CN101270134B - Method for preparing pericarpium lagenariae theine - Google Patents
Method for preparing pericarpium lagenariae theine Download PDFInfo
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- CN101270134B CN101270134B CN2008100110947A CN200810011094A CN101270134B CN 101270134 B CN101270134 B CN 101270134B CN 2008100110947 A CN2008100110947 A CN 2008100110947A CN 200810011094 A CN200810011094 A CN 200810011094A CN 101270134 B CN101270134 B CN 101270134B
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- triquetri
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Abstract
The present invention provides a method for preparing triquetin. In the method, firstly, acetone-aqueous solution with the concentration of 40 percent to 80 percent is used to extract ground tickclover material, the dosage of the extraction solvent is in accordance with the solid-liquid ratio of (g:ml) equal to 1:6 to 10, the extraction temperature is 30 DEG C to 80 DEG C, and the extraction period is 1.5 hours to 9 hours; extract, which is produced after extracting solution is condensed and dried, is resolved in water and then filtered, filtrate is absorbed by D101 macroporous resin and theneluted by deionized water until effluent liquid becomes colorless, 10 percent to 30 percent of ethanol water then elutes six to eight column volumes at the flowing speed of 1 BV/h to 2 BV/h, and after alcoholic solution eluent is collected, a triquetin product is produced by condensation and drying. Suitable for mass production, the preparation method of the present invention has the advantages of simplicity and low cost, and acetone, ethanol and macroporous resin can all be recycled.
Description
Technical field
The present invention relates to extraction of active ingredients preparation method in the natural plant gourds tea, relate in particular to the preparation of polyphenols.
Background technology
The Herba Desmodii Triquetri (Herba Tadehagi Triquetri) prime system extracts the Polyphenols composition that enrichment obtains in Herba Desmodii Triquetri (Herba Tadehagi Triquetri) herb and root.Herba Desmodii Triquetri (Herba Tadehagi Triquetri) Tadehagi triquetrum (Linn.) Ohashi is a pulse family Herba Desmodii Triquetri (Herba Tadehagi Triquetri) platymiscium.This genus has 6 kinds approximately, is distributed in the torrid areas, Asia, Pacific Islands and Australia.China has 2 kinds, i.e. Herba Desmodii Triquetri (Herba Tadehagi Triquetri) and viticula Herba Desmodii Triquetri (Herba Tadehagi Triquetri) T.pseudatriquetrum (DC.) Yang et Huang.Be distributed in ground such as Guangxi, Guangdong, Yunnan, Hainan, Fujian, Jiangxi, Guizhou, Sichuan, Hunan, Taiwan.Record the only Herba Desmodii Triquetri (Herba Tadehagi Triquetri) for medicine, medicinal part is herb (title Herba Desmodii Triquetri (Herba Tadehagi Triquetri)) and root (title Radix Desmodii triquetri), also is that Dai Nationality's medicine and watt medicine are contained.
Herba Desmodii Triquetri (Herba Tadehagi Triquetri): bitter and puckery flavor, cold.Have heat clearing away, dampness removing, function stagnant, parasite killing disappears.Be used for the treatment of flu, pharyngalgia, pneumonopathy hemoptysis, enteritis, dysentery, jaundice, rheumatic arthralgia, ancylostomiasis, vomiting during pregnancy, infantile malnutrition, furuncle.Radix Desmodii triquetri: property is flat, the mildly bitter flavor suffering.Function with heat-clearing and toxic substances removing, dampness removing cough-relieving.Be used for the treatment of the cough due to pathogenic wind-heat, lung abscess, jaundice, carbuncle, scrofula consumptive disease, bone tuberculosis.
Though the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) medicinal history is long, research is very few both at home and abroad.Up to 20 end of the centurys, domesticly just to see report successively, but focus mostly in to farming and animal husbandry aspects such as Mollusca, herding anthelmintics, medical value research is very few.
Contain tannin 7.1～8.6% in the document record calabash Folium Camelliae sinensis, its anti-Mollusca and anthelmintic action cause the interest that we are very big especially.Though because Herba Desmodii Triquetri (Herba Tadehagi Triquetri) research seldom, the research of plant polyphenol is a lot, to medicine, application is very extensive from process hides, food, daily-use chemical industry.Polyphenol is becoming one of focus of current natural product research in research pharmaceutically.Antibacterial, the antiviral of polyphenol, antimutagenic, anticancer, resisting cardiovascular disease, protect the liver kidney tonifying, the anti-ageing curative effect of waiting for a long time is noticeable.Be still the thing that attracts tremendous attention so from natural resources, seek new polyphenol resource.This is rich in the plant resources of polyphenol for further development and use, is necessary extraction, enrichment, the purifying process based on the polyphenol of pericarpium lagenariae theine in Herba Desmodii Triquetri (Herba Tadehagi Triquetri) and the root carried out in depth studying.
