CN101333241B - Process for extracting dioscin, preparation thereof and use - Google Patents
Process for extracting dioscin, preparation thereof and use Download PDFInfo
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- CN101333241B CN101333241B CN2008101083595A CN200810108359A CN101333241B CN 101333241 B CN101333241 B CN 101333241B CN 2008101083595 A CN2008101083595 A CN 2008101083595A CN 200810108359 A CN200810108359 A CN 200810108359A CN 101333241 B CN101333241 B CN 101333241B
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Abstract
The invention relates to a method for extracting dioscorea zingiberensis diosgenin in traditional Chinese medicine peltate yam, a preparation agent, and the application of the dioscorea zingiberensis diosgenin in preparing drugs in prevention and treatment of cardiovascular diseases. The dioscorea zingiberensis diosgenin extraction method of the invention adopts enzyme to remove coarse impurities, and then uses weak-polar macroporous resin to extract the dioscorea zingiberensis diosgenin. The method of the invention can significantly improve the purity and extraction rate of dioscorea zingiberensis diosgenin to reduce the production cost. The dioscorea zingiberensis diosgenin of the invention can also prepare coated tablets, syrup, oral solution, drops or capsules; compared with the prior art, the dioscorea zingiberensis diosgenin prepared through the method of the invention has better efficacy and is conducive to the transport and storage. Clinical trials prove that the dioscorea zingiberensis diosgenin extracted in the invention has a significant effect on coronary heart disease, hyperlipidemia and other cardiovascular diseases.
Description
Technical field
The present invention relates to a kind of processing method of the extraction dioscin from the Chinese medicine Rhizome of Peltate Yam, pharmaceutical preparation and preparation method thereof, with and application in preparation control cardiovascular disease treating medicine, belong to the field of Chinese medicines.
Background technology
Rhizome of Peltate Yam (Rhizoma Dioscoreae Zingiberensis) is Dioscoreaceae plant Rhizome of Peltate Yam (latin name Dioscorea Zingiberensis C.H.Wright) rhizome, effects such as Rhizome of Peltate Yam has activating blood and relaxing tendons, the Li Shui that helps digestion, and contain abundant steroidal saponin.
Dioscin is to extract to obtain from medicinal Rhizome of Peltate Yam, plant Ningpo Yam Rhizome etc., has characteristics such as chemical structure is clear and definite, oral absorption availability height.In the prior art, the method of extracting dioscin from Rhizome of Peltate Yam has a lot, major part all is to adopt the method for traditional water extract-alcohol precipitation, perhaps as CN02146284.4, adopt the method for alcohol reflux, but there is the too much problem of impurity in most of such method: because natural botanical extraction liquid is extracted into exceptionally except containing, also contain starch, protein, pectin, natural gum, resin, lymphatic temperament etc., the existence of these compositions often makes extracting solution be suspension, and influence the filtyration velocity of extracting solution, will implement removal of impurities, method commonly used has centrifuging for this reason, the finings method, alcohol deposition method, macroreticular resin absorbing method, ion exchange method, little lonely L filter membrane filters method and ultrafiltration process or the like.This has had a strong impact on the purity of extracting the fried and final product of composition, often needs to implement complicated removal of impurities process for addressing this problem, and has increased intermediate steps, increased the weight of the producer's burden, and influence contains the quality control of dioscin medicament.In recent years, the combined acid hydrolysis was studied after some investigators adopted the single enzyme preparation that the Chinese yam raw material is carried out the enzyme processing both at home and abroad, the result can make in the medicinal material more dioscin extract, but the specificity of enzymic catalytic reaction is stronger, the kind and the structure more complicated of dioscin bonded sugar in the while medicinal material, and by some pectin, impurity such as protein and vegetable fibre closely wraps up, therefore the poor effect that adopts single enzyme to react, thus limited the raising of dioscin yield.
In addition, disclose the method for utilizing polar macroporous production of resins dioscin (Dioscin), but do not had the concrete open wherein content of dioscin as patent CN02146284.2, CN02146284.4 and CN200510016775.9.The low shortcoming of content of the dioscin that this resin existence is little to the adsorptive capacity of dioscin, desorption efficiency is low and make.
Wherein macroporous adsorbent resin be by vinylbenzene, a-methyl methacrylate, propionitrile etc. for raw material adds the spherical particle that a certain amount of pore-creating agent divinylbenzene is polymerized, diameter is generally between 0.3-1.25nm.Now activeconstituents in the purifying natural plant is extracted in widespread use, as saponin(e, brass etc.According to the macroporous resin structure not with or have the surface properties of the functional group and the resin of opposed polarity, usually macroporous resin is divided into types such as nonpolar, low-pole and Semi-polarity.At present major part all is the macroporous resin production that utilizes polarity stronger, thus adsorptive capacity little.
And the deficiency that the coating tablet of prior art dioscin exists in actual applications is, (1) label medicine dissolution rate is slow, and the medicine produce effects is slow; (2) moisture absorption easily influences stability of drug and storage period; (3) dressing color and luster instability, easily oxidized and influenced the proterties of medicine; (4) dressing disperses all heterogeneities, and the opacity difference causes drug smell to distribute loss, has influenced the result of treatment of medicine.
Summary of the invention
The objective of the invention is the defective and the deficiency that exist at above-mentioned prior art, provide that a kind of can to extract impurity from the Chinese medicine Rhizome of Peltate Yam few, stable performance, the method for the dioscin that purity is high.
Another object of the present invention provides a kind of preparation method of dioscin preparation.
Further purpose of the present invention provides above-mentioned dioscin and the dioscin preparation is preparing the application that prevents and treats in the cardiovascular disease medicine.
