CN104059034A - Production system and process for nontoxically extracting taxol through ultrasonic wave countercurrent extraction - Google Patents
Production system and process for nontoxically extracting taxol through ultrasonic wave countercurrent extraction Download PDFInfo
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- CN104059034A CN104059034A CN201410257538.0A CN201410257538A CN104059034A CN 104059034 A CN104059034 A CN 104059034A CN 201410257538 A CN201410257538 A CN 201410257538A CN 104059034 A CN104059034 A CN 104059034A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
- C07D305/14—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms condensed with carbocyclic rings or ring systems
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Abstract
The invention relates to a production system and process for nontoxically extracting taxol through ultrasonic wave countercurrent extraction. The production system comprises extracting equipment, detoxication equipment, recovering equipment and cooling equipment. The process comprises an ultrasonic wave countercurrent extracting process, an oxidization detoxication and adsorption process and a finished product recovering and concentrating process. By using the production system and process provided by the invention, the extraction rate of taxol is high, the content of taxol in a product can reach 95-98 percent, the pesticide residue and 'taxus chinensis essential oil' in a raw material are effectively oxidized, and the quantity, quality, precision and purity of the produced taxol completely reach the requirement of a biological medicine product.
Description
Technical field
The present invention relates to take Ramulus et folium taxi cuspidatae plant as raw material, extract the production equipment and process of taxol, relate in particular to production system and the technique of the nontoxic extraction taxol of a kind of ultrasonic wave adverse current, belong to medical biotechnology field.
Background technology
Taxol is a kind of anticancer natural plant product with unique curative effect obtaining from Ramulus et folium taxi cuspidatae plant, its novel structure, mechanism of action uniqueness, active strong, the demand of clinical application is increasing, and prior art is not strong to the extractive technique of taxol, the medicine supply breach that the taxol of take is composition is quite large.
While extracting taxol with prior art at present, general employing in chemical method and laboratory test obtained on a small quantity, traditional technology mostly adopts in spacious cooking-pot type extractor and places Ramulus et folium taxi cuspidatae, add and extract solvent and be heated with stirring to certain temperature, to after extracting liquid filtering, be stored in hold-up vessel, through repeatedly adding, extraction solvent extracts repeatedly, concentrate drying is made finished product.But this conventional production technique extraction time of extracting taxol is long, and extraction yield is low, and solvent-oil ratio is large, and energy consumption is large, and technical process is long, to produce discontinuously, occupation area of equipment is large, and level of automation is low.Chinese patent CN101367852A discloses a kind of method of ultrasonic wave countercurrent extraction steviol glycoside.Its method is extracted solvent from bottom to top to steviol glycoside through sweet Stevia, solution and Folium Chrysanthemi remain high density gradient, in leaching process, utilize hyperacoustic cavatition that liquid is pulled into hole simultaneously, formed frictional belt while effectively breaking effective constituent stripping solid, effectively increase molecular motion of material frequency and speed, increase solvent penetration power, accelerate the velocity of diffusion of effective constituent, thereby improve extraction rate.But above technological process is not suitable for the extraction of taxol, because production process not can be automated operation, while repeatedly extracting, be easily subject to the interference of extraneous bacterium, impurity, particularly in Ramulus et folium taxi cuspidatae plant, also contain the toxic substances such as pesticide residue and " beans shirt essential oil ", taxol quantity, quality, precision and the purity making does not reach the requirement of biological medical product.
Summary of the invention
The object of the invention is to solve prior art deficiency, a kind of production equipment system and technique of nontoxic extracted with high accuracy taxol are provided, it is raw material through the crude product cleaning and crush after processing that this system and technique be take Taxus plant, first carry out ultrasonic wave countercurrent extraction, then utilize detoxification dryer to be oxidized the Methods For Purification taxol of detoxification, further optimize extraction process, reached object pollution-free, that high purity is extracted taxol.
