Investigation On Supercritical Anti-solvent Preparation And Equipment For Nanometer Particle Of The Camptochecin

This article to the camptotheca acuminata alkali nature, the anti-cancer mechanism, the nanometer research background and the supercritical fluid technology preparation ultramicro pellet research has carried on the synthesis elaboration and the analysis.The camptotheca acuminata alkali enemy pate tumor, the arm dim cancer and the leukemia and so on many kinds of malignant tumors have the curative effect Has the important physiological action and the clinical practice value, the camptotheca acuminata alkali and the derivative anti-cancer function mechanism is as affects the target take topological isomerase (Topol) to suppress DNA the synthesis, Many derivatives arise at the historic moment, become the anti-cancer domain research the new hot spot, at present camptotheca acuminata alkalis medicine oneself enters the clinical stage, and attains American food and the drugs administrative bureau FDA authorization, after becomes continues the anti-cancer active natural medicine which taxus mellow second is allowed to go on the market.The supercritical fluid technology, is the preparation ultra fine dust body material new method which the recent years proposed.Rapid Expansion of Supercritical Solution andSupercritical Anti-Solvent Crystallizatio is two research quite thorough methods.RESS and the SAS technology is two supplementary methods, the former needs the solute to have the good solubility in the supercritical fluid, the latter request insoluble or the solubility is very small in the supercritical fluid.This article mainly conducts the research to the supercritical fluid anti-solvent crystallization technology.It pollutes slightly, the condition is flexible, to the biological activity strong, the temperature sensitive and so on the materials is suitable especially, in the chemical industry, the bio-engineering, the medical service and the drugs manufacture and so on each domain has the widespread application prospect.But its equipment aspect, Shang You were very many the place which needed to improve enhances.Through a SAS process preparation camptotheca acuminata alkali nanometer particle, carries on the optimization to equipment each part, regarding this parameters and so on in process temperature, pressure, spray nozzle diameter carry on the exploration, developed the quite advanced supercritical fluid anti-solvent crystallization technology to prepare the ultra refinement equipment, has grasped various parameters to the particle shape, the particle size and the grain-size distribution influence rule.And used the entire filter diaphragm sample deliquescent material tube, has been possible the continual specimen handling negative pressure automatic specimen handling and the double dissolved cauldron system, aspect and so on receive spot cyclone collector equipment transformations.Has formed the technological breakthrough and the innovation superiority.In camptotheca acuminata alkali SAS preparation process,Carries on screening desolvation method condition and the light microscope, the atomic force microscope, the Fourier infrared spectroscope and the X-ray meter through the orthogonal experiment, according to the time and so on the major effect factor and through the camptotheca acuminata alkali physico-chemical properties which known and examines, has carried on 4 factor 5 level 16 experiments, most completion of three year mourning period for one's parents smallest 390 nanometer particles,And utilizes returns gradually carries on the regression analysis determination equation to 16 experimental point response value the regression coefficient.The orthogonal experiment has determined the best preparation condition: Solution concentration 3.75mg/ml, feeding speed of flow 15ml/min, crystallizes the cauldron temperature 57°C, crystallizes cauldron pressure 15Mpa, spray nozzle aperture 300nm.And obtains the confirmation after the experiment.Rate and the solvent returns-ratio conduct the research through the orthogonal experiment and the variance analysis to the nanometer camptotheca acuminata alkali powder body.Determined various factors are superior to the level combination: Solution concentration 2.5mg/ml, feeding speed of flow 30ml/min, crystallizes the cauldron temperature 46°C, crystallizes cauldron pressure 25Mpa, spray nozzle aperture 150nm, the solvent returns-ratio is A₂B₂C₁D₃E₁:Solution concentration 2.5mg/ml, feeding speed of flow 15ml/min, crystallizes the cauldron temperature 35°C, crystallizes cauldron pressure 20Mpa, spray nozzle aperture 150nm.Simultaneously may see the nanometer camptotheca acuminata alkali powder body rate high is equally 97.65%, the solvent returns-ratio is high equally is 96.67%, also obtains the experiment to confirm.After the infrared spectrum examination, the LC/MS/MS examination, the X-Ray test, the camptotheca acuminata alkali bulk density research discovered that,The nanometer around camptotheca acuminata alkali functional group structure change, its chemical property have not had the change;After the nanometer camptotheca acuminata alkali molecular structure has not changed; After the nanometer camptotheca acuminata alkali powder body crystallinity had to be lower than the primitive camptotheca acuminata alkali is far the camptotheca acuminata alkali particle size changes small has caused the crystal structure change; After the primitive camptotheca acuminata alkali bulk density is nanometer sample bulk density 19.98 times.After this article research, prepared the ultra fine dust body for the camptotheca acuminata alkali supercritical anti-solvent crystallization to provide the essential data foundation data, applied for the supercritical anti-solvent crystallization technology in the actual production, has provided the model.