The present invention is implemented by following technical proposals:
From Rhizome of Peltate Yam, extract the method for dioscin, may further comprise the steps:
1) gets exsiccant Rhizome of Peltate Yam powder, add certain water gaging, the back adding that stirs is dissolved required multi-functional concise enzyme DMA with 20-60 ℃ of water earlier, add the cold water regulating pondage then, add needed hydrogen peroxide and washing composition, stir, be warming up to 60-100 ℃ of insulation and obtain the thick liquid of Rhizome of Peltate Yam after 30min-1.5 hour;
2) the thick liquid of Rhizome of Peltate Yam is added 6-15 times of water gaging or 10%-30% ethanol, heating and refluxing extraction 2-4 time, each 1-3h filters, and united extraction liquid is concentrated into 0.25-2.0g crude drug/ml; Filtration or centrifugal back are by being filled with the chromatography column of low-pole macroporous resin, and extracting solution is 1 in the ratio of dioscin content and dried resin: 5-10, and last column flow rate 1-4BV/h, resin path height ratio are 1: 3-1: 9; Wash resin 3-8BV with water, elution flow rate is 2-4BV, and water elution liquid discards; With containing 30-95% aqueous ethanol wash-out, flow velocity is 2-4BV, collects ethanol eluate; It is 1.1-1.25 that ethanol eluate is evaporated to relative density, and decompression or spraying drying get dioscin.
Wherein centrifugal rotation speed is 4000-16000 rev/min.The low-pole macroporous resin is preferably polystyrene type low-pole macroporous resin.
Dioscin extract of the present invention can be a said preparation on any pharmaceutics of preparation.Described dioscin extract is made sugar coated tablet, syrup, oral liquid, drops or capsule.
According to an aspect of the present invention, the preparation method of dioscin coated tablet is: (1) gets dioscin 100-200 part, pulverizes, add calcium sulfate 1-20 part, carboxymethylstach sodium 20-60 part, mix, moistening with 95% ethanol, be rotated further 15 seconds-30 minutes, and be prepared into wet granular;
(2) wet granular is sieved through the 10-40 order;
(3) particle after sieving is 20-80 ℃ of drying;
(4) dried particle is through tabletting machine compression moulding, sugar coating, promptly.
The preparation method of preferred described dioscin coated tablet is: (1) gets 160 parts of dioscins, pulverizes, and adds 10 parts in calcium sulfate, 40 parts of carboxymethylstach sodiums, mixes, and is moistening with 95% ethanol, is rotated further 10 minutes, is prepared into wet granular;
(2) wet granular is granulated through 14 order stainless steel sifts,
(3) particle after sieving is 50 ℃ of dryings,
(4) dried particle is through tabletting machine compression moulding, sugar coating, promptly.
According to another aspect of the present invention, the application of dioscin preparation in the preparation cardiovascular disease treating medicine.Cardiovascular diseases comprises diseases such as coronary heart disease, myocardial infarction, heart strand, cerebral thrombosis.
Wherein, the low-pole macroporous resin is the polymeric adsorbent that contains ester group, and its surface has hydrophobic and hydrophilic two portions concurrently, both can be by having adsorbed apolar substance in the polar solvent, again can be by adsorbing polar material in the non-polar solution, thereby range of application is more extensive.
Positive progressive effect of the present invention is: the enzyme process removal of impurities is the novel method of separation and purification, this method is kind, the character according to impurity in the natural goods extracting solution, adopt corresponding enzyme targetedly, these impurity are decomposed or remove, to improve the clarity of liquid product, improve the stability of product.Because enzyme reaction has the specificity of height, determined the high efficiency of enzyme solution removal of impurities.Multi-functional concise enzyme DMA is made up of enzyme and some chemical assistants of single-minded Decomposition impurity such as Mierocrystalline celluloses multiple, has biocatalysis characteristic efficiently, comprise amylase, polygalacturonase, lipase, proteolytic enzyme, the compound composition of cellulase, these all are to belong to lytic enzyme, under their acting in conjunction, can effectively remove the various impurity in the Rhizome of Peltate Yam powder, the preliminary raising.
The multi-functional concise enzyme DMA that the present invention promptly adopts before with extraction using alcohol carries out enzymolysis, non-pharmaceutical cpds such as the vegetable fibre in the tubers plants such as Chinese yam, pectin, starch are removed, improve the purity of the thick liquid of Chinese yam greatly, utilize the low-pole macroporous resin characteristics big then to the adsorptive capacity of dioscin, complete by desorb, the content height of gained total saponins, the extracting method loss is little, technology simply, is not used toxic organic solvent, dioscin purity height than traditional alcohol extracting method proposition, content is big, and the one-time investment cost is low, be easy to industrialized production.
Extracting method of the present invention product cut size of the present invention makes existing dioscin have better stability to light and heat between 80-500nm.And extract dioscin coated tablet advantage of the present invention is: (1) label adopts the extraction process of several different methods, has improved the effective constituent of label medicine greatly, has improved the dissolution rate of medicine in the process of clinical application greatly, makes the medicine produce effects faster.(2) owing to adopt the film-forming process of new film-coat, film-formation result is good, can effectively prevent the infiltration of moisture in the damp atmosphere, has increased stability of drug.(3) adopt new thin-film material prescription, strengthened anti-oxidant discoloration, kept tablet appearance bright in luster, stablized the medicine shape.(4) owing to the optimization of film forming material, film forming material is easy to atomizing, disperses homogeneous, and film forming is fast, hides, and can effectively cover the unpleasant odor of Chinese medicine, is beneficial to and takes.(5) owing to label effective constituent height, the clothing layer is thin pliable and tough firmly smooth, and the great big minimizing of sheet helps transportation and storage more.
Description of drawings
Fig. 1 is that test group and control group compare histogram to two groups of blood fat somatotypes of coronary heart disease curative effect;
Fig. 2 is that test group and control group compare histogram to two groups of every traditional Chinese medical science primary symptom improvement situations of coronary heart disease;
Fig. 3 is that test group and control group compare histogram to two groups of blood lipid level improvement of coronary heart disease situation;
Fig. 4 is that test group and control group are to two groups of each laboratory safety index detected result histograms of coronary heart disease;
Fig. 5 is that test group and control group compare histogram to two groups of individual event tcm symptoms of treatment stenocardia curative effect;
Fig. 6 is that test group and control group compare histogram to two groups of hemorheology index changing conditions of treatment stenocardia;
Fig. 7 is that test group and control group are to two groups of each laboratory safety index detected result histograms of treatment stenocardia.
