CN106674272A - Processing method for amifostine - Google Patents

Processing method for amifostine Download PDF

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Publication number
CN106674272A
CN106674272A CN201611223892.7A CN201611223892A CN106674272A CN 106674272 A CN106674272 A CN 106674272A CN 201611223892 A CN201611223892 A CN 201611223892A CN 106674272 A CN106674272 A CN 106674272A
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CN
China
Prior art keywords
amifostine
drier
crystallizing tank
tank
deg
Prior art date
Application number
CN201611223892.7A
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Chinese (zh)
Inventor
徐继嗣
Original Assignee
张家港市华天药业有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 张家港市华天药业有限公司 filed Critical 张家港市华天药业有限公司
Priority to CN201611223892.7A priority Critical patent/CN106674272A/en
Publication of CN106674272A publication Critical patent/CN106674272A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/16Esters of thiophosphoric acids or thiophosphorous acids
    • C07F9/165Esters of thiophosphoric acids
    • C07F9/1651Esters of thiophosphoric acids with hydroxyalkyl compounds with further substituents on alkyl

Abstract

The invention discloses a processing method for amifostine. Through control of temperature and time parameters during crystallization, amifostine doesn't undergo other chemical reactions during crystallization, so that amifostine is high in crystallization efficiency. A single-cone vacuum dryer is arranged and can effectively purify and dry amifostine crystal to prepare an amifostine powder product.

Description

A kind of processing method for Amifostine

Technical field

The present invention relates to a kind of processing method for Amifostine.

Background technology

Amifostine in radiotherapy or chemotherapy process, is killing cancer as chemotherapy cytoprotection medicine and radiation therapy protective reagents Normal tissue cell can be optionally protected during cell, patient is continuously received treatment.Kidney poison for releasing anticarcinogen, The toxicities such as hemopoietic system, immunologic mjury that preventive radiotherapy causes have certain effect, are also used for reducing and neutrocyte Reduce the related infection of disease.

Amifostine as cell-protecting, for chemotherapy to kidney, marrow, heart protection.

The existing processing to Amifostine, processing step is complex, and equipment is costly, relatively costly, and easily exists Amifostine is chemically reacted during crystallization, cause the waste to Amifostine raw material, improve processing cost, and reduce ammonia phosphorus The production and processing efficiency of spit of fland product.

The content of the invention

It is an object of the invention to provide a kind of processing method for Amifostine, step is simple, and processing efficiency is higher.

To reach above-mentioned purpose, the technical solution adopted by the present invention is:

A kind of processing method for Amifostine, comprises the following steps:

(1)Dissolution filter:1 part of Amifostine raw material is put into dissolving tank, and adds 1-3.5 parts of water, preheat the dissolving tank extremely 20-60 DEG C makes Amifostine dissolution of raw material, then adds the dissolving after 0.1-0.8 parts of water is mixed with 0.01-0.15 parts of activated carbon In tank, 20-60 DEG C of temperature is kept, the mixture in the dissolving tank is stirred, the Amifostine raw material press filtration that will be dissolved Into crystallizing tank;

(2)Crystallization:The crystallizing tank is heated to 20-60 DEG C, then to the second of 95% concentration that 0.1-10 parts is added dropwise in the crystallizing tank Alcohol, keeps 20-60 DEG C of temperature, and 0.1-2.5h is stirred to the mixture in the crystallizing tank, then slow to the crystallizing tank Slow cool down, makes the crystallizing tank that 0-15 DEG C is cooled in 2.5-6.5h, by obtained Amifostine crystallization press filtration to drier;

(3)Dry:The vavuum pump for vacuumizing is provided in the drier, is provided for taking out second in the drier bottom The vacuum valve of alcohol, is provided for the rabbling mechanism of stirring in the drier, and portion is provided for week on the outside of the drier The hot water circulating pump of heat drying;

First by the vavuum pump to being vacuumized inside the drier, secondly open the vacuum valve and extract ethanol, then Open the rabbling mechanism to be stirred with the rotating speed of 5-35r/min, then start the hot water circulating pump with 20-55 DEG C of temperature Degree dries 1-12h to the drier, finally closes the hot water circulating pump and the rabbling mechanism, takes out Amifostine finished product.

