CN101485814B - Supercritical CO2 extraction method for saponin component in Paris polyphylla var. yunnanensis - Google Patents
Supercritical CO2 extraction method for saponin component in Paris polyphylla var. yunnanensis Download PDFInfo
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- CN101485814B CN101485814B CN2009100142317A CN200910014231A CN101485814B CN 101485814 B CN101485814 B CN 101485814B CN 2009100142317 A CN2009100142317 A CN 2009100142317A CN 200910014231 A CN200910014231 A CN 200910014231A CN 101485814 B CN101485814 B CN 101485814B
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Abstract
The invention discloses a method for extracting a saponin composition in rhizoma paridis by supercritical CO2 extraction. The rhizoma paridis is pulverized by a pulverizer to form coarse powder; 50 g of the coarse powder with 20 to 40 meshes is weighed and is placed in an extraction kettle of a supercritical extraction instrument; a polynary cosolvent is pumped into the extraction kettle by a metering pump; the polynary cosolvent consists of a composite surfactant, a mixed solution and distilled water which are in proportion; the coarse powder of the rhizoma paridis and the polynary cosolventare placed in the extraction kettle of the supercritical extraction instrument in a fixed ratio of mass to volume; and certain temperature and pressure are set for extracting saponin. The method has convenient operation, high extraction rate, high product purity, simple flow, low organic solvent remained in an extract, safety, stability, and environmental protection benefit, provides a high-efficiency extraction means for traditional Chinese medicine modernization, and has wide application prospect in the field of separation and extraction of a natural drug and a traditional Chinese medicine compound composition.
Description
Technical field
The present invention relates to the extraction process of a kind of natural Chinese medicinal herb, the supercritical CO of saponin component in a kind of specifically Rhizoma Paridis
2Extracting process is meant the employing supercritical CO
2Saponin component in the extract and separate Rhizoma Paridis belongs to effective ingredient in Chinese extractive technique field.
Background technology
Rhizoma Paridis is stated from Shennong's Herbal with the name beginning of Rhizoma Paridis, is the dry rhizome of liliaceous plant Rhizoma Paridis or Rhizoma Paridis, has taken in version " Chinese pharmacopoeia in 2005.This product bitter in the mouth is slightly cold, and is slightly poisonous, returns Liver Channel.Have effects such as heat-clearing and toxic substances removing, reducing swelling and alleviating pain, the arresting convulsion of cool liver, be used for cards such as the swollen carbuncle of furuncle, laryngopharynx swelling and pain, venom, convulsion with spasms.Modern pharmacological research shows, that Rhizoma Paridis has is antibiotic, antiviral, hemostasis, calmness, ease pain, relieving asthma, antitumor, immunoregulation effect etc.Total saponins is the main active of Rhizoma Paridis, and in recent years, this medicine causes numerous scholars' attention and concern in the research of anti-tumor aspect.
The existing method of extracting total Saponin in the Rhizoma Paridis mainly contains infusion process, heating reflux method, ultrasonic extraction, and solvent for use is organic solvents such as ethanol, methanol.Application number is in 200810052092.2 the Chinese invention patent, discloses a kind of Rhizoma Paridis utilization dipping, refluxing adds the method that the macroporous adsorbent resin chromatography purification prepares saponin extract; Application number is in 03135590.0 the Chinese invention patent, discloses a kind of Rhizoma Paridis and has used warm water soaking earlier, utilizes the method for finite concentration ethanol and α-Dian Fenmei reflux, extract, saponin again; Application number is in 200610052223.8 the Chinese invention patent, discloses a kind of Rhizoma Paridis prepares total saponins by alcohol extracting-water precipitating and deionized water wash precipitation method; Application number is in the Chinese invention patent of 0.135589.7, discloses a kind of Rhizoma Paridis prepares total saponins through steps such as ethanol extraction, membrane filtration, adsorbent resin, decolorizing resin and active carbon combination decolourings method.By the extract that these methods obtain, often need further to carry out purification refine, and have organic solvent residual, extraction time is long, and extraction efficiency is low, and ultrasonic method is extracted and is difficult to realize industrialized problem again in addition.
