CN100500196C - Method for preparing paris polyphylla total saponin - Google Patents
Method for preparing paris polyphylla total saponin Download PDFInfo
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- CN100500196C CN100500196C CNB2006100522238A CN200610052223A CN100500196C CN 100500196 C CN100500196 C CN 100500196C CN B2006100522238 A CNB2006100522238 A CN B2006100522238A CN 200610052223 A CN200610052223 A CN 200610052223A CN 100500196 C CN100500196 C CN 100500196C
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- rhizoma paridis
- supernatant
- total saponins
- resin
- merge
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- 238000002360 preparation method Methods 0.000 claims abstract description 14
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Abstract
The present invention discloses preparation process and use of Chinese paris rhizome total saponin as the effective component. The preparation process of the present invention is one simplified one comprising alcohol extraction, water precipitation, and deionized water washing and depositing. The preparation process has lowered alcohol consumption, obviously reduced production cost, no use of acetone, high effective component yield, high product purity and stable quality. The present invention also relates to the application of Chinese paris rhizome total saponin in preparing externally applied medicine for diminishing inflammation, eliminating swelling and relieving pain, antiviral medicine, and anti-tumor medicine.
Description
Technical field
The invention belongs to pharmaceutical field, particularly disclose a kind of preparation method and its usage of Rhizoma Paridis effective site-total saponins.
Background technology
Rhizoma Paridis is the dry rhizome of liliaceous plant Rhizoma Paridis Paris polyphylla Smith var.yunnanensis (Franch.) Hand.M azz. and Rhizoma Paridis P.polyphylla Smith var.chinensis (Franch.) Hara.In China, Rhizoma Paridis is multiple famous Chinese patent medicine, as the main composition medicine of Yunnan BAIYAO, jidesheng sheyao tablets, GONGXUENING JIAONANG etc.But these medicines are still basically with after Rhizoma Paridis and the other medicines compatibility, adopt water or the direct preparation of alcoholic acid extract to form, and are keeping the preparation method of Chinese medicine.Rhizoma Paridis total saponins is the main effective ingredient of the multiple pharmacological action of Rhizoma Paridis, and Rhizoma Paridis effective site is exactly to use modern science and technology total saponins constituents wherein is enriched to 50% above content.The medicine of being made by Rhizoma Paridis total saponins has multiple advantages such as dose is few, the preparation performance is good, and it is big to have overcome the Chinese medicine consumption, many shortcomings that technology is thick.At present, the drug main of being made by Rhizoma Paridis total saponins will be used for the treatment of metrorrhagia.In the existing technology of preparing, the content that has two kinds of methods to reach to make total saponins in the Rhizoma Paridis extract surpasses 50% requirement.These two kinds of methods are respectively simple resin adsorption method and membrane filtration binding resin absorption methods.Simple resin method is that the extracting solution of Rhizoma Paridis is concentrated, centrifugal, resulting supernatant prepares Rhizoma Paridis total saponins by macroporous resin column, the defective of this method is: because the Rhizoma Paridis total saponins poorly water-soluble, a large amount of Rhizoma Paridis total saponins are precipitated out when extracting solution concentrates, thereby only kept the part total saponins in the supernatant after causing concentrated solution centrifugal, made to prepare Rhizoma Paridis total saponins by this method, the extraction recovery of effective ingredient is only less than 50%.Membrane filtration binding resin absorption method improved the simple resin method effective ingredient response rate low deficiency, but processing step is loaded down with trivial details, the ethanol consumption is many in the production process, and along with skyrocketing of energy prices, complicated, the ethanol consumption of technology crossed and mostly made big industrial cost significantly improve.In addition, when decolouring, use acetone and other organic solvent in this technology, also increased production cost and danger to a certain extent.
Summary of the invention
Purpose of the present invention is exactly the deficiency that overcomes in the existing Rhizoma Paridis total saponins production technology, and a kind of preparation method of Rhizoma Paridis effective site-total saponins is provided, and the new purposes of Rhizoma Paridis total saponins in pharmacy is provided simultaneously.
