CN1162421C - New process for extracting high purity puerarin by pure water method - Google Patents

Abstract

The present invention relates to new process for extracting high purity puerarin by a pure water method. The present invention has a flow path of the drying and the grinding of raw materials, the rough extraction of a liquid phase, the fine extraction by separation and purification milling. The present invention is characterized in that the fine extraction process by separation is a column chromatography or elution method which uses a dextran gel molecular sieve with the molecular weight of 800 to 1200 as filler, and diluent which is obtained by the rough extraction of the liquid phase is processed in a chromatography and elution mode so that a paste body of the fine extraction is prepared; the rough extraction of the liquid phase comprises a high temperature soaking filtering separation procedure and a depressurization concentrating procedure; the purification milling comprises a repeated crystallization procedure of the fine extracted paste body, and a drying milling procedure; water for the liquid phase, which is used by each flow path and procedure in the new process for extracting high purity puerarin by the pure water method, is purified water. The process flow path of the present invention can produce finished products which are required by export, and organic and inorganic acid and alkali are not used. Environmental pollution can not be generated in the production process, and toxic adsorbent and inflammable and easy explosive substances are not used. The present invention has the advantages of safety, high efficiency, optimized procedures, reasonable, simple and swift connection and easy popularization.

Description

The novel process of extracting high purity puerarin by pure water method

Technical field: the present invention relates to plants ' medicinal component process for extracting field, relate in particular to the improvement and the innovation of the process for extracting of herbal medicine puerarin.

Background technology: the root of kudzu vine is a kind of time-honored traditional herbal medicine, abroad control cancer drug effect pay attention to day by day in recent years for its mystery, the demand for exports of high-purity extract of the root of kudzu vine just growing, has also been proposed more and more higher requirement for quality product simultaneously; Domestic extraction for total flavones in the root of kudzu vine and puerarin is wherein also carried out for many years, obtained certain effect, but because there are variety of problems in processing method that adopts and extraction medicament, so that extract the puerarin finished product that obtains, no matter from extracting medicament, purity, the residual angle of nuisance, all be difficult to reach the standard that requires, also influence domestic patient treatment effect to developed country's outlet.Extract the technology of total flavones as proposing the heavy method of a kind of wine in China Patent No. 91110602.2 files, its shortcoming is: technology is from first to last used a large amount of alcohol, inflammable and explosive dangerous, extract is total flavones but not wherein effective constituent puerarin, and total flavones purity only is 30%～80%, far can not adapt to existing market and puerarin is higher than 97% demand; The extraction process of a kind of water extract-alcohol precipitation, polyamide column chromatography wash-out is and for example proposed in China Patent No. 95110343.1 files, though it is said that content of puerarin can reach more than 90% in the finished product, but because of its chromatography column filler that uses is polymeric amide, and polymeric amide is judged to the neurotoxicity molecule by international medical community, can cause the pollution that is difficult to eliminate to the puerarin finished product, and puerarin content still is lower than 97% market demands; Have again and propose a kind of propyl carbinol solubilising extraction, the spissated extraction process of aluminium sesquioxide chromatography column in China Patent No. 96100953.5 files, it is said that its product purity can reach more than 97%, but because of its propyl carbinol that adopts has neurotoxicity, aluminium sesquioxide is also harmful to human body, and the ppb magnitude that they be removed to reach approval in the world is very difficult; Have recently to mention in China Patent No. 99115790.7 files crude extract is carried out the sedimentation filtration with the natural settling agent, but wherein to use ethyl acetate, propyl carbinol or methyl alcohol as solvent, and it is well-known, above-mentioned solvent is all inflammable and explosive, have potential safety hazard, and has great neurotoxicity, be difficult to from finished product, its removal be reached the ppb magnitude, and undocumented natural settling agent is difficult to estimate, is difficult to adapt to the requirement of domestic and international market.

Summary of the invention: at the above-mentioned shortcoming that prior art exists, technical problem to be solved by this invention is: a kind of nontoxic, safe extraction medicament, the finished product of energy production export requirement and novel process of the simple extracting high purity puerarin by pure water method of technology of adopting is provided.

For this reason, technical scheme of the present invention is: a kind of novel process of extracting high purity puerarin by pure water method, be made up of in regular turn following flow process: raw material drying pulverizing → liquid phase is slightly put forward → is separated essence and carry → purifying powder process, it is characterized in that: the smart flow process of carrying of described separation is to adopt column chromatography/elution method of making filler with the dextrane gel molecular sieve, liquid phase is slightly carried the diluent of gained and done chromatography, elution, make essence and carry lotion.

The molecular weight of described dextrane gel molecular sieve is 800～1200, preferred 1000; The liquid phase that wash-out adopted in described column chromatography/elution method is a pure water.

Described liquid phase is slightly put forward flow process and comprised in regular turn: temperature is soaked filtering separation operation, concentrating under reduced pressure operation, and described purifying flour mill flow comprises in regular turn: essence is put forward lotion recrystallization operation, dry powder process operation.

Described temperature is soaked in the filtering separation operation, keeps warm immersion liquid phase temperature at 40 ℃～65 ℃, and filtering and collecting filter liquid adopts the further separating filtrate of low-speed centrifugation to get supernatant fluid filtrate; Described concentrating under reduced pressure operation is that controlled temperature is lower than under 130 ℃, supernatant fluid filtrate is vacuumized and makes and slightly carry lotion, and then water will slightly to propose the paste dissolves dilution be that 5% diluent is treated chromatography; It is essence to be carried lotion repeat two, three times and make moist crystallizate with low-concentration ethanol-aqueous solution through the low temperature recrystallization that described essence is put forward lotion recrystallization operation; Described dry powder process operation is with the dehydration of gained moist crystallizate drying, makes the pure product of powdery.