Summary of the invention
Technical problem to be solved by this invention provides the supercritical CO of saponin component in a kind of Rhizoma Paridis
2Extracting process is the high extracting method of a kind of extraction efficiency.
In order to achieve the above object, the present invention realizes by following measures:
A) with pulverizer Rhizoma Paridis is ground into coarse powder, took by weighing 20～40 purpose coarse powder, place the extraction kettle of supercritical extraction instrument;
B) pump into the polynary cosolvent of 0.06mol/L in the extraction kettle with dosing pump;
C) Rhizoma Paridis coarse powder and polynary cosolvent place the extraction kettle of supercritical extraction instrument by 1: 2 proportioning of the ratio of quality (g) and volume (ml);
D) polynary cosolvent is made up of complexed surfactant, mixed solution and distilled water, complexed surfactant in the polynary cosolvent is by dihexyl sodium sulfosuccinate and two kinds of materials of polyoxyethylene nonyl 2, 2-Oxydiphenol, make than (mol) 5: 3 proportionings by amount of substance, mixed solution in the polynary cosolvent is by n-butyl alcohol (analytical pure AR) and two kinds of solution of 95% ethanol (analytical pure AR), (ml) is that 3: 4 proportionings are made by volume, with complexed surfactant with after mixed solution mixes, with distilled water by volume (ml) be that 5: 1 proportionings are made polynary cosolvent;
E) regulate extraction kettle, make extraction temperature be controlled at 40 ℃, extracting pressure is controlled at 35MPa, CO
2Flow-control extracts under the condition of 2.5L/h, and the extraction time is 4h;
F) the Rhizoma Paridis coarse powder after will extracting is presented to separating still, takes the secondary clastotype.Regulate separation reactor I, make separation temperature be controlled at 55 ℃, separating pressure is controlled at 9MPa, CO
2Flow-control separates the total Saponin of Rhizoma Paridis under the condition of 2.5L/h; Regulate separation reactor I I, make separation temperature be controlled at 55 ℃, separating pressure is controlled at 5MPa, CO
2Flow-control separates solvent and other components under the condition of 2.5L/h, the extraction yield of gained pariphyllin constituents is 5.66%.
The present invention in the present invention, the Rhizoma Paridis medical material is put into extraction kettle after treatment, adopts supercritical CO
2Extracting process, supercritical CO
2Saponin component in the/surfactant extraction Rhizoma Paridis medical material, take the secondary blood pressure lowering to resolve separating effective ingredient, the inventive method is easy to operate, the extraction ratio height, the product purity height, flow process is simple, organic solvent residual is low in the extract, safety and stability and have environmental benefit for the modernization of Chinese medicine provides a kind of means of extracting efficiently, is with a wide range of applications at natural drug and Chinese medicine compound component separating extraction field.Because Rhizoma Paridis saponin is a steroidal saponin, polar phase can adopt supercritical CO to less under the assistance of entrainer
2Extract.The present invention joins CO with surfactant and cosurfactant
2In, formed supercritical CO
2The reverse microemulsion system has greatly been improved supercritical CO
2Extraction efficiency to saponin component.
Below in conjunction with the specific embodiment to technical scheme further instruction of the present invention:
The specific embodiment
Embodiment, the supercritical CO of saponin component in a kind of Rhizoma Paridis
2Extracting process, its experimental procedure is as follows:
Experiment 1 changes raw material granularity the experimental result that total Saponin extraction yield in the Rhizoma Paridis influences is seen Table 1.
Table 1 raw material granularity is to the influence of total Saponin extraction yield in the Rhizoma Paridis
| Sample granularity | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 10～20 | 5.39 5.48 5.56 | 5.48 | 1.55 |
| 20～40 | 5.69 5.62 5.68 | 5.66 | 0.67 |
| 40～60 | 5.64 5.67 5.51 | 5.61 | 1.52 |
| 60～80 | 5.49 5.63 5.52 | 5.55 | 1.33 |
The result shows: along with the increase of raw material powder particle size order number, total Saponin extraction ratio progressively increases, but granularity greater than 40 orders after, extraction ratio begins to reduce.By finding out that granularity total Saponin extraction yield when 20～40 orders is the highest in the table, therefore selecting the granularity of Paris Root is 20～40 orders.
