CN101125126A - Method for preparing medical freeze-dried powder (injection) preparation - Google Patents
Method for preparing medical freeze-dried powder (injection) preparation Download PDFInfo
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- CN101125126A CN101125126A CNA2006100104097A CN200610010409A CN101125126A CN 101125126 A CN101125126 A CN 101125126A CN A2006100104097 A CNA2006100104097 A CN A2006100104097A CN 200610010409 A CN200610010409 A CN 200610010409A CN 101125126 A CN101125126 A CN 101125126A
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Abstract
The present invention aims at adding energy for the liquid water and /or solid water ingeniously from multi-angle and providing a new perspective which is conductive to the escape of the water molecules from the solid ice, the present invention starts from the four angles of ultrasonic disruption, infrared energy adding, microwave activating and magnetization processing, introduces the advantages and the characteristics of the magnetized water, small water molecule clusters and high-energy water into the medical frozen powder (injection) preparations which are produced industrially in a most economical method and to the maximum extend, so as to explore a new path for shortening the production cycle of the normal vacuum frozen drying and further reducing the energy consumption. On the basis, the present invention also provides: a preparation method of medical frozen powder (injection) preparations by infrared vacuum frozen drying, a preparation method of medical frozen powder (injection) preparations by microwave vacuum frozen drying etc.. The two new methods completely overcome the deficiencies of the single channel for transferring the energy of the traditional vacuum frozen drying and can possibly further greatly shorten the production period of the industrial production of the medical frozen powder (injection) preparations, reduce the energy consumption and improve the inherent quality of the products.
Description
Technical field
The present invention relates to the preparation method of a kind of medical lyophilized powder (pin) preparation, belong to field of pharmaceutical preparations.
Background technology
The powder medicine of vacuum lyophilization is compared with aqueous solvent medicine (as Blood Preparations, antibiotics, antitoxin, hormone, strain, live biological product and Chinese patent medicines such as malicious vaccine, cancer therapy drug), have: 1) a little less than the enzymology effect, original chemistry, physiological property are stablized; 2) can restore after adding water, be convenient to long-distance transport and preserve; 3) storage life can extend to the several years from several weeks or several months; 4) the energy accurate quantification in automatic packer of the aqueous solution before the medicine drying; 5) dry production process sterilizationization is easy, can the strict advantages such as asepticize of controlling batch pharmacy container and personnel.
Compare with the exsiccant powder of alternate manner (pin) agent and to have: stable in properties, the advantage that quality is good, active constituent content is high, rapid-action, bioavailability is high.
But, thereby because there are long, shortcomings such as energy consumption is high, the per unit area yield ability is little, production cost height of production cycle in Freeze Drying Technique. limited its extensive use.
For the analysis problem, improve operant level, shorten the production cycle, cut down the consumption of energy A Likan: brief talk Vacuum Freezing ﹠ Drying Technology. vacuum. (J) .2002, (4): as described below the boosting and the facing a difficult choice of blood pressure lowering that has provided existing vacuum lyophilization in 43～45:
" 2.2.3 sublimation stage pressure
In sublimation process, not only shelf temperature needs control, and the storehouse internal pressure also is the parameter that needs control.Lyophilizing storehouse pressure size influences the heat and mass of sublimation drying process.The pressure height, heat-transfer effect is good, but is unfavorable for the effusion of water vapour.Pressure is low, and heat-transfer effect is poor, helps the effusion of water vapour. and whole sublimation process is exactly a heat and mass transfer process, has only pressure suitable, and an economic dry rate just can be arranged.
When sublimation temperature is constant, when the storehouse internal pressure was lower than certain value, pressure reduced rate of sublimation and also no longer increases.And sublimation pressure is when low, and the heat exchange weak effect just needs high shelf temperature for identical heat is provided.We know that high shelf temperature causes the thawing disintegrate of material easily the front.Usually should pressure be controlled at a little less than the highest sublimation temperature 1/2nd force value of corresponding saturated vapor pressure be dryness storehouse inner control pressure.Generally between 30～90Pa.For example the material sublimation temperature is that its saturated vapor pressure of subzero 20c. is 103.5Pa, and the dryness storehouse internal pressure should be controlled at 52Pa.”
At aforesaid dilemma, Zhao Lanping etc. in freezing process and cryodesiccated relation. cryogenic engineering .1999, (4): provide the approach that improves dry rate in 105～108:
" 4 improve the approach of dry rate
The center of the energy-saving and cost-reducing research of lyophilization is to shorten drying time, just improves dry rate.Optimum pressure method, circulating pressure method, pressure and to add heat Comprehensive Control method and reduce the condensation vapor actuator temperature be the conventional route that improves speed.And freezing process is taken into account, also be one of energy-conservation approach of lyophilization.By analysis above. we find: before drying. strike off the product surface enriched layer, can reduce steam and transmit resistance; Under the prerequisite of ensuring the quality of products, the fltting speed and the thermograde of frozen interface make the ice crystal size big as far as possible in the control freezing process, can improve dry rate.
Because people are not clear to the understanding of freezing dynamic process, want to improve dry rate by optimizing freezing process, just need do more deep research to freezing process.”
" magnetic treatment of water system " (Soviet Union) B.N. carat suffering: JIUYUE was the 1st edition in 1988, the 83rd page " result shows that the evaporation rate of magnetized water is higher by 11% than the evaporation rate of untreated water ".Can see that magnetic water is twice than the crystallization weight of unmagnetized water in the 84th page " having shortened 25～40% " and the chart at this page at the crystallization time that permanent magnetic field Zhong Shui becomes ice.