The liquid phase water that each flow process, operation adopted in the novel process of described extracting high purity puerarin by pure water method is pure water.

Because above-mentioned process modification, the present invention has following remarkable advantage:

Whole technology is from initial until finished product, a large amount of and the main extraction agent that adopts is water and is pure water, basically eliminate the unsafe factor of initiation fire, blast etc., and, stopped in leaching process, may introduce an important channel of pollutent from the outside because of having removed heavy metal or other organic pollutant in the pure water;

Carry the dextrane gel molecular sieve filling post that has adopted non-toxic and safe in the flow process in the separation essence and carry out chromatography/wash-out, the high efficiency that had both kept chromatographic separation, stopped in leaching process, to introduce another possibility approach of pollutent again, thereby guaranteed the extreme high purity and the residual symbol International Drug standards that closes of pollutent of final finished from the outside; Puerarin purity 〉=98% of actual measurement final finished;

Any organic and inorganic soda acid is not used in technical process of the present invention, can not produce environmental pollution in the production process, does not use poisonous sorbent material, does not use inflammable, explosive material, safe and efficient, process optimization, and it is reasonable, simple and direct to be connected, and is easy to promote.

Embodiment: embodiment 1: get wild dried Pueraria lobota sheet, be ground into meal, → → add,, pure water soaked 10～20 hours under 50 ℃ of temperature, repeat 2～3 times, vat liquor is for several times collected together, sent into whizzer, collect supernatant fluid filtrate through the 1000rpm low-speed centrifugal, → supernatant fluid filtrate is made the high-temperature vacuum concentrating under reduced pressure at 125 ℃, slightly carried lotion, will slightly carry lotion and obtain 5% concentration crude extract with pure water dilution, → → crude extract is crossed molecular weight is 1000 dextrane gel molecular sieve chromatography, obtain adsorptive on the post, use the pure water wash-out, repeatedly twice, the smart lotion of carrying, → → in essence carried in the lotion and to be added 20% alcohol-water solution, under comparatively high temps, dissolve, place crystallization then at low temperatures, repeat twice, obtain moist crystallizate, → moist crystallizate is carried out drying and dehydrating, and to make content be the pure product of 98.6% powdery.

Embodiment 2: get wild dried Pueraria lobota sheet, be ground into meal, → → add,, pure water soaked 8～10 hours under 65 ℃ of temperature, repeat 2～3 times, vat liquor is for several times collected together, sent into whizzer, collect supernatant fluid filtrate through the 1000rpm low-speed centrifugal, → supernatant fluid filtrate is made the high-temperature vacuum concentrating under reduced pressure at 125 ℃, slightly carried lotion, will slightly carry lotion and obtain 5% concentration crude extract with pure water dilution, → → crude extract is crossed molecular weight is 800 dextrane gel molecular sieve chromatography, obtain adsorptive on the post, use the pure water wash-out, repeatedly twice, the smart lotion of carrying, → → in essence carried in the lotion and to be added 10% alcohol-water solution, under comparatively high temps, dissolve, place crystallization then at low temperatures, repeat twice, obtain moist crystallizate, → moist crystallizate is carried out drying and dehydrating, and to make content be the pure product of 98.2% powdery.

Claims (5)

1, a kind of novel process of extracting high purity puerarin by pure water method, be made up of in regular turn following flow process: raw material drying pulverizing → liquid phase is slightly put forward → is separated essence and carry → purifying powder process, the smart flow process of carrying of described separation is to adopt column chromatography/elution method of making filler with the dextrane gel molecular sieve, liquid phase is slightly carried the diluent of gained and made chromatography, elution, make essence and carry lotion, it is characterized in that the vat liquor that described liquid phase is slightly carried in the flow process is a water, liquid phase is slightly proposed the paste dissolves dilution for treating that chromatography diluent solvent for use is a water, and the liquid phase that wash-out adopted in described column chromatography/elution method is a water.

2, the novel process of extracting high purity puerarin by pure water method as claimed in claim 1 is characterized in that: the molecular weight of described dextrane gel molecular sieve is 800～1200.

3, the novel process of extracting high purity puerarin by pure water method as claimed in claim 1 or 2, it is characterized in that: described liquid phase is slightly put forward flow process and comprised in regular turn: temperature is soaked filtering separation operation, concentrating under reduced pressure operation, and described purifying flour mill flow comprises in regular turn: essence is put forward lotion recrystallization operation, dry powder process operation.

4, the novel process of extracting high purity puerarin by pure water method as claimed in claim 3, it is characterized in that: described temperature is soaked in the filtering separation operation, keep warm immersion liquid phase temperature at 40 ℃～65 ℃, filtering and collecting filter liquid adopts the further separating filtrate of low-speed centrifugation to get supernatant fluid filtrate; Described concentrating under reduced pressure operation is that controlled temperature is lower than 130 ℃ to 125 ℃, supernatant fluid filtrate is vacuumized and makes and slightly carry lotion, and then water will slightly to propose the paste dissolves dilution be that 5% diluent is treated chromatography; It is essence to be carried lotion to repeat two, three times be that 10%～20% alcohol-water solution makes moist crystallizate through the low temperature recrystallization with concentration that described essence is put forward lotion recrystallization operation; Described dry powder process operation is with the dehydration of gained moist crystallizate drying, makes the pure product of powdery.

5, the novel process of extracting high purity puerarin by pure water method as claimed in claim 4 is characterized in that: the liquid phase water that each flow process, operation adopted in the novel process of described extracting high purity puerarin by pure water method is pure water.