The technical solution used in the present invention is: the production system of the nontoxic extraction taxol of ultrasonic wave adverse current, is characterized in that comprising the extraction equipment, detoxification equipment, recovery system and the cooling apparatus being connected respectively with them that connect successively; Described extraction equipment comprises feeder, feeding machine, mixing pump, ultrasonic extraction pipe, slag extracting machine, shingle machine, extracting solution liquid feeding pump, extracting solution storage tank and the extracting solution Pump for giving-out connecting successively; Described detoxification equipment comprises oxygen bag, detoxification dryer and the dust catcher connecting successively, the extracting solution input terminus of detoxification dryer is connected with shingle machine output terminal with the extracting solution Pump for giving-out in extraction equipment, and finished product output terminal is connected with the withdrawing can in recovery system; Described recovery system comprises solvent storage tank, solvent liquid feeding pump, withdrawing can, water-and-oil separator and vacuum concentration pot, solvent storage tank is connected with the ultrasonic extraction pipe end in extraction equipment by solvent liquid feeding pump, withdrawing can and vacuum concentration pot junction arrange water-and-oil separator, and water-and-oil separator solvent output terminal is connected with solvent storage tank; Described cooling apparatus comprises purge tank liquid feeding pump, on-line cleaning tank, extraction condenser and the detoxification recovery condenser connecting successively.
Mucking machine is installed in described detoxification dryer bottom, and mucking machine is connected with dust catcher upper end.
Described detoxification dryer wall is provided with looks object lens.
On described ultrasonic extraction pipe, filter and filtration pump are set.
The processing step that utilizes production system of the present invention to extract taxol comprises:
1. ultrasonic wave countercurrent extraction technique: Ramulus et folium taxi cuspidatae plant powder particles is sent into from ultrasonic extraction pipe one end by feeder and feeding machine, extraction solvent in solvent storage tank is inputted from ultrasonic extraction pipe end with solvent liquid feeding pump, using mixing pump to stir makes Ramulus et folium taxi cuspidatae plant powder particles fully be dissolved in solvent, under ultrasonic environment to mixing solutions indirectly heat 30 degree uninterrupted stirring, to fast instant the soaking of Ramulus et folium taxi cuspidatae plant powder particles, expand, rotary impact, impel the taxol in particle to separate out fast, ultrasonic wave adverse current is soaked molten, stir, the time of separating out is 2-3 hour,
2. be oxidized detoxification absorbing process: by being filtered by filter, slag extracting machine extracts and shingle machine shingle after extracting solution by extracting liquid feeding pump, send in detoxification dryer and heat, heating is simultaneously by oxygen bag input trioxid body, oxidation objectionable impurities " beans shirt essential oil ", the oxidation detoxification time is 1-2 hour, when liquid temperature rises to gradually 50 degree to 70 and spends, oxidized material upwards swims and builds up to center, liquid layer top, and with dust catcher, by its sucking-off, the extracting solution that is fully oxidized detoxification outputs to withdrawing can;
3. reclaim concentrated finished product technique: the extracting solution that is warming up to 70 degree in withdrawing can is sent into water-and-oil separator, and to carry out taxol crude product solution separated with solvent, reclaim solvent to solvent storage tank, taxol crude product solution after separation is injected in vacuum concentration pot, 30 degree of indirectly heating, vacuum absorption solvent and moisture, when being gruel shape, takes out wash-out mixed solution, put into stainless steel pallet, carry out cryogenic freezing, dry 24-32 hour, when moisture content is following lower than 6%, take out, fast-crushing, metering pack is finished product.
Above processing step, described Ramulus et folium taxi cuspidatae plant powder particles is preferably 80 orders; Described extraction solvent is preferably the ethanolic soln that 1000 liters of content are 75%; That described ultrasonic wave adverse current is soaked is molten, stir, the time of separating out is preferably 3 hours; Preferably 2 hours described oxidation detoxification time; Described cryogenic freezing, time of drying are preferably 32 hours, are conducive to obtain more taxol.
