CN100387285C - Refining method for caoshanhu by menbrane technology separation - Google Patents
Refining method for caoshanhu by menbrane technology separation Download PDFInfo
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- CN100387285C CN100387285C CNB2005100539569A CN200510053956A CN100387285C CN 100387285 C CN100387285 C CN 100387285C CN B2005100539569 A CNB2005100539569 A CN B2005100539569A CN 200510053956 A CN200510053956 A CN 200510053956A CN 100387285 C CN100387285 C CN 100387285C
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Abstract
The present invention relates to a method of extracting a traditional Chinese medicinal material, namely sarcandra glabra, through a membrane separation technique. Aiming at the water decoction of sarcandra glabra, high yield of the sarcandra glabra and low separation and extraction of energy consumption are realized by the membrane separation technique, namely that the water decoction of the sarcandra glabra is ultrafiltered with the organic membrane of polysulfone, acetate cellulose, polyacrylonitrile or polyimide with the intercepting molecular weight of 1000 to 20000 so as to eliminate tannin, protein, starch and resin, and penetration liquid is decompressed and concentrated through a conventional method. The present invention simplifies the extraction and refining process and has the advantages of no organic solvent consumption, simple operation, cost reduction and easy automation realization of production.
Description
Technical field
The present invention relates to the membrane separation technique extracting method of Chinese crude drug Herba Pileae Scriptae,, utilize membrane separation process to realize the high yield of Herba Pileae Scriptae, the separation and Extraction of low energy consumption promptly at the decocting liquid of Herba Pileae Scriptae.
Background technology
Herba Pileae Scriptae [Sarcandrm glabra (Thunb.) Nakai] has another name called Herba Sarcandrae, Herba Pileae Scriptae, Ramulus Sambuci Williamsii, is Chloranthaceae Herba Pileae Scriptae platymiscium.The Herba Pileae Scriptae chemical constituent shows, herb contains flavonoid glycoside, isofraxidin, Fumaric acid, succinic acid and tannic acid, and composition such as trace element manganese, in the Herba Pileae Scriptae decoction liquor, except that above-mentioned active ingredient, also there are macromolecular substances and impurity such as many microgranules, submicron and floccule such as a large amount of tannins, protein, starch, resin.The existing extraction and separation technology of Herba Pileae Scriptae mainly is to adopt decoction and alcohol sedimentation technique, as 2000 editions " in the Chinese pharmacopoeia under the method for making item of " FUFANG CAOSHANHU HANPIAN "; And for example the extraction and separation technology of " Chinese Pharmaceutical Journal " middle Herba Pileae Scriptae of JIUYUE the 29th volume the 9th interim " mouthful routed one development and the clinical practice of pasting peaceful membrane " in 1994 mainly is to adopt the different concentration ethanol percolation to extract; Publication number is that the Herba Pileae Scriptae extraction and separation technology mainly adopts water extract-alcohol precipitation in the patent documentation of CN1528389A " Grass and coral powder preparation methods ", then alcoholic solution is carried out ultrafiltration; Above method not only is difficult to eliminate impurity composition, and easy loss effective ingredient even waste a large amount of organic solvents, and yield of Ti Quing and purity are lower simultaneously; Therefore seek a kind of behaviour's technology simple, cut down the consumption of energy, highly purified extracting method seems especially urgent.
Summary of the invention
The present invention seeks to improve extract yield, raising purity, the extraction cost that reduces of Herba Pileae Scriptae, remove macromolecular substances and impurity such as many microgranules, submicron and floccule such as tannin, protein, starch, resin, adopt membrane technology to separate and separate, thereby reach the purpose of concentrated, separation, purification the conventional decocting liquid of Herba Pileae Scriptae is further refining.
The present invention is achieved through the following technical solutions:
Adopt polysulfone membrane or cellulose acetate or polyacrylonitrile, polyimide film organic membrane that Herba Pileae Scriptae decocting liquid is carried out ultrafiltration, remove tannin, protein, starch, resin, permeate is concentrating under reduced pressure according to a conventional method.
The present invention can also be achieved through the following technical solutions:
The molecular cut off of above-mentioned organic membrane is 1000～20000.
The preferred scheme of the present invention can be:
The molecular cut off of selecting film for use is that 5000～15000 polysulfone membrane or cellulose acetate membrane are carried out ultrafiltration.
The present invention has the following advantages compared to existing technology:
(1) reduces loss of active ingredients, be beneficial to the biological activity, physics and the chemical stability that keep Chinese herbal medicine effective ingredients;
(2) can remove heavy metal, the residual pesticide impurity that becomes to grade, and the effect of removing various microgranule colloids, antibacterial and pyrogen in the solution is arranged;
(3) simplify technology, shortening cycle, cut down the consumption of energy and save resource such as a large amount of ethanol, thereby reduce cost, increase economic efficiency;
(4) on the basis that guarantees the product curative effect, reduce dose.