Embodiment
The present invention is directed to existing defective workmanship and improve, at first in Rhizome of Peltate Yam crude drug powder, add multi-functional concise enzyme DMA enzymolysis and remove most of thick impurity, prepare the dioscin extract by the low-pole macroporous resin again.Dioscin content 60%-90% weight wherein, compare by processing parameter with existing two kinds of resins, the result shows that the low-pole macroporous resin obviously is better than non-polar macroporous resin D101 and HPD100 to the dioscin adsorptive capacity, and the dioscin adsorptive capacity of desorption efficiency and acquisition is also apparently higher than the product that utilizes non-polar macroporous resin D101 and HPD100 to make.The present invention also provides the prepared dioscin extract for treating coronary heart disease and the pharmacodynamics data of cardiovascular diseases simultaneously.
Prepared dioscin extract, dioscin content is not less than 60% weight, preferred 60%-90% weight, more preferably 60%-70% weight.
Low-pole macroporous resin AB-8 and nonpolar D101 and HPD100 type macroporous resin are to the comparison of dioscin adsorptive capacity, desorption efficiency and gained saponin content:
Each 5 gram of resin, wash with water to there not being the alcohol flavor, decompressing and extracting, precision claims fixed, places the triangular flask of 250ml tool mill plug mouth, and each adds the sample liquid 150ml of preparation in early stage, 25 ℃ of constant temperature vibration 24h, get the soup of absorption front and back respectively, measure saponin content, calculate resin than adsorptive capacity (mg/g dried resin).Than adsorptive capacity mgg
-1Dried resin)=(saponin(e amount before the absorption-absorption back saponin(e amount)/resin dry weight.Resin with above-mentioned saturated absorption leaches respectively, with 30ml washing, wash dried surface-moisture after, add 70% ethanol 50ml desorb (25 ℃ of constant temperature vibration 24h), get measured in solution after the desorb, calculate the desorption efficiency of ethanol to each resin.Desorption efficiency=(saponin(e amount/saturated extent of adsorption in the stripping liquid) * 100%.Stripping liquid is concentrated, drying under reduced pressure gets saponin(e.Calculate the content of saponin(e.Result such as table 1.
The dissimilar resins of table 1 are to the comparison of adsorptive capacity, desorption efficiency and the saponin content of dioscin
| The resin model | D101 | HPD100 | AB-8 |
| Resin weight in wet base (g) | 5.070 | 5.195 | 5.089 |
| Resin dry weight (g) | 1.422 | 1.507 | 1.082 |
| Saponin(e amount before the absorption | 1.917 | 1.917 | 1.917 |
| Adsorptive capacity (g) | 1.594 | 1.681 | 1.535 |
| Static state compares adsorptive capacity | 227.1 | 156.6 | 353.1 |
| Saponin(e amount in the stripping liquid | 0.288 | 0.178 | 0.370 |
| Desorption efficiency (%) | 89.16 | 75.42 | 96.85 |
| Saponin(e amount (%) | 48％ | 51％ | 66％ |
The result shows that utilize low-pole macroporous resin AB-8 to prepare saponin(e, not only adsorptive capacity is big, and the desorption efficiency height, products obtained therefrom content height.
The comparative experiments that multi-functional concise enzyme DMA enzymolysis and low-pole macroporous resin extraction method (being called for short compound extraction method) and enzymolysis process prepare dioscin
Experiment 1: get exsiccant Rhizome of Peltate Yam powder 25g, add gauge water in there-necked flask, the back that stirs adds 0.1% cellulase and polygalacturonase compound enzymic preparation down 50 ℃ of temperature and handles 12h, adds a certain amount of dense H then
2SO
4The hydrolyzed solution that is made into 2mol/L filters in 100 ℃ of 4h that are hydrolyzed, and to neutral, grind and obtain powder extract by drying with the 10%NaOH solution washing for filter residue.After extract was used apparatus,Soxhlet's refluxing extraction 8h, with the rotatory evaporator concentrated extracting solution and with the product crystallization, drying obtained dioscin in 80-100 ℃ of vacuum drying oven at last, and products obtained therefrom is carried out yield and Measurement of melting point
Experiment 2: get exsiccant Rhizome of Peltate Yam powder 25g, add gauge water in there-necked flask, the back multi-functional concise enzyme DMA in 50 ℃ of following addings 0.1% of temperature that stirs handles 12h, adds the cold water regulating pondage then, add needed hydrogen peroxide and washing composition, stir, will obtain extract and add 6 times of water gagings, heating and refluxing extraction 2 times, each 1h, filter, united extraction liquid is concentrated into 0.25g crude drug/ml; Filter the back by AB-8 type macroporous resin, extracting solution is 1: 5 by the ratio of dioscin content and dried resin, and last column flow rate 1BV/h, resin path height are 1: 3; Wash resin 3BV with water, elution flow rate is 2BV/h, and water elution liquid discards; With containing 30% aqueous ethanol wash-out 8BV, flow velocity is 2BV/h, collects ethanol eluate; It is 1.1 that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin.
Two kinds of methods of extracting dioscin of table 2 compare
| Method | Saponin(e quality/g | Yield/% | Extraction yield/% | Fusing point/C |
| Enzymolysis process | 0.5386 | 2.15 | 75.42 | 199-202 |
| Compound extraction method | 0.7563 | 3.01 | 99.01 | 206-208 |
As can be seen from Table 2, in two kinds of extracting method, the yield height of compound extraction method products obtained therefrom, nearly 99% dioscin in the Chinese yam can be extracted, and the fusing point of this method products obtained therefrom is higher, molten distance is shorter, the product purity height meets the standard of excellent superfine product.
