CN114191467A - Method for extracting high-purity alkaloid from corydalis saxicola bunting - Google Patents
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Abstract
The invention discloses an extraction and purification method for obtaining high-purity alkaloid from corydalis saxicola bunting, which comprises the following steps: (1) crushing; (2) extracting crude alkaloid from corydalis saxicola bunting with ethanol solution; (3) alkali dissolution; (4) centrifuging; (5) adsorbing and eluting by adopting macroporous resin; (6) concentrating and drying to obtain high-purity alkaloid. The method has the advantages of simple operation, mild and easily-controlled conditions, simple process route, less operation steps, less alkaloid content loss in the extraction and purification process and high product purity.
Description
Technical Field
The invention relates to a method for extracting high-purity alkaloid from corydalis saxicola bunting, belonging to the technical field of extraction and purification of bioactive components in corydalis saxicola bunting.
Background
Corydalis saxicola bunting (Latin name:Cordalis saxicolabunting) is also known as: corydalis tuber, corydalis saxicola, golden thread and chrysanthemum golden thread, which are whole herbs of corydalis saxicola bunting of corydalis genus of Papaveraceae familyPerennial herbaceous plants grow in gaps of rocks at forest borders of mountain lands, and are mainly distributed in Gansu, Hubei, Guangxi, Sichuan, Guizhou, Yunnan and other places. Meanwhile, corydalis saxicola bunting is used as a strong medicine with Guangxi characteristics, has a long application history in Guangxi folks, and is a specific medicine for folks to treat diseases such as viral hepatitis.
The main active ingredients of corydalis saxicola bunting are generally considered to be alkaloid compounds: such as berberine, dehydrocavidine, cavidine, staurosine, beta-hydroxypropamide, chelerythrine, corydaline, tetrahydrofangchinamine, protopine, galbanine, hydramine, coptisine, african tetrandrine, berberine, allocryptopine, palmatine, etc.
Corydalis saxicola bunting is used as a medicine by whole herbs, and has the effects of easing pain, calming, resisting inflammation, resisting bacteria and resisting tumors. Corydalis saxicola bunting injection taking corydalis saxicola bunting as a raw material and taking main active ingredients as alkaloid is widely applied to clinically treating a series of liver-related diseases such as liver cirrhosis, liver cancer, hepatitis and the like.
At present, the common extraction methods of corydalis saxicola bunting alkaloids comprise an acid water extraction method, an alcohol solvent extraction method, a lipophilic organic solvent extraction method, an enzyme-assisted solvent extraction method and the like, for example, in patent CN 102600247A, CN 105055534A, an enzyme-assisted ethanol extraction method is used, so that the total alkaloid yield of corydalis saxicola bunting alkaloids is improved to a certain extent, but the process steps are more complicated than that of the traditional ethanol extraction method, the operation fault tolerance rate is reduced, a series of process costs including enzymes are improved, and the industrial amplification production is not facilitated; for example, in patent CN 112656842a, the extraction process of the patent uses acid water extraction, and the acid wastewater generated in the extraction process has certain environmental protection challenges, and also affects the structural change of part of alkaloids under acidic conditions.
Meanwhile, in order to ensure the purity of corydalis saxicola bunting alkaloid, the extract must be separated and purified to meet the purity requirement in the fields of medicine and the like. The existing purification methods comprise an acid-soluble alkali precipitation method, a macroporous resin method, a silica gel column chromatography method and the like, for example, in the publication No. CN 1453277A, the macroporous resin is used for purifying the corydalis saxicola bunting alkaloid, but the whole water solubility of the sample is not ideal, and the solubility is less than 1 mg/mL.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity corydalis saxicola bunting alkaloid, which has the advantages of low cost, convenience and easiness in industrial amplification.
The invention adopts the following steps to realize the extraction and purification of the high-purity corydalis saxicola bunting alkaloid.
The solid-liquid ratio is g/mL, the concentration of ethanol is volume percent, and the concentration of sodium hydroxide solution is mass percent.
