CN103623024B - The CO of effective ingredient in a kind of Herba Sonchi Arvensis 2supercritical extraction method - Google Patents
The CO of effective ingredient in a kind of Herba Sonchi Arvensis 2supercritical extraction method Download PDFInfo
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- CN103623024B CN103623024B CN201310650018.1A CN201310650018A CN103623024B CN 103623024 B CN103623024 B CN 103623024B CN 201310650018 A CN201310650018 A CN 201310650018A CN 103623024 B CN103623024 B CN 103623024B
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Abstract
The CO of effective ingredient in a kind of Herba Sonchi Arvensis
2supercritical extraction method, belongs to Herba Sonchi Arvensis abstraction technique field.The present invention adopts and first 10 ~ 20 mesh sieves is crossed in Herba Sonchi Arvensis fragmentation, after carry out ethanol-water solution immersion, adopt two separating still CO
2supercritical extraction, setting extraction kettle temperature 35 ~ 60 DEG C, extraction kettle pressure 12 ~ 30Mpa, separation reactor I temperature 40 ~ 65 DEG C, separation reactor I pressure 8 ~ 12Mpa, separation reactor I I temperature 35 ~ 40 DEG C, separation reactor I I pressure 5 ~ 8Mpa, adding 10% ~ 95% ethanol is entrainer, and extraction time is 2 ~ 6 hours; By concentrated acquisition Herba Sonchi Arvensis extract.Method of the present invention can make general flavone content in Herba Sonchi Arvensis extract maintain high value, can reach more than 3.9mg/g.
Description
Technical field
The CO of effective ingredient in a kind of Herba Sonchi Arvensis
2supercritical extraction method, belongs to Herba Sonchi Arvensis abstraction technique field.
Background technology
Herba Sonchi Arvensis, is feverfew, has another name called Herba Sonchi Oleracei.Herba Sonchi Arvensis has effect of heat-clearing and toxic substances removing, removing heat from blood dampness removing, detumescence and apocenosis, stasis-dispelling and pain-killing, tonify deficiency cough-relieving.To prevention and therapy anemia, maintain human normal physiological activity, enhancing development and health care of relieving summer heat have good effect.Herba Sonchi Arvensis water boiling concentration ethanol extract, to acute lymphoblastic Bai Xue Bing ﹑, acute and chronic myelocytic leukemia has inhibitory action.Herba Sonchi Arvensis bitter in the mouth cold in nature, has effect of heat reliving and toxin-eliminating, removing heat from blood, dampness removing, detumescence and apocenosis, stasis-dispelling and pain-killing, tonify deficiency cough-relieving.
In prior art, the extraction of effective ingredient in Herba Sonchi Arvensis is adopted traditionally to the method for water extraction or alcohol extraction, it is higher to there is temperature in leaching process, effective ingredient in destructible medical material, at substantial water and ethanol equal solvent, consume the drawbacks such as mass energy, need badly and take advanced extraction process to extract its bioactive ingredients.
Not yet relate to the technology that Herba Sonchi Arvensis adopts supercritical extraction in prior art, its technical difficulty existed is that Herba Sonchi Arvensis is containing flavone compounds such as Quercetin, isorhamnetin, chrysoeriol, acacetin, apigenin and aesculetins; Again containing the triterpenoid compound such as oleanolic acid, ursolic acid; Containing acids, esters, alcohol constituents in its volatile oil.When Herba Sonchi Arvensis adopts supercritical extraction technique to extract in prior art, due to the bad grasp of extraction conditions, cannot ensure that flavone compound, triterpenoid compound all obtain higher yield simultaneously.Adopt in prior art and squeeze the solute of Herba Sonchi Arvensis juice as supercritical fluid, easily cause in supercritical fluid that not dissolve impurity content too high, impact extraction yield; Squeeze the flavone compound, the triterpenoid compound that filter still containing high level in the remaining residue of Herba Sonchi Arvensis juice, cause wastage of material.
Summary of the invention
The technical problem to be solved in the present invention is: the deficiency existed for above-mentioned prior art, provides the CO of effective ingredient in a kind of Herba Sonchi Arvensis
2supercritical extraction method, the method can improve the dissolubility of solute in supercritical fluid, improves the extracting power of Flavonoids.