The invention has the beneficial effects as follows: the taxol that uses production system of the present invention and technique output, extraction yield can reach 95-99%, in product, the content of taxol can reach 95-98%, color is white crystals body, the toxic substance such as the pesticide residue in raw material, " beans shirt essential oil " is removed completely, whole production system configuration on-line cleaning cooling apparatus, meets the hygienic requirements of GMP authentication to equipment, and taxol quantity, quality, precision and the purity making reaches the requirement of biological medical product completely.
Accompanying drawing explanation
Fig. 1 is production system schematic diagram of the present invention.In figure, the 1st, extraction equipment, the 2nd, detoxification equipment, the 3rd, recovery system, the 4th, cooling apparatus.
Fig. 2 is process flow diagram of the present invention.
Fig. 3 is for extracting cooling apparatus schematic diagram.In figure, the 101st, feeder, the 102nd, feeding machine, the 103rd, mixing pump, the 104th, ultrasonic extraction pipe, the 105th, slag extracting machine, the 106th, shingle machine, the 107th, extracting solution liquid feeding pump, the 108th, extracting solution storage tank, the 109th, extracting solution Pump for giving-out, the 110th, filter, the 111st, filtration pump, the 401st, purge tank liquid feeding pump, the 402nd, on-line cleaning tank, the 403rd, extract condenser, the 404th, condenser is reclaimed in detoxification.
Fig. 4 is detoxification recovery system schematic diagram.In figure, the 201st, oxygen bag, the 202nd, detoxification dryer, the 203rd, depending on object lens, the 204th, dust catcher, the 205th, mucking machine, the 301st, solvent storage tank, the 302nd, solvent liquid feeding pump, the 303rd, withdrawing can, the 304th, water-and-oil separator, the 305th, vacuum concentration pot.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
As shown in Figure 1, the production system of the nontoxic extraction taxol of ultrasonic wave adverse current, comprises extraction equipment 1, detoxification equipment 2, the recovery system 3 connecting successively and the cooling apparatus 4 being connected respectively with them; As shown in Figure 3, described extraction equipment 1 comprises feeder 101, feeding machine 102, mixing pump 103, ultrasonic extraction pipe 104, slag extracting machine 105, shingle machine 106, extracting solution liquid feeding pump 107, extracting solution storage tank 108 and the extracting solution Pump for giving-out 109 connecting successively; As shown in Figure 4, described detoxification equipment 2 comprises oxygen bag 201, detoxification dryer 202 and the dust catcher 204 connecting successively, as shown in Figure 3, the extracting solution input terminus of the detoxification dryer 202 in detoxification equipment 2 is connected with shingle machine 106 output terminals with extracting solution Pump for giving-out 109, as shown in Figure 4, detoxification dryer 202 finished product output terminals are connected with withdrawing can 303; Described recovery system 3 comprises solvent storage tank 301, solvent liquid feeding pump 302, withdrawing can 303, water-and-oil separator 304 and vacuum concentration pot 305, as shown in Figure 3, solvent storage tank 301 is connected with ultrasonic extraction pipe 104 ends by solvent liquid feeding pump 302, as shown in Figure 4, withdrawing can 303 arranges water-and-oil separator 304 with vacuum concentration pot 305 junctions, and water-and-oil separator 304 solvent output terminals are connected with solvent storage tank 301; As shown in Figure 3, described cooling apparatus comprises purge tank liquid feeding pump 401, on-line cleaning tank 402, extraction condenser 403 and the detoxification recovery condenser 404 connecting successively.
As preferred version, as shown in Figure 4, in detoxification dryer 202 bottoms, mucking machine 205 is installed, mucking machine 205 is connected with dust catcher 204 upper ends, can be using the material after extraction taxol as the raw material of producing Ramulus et folium taxi cuspidatae tea streamline.Can on detoxification dryer 202 walls, install and look object lens 203, the convenient position of observing the liquid layer that swims after " beans shirt essential oil " oxidation, so that dust catcher 204 absorption.As shown in Figure 3, filter 110 and filtration pump 111 can also be set on ultrasonic extraction pipe 104, the settling in slag extracting machine 105 is carried out to secondary filtration, extraction.
The processing step that utilizes production system of the present invention to extract taxol comprises: as shown in Figure 2, be divided into three technical process.