Relevant patent:
CN1124988C activated medical water, Preparation Method And The Use, it is less to the invention discloses a kind of water clusters, the dissolving power of water, penetration, expansionary force, metabolism power, cleaning strength all is better than the activated medical water of medical distilled water, it is through IDM activated water system by medical distilled water, the TKY activated water is handled, form after ultrasonic atomizatio processing and the magnetization processing, diluent and drug solvent that this type of activated medical water can be used as injection use, also can be used as physiological regulation agent, aesthetic health care water and medical water for cleaning, more original like product has more biological activity, the aquatic reason that meets human body changes, and is a kind of medical water of novel concept.
Patent CN1124988C introduces distilled water with the idea of magnetic water, small-micelle water, high energy water gaging, and possesses the serial advantage described in the above-mentioned patent abstract.But the activated medical water that this patent is produced is applicable in hospital, beauty parlor and uses, and is not suitable in the medical industry of producing various liquid pharmaceutical formulations and uses.Its reason has two, at first, during the treatment technology IDM activated water system of complete activated medical water, the processing of TKY activated water, ultrasonic atomizatio processing and magnetization were handled among the patent CN1124988C, two core technologies (50%) such as IDM activated water system, the processing of TKY activated water were because the charged production that can not be directly used in the liquid medicine dosage form; In addition, in the production process of each liquid dosage form of medical industry, heating hydrotropy, the heat sterilization preparation technology that is absolutely necessary.Yet in this requisite temperature was higher than 60 ℃ technical process, the various characteristics of the activated medical water that the CN1124988C patent is produced and advantage were with all gone.
CN200320107364.7 has the extraradial vacuum freeze drier of the double-sided red of fortified water flow of vapor, has changed mode of heating, and then has accelerated sublimation drying speed, has shortened drying time.
The retrieval Chinese patent database, we can find infra-red radiation is used for only this of the patent application of vacuum freeze.Yet, infra-red radiation is used for common exsiccant patent application truly has 385.Researcher of the present invention thinks that its technical impassable reason is necessarily arranged, and the inventor of above-mentioned patent may not break through on this problem yet yet.
CN03249124.7 is used for the microwave freeze-drying equipment of food production, the processing and fabricating method of CN03134811.4 lyophilized instant face and microwave freeze-drying equipment thereof; Can be shortened 5～6 times the arid cycle of food, reduce the cost of large-scale production.
It is not unique, but has its counterpart, the retrieval Chinese patent database, and we can find microwave radiation is used for only these two of the patent applications of vacuum freeze, but also are same individual application's.Yet, microwave radiation is used for common exsiccant patent application truly has 1366, presumably this anything but people ignored microwave and combined with cryodesiccated, its technical impassable reason is necessarily also arranged, and the inventor of above-mentioned patent may not break through on this problem yet yet.
Researcher of the present invention is found after deliberation:
1, to be used for the impassable technology barrier of vacuum freeze be under the prior art condition to infra-red radiation, will seriously influence the refrigerating effect of freeze drying equipment behind the shelf coating infrared radiation coating.Its reason is, in cryodesiccated pre-freeze process, heat energy in material and the environment reaches shelf by transmission, make the infrared radiation coating that is coated with on the shelf obtain energy and send infra-red radiation, because the metal shelf reflects fully to infra-red radiation, so the energy that infrared radiation coating obtained that is coated with on the shelf is reflected back toward completely again and will carries out in the system of pre-freeze.
2, microwave radiation is used for the impassable technology barrier of vacuum freeze and is, (1), will freeze metal tube and heating metal pipe of traditional vacuum freeze drying equipment places in the stainless steel metal shelf, this is the scheme of saving the energy most, also be that freeze drying equipment can be accomplished the precondition of cooling rapidly, yet for microwave, the total reflection of metal pair microwave, the serious lyophilization shelf of not supporting forms the multiple structure of thing frame, can cause serious heat skewness, be unsuitable for industrialized great production, this is a pair of insoluble contradiction.(2), CN03249124.7, CN03134811.4 be the same with common microwave stove, the incorrect heat skewness that causes of mode that microwave adds.The existing uneven basic reason of microwave heating is, the in-position of microwave is arranged on the top that is lined with metallic walls, and/or both sides; Should be in the big multiplayer microwave vacuum freeze of producing based on both sides.After microwave magnetron new ray in both sides sends, be heated in the process of material in process, the energy of microwave radiation is the state that is in decay.Add the fully reflection of the interior metallic walls of stove to microwave, the ray that at every turn reflexes on the peripheral material all is equivalent to unbated new ray, and just energy may be smaller.What intermediary material received at the beginning is exactly by the ray after the peripheral material decay, and " the new ray " that the metal wall is produced reflecting fully of microwave in the stove also will just can arrive at place, material place, center through after the peripheral material attenuation by absorption.Cause peripheral temperature of charge height, the center temperature of charge is low, and this result's generation is inevitable.
Researcher of the present invention has been decoded after deliberation and has been produced the reason of The above results, and has applied for ' can be used for the microwave vacuum freeze-drying device that food and medicine is produced ', ' infra-red radiation vacuum freeze ' two patent that can be used for food and medicine production already.
Summary of the invention
The objective of the invention is to stand in multi-angle cleverly for aqueous water and/or solid water add can, help the brand-new visual angle that hydrone is escaped from solid ice, solve the difficult problems such as production cycle length, energy consumption height of medical lyophilized powder (pin) agent suitability for industrialized production.