The technical solution adopted for the present invention to solve the technical problems is: the CO of effective ingredient in this Herba Sonchi Arvensis
2supercritical extraction method, is characterized in that, adopts following steps:
A) with disintegrating machine, Herba Sonchi Arvensis is broken, cross 10 ~ 20 mesh sieves;
B) soaked 1 ~ 8 hour by the ethanol-water solution of the Herba Sonchi Arvensis after fragmentation, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 20 ~ 65%;
C) CO is carried out by the Herba Sonchi Arvensis input supercritical extracting equipment after immersion
2supercritical extraction, extraction kettle temperature 35 ~ 60 DEG C, extraction kettle pressure 12 ~ 30Mpa, separation reactor I temperature 40 ~ 65 DEG C, separation reactor I pressure 8 ~ 12Mpa, separation reactor I I temperature 35 ~ 40 DEG C, separation reactor I I pressure 5 ~ 8Mpa, adding 10% ~ 95% ethanol is entrainer, and extraction time is 2 ~ 6 hours;
D), after extraction terminates, by concentrated under 40 ~ 60 DEG C of conditions for the extract obtained from separation reactor I, separation reactor I I, removing ethanol, obtains Herba Sonchi Arvensis extract.
In ethanol-water solution described in step b), concentration expressed in percentage by volume shared by ethanol is 30 ~ 40%.
Herba Sonchi Arvensis ethanol-water solution soak time described in step b) is 2 ~ 4 hours.
Extraction kettle temperature described in step c) 55 ~ 60 DEG C, extraction kettle pressure 15 ~ 20Mpa, separation reactor I temperature 60 ~ 65 DEG C, separation reactor I pressure 8 ~ 10Mpa, separation reactor I I temperature 35 ~ 40 DEG C, separation reactor I I pressure 6 ~ 8Mpa, adding 30 ~ 40% ethanol is entrainer, and extraction time is 4 ~ 6 hours.
Extract described in step d) concentrates 6 ~ 7 hours at 45 ~ 55 DEG C.
In ethanol during lixiviate, gained effective ingredient is minimum, and because concentration of alcohol is too high, part aqueous material cannot be suggested; In water, add the dissolubility that ethanol changes water soluble ingredient, after deliberation, when concentration expressed in percentage by volume shared by ethanol is 30 ~ 40% in ethanol-water solution, farthest can extract the effective ingredient such as the flavone in Herba Sonchi Arvensis.
CO
2supercritical extraction technique is the new and effective extraction and separation technology of a kind of advanced person, and this technology utilizes CO
2have in the supercritical state far faster than the speed of the dissolving solute of liquid and much larger than gas to the dissolving of solid matter and the feature of carrying capacity, have that diffusion coefficient is high, flowing and transmit that performance is good, advantage that solvability is strong, the extraction and isolation to plurality of active ingredients such as volatile oil, lignanoids, terpenoid in Chinese medicine can be realized at a lower temperature.Compared with the methods such as the water extraction traditional with Chinese medicine, alcohol extraction, CO
2supercritical extraction technique technological process is simple, easy to operate, pollution-free, noresidue, and extraction and fractionation process unites two into one, and product quality is high and can keep the original character of medical material, can effective enrichment Effective Component of Chinese Medicine.
The mode of two separating still is adopted in step c), and set the condition of two separating still respectively: separation reactor I temperature 40 ~ 65 DEG C, separation reactor I pressure 8 ~ 12Mpa, separation reactor I I temperature 35 ~ 40 DEG C, separation reactor I I pressure 5 ~ 8Mpa, the change to flavone compound and triterpenoid compound solvability of under different temperatures pressure condition supercritical carbon dioxide can be ensured, be separated to obtain the flavone compound of different chemical composition and triterpenoid compound.
Compared with prior art, the CO of effective ingredient in a kind of Herba Sonchi Arvensis of the present invention
2the beneficial effect that supercritical extraction method has is: the CO of effective ingredient in a kind of Herba Sonchi Arvensis of the present invention
2supercritical extraction method, the dissolubility of solute in supercritical fluid can be improved, add the extracting power of supercritical fluid to extract, thus the important biomolecule active component such as the flavonoid in Herba Sonchi Arvensis are fully extracted, also improve the content of effective ingredient in extract.In the Herba Sonchi Arvensis extract adopting this method obtained, general flavone content is at more than 3.9mg/g.Overcome flavonoids effective constituent loss in existing water extraction many, extraction efficiency is low, the shortcoming that cost is high.
