CN1208468C - Method of leaching pairs polyphylla saponin - Google Patents
Method of leaching pairs polyphylla saponin Download PDFInfo
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- CN1208468C CN1208468C CN 03135590 CN03135590A CN1208468C CN 1208468 C CN1208468 C CN 1208468C CN 03135590 CN03135590 CN 03135590 CN 03135590 A CN03135590 A CN 03135590A CN 1208468 C CN1208468 C CN 1208468C
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- Prior art keywords
- leaching
- alcohol
- rhizoma paridis
- hours
- dian fenmei
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- 238000002386 leaching Methods 0.000 title claims abstract description 34
- 229930182490 saponin Natural products 0.000 title claims abstract description 26
- 150000007949 saponins Chemical class 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims description 23
- 241000416918 Polyphylla Species 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 241000244987 Daiswa polyphylla Species 0.000 claims description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 108090000790 Enzymes Proteins 0.000 claims description 4
- 102000004190 Enzymes Human genes 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 3
- 101000925662 Enterobacteria phage PRD1 Endolysin Proteins 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 230000003625 amylolytic effect Effects 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 102000004139 alpha-Amylases Human genes 0.000 abstract 3
- 108090000637 alpha-Amylases Proteins 0.000 abstract 3
- 229940024171 alpha-amylase Drugs 0.000 abstract 3
- 235000017709 saponins Nutrition 0.000 abstract 3
- 239000000843 powder Substances 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 14
- 238000000605 extraction Methods 0.000 description 10
- 229930182470 glycoside Natural products 0.000 description 9
- 150000002338 glycosides Chemical class 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 208000002193 Pain Diseases 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000036407 pain Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 206010010904 Convulsion Diseases 0.000 description 2
- 206010042674 Swelling Diseases 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000036461 convulsion Effects 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 208000004078 Snake Bites Diseases 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000001088 anti-asthma Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002949 hemolytic effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005477 standard model Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000472 traumatic effect Effects 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Saccharide Compounds (AREA)
Abstract
The present invention discloses a method for leaching paris rhizome saponins, which comprises the following steps: (1), crushing clean and dry paris rhizome into coarse fine; (2), weighing one part by weight of paris rhizome powder, immersing the paris rhizome powder in 10 times quantity (V/W) of 40 DEG C warm water for two to three hours, filtering moisture, adding 10 parts by weight of 20% alcohol and 5 parts of alpha-amylase; then, heating and boiling the alcohol and the alpha-amylase; (3), back flowing the alcohol and the alpha-amylase for leaching for three times to obtain the desired paris rhizome saponins, wherein the leaching in each time is not less than two hours. The present invention effectively shortens leaching time and enhances leaching rate, and the leaching rate is larger than 97%; the present invention can sufficiently leach the paris rhizome saponins and greatly reduce alcohol use quantity.
Description
Technical field
The present invention relates to a kind of Paris polyphylla extraction of effective components, more particularly, the water logging that the present invention relates to Rhizoma Paridis saponin goes out method.
Background technology
Paris polyphylla is liliaceous plant Rhizoma Paridis (Pairs Polyphylla Smith Var.Yunnanensis[Franch.] Hand-Mazz) or Rhizoma Paridis (Paris Polyphylla Smith Var.Chinensis[Franch] Hara) rhizome.This product bitter is slightly cold, and is slightly poisonous; Can be clearing heat and detoxicating, swelling and pain relieving, cool liver arresting convulsion.It is swollen to be used to treat the sore carbuncle, swelling and pain in the throat, and venomous snake bite is carried, traumatic pain, convulsion with spasms.Pharmacological evaluation has antibacterial, analgesia and antiasthmatic effect; Decoction and saponin(e all have hemolytic action (seeing 2000 editions one one of the Pharmacopoeia of the People's Republic of China for details).The Paris polyphylla The Chemical Constituents is shown main effective constituent is saponin(e in the Paris polyphylla.
The leaching method of existing Rhizoma Paridis saponin is under the 95% reflow of alcohol condition with 10 times of amounts, to leach 3 times, and each extraction time is 5 hours.Extraction time is long, and the alcohol consumption is big, and this is the problem that this technical field need conscientiously be solved.
Summary of the invention
The objective of the invention is provides a kind of leaching method of improved Rhizoma Paridis saponin at the deficiencies in the prior art part.
Purpose of the present invention is achieved by following technical proposals.
Except as otherwise noted, the percentage ratio that is adopted among the present invention is weight percentage.
The invention provides a kind of extracting method of Rhizoma Paridis saponin, this method comprises the steps:
(1) clean, dry Paris polyphylla is carried out coarse reduction;
(2) take by weighing the Paris polyphylla meal of 1 weight part, 10 times of amounts (V/W) water soaked 2～3 hours down at 40 ℃, and filter solid carbon dioxide branch adds the alcohol and the 5 unit α-Dian Fenmei of 10 weight parts 20%, and described unit refers to 200 units of common enzyme activity, and heat hot is boiled;
(3) backflow is leached 3 times, is no less than 2 hours at every turn, promptly obtains required Rhizoma Paridis saponin.