The present invention is achieved in that Rhizoma Paridis decoction pieces or coarse powder, adds 6～12 times 60%～95% aqueous alcohol (V/W), reflux, extract, 2～3 times, and each extraction time is 1～3 hour, merge extractive liquid,, the extracting solution after the merging is centrifugal; Tell precipitation and supernatant, with supernatant concentration to 0.2～1.0g crude drug/ml, centrifugal after the standing over night then, get supernatant A and precipitate A '.To precipitate A ' in add the deionized water be equivalent to extract used crude drug amount 1～5 times (V/W) and stir, wash, and then centrifugal, inclining supernatant, supernatant B and deposit B '; Merge supernatant A and B, will merge supernatant behind A, the B by the chromatographic column of macroporous adsorbent resin is housed, supernatant is 1:4～1:10 by the ratio of the amount of Rhizoma Paridis total saponins and dried resin, and last column flow rate 1～4BV/h, resin path height ratio are 1:3～1:9; Wash resin 3～12BV with water, elution flow rate is 1-6BV/h, and water elution liquid discards; With containing 65～95% aquiferous ethanol (V/V) eluting, 2～6BV, flow velocity is 1～6BV/h, collects ethanol elution; It is 1.1～1.25 that ethanol elution is evaporated to relative density, with deposit B ' merge, drying promptly gets Rhizoma Paridis effective site-total saponins.
Described macroporous resin is nonpolar or the low pole macroporous resin.
The Rhizoma Paridis total saponins content that makes with said method is 50%～90%, and wherein the amount of Rhizoma Paridis saponin I and Rhizoma Paridis saponin II adds up to 10%～20%, and the response rate of Rhizoma Paridis total saponins is greater than 85%.
The present invention has changed the processing method that precipitates part in the prior art in the membrane filtration binding resin absorption method, only realize, be reduced to by steps such as alcohol extraction, membrane filtration, acetone defat, resin decolorization and finish, make preparation technology significantly simplify by alcohol extracting-water precipitating and deionized water wash precipitation.Simultaneously, reduce the ethanol consumption in the production process, significantly reduced production cost, saved the use of acetone, further reduced the danger in cost and the production; Extracts active ingredients response rate height, content height, steady quality.
Another inventive point of the present invention is that Rhizoma Paridis total saponins is as the application in preparation antiinflammatory, detumescence, analgesic external used medicine, antiviral drugs, antitumor and adjuvant therapy medicaments of tumor.
The present invention is raw material with the Rhizoma Paridis total saponins, it can be developed to the auxiliary preparation of suitable antiinflammatory, detumescence, pain relieving, antiviral, antitumor and tumor as acceptable carrier or pharmaceutic adjuvant on active component and the pharmacopedics, as capsule (soft capsule, hard capsule), gel, ointment, drop pill, tablet, granule, powder, oral liquid etc.
The pharmacodynamics test of Rhizoma Paridis total saponins
Medicine: Rhizoma Paridis ointment, content of dispersion are respectively 5%, 10%, 15%; Gel: content of dispersion is respectively 5%, 10%, 15%; Rhizoma Paridis total saponins: content 60%
Animal: new zealand white rabbit, Wister kind rat, Kunming mouse
Bacterial strain and Strain, cell strain:
People's esophageal cancer cell Eca-109, stomach cancer cell SGC-7901, leukaemia HL-60, Coxsackie virus strain (CVB
2), first
1Type (A
1) and first
3Type (A
3) influenza virus, Hela cell strain
(1) externally applied anti-inflammation, analgesic pharmacodynamics data
1. antiinflammatory test
1.1 mice auricle swelling method
Get 50 of 18-22g Kunming kind female mices, be divided into 5 groups at random, be respectively Rhizoma Paridis ointment group (high, medium and low dosage group), PIYANPINGSHUANG and excipient matched group.Medicine is applied to mouse right ear two sides 100mg/ only, behind the administration 30min, is coated with dimethylbenzene 0.1ml/ again in the mouse right ear two sides only, cause swollenly, left ear is not painted with normal ear.Taking off cervical vertebra behind the 1h and put to death mice, sweep away the disk of the same appropriate section of ears with diameter 6mm card punch, weigh, is the swelling degree with the difference of left and right ear weight, the antiinflammatory action of comparative drug.The results are shown in Table 1.