Experiment 2 changes surfactant concentration and the results are shown in Table 2 to what total Saponin extraction yield in the Rhizoma Paridis influenced.
In preliminary experiment, determined n (dihexyl sodium sulfosuccinate): n (polyoxyethylene nonyl 2, 2-Oxydiphenol)=5: 3 complexed surfactant and V (n-butyl alcohol): V (ethanol)=cosolvent that 3: 4 mixed solution is made into is best to total Saponin solubilizing effect in the Rhizoma Paridis.This cosolvent and distilled water have been formed polynary cosolvent, and the cosolvent solution of this experiment preparation variable concentrations adds with the entrainer pump in extraction beginning back.
Table 2 surfactant concentration is to the influence of total Saponin extraction yield in the Rhizoma Paridis
| Surfactant concentration | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 0.04mol/L | 5.38 5.45 5.46 | 5.43 | 0.80 |
| 0.06mol/L | 5.59 5.69 5.68 | 5.65 | 0.97 |
| 0.08mol/L | 5.57 5.68 5.74 | 5.66 | 1.52 |
The result shows: along with the raising of surfactant concentration, total Saponin extraction ratio increases gradually, but concentration 0.06mol/L and concentration 0.08mol/L extraction yield are more or less the same, and consider production cost and environmental factors, select concentration 0.06mol/L for use through taking all factors into consideration decision.
Experiment 3 changes cosolvent and distilled water volume proportion and the results are shown in Table 3 to what total Saponin extraction yield in the Rhizoma Paridis influenced.
Table 3 cosolvent and distilled water volume proportion are to the influence of total Saponin extraction yield in the Rhizoma Paridis
| Proportioning | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 7∶1 | 5.51 5.59 5.61 | 5.57 | 0.95 |
| 5∶1 | 5.55 5.69 5.70 | 5.65 | 1.48 |
| 3∶1 | 5.48 5.37 5.58 | 5.48 | 1.92 |
The result shows: along with the distilled water volume fraction improves, total Saponin extracts and takes the lead in increasing the back reduction.Because the amount of surfactant institute solubilising water is limited, adds more water and can make it from CO
2Middle phase-splitting reduces Saponin at CO
2In distribution, so cosolvent and distilled water volume proportion are decided to be 5: 1.
Experiment 4 changes Rhizoma Paridis raw materials quality and polynary cosolvent volume proportion and the results are shown in Table 4 to what total Saponin extraction yield in the Rhizoma Paridis influenced.
Table 4 Rhizoma Paridis raw materials quality and polynary cosolvent volume proportion are to the influence of total Saponin extraction yield in the Rhizoma Paridis
| Proportioning (g/mL) | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 1∶1 | 5.54 5.67 5.62 | 5.61 | 1.17 |
| 1∶2 | 5.60 5.64 5.68 | 5.64 | 0.71 |
| 1∶3 | 5.67 5.61 5.65 | 5.64 | 0.54 |
The result shows: along with Rhizoma Paridis raw materials quality and polynary cosolvent volume proportion improve, total Saponin extracts to take the lead in increasing and is in considerations such as stable, comprehensive yield and cost again, and selecting proportioning (g/mL) is 1: 2.
Experiment 5 changes CO
2Flow the results are shown in Table 5 to total Saponin extraction yield influence in the Rhizoma Paridis.
Table 5 CO2 flow is to the influence of total Saponin extraction yield in the Rhizoma Paridis
| CO2 flow (L/h) | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 1.5 | 5.53 5.56 5.64 | 5.58 | 1.02 |
| 2.5 | 5.53 5.76 5.62 | 5.64 | 2.06 |
| 3.5 | 5.52 5.63 5.75 | 5.63 | 2.04 |
The result shows: along with CO
2The increase of flow, total Saponin are extracted and are taken the lead in increasing the back reduction, because suitable flow velocity can be strengthened mass transfer effect so that extraction times increases, continue to improve but work as flow velocity, cause CO
2With extract shortening time of contact.By finding out CO in the table
2Total Saponin extraction yield height when flow is 2.5L/h.
Experiment 6, the change supercritical extraction time the results are shown in Table 6 to total Saponin extraction yield influence in the Rhizoma Paridis.
