CN100525781C - American falx extract, medicinal composition containing it and its making method - Google Patents
American falx extract, medicinal composition containing it and its making method Download PDFInfo
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Abstract
An extract of American periplaneta and its medicinal composition with high content of general amino acids are disclosed. Its preparing process includes such steps as immersing American periplaneta in petroether for removing fat, extracting in water or alcohol, and mixing with pharmacologically acceptable additives.
Description
Technical field
The present invention relates to a kind of preparation method of American-cockroach-extract, belong to field of medicaments.
Background technology
Periplaneta americana (the Latin literary fame: Periplaneta americana), its diagnostic characteristics is the adult ellipse, dorsoventrally compressed, and body is yellowish-brown, rufous or dark brown, body surface gloss.Build is big, the long 25～45mm of body, and pronotary has a big pitchy butterfly patch, and there is one " T " shape yellow cord in center line the place ahead of speckle, extands rearward to " little tail ", is lark, trailing edge mottle broad around the speckle.Original producton location: the African torrid zone or subtropical zone.China's distribution status: all there is distribution all parts of the country, and are more common with China's southern area especially.
At present, the preparation about American-cockroach-extract is the national drug standards (the 19 shows standard and be implemented as WS that National Drug Administration announces
3-B-3674-2000 (Z), on December 11st, 2000), wherein disclosing " the new liquid of rehabilitation " is " solution that the ethanol extraction of the dry polypide of periplaneta americana Periploneta amjericana is made." this standard also discloses its character item, check item, assay, function and cure mainly and specification, storage; And the quality standard of periplaneta americana ethanol extraction disclosed.Li Liping, retention-enema treatment ulcerative colitis 40 examples, the Henan traditional Chinese medical science, May in 2005, the 25th the 5th phase of volume was reported rehabilitation newly in conjunction with retention-enema treatment ulcerative colitiss such as metronidazoles.Lv Wen etc., the new liquid retention-enema treatment of rehabilitation ulcerative colitis 21 examples, have been reported the drug effect that the new liquid of rehabilitation is used for external at Chinese combination of Chinese and Western medicine digestion magazine the 11st the 2nd phase of volume of April in 2003.In addition, the new liquid of rehabilitation all has relevant report at aspects such as treatment cervical erosion, condyloma acuminatum postoperative wound surfacees.Above-mentioned document is not all reported the preparation method of the new liquid of rehabilitation (American-cockroach-extract).Because the active ingredient complexity of medical material (animal drugs or plant amedica), the drug effect of different extraction process preparations is also inequality.
The ZL03117804.9 denomination of invention: the medicinal extractum extraction process of periplaneta americana wherein discloses the medicinal extractum extraction process of a kind of periplaneta americana.It is characterized in that alcohol extraction: promptly: with the deactivation of raw material Blatta seu periplaneta hot water by A.; After the warm drying of heat, coarse pulverization, sieve; Alcohol-pickled 40～50 hours; Drop in the multi-functional extractor ethanol hot reflux extracting; Recovered alcohol; Released liquor carries out oil-water separation; Separate medicinal liquid after filtration; Filtrate concentrate, cool off extractum; B. water extraction: raw material behind the alcohol is reclaimed in alcohol extraction, inject distilled water extraction; Released liquor carries out oil-water separation; Medical filtration; Get extractum after concentrating, cooling off.The extraction process of foregoing invention is always received the cream rate and is reached 18～20% after increasing extraction process by water, exceeds about one times than carbinol extraction method yield, and extractum product total amino acids content detects up to 50.4% through national departments concerned.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing American-cockroach-extract, and the American-cockroach-extract that is got by this method preparation.
The invention provides the preparation method of American-cockroach-extract, it comprises the steps:
A, get periplaneta americana Periploneta amjericana and pulverize, add petroleum ether, soak down for 5～20 ℃ in temperature, filter, filtering residue volatilizes;
Preferably, add the petroleum ether of 3 times of amounts of periplaneta americana, soaked 3 hours under 10 ℃ of temperature, filter, filtering residue volatilizes, and is standby.