The influence of table 1 Rhizoma Paridis ointment xylol induced mice auricle edema
| Numbering | Number of animals (only) | Swelling degree (mg) |
| Vehicle group | 10 | 5.0±2.7 |
| PIYANPINGSHUANG | 10 | 1.3±0.65 |
| Rhizoma Paridis ointment 5% | 10 | 1.4±0.7 |
| Rhizoma Paridis ointment 10% | 10 | 1.1±0.7 * |
| Rhizoma Paridis ointment 15% | 10 | 1.0±0.6 ** |
Compare with the excipient matched group:
*: P＜0.05,
*: P＜0.01
1.2 Rhizoma Paridis ointment on Carrageenan is induced the test of rat paw edema
Get 50 of rats, by body weight, sex is divided into 5 groups at random.Rat right hind leg is used for fixing, makes a sign in its ankle with ball pen, the right hind of animal immerses in the sufficient volumetric measurement device, and immersion depth is the boundary with the sign place.Read the normal volume (ml) of animal right hind, be coated with medicine respectively in right hind for each treated animal, all administration 300mg only carries out subcutaneous injection 1% chondrus ocellatus Holmes glue 0.1ml/ in every Mus right hind vola mind-set ankle joint direction behind the 30min.Thereafter every 30min measures the volume of Mus hind leg, continuous 3 times, the results are shown in Table 2:
Table 2 Rhizoma Paridis ointment on Carrageenan is induced the influence of rat paw edema
Compare with the excipient matched group:
*P＜0.05,
*P＜0.01
1.3 50 of rats are got in swollen test to rat granuloma, divide 5 groups at random.Lumbar injection barbital sodium 30mg.kg-1 anesthesia, strange portion sterilizes with iodine tincture about every Mus, after 75% cotton ball soaked in alcohol takes off iodine, the osculum that each 1cm is long, soak with the autoclaving cotton balls (penicillin and streptomycin mixed liquor 0.2ml) of ophthalmology tweezers 20mg, oven dry, implant from incision subcutaneous, skin suture at random.Be coated with respectively with Rhizoma Paridis gel, excipient and PIYANPINGSHUANG the same day from operation, dosage only is 300mg/, and coating is in the granuloma place, successive administration 8d opened former otch on the 9th day cotton balls is taken out together with connective tissue on every side, rejected fatty tissue, put 70 ℃ of constant temperature dryings in the baking oven, weigh.The weight that claims is deducted the former weight of cotton balls promptly get granuloma weight.Relatively the difference of each group the results are shown in Table 3.
Table 3 Rhizoma Paridis gel is to the influence of rat granuloma
| Numbering | Number of animals (only) | Cotton balls granulation dry weight (mg) |
| Vehicle group | 10 | 69.2±5.8 * |
| PIYANPINGSHUANG | 10 | 86±4.9 |
| Rhizoma Paridis gel 5% | 10 | 75±7.2 ** |
| Rhizoma Paridis gel 10% | 10 | 68±6.5 ** |
| Rhizoma Paridis gel 15% | 10 | 63±3.6 ** |
Compare with the excipient matched group:
*: P＜0.05,
*: P＜0.01.
2. analgesic effect pharmacodynamics test
Constant temperature water bath apparatus with hot plate preheating 10min, is regulated in the analgesic test (hot plate method) of mice, make water temperature be controlled at (75 ± 0.5) ℃.Get 50 of 18-22g mices, be divided into 5 groups at random, each 1 is placed on the hot plate, and mice is from being placed on the hot plate to the pain threshold values of metapedes required time (s) as this Mus occurring licking.Licking the metapedes time gives it up less than 5s or greater than 30s or leaper.Qualified mice is divided into 5 groups at random, surveys its normal pain threshold values (being pain threshold values before the medication).The depilation coating 100mg of Rhizoma Paridis gel and vehicle group animal spine, Pethidine group mouse peritoneal injection 0.01gkg-1 after the administration 30,60s, measures mice pain threshold values respectively.Still reactionless as 60s, mice is taken out, in order to avoid scald, its pain threshold values calculates with 60s, the results are shown in Table 4.