The table 6 supercritical extraction time is to the influence of total Saponin extraction yield in the Rhizoma Paridis
| Extraction time (h) | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 3 | 5.45 5.53 5.44 | 5.47 | 0.90 |
| 4 | 5.67 5.59 5.66 | 5.64 | 0.77 |
| 5 | 5.68 5.62 5.65 | 5.65 | 0.53 |
The result shows: along with CO
2Extraction time prolongs, and total Saponin extraction yield is tending towards increasing, but difference is little between extraction time 4h and the 5h, considerations such as comprehensive yield and cost, selective extraction time 4h.
Experiment 7, total Saponin supercritical extraction process is optimized in the Rhizoma Paridis.
With total Saponin extraction yield is index, and on the basis that single factor is investigated, fixedly separated still II is at pressure 5MPa, and 55 ℃ of conditions of temperature are variable with temperature and four factors of pressure that extract, separate I, adopt L
9(3
4) orthogonal table experimentizes.
Table 7 supercritical extraction process factor level table
Table 8 supercritical extraction process orthonormal design of experiments and result
Table 9 supercritical extraction process orthonormal design of experiments analysis of variance table
Attached: F
0.01(1,2)=99 F
0.05(1,2)=19
ANOVA showed significant: the factor that has the greatest impact is A extracting pressure, D separation temperature, and that B extraction temperature, C are separated I pressure influence is not remarkable.Integrated cost, efficient, produce factor such as reality greatly, A gets A1, and B gets B1, and C gets C1, and D gets D3, and promptly extracting pressure is 35MPa, and 40 ℃ of extraction temperature are separated I pressure 9MPa, 55 ℃ of separation temperatures.
Experiment 8, total Saponin supercritical extraction process checking the results are shown in Table 10 in the Rhizoma Paridis.
The process conditions of determining according to experiment 7 experimentize, and the results are shown in Table in 10 numerical value as can be seen, and this technology stability is strong, and reproduction is acted charitably, requirement up to specification.
Total Saponin supercritical extraction process checking in table 10 Rhizoma Paridis
| The experiment number | Total Saponin extraction yield (%) | Average extraction yield (%) | RSD(％) |
| 1 | 5.64 | ||
| 2 | 5.59 | 5.63 | 0.64 |
| 3 | 5.66 |
Experiment 9, the determining of supercritical process.
With pulverizer Rhizoma Paridis is ground into coarse powder, took by weighing 20～40 purpose coarse powder 50g, place the extraction kettle of supercritical extraction instrument; Pump into the polynary cosolvent of 0.06mol/L in the extraction kettle with dosing pump; Rhizoma Paridis coarse powder and polynary cosolvent place the extraction kettle of supercritical extraction instrument by 1: 2 proportioning of the ratio of quality (g) and volume (ml); Polynary cosolvent is made up of complexed surfactant, mixed solution and distilled water, complexed surfactant in the polynary cosolvent is by dihexyl sodium sulfosuccinate and two kinds of materials of polyoxyethylene nonyl 2, 2-Oxydiphenol, make than (mol) 5: 3 proportionings by amount of substance, mixed solution in the polynary cosolvent is by n-butyl alcohol (analytical pure AR) and two kinds of solution of 95% ethanol (analytical pure AR), (ml) is that 3: 4 proportionings are made by volume, with complexed surfactant with after mixed solution mixes, with distilled water by volume (ml) be that 5: 1 proportionings are made polynary cosolvent; Regulate extraction kettle, make extraction temperature be controlled at 40 ℃, extracting pressure is controlled at 35MPa, CO
2Flow-control extracts under the condition of 2.5L/h, and the extraction time is 4h; Rhizoma Paridis coarse powder after the extraction is presented to separating still, takes the secondary clastotype.Regulate separation reactor I, make separation temperature be controlled at 55 ℃, separating pressure is controlled at 9MPa, CO
2Flow-control separates the total Saponin of Rhizoma Paridis under the condition of 2.5L/h; Regulate separation reactor I I, make separation temperature be controlled at 55 ℃, separating pressure is controlled at 5MPa, CO
2Flow-control separates solvent and other components under the condition of 2.5L/h, the extraction yield of gained pariphyllin constituents is 5.66%.
Embodiment 2, the contrast experiment of extracting method, and experimental result is seen attached list.