Get exsiccant Rhizome of Peltate Yam powder 2kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 30 ℃ of water-soluble multi-functional concise enzyme DMA30g/L, add needed 8g/L hydrogen peroxide and washing composition, stir, be warming up to 70 ℃ of insulations and obtain extract behind the 50min;
To obtain extract and add 6 times of water gagings, heating and refluxing extraction 2 times, each 1h filters, and united extraction liquid is concentrated into 0.25g crude drug/ml; Filter the back by AB-8 type macroporous resin, extracting solution is 1: 5 by the ratio of dioscin content and dried resin, and last column flow rate 1BV/h, resin path height are 1: 3; Wash resin 3BV with water, elution flow rate is 2BV/h, and water elution liquid discards; With containing 30% aqueous ethanol wash-out 8BV, flow velocity is 2BV/h, collects ethanol eluate; It is 1.1 that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin medicinal extract.Recording dioscin content is 65% (Vanillin-Glacial acetic acid, perchloric acid colour developing; The UV method; ) medicinal extract is dry under 40 ℃, dried dry extract is pulverized the gelatin hard softgel shell of packing into, can get pharmaceutical capsule.
Embodiment 3
Get exsiccant Rhizome of Peltate Yam powder 1kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 60 ℃ of water-soluble multi-functional concise enzyme DMA15g/L, add needed 10g/L hydrogen peroxide and washing composition, stir, be warming up to 80 ℃ of insulations and obtain extract behind the 60min;
To obtain extract and add 15 times of amount 30% ethanol, heating and refluxing extraction 4 times, each 3h filters, and united extraction liquid is concentrated into 2.0g crude drug/ml; Filter the back by AB-8 type macroporous resin, extracting solution is 1: 10 by the ratio of dioscin content and dried resin, and last column flow rate 4BV/h, resin path height are 1: 9; Wash resin 8BV with water, elution flow rate is 4BV/h, and water elution liquid discards; With containing 95% aqueous ethanol wash-out, flow velocity is 4BV/h, collects ethanol eluate; It is 1.25 that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin medicinal extract.Recording dioscin content is 77% (Vanillin-Glacial acetic acid, perchloric acid colour developing; The UV method; ) medicinal extract is dry under 50 ℃, dried dry extract is broken into fine powder; Add ethanol as tamanori, add starch, be pressed into granule as weighting agent.
Embodiment 4
Get exsiccant Rhizome of Peltate Yam powder 5kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 20 ℃ of water-soluble multi-functional concise enzyme DMA10g/L, add needed 5g/L hydrogen peroxide and washing composition, stir, be warming up to 60 ℃ of insulations and obtain extract behind the 30min;
To obtain extract and add 8 times of water gagings, heating and refluxing extraction 2 times, each 1h filters, and united extraction liquid is concentrated into 1.0g crude drug/ml; Centrifugal (4000 rev/mins) back is by AB-8 type macroporous resin, and soup is 1: 5 by the ratio of dioscin content and dried resin, and last column flow rate 2BV/h, resin path height are 1: 5; Wash resin 3BV with water, elution flow rate is 4BV/h, and water elution liquid discards; With containing 70% aqueous ethanol wash-out 3BV, flow velocity is 2BV/h, collects ethanol eluate; It is 1.1 (50 ℃ of heat are surveyed) that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin.Recording dioscin content is 72% (Vanillin-Glacial acetic acid, perchloric acid colour developing; The UV method; )
Get exsiccant Rhizome of Peltate Yam powder 5kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 40 ℃ of water-soluble multi-functional concise enzyme DMA18g/L, add needed 6g/L hydrogen peroxide and washing composition, stir, be warming up to 100 ℃ of insulations and obtain extract behind the 1.5h;
To obtain extract and add 10 times of amount 10% ethanol, heating and refluxing extraction 2 times, each 1.5h filters, and united extraction liquid is concentrated into 0.5g crude drug/ml; Filter the back by D201 type macroporous resin, soup is 1: 9 by the ratio of dioscin content and dried resin, and last column flow rate 3BV/h, resin path height are 1: 7; Wash resin 5BV with water, elution flow rate is 4BV/h, and water elution liquid discards; With containing 30% aqueous ethanol wash-out 10BV, flow velocity is 4BV/h, collects ethanol eluate; It is 1.25 (50 ℃ of heat are surveyed) that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin medicinal extract.Recording dioscin content is 66% (Vanillin-Glacial acetic acid, perchloric acid colour developing; The UV method; ) medicinal extract is dry under 50 ℃, dried dry extract is broken into fine powder; Add auxiliary material and make particle, and dry, spray into wetting auxiliary material, be pressed into tablet.
Get exsiccant Rhizome of Peltate Yam powder 5kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 55 ℃ of water-soluble multi-functional concise enzyme DMA18g/L, add needed 6g/L hydrogen peroxide and washing composition, stir, be warming up to 75 ℃ of insulations and obtain extract behind the 1.2h;
To obtain extract and add 15 times of water gagings, heating and refluxing extraction 2 times, each 1h filters, and united extraction liquid is concentrated into 0.25g crude drug/ml; Centrifugal (8000 rev/mins) back is by HPD450 type macroporous resin, and soup is 1: 6 by the ratio of dioscin content and dried resin, and last column flow rate 4BV/h, resin path height are 1: 9; Wash resin 2BV with water, elution flow rate is 3BV/h, and water elution liquid discards; With containing 50% aqueous ethanol wash-out 5BV, flow velocity is 3BV/h, collects ethanol eluate; It is 1.2 (50 ℃ of heat are surveyed) that ethanol eluate is evaporated to relative density, and drying under reduced pressure gets dioscin.Recording dioscin content is 70% (Vanillin-Glacial acetic acid, perchloric acid colour developing; The UV method; )
Get exsiccant Rhizome of Peltate Yam powder 5kg,, add certain water gaging, after stirring, add, add the cold water regulating pondage then with 55 ℃ of water-soluble multi-functional concise enzyme DMA18g/L, add needed 6g/L hydrogen peroxide and washing composition, stir, be warming up to 75 ℃ of insulations and obtain extract behind the 1.2h;
To obtain extract and add 5 times of water gagings and soak the back and decocted 2 hours, and filter, filter residue adds 3 times of amounts of entry again and decocts 2 times, and each 1 hour, filter, merging filtrate, concentrating under reduced pressure (70～80 ℃ ,-0.08MPa) to the clear cream of relative density 1.16 (50～60 ℃); Clear cream adds 3 times of amount 80% alcohol reflux 2 times, each 1 hour, filter, merging filtrate, decompression recycling ethanol and concentrate (60～70 ℃ ,-0.08MPa) to the clear cream of relative density 1.16 (50～60 ℃); Clear cream adds 10 times of amount 95% ethanol, leaves standstill 24 hours, filters, and supernatant liquor reclaims ethanol, precipitate dried under reduced pressure (70～80 ℃ ,-0.08MPa), pulverize, check, promptly.
