CN1216895C - Rhizoma alismatis total triterpene alcohol extract and its preparation method - Google Patents
Rhizoma alismatis total triterpene alcohol extract and its preparation method Download PDFInfo
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- CN1216895C CN1216895C CN031465331A CN03146533A CN1216895C CN 1216895 C CN1216895 C CN 1216895C CN 031465331 A CN031465331 A CN 031465331A CN 03146533 A CN03146533 A CN 03146533A CN 1216895 C CN1216895 C CN 1216895C
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- rhizoma alismatis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to a water plantain total triterpenes alcohol extract. The present invention is characterized in that the extract is an oil constituent obtained by extracting water plantain raw materials in a super critical extraction method under the super critical extraction condition that pressure is from 10 to 50MPa, extraction temperature is from 32 to 45 DGE C, and separation time is from 0.5 to 5 hours, and the specific weight of the extract is from 1.15 to 1.25. The present invention also provides a method for producing high-concentration extracts containing water plantain active constituents.
Description
Technical field
The present invention relates to the total triterpene alcohols of a kind of rhizoma alismatis extract and preparation method thereof.More particularly, relate to the total triterpene alcohols of a kind of rhizoma alismatis extract, and the method for preparing this Rhizoma Alismatis extract with carbon dioxide supercritical extraction method.
Background technology
Rhizoma alismatis is a kind of ancient Chinese medicine commonly used, and known its has reducing blood-fat, the lipotropism liver function is imitated (open referring to Japanese Patent, clear and 36-17094, clear and 36-17095, clear and 44-31590).The contained total triterpene alcohols of rhizoma alismatis is the main active ingredient of its performance reducing blood lipid.Existing working method is a water, and alcohol or other organic solvent extraction rhizoma alismatis are extracted the product component complexity that obtains like this, and the content of the total triterpene alcohols of effective constituent is low.In addition, the extraction product that obtains with existing extracting method is an ointment shape form, can not process with oily attitude, can not process with solid-state, causes very big difficulty to preparation process.And owing to effective active composition in the extraction medicinal extract is low, the patient often needs day crude drug of clothes heavy dose just can reach result of treatment.And, cause unstable product quality by the medicinal raw material that difference is criticized.These shortcomings have hindered the process of this Chinese medicine stabilization formulationsization.Up to the present, rhizoma alismatis all is to be used as one of component of compound Chinese medicine preparation with crude drug or the form of extracting medicinal extract, but never have the total triterpene alcohols of the activeconstituents of rhizoma alismatis is purified to the degree that can carry out preparationization with the amount of suitability for industrialized production, also never has the total triterpene alcohols of the activeconstituents of rhizoma alismatis separately as the report of the medicine of medicine activity component.
Summary of the invention
The present inventor is in view of above-mentioned the problems of the prior art, further investigate, through found that of a large amount of tests, can obtain the total triterpene alcohols of the rhizoma alismatis extract of high-purity high-concentration with supercritical carbon dioxide extraction method, different with the brownish black medicinal extract of the ethanol extraction of prior art, products obtained therefrom is faint yellow oily thing, and this extract can further carry out preparation processing.Finished the present invention based on this discovery.
That is, the present invention relates to following content.
1. the total triterpene alcohols of rhizoma alismatis extract, it is characterized in that, this extract is to be in the carbon dioxide upercritical fluid extraction condition with the rhizoma alismatis raw material: pressure 10～50Mpa, 32～45 ℃ of extraction temperature, the oil ingredient that 0.5～5 hour supercritical extraction of disengaging time obtains, its proportion are 1.15～1.25.
2. the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 1 extract is characterized in that this oily matter is faint yellow.
3. the above-mentioned 1 or 2 total triterpene alcohols of the rhizoma alismatis extracts described in each is characterized in that this rhizoma alismatis raw material is the pulverized particles of Chinese medicine rhizoma alismatis.
4. the above-mentioned 1 or 2 total triterpene alcohols of the rhizoma alismatis extracts described in each is characterized in that, to be rhizoma alismatis remove preextraction thing after most of useless composition is removed with ethanol or other organic solvent extraction do pre-treatment to this rhizoma alismatis raw material.
5. the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 4 extract is characterized in that, be added in this preextraction thing on the carrier after, place overcritical equipment.
6. the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 5 extract is characterized in that, this carrier is to be selected from least a in gac, diatomite, the silica gel.
7. the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 6 extract is characterized in that this carrier is a gac.
8. the total triterpene alcohols of each described rhizoma alismatis extract is characterized in that in above-mentioned 1 or 2, is contrast with Alisol B std-23 monoacetate, calculate content and be 50% or more than.