In the natural plants in the prior art of extraction of polyphenol substance purifying process, water, alcohol-water, acetone-water extract, the gelatin sedimentation method, the chromatographic isolation analytical method has had more application, but does not also have relevant report at the extraction of polyphenol substance purifying process that in this kind of plant of Herba Desmodii Triquetri (Herba Tadehagi Triquetri) with the pericarpium lagenariae theine is representative.The present invention promptly is intended to finish detailed Herba Desmodii Triquetri (Herba Tadehagi Triquetri) plant polyphenol and extracts purification scheme.
Summary of the invention
The object of the present invention is to provide a kind of complete skill scheme for preparing the high-purity pericarpium lagenariae theine.
The preparation method of pericarpium lagenariae theine of the present invention is to be that 40～80% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration earlier, extract solvent load according to solid-liquid ratio (g: ml)=1: 6～10, extract 30～80 ℃ of temperature, extraction time 1.5～9h; Gained extractum water dissolution, filtration behind the extracting solution concentrate drying, filtrate is through D
101After the macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water, uses 10～30% ethanol water then, with 6～8 column volumes of flow velocity eluting of 1～2BV/h, collects alcoholic solution part eluent, and concentrate drying gets the pericarpium lagenariae theine product
The acetone-water solution of wherein said extraction solvent preferred 50～70%, and solid-liquid ratio (g: ml) preferred 1: 8～10, extract preferred 30～50 ℃ of temperature, preferred 4.5～7.5h of extraction time.
In the wherein said purification by macroporous resin step, eluting ethanol water concentration preferred 30%.
The preferred 2BV/h of described ethanol aqueous wash separation of flow speed, preferred 6 column volumes of eluent consumption.
Specifically, the preparation method of pericarpium lagenariae theine of the present invention comprises the steps:
1. be that 50～70% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration, and solid-liquid ratio (g: ml) 1: 8～10, extract 30～50 ℃ of temperature, extraction time 4.5～7.5h;
2. extracting solution concentrate drying, with gained extractum with water dissolution, filtration;
3. filtrate is through D
101Macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water then;
4. use 30% ethanol water, with 6 column volumes of flow velocity eluting of 1～2BV/h, collect eluent, concentrate drying gets the pericarpium lagenariae theine product.
In the above-mentioned concrete operating procedure, preferred parameter combinations constitutes the most preferred scheme of the present invention, and is as follows:
1. be that 60% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration, solid-liquid ratio (g: ml) be 1: 8, extract 30 ℃ of temperature, extraction time 6h;
2. extracting solution concentrate drying, with gained extractum with water dissolution, filtration;
3. filtrate is through D
101Macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water then;
4. use 30% ethanol water, with 6 column volumes of flow velocity eluting of 1～2BV/h, collect eluent, concentrate drying gets the pericarpium lagenariae theine product.
As the part in the production decision of integrating, the recycling of resin is also extremely important, and the recovery method to the resin after using among the present invention is to adopt with behind 95% the soak with ethanol 24h, cleans repeatedly with ethanol and deionized water.
Preparation method good stability of the present invention, easy to operation, cost is low, and acetone, ethanol are recyclable, and macroporous resin is renewable, all can recycle, and is suitable for large-scale production.
Description of drawings
Accompanying drawing 1 width of cloth of the present invention, i.e. the preparation method flow chart of the pericarpium lagenariae theine of embodiment.
The specific embodiment
The present invention is further illustrated in the mode of specific embodiment below.If no special instructions, measuring method to polyphenol compound among the following embodiment all is standard substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute with the gallic acid, lot number: 120563-200412, purity 99.1%), adopt colorimetry (Unico7200 visible spectrophotometer, You Nike Shanghai Instr Ltd.) to measure.