Embodiment 8
The preparation method of sugar coated tablet may further comprise the steps:
(1) get dioscin 160g among the embodiment 6, pulverize, add calcium sulfate 10g, carboxymethylstach sodium 20g, mix, moistening with 95% ethanol, 14 order stainless steel sifts are granulated,
(2) wet granular is sieved through 14 orders;
(3) particle after sieving is 50 ℃ of dryings;
(4) dried particle adds Magnesium Stearate 3g, talcum powder 7g, and is evenly mixed, and compacting is in blocks, sugar coating, promptly.
Embodiment 9
The preparation method of sugar coated tablet may further comprise the steps:
(1) get dioscin 100g among the embodiment 6, pulverize, add calcium sulfate 2g, carboxymethylstach sodium 40g, mix, moistening with 95% ethanol, 14 order stainless steel sifts are granulated,
(2) wet granular is sieved through 10 orders;
(3) particle after sieving is 20 ℃ of dryings;
(4) dried particle adds Magnesium Stearate 3g, talcum powder 7g, and is evenly mixed, and compacting is in blocks, sugar coating, promptly.
The preparation method of sugar coated tablet may further comprise the steps:
(1) get dioscin 200g among the embodiment 6, pulverize, add calcium sulfate 20g, carboxymethylstach sodium 60g, mix, moistening with 95% ethanol, 14 order stainless steel sifts are granulated,
(2) wet granular is sieved through 20 orders;
(3) particle after sieving is 80 ℃ of dryings;
(4) dried particle adds Magnesium Stearate 3g, talcum powder 7g, and is evenly mixed, and compacting is in blocks, sugar coating, promptly.
Dioscin sugar-coat treatment coronary heart disease effect is better, owing to be used for the treatment of, the present invention furthers investigate the dioscin curative effect.
1, experimenter's selection and withdrawing from
(1) Case definition
1. Western medicine diagnose standard
According to Chinese cardiovascular diseases magazine editorial board's hyperlipemia Preventing Countermeasures special topic group " hyperlipemia control suggestion " in 1997 standard formulation.
1.1 lipid examination
Under the normal diet situation, detect the blood lipid level of fasting after 12～14 hours, when judging whether to have hyperlipidaemia, must have at least 2 blood specimen detection record in 1～2 week.
1.2 meaning is judged
Serum TC
5.20mmol/L (200mg/dl) following OK range
5.23 (201～219mg/dl) edges raise～5.69mmol/L
5.72mmol/L (220mg/dl) the above rising
Serum LDL-C
3.12mmol/L (120mg/dl) following OK range
3.15 (121～139mg/dl) edges raise～3.61mmol/L
3.64mmol/L (140mg/dl) the above rising
Serum HDL-C
1.04mmol/L (40mg/dl) following OK range
0.91mmol/L (35mg/dl) the following attenuating
Serum TG
1.70mmol/L (150mg/dl) following OK range
1.70mmol/L (150mg/dl) the above rising
1.3 the classification of hyperlipidaemia
A. clinical classification
1. hypercholesterolemiaserum serum TC level increases.2. combined hyperlipidemia familial serum TC and TG level all increase.3. hypertriglyceridemia serum TG level increases.4. low hdl mass formed by blood stasis Serum HDL-C level lowers.
B. cause of disease classification
1. Primary hyperlipemia.
2. the common cause of disease of Secondary cases hyperlipidaemia is: diabetes, hypothyroidism, nephrotic syndrome, ventilation, acute or chronic liver and gall diseases etc.
2, test method
(1) test design
This testing program adopts at random, double blinding, positive control, multi-center clinical trial method of design.Whole process is worked in coordination with and is finished by Hospital Attached to Shandong Chinese Medical Univ., the hospital of traditional Chinese hospital, Jinan City, Shandong Province, 3 hospitals of Jinan City, Shandong Province third party people hospital.
(2) title of test drug and source
The peltate leaf perhexiline sheet, Jiangsu Huang He Pharmaceutical Co., Ltd provides, lot number: 20040908.
Placebo tablets, Jiangsu Huang He Pharmaceutical Co., Ltd provides, lot number: 20040901.
The zhibituo sheet, Chengdu Diao 9 Wang pharmaceutical factory provides, lot number: 041002.
All test medications all are up to the standards.
(3) method of administration
Test group: peltate leaf perhexiline sheet, 2 slices/time, 3 times/day, warm water delivery service.
Control group: sooner or later, zhibituo sheet, 2 slices/time+noon, placebo tablet, 2 slices/time.Warm water delivery service.
(4) drug combination regulation
1. duration of test must not use and treat this sick Chinese and western drugs and methods of treatment.
2. merge other drug and methods of treatment that other diseases must continue to take, must be in the drug combination table detail record.
(5) course of treatment
A course of treatment 8 Mondays.