The influence in pain response time appears in table 4 Rhizoma Paridis gel to the mice hot plate
| Group | Dosage (mg/ only) | Animal (only) | The pain response time (second) appears |
| Vehicle group | 0 | 10 | 14±3.7 |
| PIYANPINGSHUANG | 100 | 10 | 32.0±7.0 *** |
| Rhizoma Paridis gel 5% | 100 | 10 | 15.0±3.7 |
| Rhizoma Paridis gel 10% | 100 | 10 | 19.0±8.7 * |
| Rhizoma Paridis gel 15% | 100 | 10 | 19.2±5.2 ** |
Compare with the excipient matched group:
*: P＜0.01,
*: P＜0.05
(2) Rhizoma Paridis total saponins extracorporeal antivirus effect test
1. Rhizoma Paridis total saponins is to having infected CVB
3The inhibitory action of the cell generation pathological changes of virus
In the Hela of 96 well culture plates cell monolayer, CVB is infected in every hole
3100TCID
50, the 2h hypsokinesis venom of preventing or cure a disease adds the Rhizoma Paridis total saponins of high, medium and low concentration respectively, cultivates observation of cell pathological changes behind the 96h.In another group test, every hole adds CVB earlier
3100TCID
50, ("-" represents acellular pathological changes to observe pathological changes behind the cultivation 96h; "+" expression has 25% cytopathy; " ++ " expression has 50% cell generation pathological changes, " +++" expression 75% cell generation pathological changes; " ++ ++ " expression has 100% cell generation pathological changes).The results are shown in Table 5.
Table 5 Rhizoma Paridis total saponins is to having infected CVB
3The inhibitory action of the cell generation pathological changes of virus
2. Rhizoma Paridis total saponins is to the inhibitory action of influenza virus
Rhizoma Paridis total saponins is made into high, medium and low (20mg/mL, 10mg/mL, 5mg/mL) three concentration, get people " O " type blood and be made into 0.75% concentration, with cell culture (viral liquid) 25 μ L, add on the trace V type blood-coagulation-board and carry out 2 times of dilutions, final dilution factor 1:256, the red cell suspension 50 μ L of adding 0.75%, 37 ℃ of 1h, observe red cell agglutination, with ++ be terminal point, represent with the blood clotting titre.The result shows that Rhizoma Paridis total saponins is under above three concentration, to A
1The blood clotting titre of type influenza virus is respectively 1:4,1:8,1:16, to A
3The blood clotting titre of type influenza virus is 1:4,1:4,1:8, shows that Rhizoma Paridis total saponins is to A
1And A
3The type influenza virus has the good restraining effect.
(3) Rhizoma Paridis total saponins antitumor cell test
Rhizoma Paridis total saponins (60% content) is made into high, medium and low three concentration, is object with people's esophageal cancer cell Eca-109, stomach cancer cell SGC-7901, leukaemia HL-60, carries out in-vitro cell growth inhibition test (mtt assay), the results are shown in Table 6-8.