A method for extracting high-purity alkaloid from corydalis saxicola bunting comprises the following steps:
(1) crushing: crushing the dried corydalis saxicola bunting whole grass to obtain corydalis saxicola bunting crushed grass;
(2) alcohol extraction: placing the corydalis saxicola bunting in the step (1) into an extraction container, adding 50-95% ethanol according to a solid-to-liquid ratio of 1: 6-1: 14, continuously refluxing and extracting for 1-3 hours at 50-90 ℃, extracting for 1-3 times, filtering and combining extracting solutions, and concentrating and drying filtrate under reduced pressure to obtain crude alkaloid;
(3) alkali dissolution: adding crude alkaloid in the step (2) into a mixture of crude alkaloid and crude alkaloid according to a solid-liquid ratio of 1: 2-1: 6 (g/mL) is added with alkali liquor for dissolution to obtain sample alkali liquor;
(4) centrifuging: centrifuging the sample alkali liquor in the step (3) to obtain a sample centrifugation supernatant;
(5) macroporous resin adsorption elution: adsorbing the supernatant obtained in the step (4) by using macroporous resin, then eluting by using a hydrochloric acid aqueous solution and an ethanol-hydrochloric acid-aqueous solution in sequence, and collecting an ethanol eluent to obtain a sample eluent;
(6) and (3) drying: and (5) concentrating the sample eluent in the step (5) under reduced pressure, and drying to obtain the high-purity alkaloid.
In the step (2), the concentration of the ethanol is 60-80%, the solid-to-liquid ratio (g/mL) is 1: 10-1: 14, the extraction temperature is 70-90 ℃, and the extraction time is 1-2 h. Preferably, the extraction is carried out for 3 times under the conditions that the ethanol concentration is 70%, the extraction temperature is 80 ℃, the extraction time is 1.5 h, and the material-liquid ratio is 1: 12.
In the step (3), the alkali liquor is a sodium hydroxide solution with a mass percentage concentration of 0.002-0.003%, and the solid-to-liquid ratio of the crude alkaloid to the alkali liquor is 1: 2-1: 6 (g/mL).
In the step (4), the rotating speed of the centrifugal machine is 2500-3500 r/min, and the centrifugal time is 20-40 min.
In the step (5), the macroporous resin is selected from AB-8, ADS-21, ADS-17 or D3520, the pH value of the hydrochloric acid aqueous solution is 4-6, the pH value of the ethanol-hydrochloric acid-aqueous solution is 4-6, and the concentration of the ethanol is 20-60%.
In the steps (2) and (6), the temperature of the reduced pressure concentration is 60-90 ℃, and the pressure of the reduced pressure concentration is 0.06-0.08 MPa.
In the step (6), the drying mode is freeze drying, evaporation drying, spray drying or vacuum drying.
The invention has the following advantages:
(1) the extraction method comprises the following steps: the method uses the ethanol as the extraction solvent for extraction, reduces the requirements of other methods such as an enzyme method, a microwave extraction method, acid/alkali extraction and the like on extraction instruments, simplifies the extraction steps and enlarges the application range of the method.
(2) Optimizing an extraction process: the ethanol used as the extraction solvent is safe, easy to obtain and low in cost, and meanwhile, on the basis of four single-factor experiments of extraction temperature, extraction time, ethanol concentration and extraction feed-liquid ratio, orthogonal experiments are carried out to determine the optimal extraction process so as to obtain higher-yield alkaloid.
(3) Selecting a purification method: the method is based on that various alkaloids in the corydalis saxicola bunting contain phenolic hydroxyl structures, the solubility in alkali is better, and the loss of the alkaloids can be avoided by adding a small amount of alkali for dissolution, so that the polarity of the corydalis saxicola bunting alkaloids is changed by using pH regulation by adopting an alkali-dissolution combined macroporous resin purification method, and the molecular property and the ionic property of the corydalis saxicola bunting alkaloids are gradually regulated by using the Van der Waals force adsorption characteristic of macroporous resin, so that the corydalis saxicola bunting alkaloids are purified in a grading way, and the method has the advantages of simple steps, high recovery rate, high purity, high recovery rate and good safety.
(4) In the invention, partial protein isoelectric point is precipitated by adjusting the pH value during purification, and then most of the rest protein, pigment and polysaccharide are removed by macroporous resin, so that the combination of other impurity removal methods is avoided, and the purification step is further simplified. The macroporous resin has the advantages of low cost, large sample loading amount and repeated cyclic utilization, so the purification speed is high, and the high-purity corydalis saxicola bunting alkaloid can be rapidly prepared in a large amount.
(5) The method performs orthogonal test on the basis of single-factor experiment to optimize the extraction process so as to obtain higher extraction yield. Meanwhile, most impurities are removed by an alkali dissolution-macroporous resin method, and high-purity corydalis saxicola bunting alkaloid can be obtained rapidly, efficiently and massively. The invention is amplified from gram-level extraction and purification in a laboratory to kilogram-level extraction and purification, and has certain guiding significance for industrial amplification production.
Drawings
FIG. 1 example 1 extraction temperature-absorbance plot in an orthogonal assay;
FIG. 2 graph of extraction time vs. absorbance in the orthogonal assay of example 1;
FIG. 3 plot of ethanol concentration versus absorbance in the orthogonal assay of example 1;
FIG. 4 graph of extraction time vs. absorbance in the orthogonal assay of example 1;
FIG. 5 is a process flow diagram of the present invention.