Detailed description of the invention
Embodiment 1 ~ 5 is the CO of effective ingredient in a kind of Herba Sonchi Arvensis of the present invention
2the specific embodiment of supercritical extraction method.
embodiment 1
A) get 100g Herba Sonchi Arvensis medical material crusher in crushing, cross 20 mesh sieves;
B) the Herba Sonchi Arvensis ethanol-water solution after fragmentation is steeped 2 hours, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 30%;
C) CO is carried out by the Herba Sonchi Arvensis soaked input supercritical extracting equipment
2supercritical extraction, extraction kettle temperature 60 C, extraction kettle pressure 15Mpa, separation reactor I temperature 65 DEG C, separation reactor I pressure 8Mpa, separation reactor I I temperature 35 DEG C, separation reactor I I pressure 6Mpa, adding 30% ethanol 100ml is entrainer, and extraction time is 6 hours;
D) extract obtained from two separating stills is merged, concentrate 6 hours in 50 DEG C of normal pressures, obtain Herba Sonchi Arvensis extract.
embodiment 2
A) get 100g Herba Sonchi Arvensis medical material crusher in crushing, cross 10 mesh sieves;
B) the Herba Sonchi Arvensis ethanol-water solution after fragmentation is steeped 1 hour, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 40%;
C) CO is carried out by the Herba Sonchi Arvensis soaked input supercritical extracting equipment
2supercritical extraction, extraction kettle temperature 55 DEG C, extraction kettle pressure 18Mpa, separation reactor I temperature 55 DEG C, separation reactor I pressure 10Mpa, separation reactor I I temperature 39 DEG C, separation reactor I I pressure 7Mpa, adding 30% ethanol 100ml is entrainer, and extraction time is 6 hours;
D) extract obtained from separation reactor I and II is merged, concentrate 5 hours in 55 DEG C of decompression 0.02Mpa, obtain Herba Sonchi Arvensis extract.
embodiment 3
A) get 100g Herba Sonchi Arvensis medical material crusher in crushing, cross 10 mesh sieves;
B) the Herba Sonchi Arvensis ethanol-water solution after fragmentation is steeped 8 hours, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 60%;
C) CO is carried out by the Herba Sonchi Arvensis soaked input supercritical extracting equipment
2supercritical extraction, extraction kettle temperature 40 DEG C, extraction kettle pressure 25Mpa, separation reactor I temperature 40 DEG C, separation reactor I pressure 8Mpa, separation reactor I I temperature 36 DEG C, separation reactor I I pressure 5Mpa, adding 90% ethanol 100ml is entrainer, and extraction time is 1 hour;
D) extract obtained from separation reactor I and II is merged, concentrate 7 hours in 40 DEG C of normal pressures, obtain Herba Sonchi Arvensis extract.
embodiment 4
A) get 100g Herba Sonchi Arvensis medical material crusher in crushing, cross 15 mesh sieves;
B) the Herba Sonchi Arvensis ethanol-water solution after fragmentation is steeped 6 hours, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 20%;
C) CO is carried out by the Herba Sonchi Arvensis soaked input supercritical extracting equipment
2supercritical extraction, extraction kettle temperature 60 C, extraction kettle pressure 30Mpa, separation reactor I temperature 43 DEG C, separation reactor I pressure 8Mpa, separation reactor I I temperature 40 DEG C, separation reactor I I pressure 7Mpa, adding 70% ethanol 100ml is entrainer, and extraction time is 2 hours;
D) extract obtained from separation reactor I and II is merged, concentrate 7 hours in 45 DEG C of normal pressures, obtain Herba Sonchi Arvensis extract.
embodiment 5
A) get 100g Herba Sonchi Arvensis medical material crusher in crushing, cross 20 mesh sieves;
B) the Herba Sonchi Arvensis ethanol-water solution after fragmentation is steeped 3 hours, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 35%;
C) CO is carried out by the Herba Sonchi Arvensis soaked input supercritical extracting equipment
2supercritical extraction, extraction kettle temperature 45 C, extraction kettle pressure 28Mpa, separation reactor I temperature 40 DEG C, separation reactor I pressure 10Mpa, separation reactor I I temperature 38 DEG C, separation reactor I I pressure 7Mpa, adding 35% ethanol 100ml is entrainer, and extraction time is 5 hours;
D) extract obtained from separation reactor I and II is merged, concentrate 5 hours in 58 DEG C of decompression 0.02Mpa, obtain Herba Sonchi Arvensis extract.
testing result
Obtained for embodiment 1 ~ 5 Herba Sonchi Arvensis extract is carried out composition measurement.This product is green to bottle green thick paste.Detection method is as follows, and testing result is as shown in table 1.