Wherein said α-Dian Fenmei is called Alpha-starch lytic enzyme or amylolytic enzyme again, selects high temperature modification or middle warm type for use.
Beneficial effect: the present invention is optimized by the extract technology to existing Rhizoma Paridis saponin.Content with Rhizoma Paridis saponin is index, adopts orthogonal experiment that multifactor investigation is carried out in the leaching of Rhizoma Paridis saponin.Found out the optimal conditions that leaches Rhizoma Paridis saponin by test.Shortened extraction time effectively, improved leaching yield, leaching yield＞97% can fully leach Rhizoma Paridis saponin, and reduces the alcohol consumption significantly.Extracting solution can also utilize membrane concentration to replace concentrating under reduced pressure the normal temperature brother, has reduced unnecessary alcohol loss and loss of effective components.
Embodiment
By specific embodiment given below and controlled trial thereof, can further be well understood to the present invention.But they are not limitation of the invention.
Embodiment 1
1.1 chromatographic condition HP1100 chromatographic instrument, chromatographic column: Symmetry C8 analytical column (stream of 4.6mm * 250mm) phase: acetonitrile: water=45: 55, detect wavelength: 203 μ m column temperatures: 40 ℃.
1.2 the preparation Paris polyphylla drying and crushing of need testing solution accurately takes by weighing Paris polyphylla 10 grams, soaks 2～3 times under 10 times of amounts (V/W) warm water (40 ℃), be no less than 2 hours at every turn, by orthogonal table arrangement test, in the solvent of 10 times of amounts, reflux and leach filtered while hot respectively, merging filtrate, the saturated n-butanol extraction of filtrate water is collected n-butanol layer liquid, volatilizes, in the 10ml bottle, the HPLC method is surveyed its saponin content with the dissolve with methanol constant volume.
1.3 standard control product formulations prepared from solutions (1) accurately takes by weighing the Rhizoma Paridis saponin standard model I that is dried to constant weight, II, III respectively, IV, put in the 10ml volumetric flask, add dissolve with methanol and be diluted to scale, be mixed with and contain I, II, III, the IV saponin(e is respectively 0.44,0.40,0.40, the standard specimen solution of 0.38mg/ml.(2) accurately take by weighing 10 grammes per square metre building samples, put in the 250ml round-bottomed flask, leach 4 times each 4 hours with 10 times of 95% reflow of alcohol, surely be dissolved in the 10ml volumetric flask, HPLC survey its saponin content for and this content contrasted as crude drug active constituent content and trial-product.
Embodiment 2
Get three parts of Paris polyphylla sample 10g, soak 2～3 times under 10 times of amounts (W/V) warm water (40 ℃), filter is done after each 2 hours, and water, 10% alcohol, 20% alcohol carry out leaching experiment under boiling respectively then, leach three times, are no less than 2 hours at every turn.The result: three kinds of leaching agents leach liquors for the first time are khaki color or brown viscous fluid, and are mobile poor, can't be with filter paper, cloth bag, three layers of gauze, approach mode such as cotton layer and filter, and there is a change for the better for second and third time filtrate.After adding the α-Dian Fenmei material, above-mentioned first time, leach liquor can be with above-mentioned any filter type filtration.
Orthogonal test I result investigates the amount of α-Dian Fenmei, extraction temperature, and three factors such as leaching number of times the results are shown in Table 1,2 to the influence of the total glycosides leaching yield of Paris polyphylla.
Embodiment 3
Orthogonal test II and result fix according to the result who tests I and add α-Dian Fenmei part at every turn, investigate extraction temperature, leach number of times, and three factors such as ethanol concn the results are shown in Table 3,4 to the influence of the total glycosides leaching yield of Paris polyphylla.
Table 1 level of factor table
Horizontal I (temperature) II α-Dian Fenmei III (leaching number of times)
1 60 ℃ 1 part 2
2 80 ℃ 2 parts 3
3 boil 3 part 4
Table 2 orthogonal experimental design table and result
Numbering I II III result (%)
1 1 1 1 49.76
2 1 2 2 47.27
3 1 3 3 61.17
4 2 1 2 51.90
5 2 2 3 65.49
6 2 3 1 40.60
7 3 1 3 70.82
8 3 2 2 54.00
9 3 3 1 63.76
1 part of α-Dian Fenmei, boil, leach for 4 times, leaching yield is 70.82%, optimal conditions
Solvent is a water.