Detailed Description
Example 1 orthogonal experiments
Weighing several groups of 1.0 g corydalis saxicola bunting powder, extracting according to the extraction conditions in Table 1, extracting for 3 times, diluting the extract and measuring the absorbance at 346 nm.
(1) Selection of the maximum wavelength
As dehydrocavidine is a representative alkaloid compound of corydalis saxicola bunting and has high content in corydalis saxicola bunting, the content of alkaloid in corydalis saxicola bunting extract can be indirectly reflected by an absorbance method by using dehydrocavidine as a reference. The sample solution and the dehydrocavidine standard solution are respectively scanned in the wavelength range of 200-800 nm, and the result shows that 346 nm is the maximum absorption wavelength of the two solutions. At this wavelength, the alkaloid concentration is directly proportional to the absorbance.
(2) Selection of extraction temperature
Weighing several groups of 1.0 g corydalis saxicola bunting powder, adding 80% ethanol according to a material-liquid ratio of 1:10 (g/mL), extracting at 50, 60, 70, 80 and 90 deg.C for 2 hr for 3 times, diluting the extractive solution, and measuring absorbance at 346 nm.
The result of the selection of the extraction temperature is shown in fig. 1, and it can be seen that the relative alkaloid content gradually increases with the increase of the extraction temperature, and although the relative alkaloid content is highest at 90 ℃, the excessive temperature may cause thermal decomposition of alkaloid and destroy the structure, so the optimal extraction temperature is 80 ℃.
(3) Selection of extraction time
Weighing several groups of 1.0 g corydalis saxicola bunting powder, adding 80% ethanol according to a material-liquid ratio of 1:10 (g/mL), extracting at 80 deg.C for 1, 1.5, 2, 2.5, and 3 hr for 3 times, diluting the extractive solution, and measuring its absorbance at 346 nm.
The result of the selection of the extraction time is shown in fig. 2, and it can be seen from the figure that the relative alkaloid content gradually increases with the increase of the extraction time, and meanwhile, after the extraction time exceeds 1.5 hours, the relative alkaloid content gradually tends to be stable, and the optimal extraction time is 1.5 hours in comprehensive consideration.
(4) Selection of ethanol concentration of extraction solution
Weighing several groups of 1.0 g corydalis saxicola bunting powder, adding 60%, 70%, 80%, 90% and 95% ethanol according to a material-liquid ratio of 1:10 (g/mL), extracting at 80 deg.C for 2 hr for 3 times, diluting the extractive solution, and measuring its absorbance at 346 nm.
The results of selecting ethanol concentration of the extract solution are shown in FIG. 3, which shows that the relative alkaloid content increases with the increase of ethanol concentration when the ethanol concentration is within 60-70%, but the alkaloid content decreases with the increase of ethanol concentration when the ethanol concentration is within 70-95%, and the optimal ethanol concentration is 70%.
(5) Selection of ratio of extract to liquid
Weighing a plurality of groups of 1.0 g corydalis saxicola bunting powder, and respectively mixing the powder with the liquid-material ratio of 1:6, 1:8, 1:10 and 1: 12. 1:14 (g/mL), 80% ethanol was added, extraction was carried out at 80 ℃ for 2 hours for 3 times in total, and the extract was diluted and its absorbance at 346 nm was measured.
The result of selecting the ratio of the feed to the liquid is shown in figure 4, and the figure shows that the content of alkaloid in the extracting solution is gradually increased along with the increase of the adding amount, and the ratio of the feed to the liquid reaches 1: after 12 (g/mL), the alkaloid content tends to be stable, so the optimal feed-liquid ratio is 1:12 (g/mL).
TABLE 1 orthogonal Experimental Table
The results of the orthogonal experiment are shown in table 1, and the influence of various factors on the alkaloid content of the extracting solution is shown as follows: the material-liquid ratio (D) > the extraction temperature (A) > the ethanol concentration (C) > the extraction time (B), and comprehensively considering, the optimal process condition for extracting the corydalis saxicola bunting total alkaloids by the ethanol method is A3B2C1D3, namely the optimal extraction process of the corydalis saxicola bunting total alkaloids is as follows: extracting with 70% ethanol at 80 deg.C for 1.5 hr at a ratio of 1:12 for 3 times.