The preparation method of a kind of medical lyophilized powder of the present invention (pin) agent, it is characterized in that, the present invention for the production cycle, the energy consumption that reduces medical lyophilized powder (pin) agent that further shorten medical lyophilized powder (pin) agent, improve the product interior quality of medical lyophilized powder (pin) agent, providing on the basis of method that the conventional vacuum freeze drying equipment prepares medical lyophilized powder (pin) agent, provide the method that brand-new lyophilization prepares medical lyophilized powder (pin) agent;
Wherein, the brand-new lyophilization method for preparing medical lyophilized powder (pin) agent comprises:
Infrared vacuum lyophilization prepares the method for medical lyophilized powder (pin) agent;
The method of the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent.
1, at the preparation method of the medical lyophilized powder of the old equipment of tradition (pin) agent:
Researcher of the present invention is found by a large amount of document of research, by ultrasonication, infrared add can, microwave intensifies and handle formed small-micelle water, high energy water gaging, and is very close be magnetized physical property and the biology performance of handling the formed magnetic water in back, small-micelle water, high energy water gaging of light water.
Use the conventional vacuum freeze drying equipment to produce the benefit of lyophilized powder (pin) agent enterprise for above-mentioned discovery is become, the present invention has done following improvement to the liquid preparation preparation technology of predecessor of medical lyophilized powder (pin) agent:
The present invention is under the prerequisite of the predecessor's liquid preparation technology in early stage that does not change medical lyophilized powder (pin) agent substantially, after the operation that liquid preparation need heat all early stages has been finished, or before just the medicinal liquid branch installs in the commercially available packing container shortly, in fluid reservoir, in fluid reservoir medicinal liquid circulation line and/or in fluid reservoir and pipeline that fluid reservoir links to each other and/or in fluid reservoir and pipeline that racking machine links to each other and/or in the pipeline at racking machine, to medicinal liquid carry out ultrasonication, infrared add can, activation processing such as microwave intensifies, magnetization is handled.Liquid preparation after the processing places the cold degree drying equipment of conventional vacuum to carry out the well-established law drying, can produce the effect that shortens the production cycle, cuts down the consumption of energy.If in the cold degree drying equipment of traditional vacuum shelf, be added with alnico magnets the material of pre-freeze stage, sublimation stage is magnetized effect can be better.
Wherein:
Ultrasonication: be to adopt the ultrasonication technology under the prerequisite of not destroying effective ingredient in the solution, destroy original liquefaction crystal that macromolecular mass constituted that is wrapped in the water of effective ingredient outside, make it to become the liquefaction crystal of small-micelle water.
Infrared add can: be to adopt infrared technique to produce to be described as the radiation best band of light (consistent) of life at 5～18 microns infrared ray with 9.6 microns of body surface radiation wavelengths by medical circle, produce resonance with the hydrone in the solution, big hydrone group is further diminished.Simultaneously, the energy frequency spectrum of memory in liquid crystal state water has the raising body immunity, the health-care effect that enhances metabolism.
Microwave intensifies: be the high speed concussion that utilizes microwave to intensify, give bulk macromole energy, make it division, form small-micelle water.
Magnetization is handled: by liquid perpendicular cuts magnetic line of force in magnetic field, further promote the energy grade of hydrone, make it form little and stable liquid crystal state small water molecule group, the dissolving power that further promotes liquid preparation self further improves the general curative effect of liquid preparation with stability, further promote liquid preparation at the intravital penetration of machine, expansionary force.
In said method, ultrasonication, infrared add can, four kinds of processing modes such as microwave intensifies, magnetization is handled, each can shorten the freeze-off time of handling the back medicinal liquid, increases the ice crystal size, helps hydrone the finishing smoothly of (promptly distilling) of escaping from solid ice; Four kinds of processing modes can be used separately respectively, more preferably be used in combination according to the difference of the effective ingredient of product.
2, at the preparation method of the medical lyophilized powder of novel device (pin) agent
Another contribution of the present invention is, uses infrared vacuum freeze, microwave vacuum freeze-drying device prepares medical lyophilized powder (pin) agent.
Wherein:
(1), when application new infrared vacuum freeze is produced medical lyophilized powder (pin) agent, because the new infrared vacuum freeze has replaced to the kernel of cool chamber can absorb by metal material, see through, launch ultrared heat-conducting plastic, thermal conductive ceramic, the heat conduction glass material, got through the path of heat energy infra-red radiation, can be under low pressure or under the ultralow pressure, directly provide energy by infra-red radiation to material inside, make the hydrone distillation rapidly simultaneously in the material inside and outside portion ice crystal, bring following many differences for the production overall process of medical lyophilized powder (pin) agent:
A, in the pre-freeze stage, the pallet that material layering is put into infrared vacuum freeze is arranged full in an orderly manner, closes hatch door, opens the pre-freeze valve and makes low temperature silicone oil enter system, and material is carried out pre-freeze.At this moment, the heat energy in the material will enter in the subzero silicone oil below-55 ℃ by conduction of heat, two approach of infra-red radiation via the path of material → pallet → shelf → heat pipe → silicone oil, and the low temperature silicone oil that is recycled is taken away.
In this process, the part near infrared ray that pallet gives out sees through the radiation that aqueous solution produced of vial to pre-freeze, have to make it form the effect of small-micelle water, help shortening freeze-off time, help scars and form big crystallization, help carrying out smoothly of next step distillation.
When temperature of charge drops to subzero 20～50 ℃, the operation that enters next stage.
B, sublimation stage, start vacuum pump, make that vacuum remains on 5～80Pa in the storehouse, change freezing silicone oil into hot silicone oil and via the path of silicone oil → heat pipe → shelf → pallet → material, a large amount of heat energy in the silicone oil is passed through conduction of heat, two approach of infra-red radiation, enter temperature in subzero 20～50 ℃ material, make hydrone in the material inside and outside portion ice crystal obtain energy simultaneously and distil.
