are: a method for preparing high-purity chlorogenic acid from radix Arctii comprises (3) separating and purifying chlorogenic acid by high-speed countercurrent chromatography with Homopsis TBE-3000C, pouring ethyl acetate, methanol and water at volume ratio of 4: 0.1: 4, namely ethyl acetate 1000mL, methanol 200mL and water 1000mL into a separating funnel, shaking uniformly, and standing for 30 min. The upper layer is taken as a stationary phase, and the lower layer is taken as a mobile phase.
Collecting the target compound: detecting the collected fractions to find that the target compound (chlorogenic acid) flows out within 25-43 min of high-speed counter-current chromatography.
And (3) measuring the purity of the target compound, collecting fractions of 28-37 min of high-speed countercurrent chromatography, removing an organic solvent, freeze-drying to obtain a sample of 80.1mg, and measuring the purity of 94.2% by a high performance liquid chromatography area normalization method.
Example 3:
the same parts of this embodiment as embodiment 1 will not be described again, but the differences are:
(1) preparing a crude extract of burdock root:
drying and crushing the waste outer skin of the processed burdock root, sieving the crushed burdock root with a 40-mesh sieve, sampling 50g of the crushed burdock root, and ultrasonically extracting the crushed burdock root for 1 hour by using 500mL of 1mol/L potassium hydroxide solution; repeatedly extracting once, mixing the extractive solutions, adjusting pH to 3-4 with 1mol/L hydrochloric acid, extracting with equal volume of ethyl acetate for three times, concentrating under reduced pressure, and drying to obtain radix Arctii extract 2.1 g;
(2) high-speed countercurrent chromatographic separation:
dissolving 240mg of crude extract of radix Arctii ethyl acetate prepared in (1) in 5mL of a dissolving system composed of upper and lower phases at the same amount respectively, and dissolving with ultrasound at a ratio of ethyl acetate, methanol and water of 5: 0.5: 4. The separation is carried out by high-speed countercurrent chromatography of Homopield TBE-3000C, the preparation steps and the purity detection method are the same as the example 1, 59.4mg of sample is obtained after evaporation, organic solvent and freeze drying, and the purity is 93.6 percent as measured by a high performance liquid chromatography area normalization method.
Example 4:
a method for preparing high-purity chlorogenic acid from burdock roots mainly comprises the following steps: soaking 100g of dried and crushed burdock root in 0.1 mol/L2000 mL potassium hydroxide for 30min, extracting for 60min by adopting ultrasonic, and adjusting the pH value of the extract to 12; filtering the extractive solution, loading on diethylamine anion exchange resin exchange column, eluting with 1500mL distilled water to remove impurities such as saccharide, eluting with 1500mL 0.1mol/L potassium hydroxide, and adjusting pH of the eluate to 3 with hydrochloric acid; extracting the combined eluates with ethyl acetate of the same volume for three times, combining ethyl acetate phases, and concentrating to obtain dry radix Arctii extract; mixing ethyl acetate, methanol and water at volume ratio of 5: 1: 4, standing in a separating funnel for 30min, separating the upper layer as stationary phase and the lower layer as mobile phase by high speed countercurrent chromatography of Hotan TBE-3000C; and observing a countercurrent chromatogram, collecting 10 mL/bottle of fractions when a target peak appears, monitoring the purity by using a liquid phase, combining samples with the purity of more than 90%, performing rotary concentration to remove an organic solvent, and performing freeze drying to obtain the high-purity chlorogenic acid.
A solvent system with a proper distribution coefficient is selected, and generally, the separation effect is good when the distribution coefficient K value is between 0.5 and 2. From the aspect of preparation time, on the premise of meeting the requirement of purity, the shorter the time is, the higher the preparation efficiency is, and the higher the yield value per unit time is.
And (3) K value determination: the separation system is balanced in advance, 1mL of each of the upper and lower phases is taken and placed in a 5mL centrifuge tube with a cover, and the refined burdock root (about 1-3 mg) is added and shaken to dissolve. Standing, respectively placing 0.5mL of upper and lower phase in 2mL centrifuge tube with cover, blowing with nitrogen, dissolving in 1mL methanol, performing HPLC detection, and recording peak areas of upper and lower phase as A1And A2，K= A1/A2The results are shown in Table 1.
And (3) investigating separation efficiency: the lower phase was pumped at different flow rates and the separation effect of chlorogenic acid at different flow rates was examined separately and the results are shown in table 2.
As can be seen from table 1, in the petroleum ether-ethyl acetate-methanol-water system, the distribution coefficient measured is slightly small, and it is found that the solubility in the stationary phase is too small, and when separation is performed by high-speed countercurrent chromatography using the same-field TBE-3000C, the elution rate of the target compound is too fast, and it is difficult to perform effective separation, and in the actual high-speed countercurrent separation test, it is confirmed that the solubility of the sample is insufficient and the target compound is not well separated and purified, and therefore, it is not suitable as a dissolved system for separation. As can be seen from Table 2, the target compound can be effectively separated even at a flow rate of 10mL/min, the prepared high-speed counter-current chromatogram is shown in FIG. 1, and the purity of the collected component to be detected is higher than 90% after liquid chromatography analysis.