3, experimental result
One, efficacy analysis
(1) blood fat total effects
Two groups of blood fat total effectses relatively see Table 3:
Table 3 liang group blood fat total effects relatively
Two groups of blood fat total effectses compare, and difference does not have the significance meaning, and test group is higher than control group total effective rate.
(2) blood fat somatotype curative effect
Two groups of blood fat somatotype curative effects relatively see Table 4:
Table 4 liang group blood fat somatotype curative effect relatively
Two groups of blood fat somatotype curative effects relatively, difference there are no significant meaning, as shown in Figure 1, TC increases in the type, the clinic control of test group 59 routine numbers, produce effects, effectively and the numeric ratio control group 15 routine number test group of total effective rate higher, better efficacy, in like manner TG increase with mixed type in, test group 60, test group 59 are compared control group 21 and control group 24 better effects if.
(3) tcm syndrome curative effect
Two groups of tcm syndrome curative effects relatively see Table 5:
Table 5 liang group tcm syndrome curative effect relatively
Two groups of tcm syndrome curative effects compare, and difference does not have the significance meaning, and test group is higher than control group total effective rate.
(4) every traditional Chinese medical science primary symptom is improved situation
Two groups of every traditional Chinese medical science primary symptoms are improved situation and are relatively seen Table 6:
The table 6 liang every traditional Chinese medical science primary symptom improvement situation of group relatively
The improvement situation of two groups of each traditional Chinese medical science primary symptoms compares: the interior comparing difference of group all has highly significant meaning (P＜0.01) before and after each cardinal symptom treatment; Treat between the group of back and relatively have (P＜0.05) the significance meaning, comparing difference there are no significant meaning (P＞0.05) between vexed and pareordia shouting pain group that the chest side of body is bloated except that walking to scurry two groups of differences of pain.As shown in Figure 2, in the bloated vexed type of the chest side of body, the variation difference of test group is greater than control group after the curative effect, and the test group of walking to scurry pain and pareordia shouting pain equally as seen from the figure changes difference all greater than control group, and this shows that also test group is more effective to them.
(5) the tcm symptom average integral improves situation
Two groups of tcm symptom average integrals improve situation and relatively see Table 7:
Table 7 liang group tcm symptom average integral improvement situation comparison (X ± SD)
Compare in the group of treatment front and back: two groups of treatment front and back self comparing differences all have the highly significant meaning.
Compare between the group of treatment back: comparing difference does not have the significance meaning between two groups of treatment back groups.
(6) blood lipid level improves situation
Two groups of blood lipid levels improve situation and relatively see Table 8:
Table 8 liang group blood lipid level improvement situation comparison (X ± SD, mmol/L)
Compare in the group before and after the treatment: test group HDL self comparing difference does not have the significance meaning, and all the other indexs self comparing difference all has significantly or the highly significant meaning.Between treatment back group relatively: TG treats that comparing difference has the significance meaning between the group of back, comparing difference there are no significant meaning between all the other index groups.As shown in Figure 3, compare from treatment curative effect front and back difference, the values of control groups of TC, TG, HDL, LDL and VLDL is all greater than control group, and it is also little to change difference, so better efficacy.
(7) the lipophorin level is improved situation
Two groups of lipophorin levels are improved situation and are relatively seen Table 9:
Table 9 liang group lipophorin level improvement situation comparison (X ± SD, mmol/L)
Compare in the group before and after the treatment: test group aPoA (Apo-A) self comparing difference does not have the significance meaning, and all the other indexs self comparing difference all has the highly significant meaning.
Compare between the group of treatment back: comparing difference has the significance meaning between the group of aPoA (Apo-A) treatment back; Comparing difference does not have the significance meaning between organizing after apolipoprotein B (Apo-B) is treated.
Two, safety analysis
(1) laboratory safety index detected result is analyzed
Two groups of each laboratory safety index detected result analysis in table 10:
Table 10 liang each laboratory safety index detected result of group
Laboratory safety index detected result shows:
Test group and control group normally increase the weight of index after the treatment before treatment back abnormal index or the treatment before there is no treatment unusually unusually.
Test group has 31 examples, control group that 13 routine electrocardiographic abnormality persons are arranged before treating, mostly be greatly more than 45 years old in, the elderly, question closely medical history, arteriosclerosis, coronary disease medical history are mostly arranged, not seeing has tangible cardiac insufficiency.This patient group's Electrocardioscopy is not unusual yet after the treatment, but the no abnormality seen situation increases the weight of.Test group has 6 examples, control group to have 2 routine ALT to raise before treating, and it is long that the investigator is judged as the hyperlipidaemia course of disease, due to the merging fatty liver.The treatment back is along with the decline of blood fat, and the test group control group respectively has 1 routine patient's ALT to reduce to normally.As shown in Figure 4, from routine blood test, routine urinalysis, just unusual routine number changes before and after the treatment of routine, electrocardiogram(ECG, ALT, BUN and Cr, test group is improved the unusual remarkable control group that is better than, so the test group better efficacy.
4, conclusion
Show by the clinical observation to 240 routine hyperlipidaemia (syndrome of qi stagnation and blood stasis) patients: peltate leaf perhexiline sheet treatment hyperlipidaemia (syndrome of qi stagnation and blood stasis) is safe and effective, and in the prior art of comparing than the pharmaceutical preparation better efficacy of preferable treatment coronary heart disease.
Dioscin treatment coronary heart disease effect is better, owing to be used for the treatment of, the present invention furthers investigate the process that dioscorea opposita saponin liposome sees through, and is significant to the characteristics of the targeted therapy of understanding liposome.
1, case choice criteria
(1) Case definition
1. Western medicine diagnose standard
(with reference to International Society of Cardiology and association and World Health Organization's clinical name stdn associating special topic group report " name of ischemic heart disease and Case definition " formulation)
(1) Case definition
1. fatigue stenocardia: the anginal feature of fatigue is because motion or other increase the of short duration pectoralgia outbreak of being brought out under the situation of myocardium requirementing keto quantities, and after having a rest or containing the clothes pannonit, pain often can rapidly disappear.