9. the manufacture method of the total triterpene alcohols of a rhizoma alismatis extract, it is characterized in that, use the rhizoma alismatis raw material to be: pressure 10～50Mpa, 32～45 ℃ of extraction temperature in the carbon dioxide upercritical fluid extraction condition, extract under 0.5～5 hour the supercritical extraction condition of disengaging time, separate then.
10. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 9 extract is characterized in that this rhizoma alismatis raw material is the pulverized particles of Chinese medicine rhizoma alismatis.
11. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 9 extract is characterized in that, to be rhizoma alismatis remove preextraction thing after most of useless composition is removed with ethanol or other organic solvent extraction do pre-treatment to this rhizoma alismatis raw material.
12. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 11 extract is characterized in that, be added in this preextraction thing on the carrier after, place overcritical equipment.
13. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 12 extract is characterized in that, this carrier is to be selected from least a in gac, diatomite, the silica gel.
14. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in above-mentioned 13 extract is characterized in that this carrier is a gac.
Embodiment
A first aspect of the present invention relates to the total triterpene alcohols of a kind of rhizoma alismatis extract, it is characterized in that, this extract is to be in the carbon dioxide upercritical fluid extraction condition with the rhizoma alismatis raw material: pressure 10～50Mpa, 32～45 ℃ of extraction temperature, the oil ingredient that 0.5～5 hour supercritical extraction of disengaging time obtains.The proportion of this oily matter is 1.15～1.25.
The total triterpene alcohols of this rhizoma alismatis extract, it is a kind of brand-new extract, be to pass through carbon dioxide supercritical extraction method, under specific extraction conditions, be pressure 10～50Mpa, 15～50Mpa more preferably, 32～45 ℃ of extraction temperature, more preferably 32～42 ℃, a kind of extract that disengaging time extracted in 0.5～5 hour.
The accurate title of this oily matter is fixed, add ethanol and make the solution of 30 μ g/ml, precision is measured 10ml, evaporate to dryness in water-bath, add sulfuric acid 10ml dissolving, heating is 3 hours in 60 ℃ of water-baths, measures optical density at the 316nm place with spectrophotometry, with Alisol B std-23 monoacetate is contrast, calculate content 50% or more than.
This extract high density high purity contains the total triterpene alcohols of rhizoma alismatis, compare with ethanol extraction in the past, have following obvious characteristic: 1) ethanol extraction is black or brown medicinal extract, thickness, non-oily matter is also non-solid, can't carry out further preparation production, and the total triterpene extracts of rhizoma alismatis of the present invention, physical aspect is faint yellow oily thing, can carry out further preparationization.2) complicated component in the ethanol extraction, active constituent content is low, and the total triterpene alcohols of rhizoma alismatis of the present invention extract contains the total triterpene alcohols of main active component of rhizoma alismatis with the high density high purity, is the extract of having concentrated the rhizoma alismatis main active ingredient.If such extract further carry out preparationization, such as making capsule and pill, can obtain steady quality, the Chinese medicine new formulation of easy administration.
Supercritical carbon dioxide extraction method possesses the low temperature inert environments, does not influence the effective constituent activity, and is nontoxic nonflammable, safe in utilization, do not pollute the environment no solvent residue, multiple advantages such as heavy metal free ion.Extract though super critical CO 2 technology has been used to some traditional Chinese medicine ingredients, also do not have report to use it for the rhizoma alismatis extraction of active ingredients.The inventor at first expects extracting the rhizoma alismatis activeconstituents with supercritical extraction method, and through a large amount of tests, has found out the supercritical extraction condition that is suitable for extracting the rhizoma alismatis activeconstituents, thereby finished the present invention.
Promptly, another aspect of the present invention relates to the manufacture method of the total triterpene alcohols of rhizoma alismatis extract, it is characterized in that, use the rhizoma alismatis raw material to be: pressure 10～50Mpa in the carbon dioxide upercritical fluid extraction condition, 32～45 ℃ of extraction temperature, extract under 0.5～5 hour the supercritical extraction condition of disengaging time, separate.
This supercritical extraction method can be divided into two kinds again.First kind is direx process.Being about to the Chinese medicinal materials rhizoma alismatis, to be ground into red bean granular, places supercritical extraction equipment directly to extract with carbonic acid gas, and extraction conditions is extracting pressure 10～50MPa, further preferably at 15～50Mpa, 32～45 ℃ of extraction temperature, further preferably at 32～42 ℃, disengaging time 0.5～5 hour.Second method is that rhizoma alismatis is done pre-treatment with ethanol or other organic solvent extraction, the composition that major part is useless is removed, use the intensive preextraction thing of total triterpene alcohols content as raw material, make carrier with gac, diatomite, silica gel etc., extractive with organic solvent is invested in the carrier, insert supercritical extraction equipment, with the total triterpene alcohols of effective constituent from wherein separating.Wherein carrier is preferably gac.The extract composition that obtains with above two kinds of methods is identical, and outward appearance all is faint yellow oily thing.The ratio weight average of oily matter is between 1.15～1.25.