Embodiment 1: 1. ultrasonic wave countercurrent extraction technique: as shown in Figure 3, to be ground into 60 object Ramulus et folium taxi cuspidatae plant powder particles sends into from ultrasonic extraction pipe 104 one end by feeder 101 and feeding machine 102, the ethanolic soln that is 75% 1000 liters of content in solvent storage tank 301 is inputted from ultrasonic extraction pipe 104 ends with solvent liquid feeding pump 302, using mixing pump 103 to stir makes Ramulus et folium taxi cuspidatae plant powder particles fully be dissolved in ethanol, under ultrasonic environment to mixed solution indirectly heat 30 degree uninterrupted stirring, to fast instant the soaking of Ramulus et folium taxi cuspidatae plant powder particles, expand, rotary impact, impel the taxol in particle to separate out fast, ultrasonic wave is soaked molten, stir, the time of separating out is 2 hours,
2. be oxidized detoxification absorbing process: as shown in Figure 3,4, extracting solution after filter 110 filtrations, slag extracting machine 105 extractions and shingle machine 106 shingles is sent into heating in detoxification dryer 202 by extracting solution liquid feeding pump, heating is simultaneously by oxygen bag 201 input trioxid bodies, oxidation objectionable impurities " beans shirt essential oil ", the oxidation detoxification time is 1 hour, when liquid temperature rises to gradually 50 degree to 70 and spends, oxidized material upwards swims and builds up to center, liquid layer top, with dust catcher 204, by its sucking-off, the extracting solution that is fully oxidized detoxification outputs to withdrawing can 303;
3. reclaim concentrated finished product technique: the extracting solution that is warming up to 70 degree in withdrawing can 303 is sent into water-and-oil separator 304, and to carry out taxol crude product solution separated with solvent, reclaim solvent to solvent storage tank 301 simultaneously, taxol crude product solution after separation is injected in vacuum concentration pot 305, 30 degree of indirectly heating, vacuum absorption solvent and moisture, when being gruel dress, takes out wash-out mixed solution, put into stainless steel pallet, carry out cryogenic freezing, dry 24 hours, when moisture content is following lower than 6%, take out, fast-crushing, metering pack is finished product, make white crystals body taxol powder 20kg, product content of taxol 95%.
Embodiment 2: its processing step except ultrasonic wave soak molten, stir, the time of separating out is 2.5 hours, the oxidation detoxification time is 1.5 hours, cryogenic freezing, dry 30 hours are outer, and all the other are identical, can make white crystals body taxol powder 25kg, product content of taxol 96%.
Embodiment 3: its processing step except ultrasonic wave soak molten, stir, the time of separating out is 3 hours, the oxidation detoxification time is 2 hours, cryogenic freezing, dry 32 hours are outer, and all the other are identical, can make white crystals body taxol powder 30kg, product content of taxol 98%.
Claims (10)
1. the production system of the nontoxic extraction taxol of ultrasonic wave adverse current, is characterized in that comprising the extraction equipment (1), detoxification equipment (2), the recovery system (3) and the cooling apparatus being connected respectively with them (4) that connect successively; Described extraction equipment (1) comprises feeder (101), feeding machine (102), mixing pump (103), ultrasonic extraction pipe (104), slag extracting machine (105), shingle machine (106), extracting solution liquid feeding pump (107), extracting solution storage tank (108) and the extracting solution Pump for giving-out (109) connecting successively; Described detoxification equipment (2) comprises oxygen bag (201), detoxification dryer (202) and the dust catcher (204) connecting successively, the extracting solution input terminus of detoxification dryer (202) is connected with shingle machine (106) output terminal with the extracting solution Pump for giving-out (109) in extraction equipment (1), and finished product output terminal is connected with the withdrawing can (303) in recovery system (3); Described recovery system (3) comprises solvent storage tank (301), solvent liquid feeding pump (302), withdrawing can (303), water-and-oil separator (304) and vacuum concentration pot (305), solvent storage tank (301) is connected with ultrasonic extraction pipe (104) end in extraction equipment (1) by solvent liquid feeding pump (302), withdrawing can (303) arranges water-and-oil separator (304) with vacuum concentration pot (305) junction, and water-and-oil separator (304) solvent output terminal is connected with solvent storage tank (301); Described cooling apparatus comprises purge tank liquid feeding pump (401), on-line cleaning tank (402), extraction condenser (403) and the detoxification recovery condenser (404) connecting successively.