Below be the antiinflammatory action drug effect contrast experiment of the different extraction processes of Herba Pileae Scriptae:
Method: adopt the implantation cotton balls to cause rat granulation tissue hyperplasia method, observe the effect of medicine to chronic inflammatory disease; Adopt carrageenin to cause the rat paw edema method and observe medicine acutely inflamed effect.The result: Herba Pileae Scriptae can obviously suppress by the rat chronic inflammation granulation tissue hyperplasia due to the implantation cotton balls; Also can suppress by the rat paw edema due to the carrageenin. and two groups of drug effect no significant differences.
1 test material
Animal: the SD rat is provided by Jiangxi Medical College's animal center
Medicine and reagent: Herba Pileae Scriptae extractum is provided by Jiangzhong Pharmaceutical Co., Ltd.; Carrageenin
Test apparatus: electronic balance; Slide gauge (0.02mm)
Experimental condition: before and after the administration, the experimental rat sub-cage rearing is provided by full-valence pellet feed (being provided by Jiangxi Medical College's animal center), freely drinks water 22 ± 3 ℃ of room temperatures, relative humidity 45-65%.
Grouping and level prescription method: with 50 of SD rats, be divided into 5 groups at random, 10 every group, irritate stomach respectively and give Herba Pileae Scriptae extractum water ultrafiltration 19.11,38.22mg/kg, Herba Pileae Scriptae extractum water extract-alcohol precipitation 19.11,38.22mg/kg and isometric water.
Statistical method: (X ± S) expression adopts and designs the t check relatively of two sample averages in groups experimental result with mean ± standard deviation.
2 test methods
Cotton balls is implanted experiment: male SD rat, and body weight 130-180g, the ether light anaesthesia is made abdominal incision under aseptic condition, and with 23mg cotton balls autoclaving, each cotton balls adds ampicillin 1mg/0.1ml again, and after 50 ℃ of oven dry, it is subcutaneous to implant groin.Performing the operation began administration the same day, every day 1 time, and continuous 7 days, to weigh earlier in the 8th day, 1h takes off cervical vertebra execution with rat after the administration, peels off and take out the granuloma induced by implantation of cotton pellets tissue, weighs after dry in 60 ℃ of baking ovens, deducts the weight of former cotton balls, is the granuloma net weight.
Carrageenin causes the rat paw edema experiment: get male SD rat, body weight 130-160g.1h after the administration in the right back sufficient plantar subcutaneous injection carrageenin 0.1ml/ of rat only, causes scorching back 1h, 2h, 4h, 6h, measures sufficient sole of the foot portion thickness respectively, calculate swelling value=cause scorching back thickness-cause scorching before thickness, thickness before swelling rate=swelling value/cause is scorching.
3 results
To the swollen outgrowth influence of rat granuloma: Herba Pileae Scriptae extractum water is put forward ultrafiltration and the heavy dose of group of water extract-alcohol precipitation can illustrate that it has certain inhibitory action to chronic inflammatory disease by the rat chronic granulation tissue hyperplasia of implanting due to the cotton balls.And the drug effect no significant difference of two groups of extractum.The results are shown in Table 1:
Table one Herba Pileae Scriptae is to the bullate influence of rat granuloma (X ± S)
| Group | Number of animals (only) | Granuloma dry weight (mg/100g) | Suppression ratio (%) |
| Blank group | 10 | 30.26±8.57 | |
| Herba Pileae Scriptae extractum water is put forward dosage group in the ultrafiltration | 10 | 24.37±7.30 | 19.46％ |
| Herba Pileae Scriptae extractum water is put forward the heavy dose of group of ultrafiltration | 10 | 21.65±4.50 * | 28.45％ |
| Dosage group in the Herba Pileae Scriptae extractum water extract-alcohol precipitation | 10 | 24.64±5.34 * | 18.57％ |
| The heavy dose of group of Herba Pileae Scriptae extractum water extract-alcohol precipitation | 10 | 19.66±5.02 * | 35.03％ |
Compare with matched group,
*P＜0.05
On Carrageenan causes the influence of rat paw edema: Herba Pileae Scriptae extractum water is put forward the heavy dose of group of ultrafiltration and water extract-alcohol precipitation can obviously suppress rat paw edema due to the carrageenin, generally 1h onset after administration, and effect lasts till 6h.And the drug effect no significant difference of two groups of extractum.The results are shown in Table 2:
Table 2 Herba Pileae Scriptae on Carrageenan cause the rat paw edema rate influence (X ± S, n=10)
| Group | Swelling rate 1 hour | 2 hours swelling rates | 4 hours swelling rates | 6 hours swelling rates |
| Blank group | 0.26±0.12 | 0.51±0.15 | 0.41±0.15 | 0.31±0.11 |
| Herba Pileae Scriptae extractum water is put forward dosage group in the ultrafiltration | 0.23±0.06 | 0.44±0.07 | 0.41±0.06 | 0.31±0.07 |
| Herba Pileae Scriptae extractum water is put forward the heavy dose of group of ultrafiltration | 0.17±0.07 * | 0.36±0.07 * | 0.35±0.08 * | 0.23±0.06 * |
| Dosage group in the Herba Pileae Scriptae extractum water extract-alcohol precipitation | 0.22±0.10 | 0.43±0.14 | 0.34±0.10 | 0.28±0.09 |
| The heavy dose of group of Herba Pileae Scriptae extractum water extract-alcohol precipitation | 0.21±0.06 * | 0.41±0.08 * | 0.34±0.11 * | 0.26±0.09 * |
Compare with matched group,
*P＜0.05
4 conclusions
The test of Herba Pileae Scriptae antiinflammatory shows that this product can obviously suppress by the rat chronic inflammation granulation hyperplasia due to the implantation cotton balls, and suppression ratio can reach 35.03%, illustrates that it has good inhibitory effect to chronic inflammatory disease.This product also can suppress to illustrate that by the rat paw edema due to the carrageenin it has good inhibitory effect to acute inflammation.Above-mentioned pharmacological action has constituted the pharmacological basis of its treatment pharyngitis.And the drug effect no significant difference of two groups of extractum.