Table 6 suppresses esophageal cancer cell Eca-109 growth test result
| Concentration (μ g/ml) | Suppression ratio (%) | Whether effective |
| 10 | 27.13 | |
| 100 | 74.16 | * |
| 300 | 86.82 | ** |
Table 7 suppresses stomach cancer cell SGC-7901 growth test result
| Concentration (μ g/ml) | Suppression ratio (%) | Whether effective |
| 10 | 12.18 | |
| 100 | 53.88 | * |
| 300 | 76.90 | ** |
Table 8 suppresses leukaemia HL-60 growth test result
| Concentration (μ g/ml) | Suppression ratio (%) | Whether effective |
| 10 | 15.04 | |
| 100 | 77.40 | * |
| 300 | 85.39 | ** |
The specific embodiment
Embodiment 1
Its Rhizoma Paridis decoction pieces 1kg, the ethanol that adds 6 times of amounts 60%, reflux, extract, 2 times, each extraction time is 1 hour, merges ethanol extract, centrifugal (4000 rev/mins of the rotating speeds of ethanol extract after the merging, 30 minutes time), tell the precipitation and supernatant, with supernatant concentration to 0.25g crude drug/ml, centrifugal after the standing over night, get supernatant A and precipitate A '.To precipitate A ' in add the deionized water be equivalent to extract used crude drug amount 1 times (V/W) and stir, wash, and then centrifugal (4000 rev/mins of rotating speeds, 30 minutes time), inclining supernatant, supernatant B and deposit B '; Merge supernatant A and B, will merge supernatant behind A, the B by the chromatographic column of D101 type macroporous adsorbent resin (nonpolar) is housed, supernatant is 1:4 by the ratio of the amount of Rhizoma Paridis total saponins and dried resin, and last column flow rate 1BV/h, resin path height ratio are 1:3; Wash resin 3BV with water, elution flow rate is 1BV/h, and water elution liquid discards; With the ethanol elution 2BV that contains 65%, flow velocity is 1BV/h, collects ethanol elution; It is 1.1 that ethanol elution is evaporated to relative density, with deposit B ' merge, vacuum drying (75 ℃, 6h), promptly.The content of total saponins is 50% in the prepared Rhizoma Paridis sample, and the amount of Rhizoma Paridis saponin I and Rhizoma Paridis saponin II adds up to 10%.
Embodiment 2
Get Rhizoma Paridis drink coarse powder 1kg, add the ethanol of 12 times of amounts 95%, reflux, extract, 3 times, each extraction time is 3 hours, merges ethanol extract, the ethanol extract after the merging centrifugal (10000 rev/mins of rotating speeds, 90 minutes time); Tell precipitation and supernatant, with supernatant concentration to 1.0g crude drug/ml, centrifugal after the standing over night, get supernatant A and precipitate A ', to precipitate A ' in add the deionized water be equivalent to extract used crude drug amount 5 times (V/W) and stir, wash, and then centrifugal (10000 rev/mins of rotating speeds, 90 minutes time), inclining supernatant.Get supernatant B and deposit B '; Merge supernatant A and B, will merge supernatant behind A, the B by the chromatographic column of AB-8 type macroporous adsorbent resin (low pole) is housed, supernatant is 1:10 by the ratio of the amount of Rhizoma Paridis total saponins and dried resin, and last column flow rate 4BV/h, resin path height ratio are 1:9; Wash resin 12BV with water, elution flow rate is 6BV/h, and water elution liquid discards; With the ethanol elution 6BV that contains 95%, flow velocity is 6BV/h, collects ethanol elution; It is 1.25 that ethanol elution is evaporated to relative density, with deposit B ' merge, vacuum drying (75 ℃, 6h), promptly.The content of total saponins is 90% in the obtained sample, and the amount of Rhizoma Paridis saponin I and Rhizoma Paridis saponin II adds up to 20%.
Embodiment 3
Get Rhizoma Paridis decoction pieces 1kg, add the aqueous alcohol of 8 times of amounts 70%, reflux, extract, 2 times, each extraction time is 2 hours, merges ethanol extract, filters; Ethanol extract after filtering is concentrated into 0.5g crude drug/ml, and standing over night is filtered, the deionized water that adding is equivalent to extract 2 times of amounts of used crude drug amount (V/W) in supernatant A and the precipitate A ', to precipitate A ' stirs, washs, centrifugal, inclining supernatant, gets supernatant B and deposit B '; Merge supernatant A and B, will merge supernatant behind A, the B by D101 type macroporous adsorbent resin (nonpolar) chromatographic column is housed, supernatant is 1:7 by the ratio of the amount of Rhizoma Paridis total saponins and dried resin, and last column flow rate 2BV/h, resin path height ratio are 1:5; Wash resin 5BV with water, elution flow rate is 3BV/h, and water elution liquid discards; With the ethanol elution 4BV that contains 70%, flow velocity is 3BV/h, collects ethanol elution; It is 1.15 that ethanol elution is evaporated to relative density, with deposit B ' merge, vacuum drying (75 ℃, 6h), promptly.The content of total saponins is 65% in the obtained sample, and the amount of Rhizoma Paridis saponin I and Rhizoma Paridis saponin II adds up to 17%.