B, get step a gained filtering residue, adopt decoction and alcohol sedimentation technique or ethanol extract from water precipitation to extract, leave standstill; Medicinal liquid after leaving standstill is abandoned the upper strata oils and fats, filters, and gets lower floor's medicinal liquid;
Wherein, decocting amount of water in the decoction and alcohol sedimentation technique is 3～5 times, 60～80 ℃ of immersions, and soak time 0.5～2 hour, decocting time 4～8 hours decocts number of times 1～3 time; Further, decoct with water and add four times of water gagings first, 70 ℃ of soaking temperatures soaked 1 hour, decocted 8 hours; Add 3 times of water gagings for the second time at every turn, soak the back and decocted 4～6 hours;
In addition, adding ethanol alcohol precipitation concentration is: 75%～95%, and addition is 3 times of amounts; Preferred alcohol concentration is 95%w/w;
Wherein, in the ethanol extract from water precipitation, ethanol extraction adds 3～8 times of amount 60～80%w/w ethanol when decocting, 60～80 ℃ of immersions, and soak time 0.5～2 hour, decocting time 6～10 hours decocts number of times 1～3 time; Further, ethanol decocts and adds four times of amount 70%w/w ethanol first, and 70 ℃ of soaking temperatures soaked 1 hour, decocted 8 hours; Add 3 times of amount 70%w/w ethanol for the second time at every turn, soak the back and decocted 6 hours; Extracting method also can use percolation.
C, gained b step gained medicinal liquid, being concentrated into relative density is 1.20～1.25, gets clear paste;
D, use the usefulness of 40～60ml glycerol to measure glycerol, mixes with the described clear paste of c step by every 1000g periplaneta americana, must American-cockroach-extract of the present invention.
Further, the glycerol consumption preferably uses 50ml glycerol in the every 1000g periplaneta americana of periplaneta americana.
Temperature range in the preparation method of the present invention among step a～d is: 60～85 ℃, preferred temperature is 70 ℃.
Another technical problem solved by the invention has provided the American-cockroach-extract that is got by method for preparing.
Another technical problem solved by the invention has provided a kind of pharmaceutical composition with promoting blood circulation, and it is that American-cockroach-extract by effective dose is an active component, adds the medicament that acceptable accessories or complementary composition are prepared from.
Wherein, described medicament is topical agent, medicinal preparation for oral administration.
American-cockroach-extract preparation method of the present invention is simple, easy to operate, receives cream rate height in the preparation process, and product is limpid, total amino acids content height, for clinical preparation American-cockroach-extract provides a kind of new selection.
Obviously, according to foregoing of the present invention,,, can also make modification, replacement and the change of other various ways not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite according to the ordinary skill knowledge and the customary means of this area.
The specific embodiment of form is described in further detail foregoing of the present invention again by the following examples.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
The specific embodiment
The preparation of embodiment 1 periplaneta americana ethanol extraction
With exsiccant periplaneta americana coarse crushing 1000kg, add 4 times of amount 70% ethanol, to soak after 1 hour, 70 ℃ of temperature are extracted secondary, 8 hours for the first time; For the second time add 3 times of amounts of ethanol, extract 6 hours merging secondary raffinates, filter, when filtrate is concentrated into relative density and is the clear paste of 1.09～1.16 (70 ℃), add entry, 70 ℃ of insulated and stirred 60 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol is evaporated to relative density and is 1.16～1.22 medicinal liquid (70 ℃), every 1000ml adds 50ml glycerol, stir, filter, after filtrate is boiled 30 minutes, be distributed into bottle, through 125 ℃, pressure is 0.1Mpa again, sterilizes 30 minutes, be chilled to room temperature, promptly.
The preparation of embodiment 2 periplaneta americana ethanol extractions
With exsiccant periplaneta americana coarse crushing 1000kg, every 100kg coarse powder adds 400kg water, soaks after 1 hour, and temperature is extracted three times about 70 ℃, 8 hours for the first time; For the second time add water 300kg, extracted 6 hours; Add water 300kg for the third time, extracted 4 hours.Merge three times extracting solution, filter, when filtrate is concentrated into relative density and is 1.10～1.20 (70 ℃), add 95% ethanol, 70 ℃ of insulated and stirred 30 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol, being evaporated to relative density is 1.20～1.25 (70 ℃), add purified water and glycerol (every 1000ml adds 50ml), stir, filter, promptly.
The preparation of embodiment 3 periplaneta americana ethanol extractions
With exsiccant periplaneta americana coarse crushing 1000kg, every 100kg coarse powder adds 500kg water, soaks after 2 hours, and temperature is extracted three times about 80 ℃, 8 hours for the first time; For the second time add water 300kg, extracted 6 hours; Add water 300kg for the third time, extracted 4 hours.Merge three times extracting solution, filter, when filtrate is concentrated into relative density and is 1.10～1.20 (70 ℃), add 95% ethanol, 70 ℃ of insulated and stirred 30 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol, being evaporated to relative density is 1.20～1.25 (70 ℃), add purified water and glycerol (every 1000ml adds 60ml), stir, filter, promptly.