2. the production system of the nontoxic extraction taxol of ultrasonic wave adverse current as claimed in claim 1, is characterized in that described detoxification dryer (202) bottom installation mucking machine (205), and mucking machine (205) is connected with dust catcher (204) upper end.
3. the production system of the nontoxic extraction taxol of ultrasonic wave adverse current as claimed in claim 1 or 2, is characterized in that installing and looking object lens (203) on described detoxification dryer (202) wall.
4. the production system of the nontoxic extraction taxol of ultrasonic wave adverse current as claimed in claim 1 or 2, is characterized in that arranging on described ultrasonic extraction pipe (104) filter (110) and filtration pump (111).
5. utilize as arbitrary production system in claim 1 or 2 and extract the technique of taxol, it is characterized in that comprising the following steps:
1. ultrasonic wave countercurrent extraction technique: Ramulus et folium taxi cuspidatae plant powder particles is sent into from ultrasonic extraction pipe (104) one end by feeder (101) and feeding machine (102), extraction solvent in solvent storage tank (301) is inputted from ultrasonic extraction pipe (104) end with solvent liquid feeding pump (302), using mixing pump (103) to stir makes Ramulus et folium taxi cuspidatae plant powder particles fully be dissolved in solvent, under ultrasonic environment to mixing solutions indirectly heat 30 degree uninterrupted stirring, to fast instant the soaking of Ramulus et folium taxi cuspidatae plant powder particles, expand, rotary impact, impel the taxol in particle to separate out fast, ultrasonic wave adverse current is soaked molten, stir, the time of separating out is 2-3 hour,
2. be oxidized detoxification absorbing process: the extracting solution after filter (110) filtration, slag extracting machine (105) extraction and shingle machine (106) shingle is sent into heating in detoxification dryer (202) by extracting liquid feeding pump (109), heating is simultaneously by oxygen bag (201) input trioxid body, oxidation objectionable impurities " beans shirt essential oil ", the oxidation detoxification time is 1-2 hour, when liquid temperature rises to gradually 50 degree to 70 and spends, oxidized material upwards swims and builds up to center, liquid layer top, with dust catcher (204), by its sucking-off, the extracting solution that is fully oxidized detoxification outputs to withdrawing can (303);
3. reclaim concentrated finished product technique: the extracting solution that is warming up to 70 degree in withdrawing can (303) is sent into water-and-oil separator (304), and to carry out taxol crude product solution separated with solvent, reclaim solvent to solvent storage tank (301), taxol crude product solution after separation is injected in vacuum concentration pot (305), 30 degree of indirectly heating, vacuum absorption solvent and moisture, when being gruel shape, takes out wash-out mixed solution, put into stainless steel pallet, carry out cryogenic freezing, dry 24-32 hour, when moisture content is following lower than 6%, take out, fast-crushing, metering pack is finished product.
6. production system as claimed in claim 5 is extracted the technique of taxol, it is characterized in that Ramulus et folium taxi cuspidatae plant powder particles is 80 orders.
7. production system as claimed in claim 5 is extracted the technique of taxol, and it is characterized in that extracting solvent is 1000 liters of ethanolic solns that content is 75%.
8. production system as claimed in claim 5 is extracted the technique of taxol, it is characterized in that ultrasonic wave adverse current soak molten, stir, the time of separating out is 3 hours.
9. production system as claimed in claim 5 is extracted the technique of taxol, and it is characterized in that being oxidized the detoxification time is 2 hours.
10. production system as claimed in claim 5 is extracted the technique of taxol, it is characterized in that cryogenic freezing, time of drying are 32 hours.
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Application publication date: 20140924 |