Below, enumerate embodiment and further describe the present invention, but the present invention is not limited to these embodiment.
In the following embodiments, the preparation method of Alisol B std-23 monoacetate reference substance is as follows.
Rhizoma alismatis, use 98% extraction using alcohol, the extract petroleum ether degreasing is used acetic acid ethyl dissolution, washes with water, remove the back silica gel column chromatography that desolvates, with sherwood oil and ethyl acetate (8: 1) is eluent, and target fraction is collected in the thin-layer chromatography calibrating, removes the back recycle silicon plastic column chromatography that desolvates, benzene and acetone (10: 1) are eluent, and the target flow point is collected in the thin-layer chromatography calibrating.Remove and desolvate, freezing and crystallizing gets Alisol B std-23 monoacetate reference substance with sherwood oil and re-crystallizing in ethyl acetate.
Outward appearance: be colourless prism-shaped crystallization.
Fusing point: 162～164 ℃.
UVλmax(MeOH)nm：205.
Infrared absorption peak cm
-1: 3470 (OH), 1745 (acetyl), 1700 (ring ketone).
EIMS?m/z：514(M
+)。
Embodiment 1
The Chinese medicine rhizoma alismatis that will meet national standard is granular through being ground into red bean, takes by weighing 25Kg, in the extractor of the carbon dioxide upercritical fluid extraction equipment of packing into, and the input carbonic acid gas, extracting pressure is 15MPa, 40 ℃ of extraction temperature, continuous extraction 5 hours.The carbonic acid gas input separator that will contain extract separates to obtain the total triterpene alcohols of rhizoma alismatis oily matter 106g from separator, be 0.42% with respect to the yield of raw material input amount.Gained oily matter is light yellow oil, proportion 1.15.
It is fixed to get the accurate title of this product, adds the solution that ethanol is made 30 μ g/ml, and precision is measured 10ml, evaporate to dryness in water-bath adds sulfuric acid 10ml dissolving, and heating is 3 hours in 60 ℃ of water-baths, measuring optical density at the 316nm place with spectrophotometry, is contrast with Alisol B std-23 monoacetate, and calculating content is 51%.
Embodiment 2
With embodiment 1 operation, different is, charging capacity is a 100Kg rhizoma alismatis particle, and extracting pressure is 30MPa, and extraction temperature is 32 ℃, and the extraction time is 2 hours, and products therefrom is faint yellow oily thing, and 412g is 0.412% with respect to the yield of raw material input amount.Proportion 1.17.With Alisol B std-23 monoacetate is contrast, and calculating content is 60%.
Embodiment 3
With embodiment 2 operation different be, extracting pressure is 20MPa, extraction temperature is 42 ℃, the extraction time is 1 hour, products therefrom is faint yellow oily thing, 398g is 0.412% with respect to the yield of raw material input amount.Proportion 1.25.With Alisol B std-23 monoacetate is contrast, and calculating content is 58%.
Embodiment 4
With embodiment 1 operation, different is that charging capacity is 50Kg, and extracting pressure is 50MPa, and extraction temperature is 35 ℃, and the extraction time is 3 hours, and products therefrom is faint yellow oily thing, and 217g is 0.434% with respect to the yield of raw material input amount.Proportion 1.20.With Alisol B std-23 monoacetate is contrast, and calculating content is 65%.
Embodiment 5
It is granular that the Chinese medicine rhizoma alismatis 100Kg that will meet national standard is ground into red bean, and with 80% ethanol 150Kg seepage flow 2 times, underpressure distillation removes and desolvates, the 7.2Kg black paste.With 10L petroleum ether 3 times, use ethyl acetate and water (1: 1) washing 3 times then, the reject water, underpressure distillation removes and desolvates, 2.86Kg brown oil paste, added activated carbon by weight 1: 2 and carry out carbon dioxide upercritical fluid extraction.Extracting pressure is 15MPa, 32 ℃ of extraction temperature, and 1.5 hours extraction time, the gained extract is faint yellow oily thing, 405g is 0.405% with respect to the yield of raw material input amount.Proportion is 1.23.With Alisol B std-23 monoacetate is contrast, and calculating content is 58%.