Conduction of heat via silicone oil → heat pipe → shelf → pallet → material path can make rate of sublimation reach the cryodesiccated level of conventional vacuum; Can penetrate vial from the near infra-red thermal radiation that shelf, pallet produced heats material inside and outside losslessly simultaneously.Thereby can shorten the consuming time of sublimation stage greatly, reduce the power consumption of sublimation stage greatly.
When temperature of charge leveled off to zero degree, sublimation stage finished.
C, desorption phase, icing because of not existing in the material, product temperature can rise rapidly up to the highest permissive temperature to product.In this process, to constantly reduce the temperature of silicone oil or turn the flow of silicone oil down, and when reaching the highest permissive temperature of product, keep a period of time, the water that makes bound water and be adsorbed in the drying layer obtains enough energy, from Molecular Adsorption, desorb, finish the overall process of the infrared vacuum lyophilization of medical lyophilized powder (pin) agent.
The whole story of three phases operations such as above-mentioned pre-freeze, distillation, desorbing, can judge by temperature, also can judge by the pressure reduction in vacuum pressure in the storehouse or two storehouses.
(2), when application novel microwave radiation heating vacuum freeze is produced medical lyophilized powder (pin) agent, because the following characteristic that novel freeze drying equipment had:
A, main microwave heating source is arranged on do not have the material of metallic walls center
Refrigerator pipes in b, the shelf 6, auxilliary heating tube, shelf, pallet is made by heat-conducting plastic, heat conduction glass, the thermal conductive ceramic of the anti-microwave that does not absorb microwave radiation energy; Made by plastics, glass, the ceramic material of the anti-microwave that does not absorb microwave radiation energy in crane main body, the built-in microwave magnetron supporter every, microwave magnetron supporter, the refrigerator pipes that links to each other with microwave magnetron.
C, the present invention introduce vacuum freeze with the infrared ray sensor technology, infrared sensor 5 is in the production overall process of cryodesiccated pre-freeze stage, sublimation stage, desorption phase, temperature to the material surface is carried out real-time sensing, and the fair supply of energy is adjusted in real time, controlled by voltage by the preset program of micro computer.
The path of heat energy microwave radiation has been got through in above-mentioned change, can be under low pressure or under the ultralow pressure, directly provide energy by microwave radiation to material, and make the hydrone distillation rapidly simultaneously in the material inside and outside portion ice crystal.Increase the real-time control of the real-time sensing and the micro computer of infrared sensor simultaneously, compared for the production overall process of medical lyophilized powder (pin) agent to bring with traditional lyophilization many different, seen the following specific embodiment for details.
Comparable advantage
The preparation method of a kind of medical lyophilized powder of the present invention (pin) agent, from ultrasonication, infrared add can, microwave intensify, magnetize the processing four angles start with, in the hope of to greatest extent magnetic water, small-micelle water, high energy water gaging advantage and characteristics being introduced in medical lyophilized powder (pin) agent of suitability for industrialized production with economic way, for shortening the cryodesiccated production cycle of conventional vacuum, further cut down the consumption of energy and opened up a new road.On this basis, the present invention gives: infrared vacuum lyophilization prepares the method for medical lyophilized powder (pin) agent, two kinds of new method such as method of the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent.Two kinds of new method overcome has fully fallen the single pass deficiency of traditional vacuum lyophilization energy delivery, has broken through the pressure height of normal freeze-drying, and heat-transfer effect is good, but is unfavorable for the effusion of water vapour; Pressure is low, and heat-transfer effect is poor, helps the facing a difficult choice of effusion of water vapour.Make production cycle, the energy consumption that reduces medical lyophilized powder (pin) agent that further significantly shortens medical lyophilized powder (pin) agent, the product interior quality that improves medical lyophilized powder (pin) agent become possibility.
The specific embodiment
For further specifying the present invention, not limited provide following kind of the present invention and the embodiment of being suitable for:
Embodiment 1, the scope of application of the present invention