Can be divided three classes:
First hair style fatigue stenocardia: the course of disease is in one month.
Stable form fatigue stenocardia: the course of disease was stabilized in more than one month.
Deterioration type fatigue stenocardia: number of times, severity and time length that the equal extent fatigue is brought out increase the weight of suddenly.
2. spontaneous angina pectoris: the feature of spontaneous angina pectoris is that the pectoralgia outbreak does not have obvious relation with the increase of myocardium requirementing keto quantity.Compare with fatigue stenocardia, this pain general persistence is longer, and degree is heavier, and does not alleviate for pannonit.This type is not seen enzymic change, and electrocardiogram(ECG often occurs that some temporary ST section is forced down or the T ripple changes.Spontaneous angina pectoris can take place separately or merge existence with fatigue stenocardia.
Spontaneous angina pectoris patient's pain seizure frequency, time length and pain degree can have different clinical manifestations, and the patient can have the pectoralgia outbreak that continues than long sometimes, similar myocardial infarction, but do not have the characteristic of electrocardiogram(ECG and enzyme to change.
Some spontaneous angina pectoris patient the S-T section of transience occurs and raises when outbreak, often be called ariant angina.But when myocardial infarction records this ECG pattern in early days, can not use this title.
Just hair style fatigue stenocardia, deterioration type fatigue stenocardia and spontaneous angina pectoris often are referred to as " unstable angina pectoris ".
(2) calibration, grading diagnosis standard (standard formulation of reference in September, 1979 whole nation prevention and treatment in traditional Chinese and western coronary heart disease and angina pectoris, irregular pulse research symposium revision)
1. exertional angina pectoris
The I level: cause stenocardia than daily routines physical exertion heavily, daily routines are asymptomatic, trot as the level land, and quick or prudent thing Shang Sanlou, last abrupt slope etc. causes stenocardia.
The II level: daily physical exertion causes stenocardia, and daily routines are restricted slightly.Cause stenocardia as often trot going 3-4 station (3-4 li), Shang Sanlou, upward slope under normal operation.
The III level: the physical exertion light than daily routines causes stenocardia, and daily routines are obviously limited.1-2 stands (1-2 li), upward second floor, clivia cause stenocardia as often trot going under normal operation.
The IV level: slight physical exertion (as in indoor jogging) causes stenocardia, and stenocardia also takes place during the severe patient rest.
2. non-EA
Slightly: have than the classical angina outbreak, continue several minutes at every turn, show effect 2-3 time at least weekly, or show effect 1-3 time every day, but pain is not heavy, need obey pannonit sometimes.
Moderate: have every day repeatedly than the classical angina outbreak, each time length number is minute heavier to 10 minutes pain, generally need contain the clothes pannonit.
Severe: classical angina outbreak is arranged repeatedly every day, thereby influence activities of daily living (for example defecate, wear the clothes etc.), the time length of at every turn showing effect is longer, need repeatedly suck pannonit.
2, test method
(1) test design
This testing program adopts at random, double blinding, positive control, multi-center clinical trial method of design.Whole process is worked in coordination with and is finished by Hospital Attached to Shandong Chinese Medical Univ., the hospital of traditional Chinese hospital, Jinan City, Shandong Province, 3 hospitals of Jinan City, Shandong Province third party people hospital.
(2) title of test drug and source
The peltate leaf perhexiline sheet, Jiangsu Huang He Pharmaceutical Co., Ltd provides, lot number: 20040908.
FUFANG DANSHEN PIAN, the ferreous pharmaceutical factory in Heilongjiang Province provides lot number: 20041002.
All test medications all are up to the standards.
(3) method of administration
Test group: peltate leaf perhexiline sheet, 3 slices/time (being equivalent to 2 slices/time of primary standard crude drug doses), 3 times/day, warm water delivery service.
Control group: FUFANG DANSHEN PIAN, 3 slices/time, 3 times/day, warm water delivery service.
(4) drug combination regulation
1. duration of test must not use and treat this sick Chinese and western drugs and methods of treatment.
2. merge other drug and methods of treatment that other diseases must continue to take, must be in the drug combination table detail record.
(5) course of treatment
A course of treatment 8 Mondays.
2, experimental result
One, efficacy analysis
(1) curative effect to treat angina pectoris
Two groups of patient's curative effect to treat angina pectoris relatively see Table 11:
Table 11 liang group patient curative effect to treat angina pectoris relatively
Two groups of curative effect to treat angina pectoris compare, and difference does not have the significance meaning.
(2) ECG curative effect
Two groups of ECG curative effect relatively see Table 12:
Table 12 liang group ECG curative effect relatively
Two groups of ECG curative effect compare, and difference does not have the significance meaning.
(3) tcm syndrome curative effect
Two groups of tcm syndrome curative effects relatively see Table 13:
Table 13 liang group tcm syndrome curative effect relatively
Two groups of tcm syndrome curative effects compare, and difference does not have the significance meaning.
(4) tcm symptom curative effect
1. individual event tcm symptom curative effect
Two groups of individual event tcm symptom curative effects relatively see Table 14:
Table 14 liang group individual event tcm symptom curative effect relatively
Two groups of each individual event tcm symptom curative effects relatively, difference there are no significant meaning, as shown in Figure 5,, fullness and distention in the chest and hypochondrium uncomfortable in chest and palpitaition symptom from the treatment pectoralgia, test group produce effects ratio is higher than control group, so it is to these symptom better efficacy.
2. the tcm symptom integration improves situation
Two groups of tcm symptom integrations improve situation and relatively see Table 15:
Table 15 liang group tcm symptom integration improvement situation comparison (X ± SD)
Two groups of tcm symptom integrations improvement situations, comparing two groups in the treatment front and back are organized all has highly significant meaning (P＜0.01), and comparing difference does not have significance meaning (P＞0.05) between organizing after treating.