The preparation method of purity pericarpium lagenariae theine of the present invention is to put into container after the raw material Herba Desmodii Triquetri (Herba Tadehagi Triquetri) drying and crushing, and (g: ml), extract temperature, time lixiviate, leaching process can stir according to the solvent of setting, solid-liquid ratio; Separation and Extraction liquid also reclaims solvent, and the product lyophilization gets rough pericarpium lagenariae theine.With the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) extracting solution through D
101Behind the absorption with macroporous adsorbent resin, it is colourless to be eluted to effluent with deionized water, and carries out eluting with eluent, the eluting material ratio condition set, gathers eluent and reclaims solvent and freezing vacuum drying, gets light yellowish brown graininess pericarpium lagenariae theine.
Following specific embodiment divides other detailed description to extraction and resin purification step.
One, pericarpium lagenariae theine extraction process embodiment
According to above-mentioned concrete operations step, at the extraction pericarpium lagenariae theine down that imposes a condition, extracting solvent is the acetone-aqueous solution of variable concentrations, and yield calculates according to following formula:
Yield=(pericarpium lagenariae theine quality/raw materials quality) * 100%
Actual conditions is set and is extracted and the results are shown in Table 1:
Table 1
Embodiment 21
Present embodiment is an orthogonal experiment of investigating extraction process, and the extraction process step is with aforementioned embodiment 1～20, according to the result of previous embodiment 1～20,4 factors is selected 3 levels suiting respectively, adopts L
9(3
4) orthogonal experiment calendar investigation optimum process condition.The arrangement of orthogonal experiment factor level sees Table 2, and experimental result sees Table 3 respectively:
Table 2
Table 3
The above result of analysis-by-synthesis, the primary and secondary that influences of each factor is A＞B＞C＞D, promptly extracts temperature＞concentration＞time＞volume.Therefore optimised process combination A1B1C1D2, promptly 8 times of amount 50% acetone water extract 6h for 30 ℃, and the pericarpium lagenariae theine yield is about 6%, is fit to the extraction of pericarpium lagenariae theine.
Two, D
101The process conditions of purification by macroporous resin pericarpium lagenariae theine and parameter are investigated embodiment
This part embodiment includes D
101Pretreatment and recovery post-processing step before the use of macroporous resin, pretreated method is: get a certain amount of D
101Macroporous resin, 95% soak with ethanol 24 hours in its resin column that cleans in advance of packing into, is washed till effluent with 95% ethanol earlier and adds 3 times of no white casse phenomenons of the constant muddiness of water, uses distilled water flushing then instead to there not being the alcohol flavor, can use.Use the method for back recycling to be: behind 5% the soak with ethanol 24h, to clean repeatedly with ethanol and deionized water.
In order to optimize the use of resin, present embodiment is at first investigated the resin property parameter, comprising:
1, determining of static adsorption capacity: in the conical flask of 250ml, add the pretreated D of 5g (dry weight 1.479g)
101Macroporous adsorbent resin and 100ml sample solution (concentration is 9.73mg/ml).The room temperature vibration is got 1ml at set intervals and is measured polyphenol content remaining in the solution, draws unit adsorbance and time curve.And according to following formula calculating material balance adsorbance
q＝(C1-C2)V/G
The concentration (mg/ml) of total polyphenols in solution when wherein, C1 and C2 are initial and balance respectively;
V is the volume (ml) of test sample liquid; G is an amount of resin.
Experiment records D
101The static adsorption capacity of resin is 272.5mg/ml.
2, the dynamic adsorption amount determines
The investigation of last sample flow velocity: the resin column that to get 4 internal diameters be 2.5cm, the pretreated D of 15g respectively packs into
101Macroporous adsorbent resin, adding 50ml concentration respectively is the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) solution of 9.36mg/ml, regulates different flow velocitys, the sample flow velocity is to the influence of absorption with macroporous adsorbent resin pericarpium lagenariae theine in the investigation.Find D according to experimental result
101The adsorption capacity of resin is along with the increase of flow velocity slowly descends, when flow velocity is 1～2BV/h, and D
101The adsorption capacity of resin changes little, is 103.5mg/g, and when flow velocity was brought up to 4BV/h, its adsorbance reduced to some extent, was 91.8mg/g.Comprehensive post is imitated and the production time cost consideration, and flow velocity selects to be controlled at 1～2BV/h.