The present invention is applicable to any lyophilization that needs, and need in freezing dry process to use that method of the present invention further improves the product interior quality, further shortens the production cycle, the medical freeze dried powder that further cuts down the consumption of energy, medical lyophilized injectable powder.Be example now with medical lyophilized injectable powder; not limited provide the following kind of the present invention that is suitable for: acyclovir; azithromycin; oxaliplatin; Omeprazole Sodium; aztreonam; amifostine; amrinone; atracurium besilate; sodium ozagrel; sodium ferulate; ornidazole; tranexamic acid; aminomethylbenzoic acid; the azithromycin sodium dihydrogen phosphate; aminobutyric acid; sodium ampicillin; amipicloxacillin sodium; Aspirin-arginin; arfonad; amycin; aklavine; amrinone; oxiracetam; hyaluronidase, sodium phenobarbital, phenytoin Sodium; the Gallate propyl ester; white-browed snake venom blood coagulation enzyme, C14H25N4NaO11P2, alarelin; the C14H25N4NaO11P2 inosine; alanyl glutamine, bumetanide, betamethasone sodium phosphate; benzathine benzylpenicillin; bristopen, bleomycin, epirubicin; cloth Salmonella live vaccine; interleukin, Radix Isatidis, recombination human interleukin-2; recombined human granulocyte-macrophage stimulating factors; the recombinant human somatropin, hepatocyte growth-promoting factors, Andrographolide; recombinant mutant human tumor necrosis factor; vinpocetine, thyroliberin, octreotide acetate; Vinorelbine monotartrate; bulleyaconitine A, superoxide dismutase, vincaleucoblastine; Radix Et Caulis Acanthopanacis Senticosi; Rhizoma Dioscoreae Nipponicae, andrographolide, Radix Bupleuri; DANHONG; to Aminosalicylic sodium, isosorbide mononitrate, breviscapine; low molecular weight heparin sodium; Radix Salviae Miltiorrhizae, single phosphoric acid cytosine arabinoside, dacarbazine; docetaxel; salvianolate, doxofylline, dexamethasone sodium phosphate; scopolamine butylbromide; various trace elements (II), dacarbazine, pralidoxime iodide; dopamine; Pheretima, sodium tanshinone IIA sulfate, polyene phosphatidylcholine; Calcium Dibutyryladenosine Cyclophosph-ate; diprophylline, diacetayl amide acetic ethylenediamine, dimercaptosuccinic acid; Oleum Curcumae; coenzyme A, fluorine cytidine, actinomycin D; fleroxacin; famotidine, Venenum apis, Coenzyme Complex; compound three-vitamines B; sodium amidotrizoate, etamsylate, fluconazol; fluorouracil; compound monoammonium glycyrrhizinate S, floxuridine, sodium fusidate; fotemustine; voriconazole, compound diisopropylamine dichloroacetate, SNMC; furosemide; floxapenstaphylex, furbenicillin, compound quinine; Compound recipe Radix Isatidis; coenzyme Q10, compound recipe methionine-vitamin B 1, Fructose Diphosphate sodium; gonadorelin; puerarin, CMNa, Carbamaid peroxide; mannatide; ganciclovir, bone peptide, norfloxacin glutamate; adenosine cyclophosphate; homoharringtonine, glycyrrhizic acid diamidogen, fructose; bone-melon extract; Kaglutam, calciparine, bacitracin; glucagon; interferon, dactinomycin, mithramycin; glutathione; mannomustin, cyclophosphamide, reduced glutathion; ribonucleic acid; adenosine cyclophosphate, sulfomercaprine sodium, meglumine adenosine cycle phosphate; astragalus polysaccharides; Carthamus yellow, riboflavin sodium phosphate, kedacillin; nootkatin; ribostamycin, ancitabine, sulfatodiamino cyclohexane platinum; erythromycin; the Radix Astragali, Radix Illicii Lanceolati, methotrexate; the metronidazole sodium phosphate; the methoxy isonitrile, Urbason Solubile, phentolamine mesylate; pefloxacin mesilate; pentoxifylline, sodium citrate, collagenase; Gatifloxacin; Kitasamycin tartrate, inosine, spectinomycin hydrochloride; mecobalamin; Pazufloxacin Mesilate, sarcosine peptide aglycone, methionine vitamin B 1; gabexate mesilate; s-ropivacaine mesylate, phloroglucinol, thiamphenicol; kitasamycin tartrate; formyl hydrogen Calcium Folinate-SF, influenza A vaccine, old tuberculin; dihydroergotoxine methanesulfonate; cimetidine, methyl prednisone sodium succinate, human normal plasma; refined tetanus antitoxin; refined diphtheria antitoxin, Antirobies Serum, Flos Trollii; clindamycin phosphate; carboplatin, Cobratide, bacillus calmette-guerin vaccine; anti-hepatitis B immune ribonucleic acid; kurarinone, matrine, captopril; carbazochrome sodium sulfonate; card nitrogen is situated between bekanamycin, antilymphocyte globulin; rabies vaccine; AT 581., BCG-polysaccharide nucleic acid, Netilmicin Sulfate; aspisol; kanamycin sulfate, amikacin sulfate, Vistamycin; the plain sodium of phosphorus enzyme; sodium prasterone sulfate, Azithromycin Sulfate, vindesine sulfate; vincristine sulfate; tiopronin, sodium thiosulfate, kangdisu sulfas; amphotericin B; penthiobarbital, Etimicin sulfate., Bacterium prodigiosum polysaccharide; capreomycin sulfate Capastat sulfate; aerosporin, chondroitin sulfate, AM Bison; terbutaline sulphate; ligustrazine phosphate, lecithin, Micronomicin Sulfate; foscarnet sodium; lornoxicam, rifampicin, phosphoric acid etoposide; rifamicina; armillarisin A, fludarabine phosphate, cervus and cucumis polypeptide; Long Ruikelin; potassium chloride, cloxacillin sodium, streptomycin sulfate; amikacin sulfate; the sulphuric acid oleandomycin, many glutinosins of sulphuric acid E, sulphuric acid AEROSPORIN; vinblastine sulfate;, Clomipramine, fosfomycin sodium; meclofenoxane; aspisol, streptokinase, prodigiosin; streptomycin; ethacrynate sodium, malaridine, ribavirin; Roxithromycin; ropivacaine, asparaginase, maleic acid Archie enzyme element; meropenem; Chymotrypsin, mezlocillin sulbactam sodium, motassium magnessium aspartate; aspartic acid ornithine; Mycophenolate Mofetil, asparaginase, thioctic acid; xylitol; Chymotrypsin, Trypsin-chymotrypsin, chymopapain; immune ribonucleic acid; nimustine, metadoxine, milrinone; Moxifloxacin; urokinase, brain heart health, nedaplatin; nicergoline; menotrophin, naproxen sodium, carbamide; Clistin-M Vial; Energy mixture, meningococcal polysaccharide