(5) pannonit stops lapse rate
Two groups of pannonits stop lapse rate and relatively see Table 16:
Table 16 a liang group pannonit stops lapse rate relatively
Two groups of pannonits stop lapse rate relatively, and difference does not have the significance meaning.
(6) to the influence of angina pectoris attacks frequency, time length
1. to the influence of angina pectoris attacks frequency
Two groups of angina pectoris attacks frequency ratios see Table 17:
Table 17 liang group angina pectoris attacks frequency ratio is (inferior/week)
Two groups of angina pectoris attacks frequency ratios, before and after the treatment in the group relatively two groups highly significant meaning (P＜0.01) is all arranged, treat that comparing difference does not have significance meaning (P＞0.05) between the group of back.
2. to the influence of stenocardia time length
Two groups of stenocardia time length relatively see Table 18:
The table 18 liang group stenocardia time length is (min/ time) relatively
Two groups of stenocardia time length situations compare, and comparing two groups in the treatment front and back are organized all has highly significant meaning (P＜0.01), and comparing difference does not have significance meaning (P＞0.05) between organizing after treating.
(7) influence of hemorheology index
Two groups of hemorheology index changing conditions relatively see Table 19:
Table 19 liang group hemorheology index changing conditions relatively
Two groups of hemorheology changing conditions compare: compare in the group before and after the treatment outside the dehematize pulp fibres proteinogen, all the other indexs are improved situation for two groups all highly significant meaning (P＜0.01); Treat between the group of back more every index group difference there are no significant meaning (P＞0.05).As shown in Figure 6, from the numerical value of the whole blood viscosity high value of cutting, the low value of cutting of whole blood viscosity, plasma viscosity, plasma fibrinogen and pcv, the difference of control group before and after treatment is significantly higher than control group, so its better efficacy.
(8) influence of blood lipids index
Two groups of blood lipids index changing conditions relatively see Table 20:
Table 20 liang group blood lipids index changing conditions is (mmol/L) relatively
Two groups of blood lipids index changing conditions compare: compare in the group before and after the treatment, except that the total triglyceride level difference of control group serum does not have the significance meaning, significantly (P＜0.05) or highly significant meaning (P＜0.01) are arranged more all in two groups of groups of all the other indexs; Treat between the group of back relatively two index differences there are no significant meaning (P＞0.05).
Two, safety analysis
(1) laboratory safety index detected result is analyzed
Two groups of each laboratory safety index detected result analysis in table 21:
Table 21 liang each laboratory safety index detected result of group
Laboratory safety index detected result shows:
Test group and control group normally increase the weight of index after the treatment before treatment back abnormal index or the treatment before there is no treatment unusually unusually.Test group has 6 examples, control group that 2 routine ALT risings are arranged before treating, and treating the back test group has 1 routine patient's ALT to reduce to normally, and all the other are still higher, but the preceding nothing of treatment increases the weight of.The investigator is judged as and merges due to liver cirrhosis, the fatty liver through questioning closely medical history.As shown in Figure 7, from routine blood test, routine urinalysis, just unusual routine number changes before and after the treatment of routine, ALT, BUN and Cr, test group is improved the unusual remarkable control group that is better than, so the test group better efficacy.
3, conclusion
Show by the clinical observation to 240 routine coronary heart disease and angina pectoris (syndrome of qi stagnation and blood stasis) patients: peltate leaf perhexiline sheet treatment coronary heart disease and angina pectoris (syndrome of qi stagnation and blood stasis) is safe and effective, and in the prior art of comparing than the anginal pharmaceutical preparation better efficacy of preferable treatment.
Claims (3)
1. method of extracting dioscin from Rhizome of Peltate Yam is characterized in that may further comprise the steps:
1) gets exsiccant Rhizome of Peltate Yam powder, add certain water gaging, after stirring, add with the 20-60 ℃ of multi-functional concise enzyme DMA 10-30g/L of suitable quantity of water dissolved, add the cold water regulating pondage then, add needed 5-10g/L hydrogen peroxide and washing composition, stir, be warming up to 60-100 ℃ of insulation and obtain the thick liquid of Rhizome of Peltate Yam after 30min-1.5 hour;
2) the thick liquid of Rhizome of Peltate Yam is added 6-15 times of water gaging or 10%-30% ethanol, heating and refluxing extraction 2-4 time, each 1-3h filters, and united extraction liquid is concentrated into 0.25-2.0g crude drug/ml; Filtration or centrifugal back are by being filled with the chromatography column of low-pole macroporous resin, and extracting solution is 1 in the ratio of dioscin content and dried resin: 5-10, and last column flow rate 1-4BV/h, resin path height ratio are 1: 3-1: 9; Wash resin 3-8BV with water, elution flow rate is 2-4BV, and water elution liquid discards; With containing 30-95% aqueous ethanol wash-out, flow velocity is 2-4BV, collects ethanol eluate; It is 1.1-1.25 that ethanol eluate is evaporated to relative density, and decompression or spraying drying get dioscin.
2. method according to claim 1 is characterized in that described centrifugal rotation speed is 4000-16000 rev/min.
3. method according to claim 1 is characterized in that described low-pole macroporous resin is a polystyrene type low-pole macroporous resin.
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| CN1415625A (en) * | 2002-10-21 | 2003-05-07 | 吉林天药科技股份有限公司 | Method for preparing yam saponin, medicinal preparation and new usage in medication |
| CN1416816A (en) * | 2002-11-08 | 2003-05-14 | 吉林天药科技股份有限公司 | Antineoplastic effect and medicine prepn of dioscin |
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| CN1415625A (en) * | 2002-10-21 | 2003-05-07 | 吉林天药科技股份有限公司 | Method for preparing yam saponin, medicinal preparation and new usage in medication |
| CN1416816A (en) * | 2002-11-08 | 2003-05-14 | 吉林天药科技股份有限公司 | Antineoplastic effect and medicine prepn of dioscin |
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