Preferably, in the step(1)In, will dissolve Amifostine raw material press filtration to the crystallizing tank in after, then To water the cleaning activated carbon and the dissolving tank that 0.1-0.6 parts is added in the dissolving tank, the Amifostine raw material that will be remained After dissolving in press filtration to the crystallizing tank.

Preferably, in the step(2)In, after obtained Amifostine is crystallized in press filtration to the drier, then To the ethanol of 95% concentration that 0.1-0.5 parts is added in the crystallizing tank, after being cleaned to the inside of the crystallizing tank, then In press filtration to the drier.

Preferably, in the step(2)In, the crystallizing tank is being cooled to 0-15 DEG C afterwards in 2.5-6.5h, make The crystallizing tank maintains 0-15 DEG C, and continues 1-8h, then again by obtained Amifostine crystallization press filtration to the drier.

Preferably, in the step(3)In, the drier is single cone vacuum desiccator of the shape in back taper.

Preferably, in the step(3)Afterwards, Amifostine finished product is slowly fitted into sterile bag, the sterile bag is located at In Aluminum Bottle, the Aluminum Bottle is weighed by weighing mechanism, when weight reaches setting value, tie the sterile bag, and cover Upper aluminium lid.

It is highly preferred that the aluminium lid is tightened on the Aluminum Bottle by Cover-rolling machine.

Due to the utilization of above-mentioned technical proposal, the present invention has following advantages compared with prior art:A kind of use of the invention In the processing method of Amifostine, by controlling temperature parameter and time parameter during crystallization, Amifostine is set not sent out in crystallization Raw other chemical reactions, crystalline rate is high;By setting single cone vacuum desiccator, efficiently Amifostine crystallization can be carried Pure drying, so that powdery Amifostine product is obtained.

Brief description of the drawings

Accompanying drawing 1 is the process chart of the inventive method.

Specific embodiment

The technical solution of the present invention will be further described below with reference to the accompanying drawings.

Shown in Figure 1, here is a kind of for Amifostine(C5H21N2O6PS)One of processing method specific implementation Example, the method is comprised the following steps:

(1)Dissolution filter:The Amifostine raw material that quality is 1 part is put into dissolving tank, and to 2 parts of water are added in dissolving tank, in advance The hot dissolving tank makes Amifostine dissolution of raw material in water to 40 DEG C, then after 0.5 part of water mix with 0.08 part of activated carbon addition this In dissolving tank, dissolving tank is kept 40 DEG C of temperature, the mixture in dissolving tank is stirred, the Amifostine raw material that will be dissolved In press filtration to crystallizing tank;After in Amifostine raw material press filtration to the crystallizing tank that will be dissolved, then to adding 0.3 part in dissolving tank Inside water cleaning active charcoal and dissolving tank, after the Amifostine dissolution of raw material that will be remained also in press filtration to crystallizing tank;The step is molten Carried out between solution, the clean rank between dissolving is C grades;

(2)Crystallization:Heating crystalline tank protects crystallizing tank to 50 DEG C, then to the ethanol of 95% concentration that 5 parts are added dropwise in the crystallizing tank 50 DEG C of temperature is held, 1.5h is stirred to the mixture in crystallizing tank, then to crystallizing tank Slow cooling, make crystallizing tank in 4.5h Inside it is cooled to 0-15 DEG C;Crystallizing tank is being cooled to 0-15 DEG C afterwards in 4.5h, crystallizing tank is kept 0-15 DEG C of temperature, and Continue 4.5h, then by obtained Amifostine crystallization press filtration to drier;Obtained Amifostine is being crystallized into press filtration to drying After in device, then to the ethanol of 95% concentration that 0.3 part of normal temperature is added in crystallizing tank, the inside to crystallizing tank carries out cleaning Afterwards, then by residue press filtration to drier;The step between crystallization in carry out, the clean rank between crystallization be A grades or B grades;