The invention finds that the measured distribution coefficient is more suitable in the separation system of ethyl acetate-methanol-water and ethyl acetate-ethanol-water, so the system is selected as a solvent system for separating chlorogenic acid. Through experiments, the target compound with higher purity can be separated and purified by the ethyl acetate-methanol-water (4-5: 0-1: 4-5) compared with other proportion systems at a high preparation flow rate of 10 mL/min.
TABLE 2 Peak time for different flow rates to prepare target Components
Comparative example one:
according to Chinese patent application No. CN03111946.8, 100g of dried and pulverized burdock root is respectively extracted by 2 times of 2000mL of ethanol (pH 2) at 78 ℃ for 2h and 1h under reflux, the filtrate is combined after each extraction, and the crude extract of the burdock root is concentrated under reduced pressure. Loading the crude extract of radix Arctii on polyamide column, eluting with water and methanol, concentrating and refining the eluate to obtain high-purity chlorogenic acid.
Comparative example two:
according to Chinese patent application No. CN200510000484.0, adding 100g of dried and pulverized radix Arctii into 1300mL of chloroform, reflux-extracting for 80 min, filtering, and discarding the chloroform layer; adding a chloroform-extracted sample into 1200 mL of sulfuric acid water solution with the pH value of 3.5, refluxing and extracting for 2 hours, and concentrating to 100mL of crude extract; extracting the crude extract with 2000mL ethyl acetate for 4 times, and discarding the ethyl acetate part; passing the residual solution through AB-8 macroporous resin, and eluting with acid water with pH of 3.5 and 30% ethanol respectively; concentrating the ethanol eluate, loading onto AB-8 macroporous resin, eluting with acid water with pH of 3.5 and 30% ethanol, concentrating, and recrystallizing to obtain high purity chlorogenic acid.
Comparative example three:
according to the research of separating and purifying chlorogenic acid by high-speed counter-current chromatography (food science, Chengdi et al, 2008), 50g of burdock root is crushed and then accurately weighed, 70% ethanol solution is used for extracting for 2 times in 70 ℃ water bath with the material-liquid ratio of 1: 10 and the pH value of 4, the extraction is carried out for 1.5h each time, the filtrates are combined, the filtrate is decompressed and concentrated to about 100ml at the temperature of 60 ℃, petroleum ether and ethyl acetate are sequentially used for extracting for three times respectively, and the ethyl acetate layer is decompressed and concentrated at the temperature of 60 ℃. Separating with n-butanol-glacial acetic acid-water (4: 1: 5, V/V) system to obtain high purity chlorogenic acid.
A large number of test results show that only the technical scheme of the invention can obtain the chlorogenic acid with the purity of more than 90 percent from the burdock roots within 60 min.
Claims (3)
1. A method for separating and purifying chlorogenic acid from burdock roots is characterized by comprising the following steps:
(1) preparing a burdock root extracting solution;
pulverizing dried radix Arctii, soaking in alkaline water for 30min, extracting with ultrasound or microwave, and adjusting pH of the extractive solution to 11-12;
(2) purifying and enriching;
loading the extracting solution obtained in the step (1) to an anion exchange column, wherein the column filler in the anion exchange column is weakly alkaline anion resin, sequentially eluting with distilled water to remove impurities such as saccharides and the like, eluting with alkali liquor, adjusting the pH of the eluent with acid water to 2-5, extracting with ethyl acetate with the same volume for three times, combining ethyl acetate phases, concentrating under reduced pressure and drying to obtain a burdock root extract; the weak base anion resin is diethylamine anion exchange resin, macroporous weak base styrene anion exchange resin or weak base anion exchange resin D301;
(3) separating and purifying chlorogenic acid by adopting high-speed counter-current chromatography: the flow rate of a mobile phase of the high-speed countercurrent chromatograph is 5-12 mL/min; ethyl acetate, methanol and water are mixed according to a volume ratio of 4-5: 0.1-1: 4-5, placing the mixed solution in a separating funnel, standing for 30min, taking the upper layer as a stationary phase, and taking the lower layer as a mobile phase; pumping the stationary phase, filling the high-speed counter-current chromatographic column with the stationary phase, starting a rotating speed regulator, pumping the mobile phase, dissolving the burdock root extract obtained in the step (2) in the stationary phase and the mobile phase which are equal in number when the mobile phase flows out and the reading of the ultraviolet detector is stable, carrying out sample injection, observing a chromatogram, collecting fractions when a target peak appears, carrying out rotary concentration to remove an organic solvent, and carrying out freeze drying to obtain the high-purity chlorogenic acid.
2. The method for separating and purifying chlorogenic acid from burdock root according to claim 1, characterized in that the alkali in the alkaline water in step (1) is potassium hydroxide, sodium carbonate, potassium carbonate, sodium methoxide and sodium ethoxide alkaline samples, and the concentration is 0.1mol/L-1 mol/L.
3. The method for separating and purifying chlorogenic acid from burdock root as claimed in claim 1, wherein in step (2), the acid water for adjusting the pH value of the eluent is hydrochloric acid, sulfuric acid, phosphoric acid, formic acid of 1mol/L-5 mol/L.
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