Example 2
Pulverizing corydalis saxicola bunting, weighing 40.0 g corydalis saxicola bunting, adding 560 mL of 60% ethanol each time, leaching at 80 deg.C for 2.5 h for three times, mixing extractive solutions, filtering, and concentrating the filtrate under reduced pressure to obtain crude corydalis saxicola bunting alkaloid 6.5 g with purity of 65.3%. Weighing 5.0 g of crude alkaloid, adding 10 mL of 0.002% sodium hydroxide solution for fully dissolving, centrifuging for 30 min in a centrifuge with the rotating speed of 3000 r/min, taking supernate, adsorbing by adopting ABS-8 macroporous resin, sequentially eluting by using hydrochloric acid with the pH =5 and ethanol (pH = 5) solution with the concentration from low to high, collecting 20-50% ethanol (pH = 5) eluent, concentrating under reduced pressure, and freeze-drying to obtain 3.1 g of high-purity alkaloid with the purity of 88.3%.
Example 3
Crushing corydalis saxicola bunting whole grass, weighing 2.0 kg corydalis saxicola bunting, adding 25L of 60% ethanol each time, leaching at 80 ℃ for 2.5 h for three times, combining and filtering the extracting solutions, concentrating the filtrate under reduced pressure to obtain 273.2 g of crude corydalis saxicola bunting alkaloid with the purity of 63.4%, weighing 250.0 g of crude alkaloid, adding 1L of 0.002% sodium hydroxide solution to fully dissolve, centrifuging at a rotation speed of 3000 r/min for 30 min, taking the supernatant, adsorbing by using AB-8 macroporous resin, sequentially eluting by using hydrochloric acid with the pH =5 and ethanol (pH = 5) solution with the concentration from low to high, collecting 20-50% ethanol (pH = 5) eluent, concentrating under reduced pressure, and freeze-drying to obtain 151.5 g of high-purity alkaloid with the purity of 86.5%.
Claims (10)
1. A method for extracting high-purity alkaloid from corydalis saxicola bunting is characterized by comprising the following steps:
(1) crushing: crushing the dried corydalis saxicola bunting whole grass to obtain corydalis saxicola bunting crushed grass;
(2) alcohol extraction: placing the corydalis saxicola bunting in the step (1) into an extraction container, adding 50-95% ethanol according to a solid-to-liquid ratio of 1: 6-1: 14, continuously refluxing and extracting for 1-3 hours at 50-90 ℃, extracting for 1-3 times, filtering and combining extracting solutions, and concentrating and drying filtrate under reduced pressure to obtain crude alkaloid;
(3) alkali dissolution: adding crude alkaloid in the step (2) into a mixture of crude alkaloid and crude alkaloid according to a solid-liquid ratio of 1: 2-1: 6, adding alkali liquor to dissolve to obtain sample alkali liquor;
(4) centrifuging: centrifuging the sample alkali liquor in the step (3) to obtain a sample centrifugation supernatant;
(5) macroporous resin adsorption elution: adsorbing the supernatant obtained in the step (4) by using macroporous resin, then eluting by using a hydrochloric acid aqueous solution and an ethanol-hydrochloric acid-aqueous solution in sequence, and collecting an ethanol eluent to obtain a sample eluent;
(6) and (3) drying: and (5) concentrating the sample eluent in the step (5) under reduced pressure, and drying to obtain the high-purity alkaloid.
2. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (2), the concentration of ethanol is 60-80%, the solid-to-liquid ratio is 1: 10-1: 14, the extraction temperature is 70-90 ℃, and the extraction time is 1-2 hours.
3. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 2, wherein the extraction step comprises the following steps: extracting with 70% ethanol at 80 deg.C for 1.5 hr at a ratio of 1:12 for 3 times.
4. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (3), the alkali liquor is a sodium hydroxide solution with the mass percentage concentration of 0.002-0.003%, and the solid-to-liquid ratio of the crude alkaloid to the alkali liquor is 1: 2-1: 6.
5. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (4), the rotating speed of the centrifugal machine is 2500-3500 r/min, and the centrifugal time is 20-40 min.
6. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (5), the macroporous resin is selected from AB-8, ADS-21, ADS-17 or D3520.
7. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (5), the step (c),
the pH value of the hydrochloric acid aqueous solution is 4-6, and the pH value of the ethanol-hydrochloric acid-aqueous solution is 4-6.
8. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (5), the concentration of the ethanol is 20-60%.
9. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the steps (2) and (6), the temperature of the reduced pressure concentration is 60-90 ℃, and the pressure of the reduced pressure concentration is 0.06-0.08 MPa.
10. The method for extracting high-purity alkaloid from corydalis saxicola bunting according to claim 1, wherein the method comprises the following steps: in the step (6), the drying mode adopts freeze drying, evaporation drying, spray drying or vacuum drying.
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