Rigid condition: get 20-40 purpose Rhizoma Paridis raw material 50g; The supercritical extraction parameter that experiment relates to is selected according to example 9, and analytical method is measured the extraction yield of pariphyllin constituents in accordance with regulations.
Experimental technique 1 ethanol refluxing process extracts the total Saponin of Rhizoma Paridis, and 10 times of amounts of twice, the 1 usefulness of 70% ethanol extraction are extracted 2h, and 8 times of amounts of the 2nd usefulness are extracted 1.5h, merge extractive liquid,, and decompression recycling ethanol gets extract.
Experimental technique 2 supercritical COs
2The total Saponin of extraction Rhizoma Paridis Rhizoma Paridis uses pure CO
2Entrainer and surfactant are not used in extraction.
Experimental technique 3 supercritical COs
2The total Saponin of/entrainer extraction Rhizoma Paridis selects 95% ethanol to make entrainer, adds with the entrainer pump in extraction beginning back.
Experimental technique 4 adopts the total Saponin of experimental technique extraction Rhizoma Paridis of the present invention.
The comparison of total Saponin extracting method in the subordinate list Rhizoma Paridis
The result shows: supercritical CO
2The surfactant extraction is better than other extracting method.
Claims (1)
1. the supercritical CO of saponin component in the Rhizoma Paridis
2Extracting process is characterized in that, the step of this extracting process is as follows:
A) with pulverizer Rhizoma Paridis is ground into coarse powder, took by weighing 20～40 purpose coarse powder, place the extraction kettle of supercritical extraction instrument;
B) pump into the polynary cosolvent of 0.06mol/L in the extraction kettle with dosing pump;
C) Rhizoma Paridis coarse powder and polynary cosolvent place the extraction kettle of supercritical extraction instrument by 1: 2 proportioning of the ratio of quality g and volume ml;
D) polynary cosolvent is made up of complexed surfactant, mixed solution and distilled water, complexed surfactant in the polynary cosolvent is by dihexyl sodium sulfosuccinate and two kinds of materials of polyoxyethylene nonyl 2, 2-Oxydiphenol, make than 5: 3 proportionings of mol by amount of substance, mixed solution in the polynary cosolvent is the two kinds of solution of 95% ethanol by the n-butyl alcohol of analytical pure AR and analytical pure AR, ml is that 3: 4 proportionings are made by volume, with complexed surfactant with after mixed solution mixes, with distilled water by volume ml be that 5: 1 proportionings are made polynary cosolvent;
E) regulate extraction kettle, make extraction temperature be controlled at 40 ℃, extracting pressure is controlled at 35MPa, CO
2Flow-control extracts under the condition of 2.5L/h, and the extraction time is 4h;
F) the Rhizoma Paridis coarse powder after will extracting is presented to separating still, takes the secondary clastotype, regulates separation reactor I, makes separation temperature be controlled at 55 ℃, and separating pressure is controlled at 9MPa, CO
2Flow-control separates the total Saponin of Rhizoma Paridis under the condition of 2.5L/h; Regulate separation reactor I I, make separation temperature be controlled at 55 ℃, separating pressure is controlled at 5MPa, CO
2Flow-control separates solvent and other components under the condition of 2.5L/h, the extraction yield of gained pariphyllin constituents is 5.66%.
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| CN106367374B (en) * | 2016-09-22 | 2019-04-09 | 中南民族大学 | The Escherichia coli clx-6 bacterial strain and application thereof of one plant of production polyphyllin Ⅵ |
| CN106866831A (en) * | 2017-01-22 | 2017-06-20 | 嵊州市派特普科技开发有限公司 | The Preparation method and use of Poria cocos acidity polyoses extract |
| CN106831933A (en) * | 2017-01-22 | 2017-06-13 | 嵊州市派特普科技开发有限公司 | The method that thick Total saponin is extracted from Chinese yam class plant |
| CN106832031A (en) * | 2017-01-22 | 2017-06-13 | 嵊州市派特普科技开发有限公司 | The preparation method of plantago asiatica linne polyoses extract |
| CN109453099B (en) * | 2018-12-27 | 2021-08-24 | 神农架林区中医医院 | Paris polyphylla composition and preparation method thereof |
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