vaccin, Cerebrolysin Vial; nimodipine; nizatidine, Protirelin, Pantoprazole Sodium; pamidronic acid acyl disodium; piracetam, sodium glucuronate, Enoxacin Gluconate; pemetrexed disodium; the Pamidronic Acid disodium, procaine benzylpenicillin, avocin; piperazine ketone sodium; Bleomycin A5, pirenzepine, dandelion; aescine; hydrocortisone sodium succinate, Alprostadil, dianhydrodulcitol; hydroxycamptothecin; mouse nerve growth factor, QINGKAILING, troxerutin; lappaconitine hydrobromide; Injectio natarii norcantharidatis, benzylpenicillin potassium, penicillin sodium; rolitetracycline; rolitetracycline nitrate, globoroseomycin, penicillin; the zinc hydroxide thyroliberin; gentamycin, penicillinase, dextromethorphan hydrobromide; erythromycin lactobionate; chorionic gonadotrophin, ethacridine lactate, reteplase; zidovudine; Norfloxacin Lactate, Rui Sixi butyl hydrogen sulphate salt, chorionic gonadotrophin; daunorubicin; sarcolycin, lactobionic acid azithromycin, lysozyme; the human albumin; blood albumin of human placenta, human, human fiber's proteinogen; adenosine triphosphate disodium salt; cisplatin, water soluble vitamins, ethylenedicysteine; SHUANGHUANLIAN; ethyl cysteinate dimer, sulbactam sodium, adenosine triphosphate coenzyme insulin; somatostatin; dipyridamole, oxytocin, diclofenac sodium lignocaine; huperzine A; along the benzenesulfonic acid atracurium, hetacillin potassium, carboxylic benzyl sodium penem; licarcillin sodium; thiophene oxime sodium, dibekacin, streptokinase-streptodornase; Calcium Dibutyryladenosine Cyclophosph-ate; adenosine triphosphate, GTP (guanosine triphosphate), cytidine; harringtonine; sultopride is given birth to arteries and veins, arsenic trioxide; Moschus; hirudin, ftorafur impersonates the Lamine; cefonicid sodium; placental lipo-glucosaminoglycan, gastrodine, cefpiramide; cephalothin sodium; Elastase, cefaloridine, cefazolin sodium; cefradine, cefacetrile sodium.Cephapirin sodium, cefathiamidine, cefuroxime, cefoxitin, cefotiam, ceftazidime, cefotaxime, cefmenoxime, cefsulodine sodium, cefmetazole, parotin, carboplatin, sodium bicarbonate, cefamandole nafate, torasemide, Ro 15-8074/001, ketone Lip river phenol, salmon calcitonin see calcimar, ulinastatin, vitamin B6, vecuronium bromide, vitamin C, cytochrome C, thymosin, lentinan, neoarsphenamine, XUESAITONG, nitrocaphane, cobamamide, sodium nitroprusside, angiotensin, Thymopentin, cimetidine, neo-houttuyninum, asarone, calf blood protein-removed extraction, antostab, fibrinoclase, thymosin, ametycin, nitrocaphanum, sorbide nitrate, nifedipine, energy fruit acid, scorpion venom, Herba Saussureae Involueratae, cidofovir, Amiodarone Hydrochloride, the human normal immunoglobulin, gemcitabine hydrochloride, tetracaine hydrochloride, spectinomycin hydrochloride, norvancomycin hydrochloride, ofloxacin, kallidinogenase, levofloxacin hydrochloride, mitoxantrone hydrochloride, Ondansetron Hydrochloride, calcium folinate, inferior stannum sodium phytate, methylenediphsphonate and stannous chloride, inferior stannum gluceptate sodium, inferior stannum pentetic acid, sodium pyrophosphate and stannous chloride, aprotinin, lomefloxacin hydrochloride, Buflomedil Hydrochloride, cefotiam hydrochloride is fixed, meclofenoxate hydrochloride, quadracycline, topotecan hydrochloride, inferior stannum sodium dimercaptosuccinate, inferior stannum Dextran 10 5, inferior stannous gluconate acid calcium, isoniazid, cytarabine hydrochloride, Retilian Simplex, irinotecan hydrochloride, ketalar, the how gentle pyrrole star of andrographolide, Antiradon, hydrochloric acid, ifosfamide, remifentanil hydrochloride, Betahistine Hydrochloride, the different dried meat of inferior stannum methoxy, ligustrazine hydrochloride, the ethamine uride, diltiazem hydrochloride, verapamil hydrochloride, dopamine hydrochloride, divalvon-D, esmolol hydrochloride, idarubicin hydrochloride, nicotinic acid, nicotiamide, sodium etacrynate, aceglutamide, hydrochloric acid replaces fourth for the Buddhist nun, dimefline hydrochloride, nefopam hydrochloride, Boanmycin Hydrochloride, Nimustine, lysine hydrochloride, tramadol hydrochloride, inferior stannum etifenin, indole Pu is green, sotalol hydrochloride, hydrochloric acid glucagon, Granisetron Hydrochloride, Bisolvon, Ramosetron HCl, arginine hydrochloride, Arterenol (Hoechst)., labetalol hydrochloride, Tiapride Hydrchloride, ambroxol hydrochloride, naloxone hydrochloride, papaverin hydrochloride, doxapram hydrochloride, Imipenem-cilastatin sodium, Propacetamol Hydrochloride, dexrazoxane, etoposide, Dextran 40, hydrochloric acid is for how non-class, Navoban (Soz), hydrochloric acid horse traction ground that, folic acid, abadox, minocycline hydrochloride, Lyphocin (Fujisawa), methylphenidate hydrochloride, procaine hydrochloride, clonidine hydrochloride, dobutamine hydrochloride, hydrochloric acid vidarabine, edetate sodium, ciprofloxacin, insulin, trypsin, hydrochloric acid L-cysteine, Lumbrukinase, hydrochloric acid Ni Keli is fixed, Sodium Houttuyfonate, bilobalide, minocycline hydrochloride, Incadronate, mattress Cape jasmine Huang, leucovorin sodium, Herba Houttuyniae, itraconazole, Flos Chrysanthemi Indici, Radix Curcumae, the U.S. phenol of hydrochloric acid sodium, transfer factor, Paclitaxel liposome, propylene glycol alginate sodium sulfate, levocarnitine, zoledronic acid, fatsoluble vitamin, Nulomoline, phytohaemagglutinin, polyporusum bellatus, levo-potassium magnesium aspartate, left cloth Buddhist nun caine.