The preparation of embodiment 4 periplaneta americana ethanol extractions
With exsiccant periplaneta americana coarse crushing 1000kg, every 100kg coarse powder adds 300kg water, soaks after 0.5 hour, and temperature is extracted three times about 60 ℃, 8 hours for the first time; For the second time add water 300kg, extracted 6 hours; Add water 300kg for the third time, extracted 4 hours.Merge three times extracting solution, filter, when filtrate is concentrated into relative density and is 1.10～1.20 (70 ℃), add 95% ethanol, 70 ℃ of insulated and stirred 30 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol, being evaporated to relative density is 1.20～1.25 (70 ℃), add purified water and glycerol (every 1000ml adds 40ml), stir, filter, promptly.
The preparation of embodiment 5 periplaneta americana ethanol extractions
With exsiccant periplaneta americana coarse crushing 1000kg, add 8 times of amount 70% ethanol, to soak after 2 hours, about 80 ℃ of temperature is extracted secondary, 8 hours for the first time; For the second time add 6 times of amounts of ethanol, extract 6 hours merging secondary raffinates, filter, when filtrate is concentrated into relative density and is the clear paste of 1.09～1.16 (70 ℃), add entry, 70 ℃ of insulated and stirred 60 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol is evaporated to relative density and is 1.16～1.22 medicinal liquid (70 ℃), every 1000ml adds 60ml glycerol, stir, filter, after filtrate is boiled 30 minutes, be distributed into bottle, through 125 ℃, pressure is 0.1Mpa again, sterilizes 30 minutes, be chilled to room temperature, promptly.
The preparation of embodiment 6 periplaneta americana ethanol extractions
With exsiccant periplaneta americana coarse crushing 1000kg, add 6 times of amount 70% ethanol, to soak after 0.5 hour, 60 ℃ of temperature are extracted secondary, 6 hours for the first time; For the second time add 4 times of amounts of ethanol, extract 4 hours merging secondary raffinates, filter, when filtrate is concentrated into relative density and is the clear paste of 1.09～1.16 (70 ℃), add entry, 70 ℃ of insulated and stirred 60 minutes left standstill 12 hours, discard the upper strata oils and fats, lower floor's medical filtration, filtrate recycling ethanol is evaporated to relative density and is 1.16～1.22 medicinal liquid (70 ℃), every 1000ml adds 40ml glycerol, stir, filter, after filtrate is boiled 30 minutes, be distributed into bottle, through 125 ℃, pressure is 0.1Mpa again, sterilizes 30 minutes, be chilled to room temperature, promptly.
Below by craft screening experiment and technology contrast experiment beneficial effect of the present invention is described.
1, defat with petroleum ether technology is investigated, and sees Table 1
Table 1 degreasing process is investigated
The result shows, carries out defat with petroleum ether under selecting 10 ℃, centrifugal effect is good.
2, ethanol decocts the screening of extraction process parameter:
The orthogonal design water-glass sees Table 2, and orthogonal experiments sees Table 3:
Table 2 orthogonal design water-glass
Table 3 orthogonal experiments
Remarks: investigate medical material amount 100g
Analysis result shows: the influence of three factors has remarkable meaning (P＜0.05), and the result knows by range analysis, and best of breed is A
2B
1C
2, promptly 4 times of amount 70% ethanol decocted 8 hours.According to this condition, carry out demonstration test, the results are shown in Table 4:
Table 4 demonstration test result
By table 4 as seen, extractum yield, amino acid content fluctuate little, this process stabilizing, reliable; In sum, ethanol extraction technology is defined as: add 4 times of amount 70% ethanol for the first time and decocted 8 hours, add 3 times of amount 70% ethanol for the second time, for the third time and decocted 6 hours.
3, investigate required soaking temperature of 70% ethanol and time
The orthogonal design water-glass sees Table 5, and orthogonal experiments sees Table 6
Table 5 orthogonal design water-glass
Table 6 orthogonal experiments
Remarks: investigate medical material amount 100g
Analysis result shows: the influence of two factors has remarkable meaning (P＜0.05), and the result knows by range analysis, and best of breed is A
2B
2C
2, promptly 70% ethanol is 70 ℃ in temperature, soaks 1 hour.In conjunction with the screening that ethanol decocts the extraction process parameter, consider that the problem of cost savings determines that at last the extraction process of American-cockroach-extract of the present invention is 4 times of amount 70% ethanol, to soak after 1 hour, 70 ℃ of temperature are extracted secondary, 8 hours for the first time; For the second time add 3 times of amounts of ethanol, extracted 6 hours.
4, the screening of glycerol consumption sees Table 7
The The selection result of table 7 glycerol
Annotate :-show against regulation; + show better; ++ express friendship.