Table 3: level of factor table
Horizontal I (ethanol concn) II (leaching number of times) III (temperature)
1 5% 2 boils
2 10％ 3 80℃
3 20% 4 boil
Table 4 orthogonal array and result
Numbering I II III result (%)
1 1 1 1 59.49
2 1 2 2 51.80
3 1 3 2 64.27
4 2 2 1 72.54
5 2 3 2 94.09
6 2 1 1 66.34
7 3 3 1 76.75
8 3 1 2 82.67
9 3 2 1 96.64
Optimal conditions 20% alcohol boils, and leaches 3 times, and leaching yield is 96.64%
Embodiment 4
Orthogonal test III and result are according to the result of test I, II, and fixedly extraction temperature is for boiling, and leaching number of times is 3 times.Investigate of the influence of two factors such as α-Dian Fenmei, ethanol concn once more, the results are shown in Table 5,6 the total glycosides leaching yield of Paris polyphylla.
Table 5 level of factor
Horizontal I (No:1) II (ethanol concn)
13 part 10%
25 part 20%
Table 6 orthogonal design and data processing
Numbering I II result 2 (%)
1 1 1 72.57
2 2 2 93.93
3 1 2 87.33
4 2 1 77.65
5 parts of α-Dian Fenmei of optimal result, 20% alcohol boil and leach three times
Interpretation of result is with 95% alcohol thermal backflow, each 10 times of alcohol volumes, 4 times, each 4 hours.Two parallel samples are measured total glycosides content and are respectively 4.6417mg/g, 4.3984mg/g, and its mean value is 4.52mg/g.The polarity of the total glycosides of Paris polyphylla is little, and the dissolving in water is very little, and water is difficult to total glycosides is leached clean as solvent fully.
Therefore in experiment II, fixedly the amount of α-Dian Fenmei suitably adds alcohol (being controlled in 20%), has investigated ethanol concn, and extraction temperature leaches the influence of number of times to total glycosides leaching yield, and the result shows that optimised process is I
3II
2III
1, influence factor is ethanol concn＞extraction temperature＞leaching number of times.From test II result as can be seen, be reference standard with the result of alcohol thermal backflow, relatively list in result 2 in the table 6 with the result of test II III.Comprehensive test I II III result, in Optimal Temperature with leach under the number of times, the contriver investigates the influence to total glycosides leaching yield of the amount of α-Dian Fenmei and ethanol concn again.Find out best leaching scheme from above-mentioned 3 test-results: promptly during boiling, reflux and leach 3 times, be no less than 2 hours at every turn, can leach the total glycosides of Paris polyphylla fully with the α-Dian Fenmei of 20% alcohol of each 10 times of amounts and 5 parts.
Embodiment 5
Under above-mentioned best leaching condition, 1 weight part Paris polyphylla, 95% alcohol consumption is: 10 * 3 * 20%=6 weight part; And under conventional leaching condition, common 95% alcohol consumption is 1: 10～15,1 weight part Paris polyphylla then, and 95% alcohol consumption is 10～15 weight parts.
Embodiment 6
Proof test: get same two parts of the test agents that supply, be optimized the preparation of need testing solution respectively, measure its content, make comparisons with the content that 95% alcohol leaches under the same conditions, Rhizoma Paridis saponin is respectively 97.4%, 100.3%, and the purpose that reaches selection process is described.
Claims (3)
1. the leaching method of a Rhizoma Paridis saponin may further comprise the steps:
(1) clean, dry Paris polyphylla is carried out coarse reduction;
(2) take by weighing the Paris polyphylla meal of 1 weight part, 10 times of amounts (V/W) water soaks under 40 ℃ 2～3 times, is no less than 2 hours at every turn, filter solid carbon dioxide branch, add the alcohol and the 5 unit α-Dian Fenmei of 10 weight parts 20%, described unit refers to 200 units of common enzyme activity, and heat hot is boiled; (3) backflow is leached 3 times, is no less than 2 hours at every turn, promptly obtains required Rhizoma Paridis saponin.
2. the leaching method of Rhizoma Paridis saponin according to claim 1, wherein said α-Dian Fenmei is called Alpha-starch lytic enzyme or amylolytic enzyme again, selects high temperature modification or middle warm type for use.
3. the leaching method of Rhizoma Paridis saponin according to claim 1, wherein to leach be at every turn with the leaching that refluxes in boiling of 20% alcohol of 10 weight parts and 5 parts of α-Dian Fenmei to the described backflow of step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135590 CN1208468C (en) | 2003-08-11 | 2003-08-11 | Method of leaching pairs polyphylla saponin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135590 CN1208468C (en) | 2003-08-11 | 2003-08-11 | Method of leaching pairs polyphylla saponin |
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| CN1490413A CN1490413A (en) | 2004-04-21 |
| CN1208468C true CN1208468C (en) | 2005-06-29 |
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| CN105997749A (en) * | 2016-07-20 | 2016-10-12 | 云南白药集团股份有限公司 | Gel having acne removing effect |
| CN108531318A (en) * | 2018-07-21 | 2018-09-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of preparation process of the soap containing paris polyphylla extract |
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