Embodiment 22～27
With 50% acetone-water solution serves as to extract solvent, according to solid-liquid ratio 1: 8, extract 30 ℃ of temperature, 6 hours extraction times were extracted pericarpium lagenariae theine from dry Herba Desmodii Triquetri (Herba Tadehagi Triquetri) material powder, extracting solution is used water dissolution, filtration after making extractum, the filtrate upper prop, it is colourless to be eluted to effluent with deionized water after absorption is finished, more respectively according to the eluting that imposes a condition, the enrichment eluent, concentrate drying gets the pericarpium lagenariae theine product, measures polyphenol content (%) in the product, and calculated yield.Actual conditions setting and result are as shown in table 4:
Table 4
Embodiment 28
The present embodiment technological process as shown in Figure 1.
With 50% acetone-water solution serves as to extract solvent, according to solid-liquid ratio 1: 8, extracts 30 ℃ of temperature, and 6 hours extraction times were extracted pericarpium lagenariae theine from dry Herba Desmodii Triquetri (Herba Tadehagi Triquetri) material powder, extraction ratio 6%; Extracting solution is used water dissolution, filtration after making extractum, the filtrate upper prop, and it is colourless to be eluted to effluent with deionized water after absorption is finished, the ethanol of reuse 30% is with 6 column volumes of flow velocity eluting of 2BV/h, enrichment eluent, concentrate drying gets the pericarpium lagenariae theine product, and pericarpium lagenariae theine content is 75%.
Claims (6)
1. the preparation method of a pericarpium lagenariae theine, it is characterized in that this method is is that 40～80% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration earlier, extract solvent load according to solid-liquid ratio (g: ml)=1: 6～10, extract 30～80 ℃ of temperature, extraction time 1.5～9h; Gained extractum water dissolution, filtration behind the extracting solution concentrate drying, filtrate is through D
101After the macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water, uses 10～30% ethanol water then, with 6～8 column volumes of flow velocity eluting of 1～2BV/h, collects alcoholic solution part eluent, and concentrate drying gets the pericarpium lagenariae theine product.
2. the preparation method of pericarpium lagenariae theine according to claim 1 is characterized in that described extraction solvent is 50～70% acetone-water solution, solid-liquid ratio (g: ml)=1: 8～10, extract 30～50 ℃ of temperature, extraction time 4.5～7.5h.
3. the preparation method of pericarpium lagenariae theine according to claim 1 and 2 is characterized in that in the described purification by macroporous resin step, eluting is 30% with ethanol water concentration.
4. the preparation method of pericarpium lagenariae theine according to claim 3 is characterized in that described ethanol aqueous wash separation of flow speed is 2BV/h, and the eluent consumption is 6 column volumes.
5. the preparation method of pericarpium lagenariae theine according to claim 1 is characterized in that this method is:
1. be that 50～70% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration, extract solvent feed than (g: ml)=1: 8～10, extract 30～50 ℃ of temperature, extraction time 4.5～7.5h;
2. extracting solution concentrate drying, with gained extractum with water dissolution, filtration;
3. filtrate is through D
101Macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water then;
4. use 30% ethanol water, with 6 column volumes of flow velocity eluting of 1～2BV/h, collect eluent, concentrate drying gets the pericarpium lagenariae theine product.
6. the preparation method of pericarpium lagenariae theine according to claim 1 is characterized in that this method is:
1. be that 60% acetone-water solution extracts the Herba Desmodii Triquetri (Herba Tadehagi Triquetri) raw material after pulverizing with concentration, extracting the solvent load solid-liquid ratio is 1: 8, extracts 30 ℃ of temperature, extraction time 6h;
2. extracting solution concentrate drying, with gained extractum with water dissolution, filtration;
3. filtrate is through D
101Macroporous resin adsorption, it is colourless to be eluted to effluent with deionized water then;
4. use 30% ethanol water, with 6 column volumes of flow velocity eluting of 1～2BV/h, collect eluent, concentrate drying gets the pericarpium lagenariae theine product.
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Non-Patent Citations (3)
| Title |
|---|
| Wei Xiang,RongTao Li,et al..Four New Prenylated Isoflavonoids in Tadehagi triquetrum.J.Agric.Food.Chem.53 2.2005,53(2),267-271. |
| Wei Xiang,RongTao Li,et al..Four New Prenylated Isoflavonoids in Tadehagi triquetrum.J.Agric.Food.Chem.53 2.2005,53(2),267-271. * |
| 姚新生."鞣质的提取与分离".《天然药物化学(第二版)》.人民卫生出版社,1995,第257页. |
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