According to 7 results, select for use 1000ml American-cockroach-extract of the present invention to add the glycerol of 50ml from multifactor considerations such as the control of cost and qualitative factor controls, and amino acid contents (in alanine) before and after adding glycerol are compared with appearance character, the results are shown in Table 8.
Changes of contents relatively before and after table 8 added glycerol
The result shows and adds that appearance character, amino acid content (in the alanine) content of medicinal liquid does not have obvious variation behind the glycerin, and it is rationally feasible as seen should to add glycerol dosage.
5, patent 03117804.9 and technology contrast experiment of the present invention
Technology of the present invention mainly contains three parts: A, petroleum ether soaks, and B, extractum extract the C glycerol adding.Get three parts of the periplaneta americanaes of same amount, get the extractum product according to the extractum extraction process of patent 03117804.9, A+B technology of the present invention, B prepared of the present invention respectively, analyze receipts cream rate, the total amino acids content of three kinds of extractum products respectively, comparing result sees Table 9:
Table 9 technology of the present invention and patent 03117804.9 technology comparing result
The result shows, receives the cream rate through A+B PROCESS FOR TREATMENT of the present invention and is higher than patent 03117804.9 extraction process extractum receipts cream rate.Receive cream rate difference and illustrate that it is not identical product that extraction and preparation technique products obtained therefrom of the present invention prepares products obtained therefrom with patent 03117804.9 extraction process, according to total amino acids assay result, the total amino acids content of A+B prepared products obtained therefrom of the present invention obviously prepares the total amino acids content of products obtained therefrom more than patent 03117804.9.Illustrate that American-cockroach-extract preparation technology of the present invention obviously is better than the preparation technology of patent 03117804.9, prepare the method for American-cockroach-extract for the public provides a kind of new extraction.
Claims (8)
1, a kind of preparation method of American-cockroach-extract, it comprises the steps:
A, get periplaneta americana and pulverize, add petroleum ether, soak down for 5～20 ℃ in temperature, filter, filtering residue volatilizes;
B, get step a gained filtering residue, adopt decoction and alcohol sedimentation technique or ethanol extract from water precipitation to extract, leave standstill; Medicinal liquid after leaving standstill is abandoned the upper strata oils and fats, filters, and gets lower floor's medicinal liquid;
Wherein, during precipitate with ethanol, the concentration of alcohol of adding is: 75～95%w/w in the decoction and alcohol sedimentation technique;
Or during ethanol extract from water precipitation, the concentration of alcohol of adding is: 60～80%w/w;
C, gained b step gained medicinal liquid, being concentrated into relative density is 1.20～1.25, gets clear paste;
D, use the usefulness of 40～60ml glycerol to measure glycerol, mix, promptly get American-cockroach-extract with the described clear paste of c step by every 1000g periplaneta americana.
2, the preparation method of American-cockroach-extract according to claim 1, it is characterized in that: the amount of water when decoction and alcohol sedimentation technique decocts among the step b is 3～5 times, 60～80 ℃ of immersions, soak time 0.5～2 hour, decocting time 4～8 hours decocts number of times 1～3 time.
3, the preparation method of American-cockroach-extract according to claim 2 is characterized in that: when adopting decoction and alcohol sedimentation technique in step b, decoct with water and add four times of water gagings first, 70 ℃ of soaking temperatures soaked 1 hour, decocted 8 hours; Add 3 times of water gagings for the second time at every turn, soak the back and decocted 4～6 hours.
4, the preparation method of American-cockroach-extract according to claim 1 is characterized in that: when adopting decoction and alcohol sedimentation technique in step b, adding the ethanol alcohol precipitation concentration is 95%w/w.
5, the preparation method of American-cockroach-extract according to claim 1, it is characterized in that: adopt during ethanol extract from water precipitation ethanol to decoct among the step b and extract, add 3～8 times of amount 60～80%w/w ethanol, 60～80 ℃ of immersions, soak time 0.5～2 hour, decocting time 6～10 hours decocts number of times 1～3 time.
6, the preparation method of American-cockroach-extract according to claim 5 is characterized in that: adopt during ethanol extract from water precipitation ethanol to decoct in step b and extract, ethanol decocts and adds four times of amount 70%w/w ethanol first, 70 ℃ of soaking temperatures soaked 1 hour, decocted 8 hours; Add 3 times of amount 70%w/w ethanol for the second time at every turn, soak the back and decocted 6 hours.
7, the preparation method of American-cockroach-extract according to claim 1 is characterized in that: the glycerol consumption described in the steps d uses 50ml glycerol in the every 1000g periplaneta americana of periplaneta americana.
8, each described method preparation of claim 1～7 and American-cockroach-extract.
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