Embodiment 4
Rhizoma Paridis total saponins 50g adds Acritamer 940 10g, triethanolamine 6g, glycerol 50g, ethanol 50g, azone 50g, ethylparaben 1g, and distilled water adds to 1000ml, makes gel after high-speed stirred is even.
Embodiment 5
Rhizoma Paridis total saponins 50g, adding hydroxypropyl emthylcellulose 50g, azone 20g, propylene glycol 50g, phenol 1g, glycerol 50g, distilled water add to 100ml, by making gel behind the equal machine mixing of breast.
Embodiment 6
Rhizoma Paridis total saponins 50g, adding lanoline 50g, ethylparaben 0.3g, vaseline add to 1000g, make ointment.
Embodiment 7
Rhizoma Paridis total saponins 50g adds stearic acid 300g, triethanolamine 40g, glycerol 80g, lanoline 40g, liquid Paraffin 250ml, distilled water 1000ml, makes ointment.
Claims (2)
1, a kind of preparation method of Rhizoma Paridis total saponins is characterized in that this method is: Rhizoma Paridis decoction pieces or coarse powder add envelope-bulk to weight ratio and are 6～12 times 60%～95% aqueous alcohol, reflux, extract, 2～3 times, each extraction time is 1～3 hour, merge extractive liquid,, and the extracting solution after the merging is centrifugal; Tell precipitation and supernatant, with supernatant concentration to 0.2～1.0g crude drug/ml, centrifugal after the standing over night then, get supernatant A and precipitate A '; To precipitate A ' in add that to be equivalent to extract used crude drug amount envelope-bulk to weight ratio be that 1～5 times deionized water stirs, washs, and then centrifugal, inclining supernatant, supernatant B and deposit B '; Merge supernatant A and B, will merge supernatant behind A, the B by the chromatographic column of macroporous adsorbent resin is housed, supernatant is 1:4～1:10 by the ratio of the amount of Rhizoma Paridis total saponins and dried resin, and last column flow rate 1～4BV/h, resin path height ratio are 1:3～1:9; Wash resin 3～12BV with water, elution flow rate is 1-6BV/h, and water elution liquid discards; With containing volume ratio is 65～95% aquiferous ethanol eluting, 2～6BV, and flow velocity is 1～6BV/h, collects ethanol elution; It is 1.1～1.25 that ethanol elution is evaporated to relative density, with deposit B ' merge, drying promptly gets Rhizoma Paridis total saponins.
2, the preparation method of a kind of Rhizoma Paridis total saponins as claimed in claim 1 is characterized in that described macroporous resin is a kind of in the nonpolar and low pole macroporous resin.
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| CN106177359A (en) * | 2016-08-25 | 2016-12-07 | 王昌利 | Nano suspension for the treatment of tumor and preparation method thereof |
| CN109735418A (en) * | 2019-03-05 | 2019-05-10 | 王忠良 | A kind of tea wine and preparation method thereof |
| CN113893303A (en) * | 2021-09-28 | 2022-01-07 | 深圳市真味生物科技有限公司 | Preparation method of rhizoma paridis extract |
| CN113842425A (en) * | 2021-10-22 | 2021-12-28 | 陕西盘龙药业集团股份有限公司 | Rhizoma paridis total saponin extract with multi-drug resistant bacteria resisting activity, and preparation method and application thereof |
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