The activation processing of embodiment 2, liquid preparation
The present invention is under the prerequisite of the predecessor's liquid preparation technology in early stage that does not change medical lyophilized powder (pin) agent substantially, after the operation that liquid preparation need heat all early stages has been finished, or before just the medicinal liquid branch installs in the commercially available packing container shortly, in fluid reservoir, in fluid reservoir medicinal liquid circulation line, and/or in fluid reservoir and pipeline that fluid reservoir links to each other, and/or in fluid reservoir and pipeline that racking machine links to each other, and/or in the pipeline of racking machine, medicinal liquid is carried out ultrasonication, infrared adding, can, microwave intensifies, the activation processing that waits one or more is handled in magnetization.The cryodesiccated production cycle of conventional vacuum is shortened more than 10%, and energy consumption reduces more than 15%.
Embodiment 3, microwave vacuum freeze seasoning prepare medical lyophilized powder (pin) agent
The liquid preparation that branch is installed places microwave vacuum freeze-drying device, open refrigerating plant, when material surface temperature during near zero degree, open 1～5 second of microwave radiation, make the macromolecular mass water in the aqueous solution become small-micelle water, help shortening freeze-off time, help scars and form big crystallization, help carrying out smoothly of next step distillation.Continue pre-freeze, make predrying material be cooled to subzero 20～50 ℃ rapidly, the pre-freeze of finishing material.
Sublimation stage starts vacuum pump, makes that vacuum remains on 5～80Pa in the storehouse in, and starting main heating source is microwave magnetron, and material is carried out the high-energy heating, impels material inside and outside to be heated, to make ice to distil rapidly simultaneously; In this process, infrared sensor carries out real-time sensing to the temperature on material surface, and according to measured result, the preset program of micro computer is adjusted in real time, controlled microwave heating dynamics, storehouse internal pressure by voltage; When temperature of charge leveled off to zero degree, sublimation stage finished.
Desorption phase, this moment, infrared sensor was further turned the microwave heating dynamics down by the preset program of micro computer, icing because of not existing in the material, product temperature is increased on can be rapidly and differs from 10～20 ℃ of the highest permissive temperatures that reach product, and this moment, infrared sensor cut out microwave heating by the preset program of micro computer; Start the insulation program that heats of silicone oil in the heat-conduction plastic pipe of anti-microwave that the supporting plate internal layer do not absorb microwave radiation energy simultaneously.Product temperature continues to rise to the highest permissive temperature of product, and under this temperature, keep a period of time, the water that makes bound water and be adsorbed in the drying layer obtains enough energy, desorbs from Molecular Adsorption, finishes the exsiccant overall process of medical lyophilized powder (pin) agent microwave vacuum freeze.
Can judge that manual voltage regulation power and energy are supplied with the whole story of three phases operations such as pre-freeze, distillation, desorbing by the vacuum pressure difference in vacuum pressure in temperature, the storehouse or two storehouses in the method for the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent; More preferably infrared sensor carries out real-time sensing to the temperature on material surface, and according to measured result, the preset program of micro computer is adjusted in real time, controlled microwave heating dynamics, storehouse internal pressure by voltage.
Claims (9)
1. the preparation method of a medical lyophilized powder (pin) agent, it is characterized in that, the present invention for the production cycle, the energy consumption that reduces medical lyophilized powder (pin) agent that further shorten medical lyophilized powder (pin) agent, improve the product interior quality of medical lyophilized powder (pin) agent, providing on the basis of method that the conventional vacuum freeze drying equipment prepares medical lyophilized powder (pin) agent, provide the method that brand-new lyophilization prepares medical lyophilized powder (pin) agent;
Wherein, the brand-new lyophilization method for preparing medical lyophilized powder (pin) agent comprises:
Infrared vacuum lyophilization prepares the method for medical lyophilized powder (pin) agent;
The method of the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent.
2. the preparation method of a kind of medical lyophilized powder according to claim 1 (pin) agent is characterized in that the conventional vacuum freeze drying equipment prepares the method for medical lyophilized powder (pin) agent; The present invention is under the prerequisite of the predecessor's liquid preparation technology in early stage that does not change medical lyophilized powder (pin) agent substantially, after the operation that liquid preparation need heat all early stages has been finished, or before just the medicinal liquid branch installs in the commercially available packing container shortly, in fluid reservoir, in fluid reservoir medicinal liquid circulation line and/or in fluid reservoir and pipeline that fluid reservoir links to each other and/or in fluid reservoir and pipeline that racking machine links to each other and/or in the pipeline at racking machine, to medicinal liquid carry out ultrasonication, infrared add can, activation processing such as microwave intensifies, magnetization is handled; Liquid preparation after the processing places the conventional vacuum freeze drying equipment to carry out the well-established law drying, can produce the effect that shortens the production cycle, cuts down the consumption of energy.
3. according to the preparation method of claim 1,2 described a kind of medical lyophilized powder (pin) agent, it is characterized in that the conventional vacuum freeze drying equipment prepares the method for medical lyophilized powder (pin) agent; The adding alnico magnets magnetize the effect meeting better to the material of pre-freeze stage, sublimation stage in traditional vacuum freeze drying equipment shelf.