The specific embodiment
Embodiment 1.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polysulfone membrane ultrafiltration, and molecular cut off is 5000, and the permeate concentrating under reduced pressure becomes 500 milliliters clear paste, promptly.
Embodiment 2.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the cellulose acetate membrane ultrafiltration, and molecular cut off is 5000, and the permeate concentrating under reduced pressure becomes 495 milliliters clear paste, promptly.
Embodiment 3.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the cellulose acetate membrane ultrafiltration, and molecular cut off is 20000, and the permeate concentrating under reduced pressure becomes 560 milliliters clear paste, promptly.
Embodiment 4.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filters, and gets 80 liters of filtrates, and filtrate is used the polyacrylonitrile membrane ultrafiltration, molecular cut off is 20000, and it is 565 milliliters of 1.24～1.26 clear paste that the permeate concentrating under reduced pressure becomes relative density, promptly.
Embodiment 5.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filters, and gets 80 liters of filtrates, and filtrate is used the polyimides membrane ultrafiltration, molecular cut off is 20000, and it is 567 milliliters of 1.24～1.26 clear paste that the permeate concentrating under reduced pressure becomes relative density, promptly.
Embodiment 6.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polyimides membrane ultrafiltration, and molecular cut off is 1000,475 milliliters of clear paste that the permeate concentrating under reduced pressure becomes, promptly.
Embodiment 7.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polyacrylonitrile membrane ultrafiltration, and molecular cut off is 1000, and the permeate concentrating under reduced pressure becomes 472 milliliters clear paste, promptly.
Embodiment 8.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polysulfone membrane ultrafiltration, and molecular cut off is 1000, and the permeate concentrating under reduced pressure becomes 460 milliliters clear paste, promptly.
Embodiment 9.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polysulfone membrane ultrafiltration, and molecular cut off is 20000, and the permeate concentrating under reduced pressure becomes 558 milliliters clear paste, promptly.
Embodiment 10.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the polysulfone membrane ultrafiltration, and molecular cut off is 15000, and the permeate concentrating under reduced pressure becomes 552 milliliters clear paste, promptly.
Embodiment 11.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the cellulose acetate membrane ultrafiltration, and molecular cut off is 1000, and the permeate concentrating under reduced pressure becomes 465 milliliters clear paste, promptly.
Embodiment 12.
Get 5 kilograms of Herba Sarcandraes, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, and gets 80 liters of filtrates, and filtrate is used the cellulose acetate membrane ultrafiltration, and molecular cut off is 15000, and the permeate concentrating under reduced pressure becomes 556 milliliters clear paste, promptly.
Claims (2)
1. the membrane technology separation and refining method of a Herba Pileae Scriptae, in Herba Pileae Scriptae decocting liquid, adopt the further refining separation of membrane technology, it is characterized in that: adopting molecular cut off is that 1000～20000 organic membrane polysulfone membrane or cellulose acetate or polyacrylonitrile or polyimide film carry out ultrafiltration to Herba Pileae Scriptae decocting liquid, removes tannin, protein, starch, resin.
2. the membrane technology separation and refining method of Herba Pileae Scriptae according to claim 1, it is characterized in that: select for use polysulfone membrane or cellulose acetate membrane to carry out ultrafiltration, the molecular cut off of film is 5000～15000.
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Non-Patent Citations (6)
| Title |
|---|
| 中华人民共和国药典. 国家药典委员会，523，化学工业出版社. 2000 |
| 中华人民共和国药典. 国家药典委员会，523，化学工业出版社. 2000 * |
| 膜分离技术在中药制剂中的应用. 杨明，刘小彬.世界科学技术-中医药现代化，第6卷第2期. 2004 |
| 膜分离技术在中药制剂中的应用. 杨明，刘小彬.世界科学技术-中医药现代化，第6卷第2期. 2004 * |
| 超滤膜分离技术在中药生产中的应用研究. 宁慧青.山西化工，第23卷第3期. 2003 |
| 超滤膜分离技术在中药生产中的应用研究. 宁慧青.山西化工，第23卷第3期. 2003 * |
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