Assay: measure according to ultraviolet visible spectrophotometry [" Chinese Pharmacopoeia " (version in 2010) annex VA]
The preparation of reference substance solution: precision takes the control substance of Rutin 25mg being dried to constant weight at 120 DEG C, put in 50ml measuring bottle, add appropriate amount of ethanol, supersound process makes dissolving, lets cool, and adds ethanol to scale, shakes up.Precision measures 20ml, puts in 50ml measuring bottle, adds water to scale, shake up, and obtains (containing anhydrous rutin 0.2mg in every 1ml).
The preparation of standard curve: precision measures reference substance solution lml, 2ml, 3ml, 4ml, 5ml, 6ml, put in 25ml measuring bottle respectively, respectively add water to 6ml, add 5% sodium nitrite solution 1ml, shake up, place 6 minutes, add 10% aluminum nitrate solution 1ml, shake up, place 6 minutes, add 4% sodium hydroxide solution 10ml, then add water to scale, shake up, place 15 minutes, take corresponding reagent as blank, immediately according to ultraviolet visible spectrophotometry (" Chinese Pharmacopoeia " 2010 editions annex VA), measure absorbance y(A at 510nm wavelength place).With absorbance y(A) be vertical coordinate, with total flavones concentration (mg/ml) for abscissa, drawing standard curve, obtains linear regression equation and calculates correlation coefficient.
Sample determination method: precision takes this product 0.5g, puts in 25ml measuring bottle, and add water 6ml, ultrasonicly makes dissolving, the method under sighting target directrix curve preparation, operates from " 5% sodium nitrite solution 1ml " in accordance with the law, surveys absorbance y(A).The content of total flavones in test sample is calculated to obtain by equation of linear regression.Extract total flavones component content is the acquisition effective ingredient that the present invention extracts acquisition---the total content of Flavonoids.
Table 1 testing result
Can find out in embodiment 1 ~ 5 that the Flavonoids content adopting method of the present invention to obtain is all higher than 3.9mg/g by table 1, the inventive method extracts Flavonoids excellent effect.
The above is only preferred embodiment of the present invention, and be not restriction invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (2)
1. the CO of effective ingredient in a Herba Sonchi Arvensis
2supercritical extraction method, is characterized in that, adopts following steps:
A) with disintegrating machine, Herba Sonchi Arvensis is broken, cross 10 ~ 20 mesh sieves;
B) soaked 2 ~ 4 hours by the ethanol-water solution of the Herba Sonchi Arvensis after fragmentation, in ethanol-water solution, concentration expressed in percentage by volume shared by ethanol is 30 ~ 40%;
C) CO is carried out by the Herba Sonchi Arvensis input supercritical extracting equipment after immersion
2supercritical extraction, extraction kettle temperature 55 ~ 60 DEG C, extraction kettle pressure 15 ~ 20Mpa, separation reactor I temperature 60 ~ 65 DEG C, separation reactor I pressure 8 ~ 10Mpa, separation reactor I I temperature 35 ~ 40 DEG C, separation reactor I I pressure 6 ~ 8Mpa, adding 30 ~ 40% ethanol is entrainer, and extraction time is 4 ~ 6 hours;
D), after extraction terminates, by concentrated under 40 ~ 60 DEG C of conditions for the extract obtained from separation reactor I, separation reactor I I, removing ethanol, obtains Herba Sonchi Arvensis extract.
2. the CO of effective ingredient in a kind of Herba Sonchi Arvensis according to claim 1
2supercritical extraction method, is characterized in that: the extract described in step d) concentrates 6 ~ 7 hours at 45 ~ 55 DEG C.
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| CN111410981A (en) * | 2019-01-07 | 2020-07-14 | 中国石油天然气股份有限公司 | Supercritical CO with entrainer assistance2Method for extracting oil in drilling waste |
| CN112341515A (en) * | 2020-11-20 | 2021-02-09 | 榆林学院 | Method for extracting taraxasterol from sow thistle |
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