4. according to the preparation method of claim 1,2 described a kind of medical lyophilized powder (pin) agent, it is characterized in that the conventional vacuum freeze drying equipment prepares in the method for medical lyophilized powder (pin) agent; Ultrasonication, infrared add can, four kinds of processing modes such as microwave intensifies, magnetization is handled, can use separately respectively, more preferably be used in combination.
5. the preparation method of a kind of medical lyophilized powder according to claim 1 (pin) agent is characterized in that, infrared vacuum lyophilization prepares the method for medical lyophilized powder (pin) agent to be finished by three phases operations such as pre-freeze, distillation, desorbings, wherein:
A, in the pre-freeze stage, the pallet that material layering is put into infrared vacuum freeze is arranged full in an orderly manner, closes hatch door, opens the pre-freeze valve and makes low temperature silicone oil enter system, and material is carried out pre-freeze; At this moment, the heat energy in the material will enter in the subzero silicone oil below-55 ℃ by conduction of heat, two approach of infra-red radiation via the path of material → pallet → shelf → heat pipe → silicone oil, and the low temperature silicone oil that is recycled is taken away; When temperature of charge drops to subzero 20～50 ℃, the operation that enters next stage;
B, sublimation stage, start vacuum pump, make that vacuum remains on 5～80Pa in the storehouse, change freezing silicone oil into hot silicone oil and via the path of silicone oil → heat pipe → shelf → pallet → material, heat energy in the silicone oil is passed through conduction of heat, two approach of infra-red radiation, enter temperature in subzero 20～50 ℃ material, make hydrone in the material inside and outside portion ice crystal obtain energy simultaneously and distil; When temperature of charge leveled off to zero degree, sublimation stage finished;
C, desorption phase, to constantly reduce the temperature of silicone oil or turn the flow of silicone oil down, and when reaching the highest permissive temperature of product, keep a period of time, the water that makes bound water and be adsorbed in the drying layer obtains enough energy, from Molecular Adsorption, desorb, finish the overall process of the infrared vacuum lyophilization of medical lyophilized powder (pin) agent.
6. according to the preparation method of claim 1,5 described a kind of medical lyophilized powder (pin) agent, it is characterized in that, infrared vacuum lyophilization prepares the whole story of two interim operations such as distillation in the method for medical lyophilized powder (pin) agent, desorbing, can judge by temperature, also can judge by the vacuum pressure difference in vacuum pressure in the storehouse or two storehouses.
7. the preparation method of a kind of medical lyophilized powder according to claim 1 (pin) agent is characterized in that, the method for the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent is finished by three phases operations such as pre-freeze, distillation, desorbings, wherein:
A, in the pre-freeze stage, the liquid preparation that branch is installed places microwave vacuum freeze-drying device, opens refrigerating plant, when material surface temperature during near zero degree, opens 1～5 second of microwave radiation; Continue pre-freeze, make predrying material be cooled to subzero 20～50 ℃ rapidly, the pre-freeze of finishing material;
B, sublimation stage start vacuum pump, make that vacuum remains on 5～80Pa in the storehouse in, and starting main heating source is microwave magnetron, and material is carried out the high-energy heating, impels material inside and outside to be heated, to make ice ice to distil rapidly simultaneously; In this process, infrared sensor carries out real-time sensing to the temperature on material surface, and according to measured result, the preset program of micro computer is adjusted in real time, controlled microwave heating dynamics, storehouse internal pressure by voltage; When temperature of charge leveled off to zero degree, sublimation stage finished;
C, desorption phase, this moment, infrared sensor was further turned the microwave heating dynamics down by the preset program of micro computer, icing because of not existing in the material, product temperature is increased on can be rapidly and differs from 10～20 ℃ of the highest permissive temperatures that reach product, and this moment, infrared sensor cut out microwave heating by the preset program of micro computer; Start the insulation program that heats of silicone oil in the heat-conduction plastic pipe of anti-microwave that the supporting plate internal layer do not absorb microwave radiation energy simultaneously; Product temperature continues to rise to the highest permissive temperature of product, and under this temperature, keep a period of time, the water that makes bound water and be adsorbed in the drying layer obtains enough energy, desorbs from Molecular Adsorption, finishes the exsiccant overall process of medical lyophilized powder (pin) agent microwave vacuum freeze.
8. according to the preparation method of claim 1,7 described a kind of medical lyophilized powder (pin) agent, it is characterized in that, the whole story of three phases operations such as pre-freeze, distillation, desorbing in the method for the dry preparation of microwave vacuum freeze medical lyophilized powder (pin) agent, can judge that manual voltage regulation power and energy are supplied with by the vacuum pressure difference in vacuum pressure in temperature, the storehouse or two storehouses; More preferably infrared sensor carries out real-time sensing to the temperature on material surface, and according to measured result, the preset program of micro computer is adjusted in real time, controlled microwave heating dynamics, storehouse internal pressure by voltage.
9. the preparation method of a kind of medical lyophilized powder according to claim 1 (pin) agent, it is characterized in that, the present invention is applicable to any lyophilization that needs, and need in freezing dry process to use that method of the present invention further improves the product interior quality, further shortens the production cycle, the medical freeze dried powder that further cuts down the consumption of energy, medical freezing in injectable powder; Be example now, not limited provide the following kind of the present invention that is suitable for medical lyophilized injectable powder:
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| CNA2006100104097A CN101125126A (en) | 2006-08-16 | 2006-08-16 | Method for preparing medical freeze-dried powder (injection) preparation |
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