Embodiment 6
With embodiment 5 operation, different is that the rhizoma alismatis add-on is 200Kg, and with 98% alcohol immersion 3 times, each 48 hours, removal of solvent under reduced pressure must 15.2Kg black cream thing.With 20L petroleum ether 3 times, use ethyl acetate and water (1: 1) washing 3 times again, get brown oil paste 6.10Kg, added gac, carry out supercritical carbon dioxide extraction by weight 1: 2, extracting pressure is 20MPa, extraction temperature is 40 ℃, and the extraction time is 1 hour, and the gained extract is faint yellow oily thing, 851g is 0.425% with respect to the yield of raw material input amount.Proportion 1.18.With Alisol B std-23 monoacetate is contrast, and calculating content is 62%.
Embodiment 7
With embodiment 5 operations, different is that the rhizoma alismatis grain heats with methyl alcohol 150L, leaches 3 times, temperature is 50 ℃, decompression removes district's solvent, obtains 7.5Kg black medicinal extract, with 10L normal hexane washing 3 times, use chloroform and water (1: 1) washing 3 times then, reject water, underpressure distillation remove and to desolvate, 3.01Kg brown oil paste product, add gac at 1: 2.5 by weight, carry out supercritical carbon dioxide extraction.Extracting pressure is 15MPa, and temperature is 32 ℃, and the time is 0.5 hour, and the gained extract is faint yellow oily thing, and 411g is 0.411% with respect to the yield of raw material input amount.Proportion 1.17.With Alisol B std-23 monoacetate is contrast, and calculating content is 51%.
Embodiment 8
Get gained brown oil paste 5Kg, pressure is 15Mpa, and temperature is 32 ℃, and the time is 2.5 hours, and the gained extract is faint yellow oily thing, and 401g is 0.401% with respect to the yield of raw material input amount.Proportion 1.19.With Alisol B std-23 monoacetate is contrast, and calculating content is 58%.
The total triterpene alcohols of the rhizoma alismatis of the present invention extract that can high productivity obtains by supercritical extraction of the present invention, be faint yellow oily thing, this extract is rich in the total triterpene alcohols of rhizoma alismatis active ingredient, with Alisol B std-23 monoacetate is contrast, calculate content and be 50% or more than, this compared with prior art, no matter be that output or effective constituent concentration all have been to improve tremendously, products obtained therefrom can carry out preparation well.
Claims (12)
1. the total triterpene alcohols of rhizoma alismatis extract, it is characterized in that, this extract is to be in the carbon dioxide upercritical fluid extraction condition with the rhizoma alismatis raw material: pressure 10～50Mpa, 32～45 ℃ of extraction temperature, the oil ingredient that 0.5～5 hour supercritical extraction of disengaging time obtains, its proportion are 1.15～1.25.
2. the total triterpene alcohols of the rhizoma alismatis described in the claim 1 extract is characterized in that, this oily matter is faint yellow.
3. the rhizoma alismatis total triterpene alcohols extract of claim 1 or 2 described in each; it is characterized in that the pulverized particles that this rhizoma alismatis raw material is the Chinese medicine rhizoma alismatis or remove preextraction thing after most of useless composition is removed with ethanol or other organic solvent extraction do pre-treatment for rhizoma alismatis.
4. the total triterpene alcohols of the rhizoma alismatis described in the claim 3 extract is characterized in that, be added in this preextraction thing on the carrier after, place overcritical equipment.
5. the total triterpene alcohols of the rhizoma alismatis described in the claim 4 extract is characterized in that, this carrier is to be selected from least a in gac, diatomite, the silica gel.
6. the total triterpene alcohols of the rhizoma alismatis described in the claim 5 extract is characterized in that, this carrier is a gac.
7. the total triterpene alcohols of each described rhizoma alismatis extract in the claim 1 or 2 is characterized in that, is contrast with Alisol B std-23 monoacetate, calculate content and be 50% or more than.
8. the manufacture method of the total triterpene alcohols of a rhizoma alismatis extract, it is characterized in that, use the rhizoma alismatis raw material to be: pressure 10～50Mpa, 32～45 ℃ of extraction temperature in the carbon dioxide upercritical fluid extraction condition, extract under 0.5～5 hour the supercritical extraction condition of disengaging time, separate then.
9. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in the claim 8 extract; it is characterized in that pulverized particles that this rhizoma alismatis raw material is the Chinese medicine rhizoma alismatis or rhizoma alismatis are removed preextraction thing after most of useless composition is removed with ethanol or other organic solvent extraction do pre-treatment.
10. the manufacture method of the total triterpene alcohols of the rhizoma alismatis extract described in the claim above-mentioned 9 is characterized in that, be added in this preextraction thing on the carrier after, place overcritical equipment.
11. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in the claim 10 extract is characterized in that, this carrier is to be selected from least a in gac, diatomite, the silica gel.
12. the manufacture method of the total triterpene alcohols of the rhizoma alismatis described in the claim 11 extract is characterized in that this carrier is a gac.
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