(3)Dry:The drier is single cone vacuum desiccator of the shape in back taper, is provided in singly cone vacuum desiccator The vavuum pump for vacuumizing, is provided for taking out the vacuum valve of ethanol, in singly cone vacuum desiccator in singly cone vacuum desiccator bottom The rabbling mechanism of stirring is provided for, portion is provided for the hot water circulating pump of heat drying week on the outside of singly cone vacuum desiccator;

First by vavuum pump to being vacuumized inside single cone vacuum desiccator, the vacuum valve for secondly opening bottom extracts waste ethanol, Waste ethanol is drained net rear rabbling mechanism of opening to be stirred with the rotating speed of 20r/min, then starts hot water circulating pump with 35 DEG C Temperature 6h is dried to single cone vacuum desiccator, finally close hot water circulating pump and rabbling mechanism, take out powdered Amifostine into Product;The step between crystallization in carry out, the clean rank between crystallization be A grades or B grades;

(4)Discharging:It is provided for exporting the valve of powdered Amifostine finished product, turning for discharging in singly cone vacuum desiccator Fortune bucket, the transferring barrel visor for observing transferring barrel state;

During discharging, slow Open valve observes material from transferring barrel visor, and valve is closed after bucket to be transported is full, unclamps docking, uses It is aseptic change trains or buses by transferring barrel be transported to packing between dispense and weigh;The step between crystallization in carry out, the clean rank between crystallization be A Level or B grades;

(5)Packing:Transferring barrel is docked with material guiding hopper valve, Aluminum Bottle is placed in the discharging opening of material guiding hopper valve, placed in Aluminum Bottle aseptic Bag, powdered Amifostine finished product is slowly fitted into sterile bag, Aluminum Bottle is weighed by weighing mechanism, in the present embodiment In, the weighing mechanism is electronic weighing balance, when the weight of Aluminum Bottle reaches setting value 10kg, ties sterile bag, and cover aluminium lid; The step between packing in carry out, the clean rank between packing be A grades;

(6)Roll lid:Aluminium lid is tightened on Aluminum Bottle by Cover-rolling machine;The step is carried out in rolling between lid, rolls the clean level between lid Wei A grades or B grades.

The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and be carried out that it is not intended to limit the scope of the present invention, all according to the present invention The equivalent change or modification that Spirit Essence is made, should all cover within the scope of the present invention.

Claims (7)

1. a kind of processing method for Amifostine, it is characterised in that:Comprise the following steps:
(1)Dissolution filter:1 part of Amifostine raw material is put into dissolving tank, and adds 1-3.5 parts of water, preheat the dissolving tank extremely 20-60 DEG C makes Amifostine dissolution of raw material, then adds the dissolving after 0.1-0.8 parts of water is mixed with 0.01-0.15 parts of activated carbon In tank, 20-60 DEG C of temperature is kept, the mixture in the dissolving tank is stirred, the Amifostine raw material press filtration that will be dissolved Into crystallizing tank;
(2)Crystallization:The crystallizing tank is heated to 20-60 DEG C, then to the second of 95% concentration that 0.1-10 parts is added dropwise in the crystallizing tank Alcohol, keeps 20-60 DEG C of temperature, and 0.1-2.5h is stirred to the mixture in the crystallizing tank, then slow to the crystallizing tank Slow cool down, makes the crystallizing tank that 0-15 DEG C is cooled in 2.5-6.5h, by obtained Amifostine crystallization press filtration to drier;
(3)Dry:The vavuum pump for vacuumizing is provided in the drier, is provided for taking out second in the drier bottom The vacuum valve of alcohol, is provided for the rabbling mechanism of stirring in the drier, and portion is provided for week on the outside of the drier The hot water circulating pump of heat drying;
First by the vavuum pump to being vacuumized inside the drier, secondly open the vacuum valve and extract ethanol, then Open the rabbling mechanism to be stirred with the rotating speed of 5-35r/min, then start the hot water circulating pump with 20-55 DEG C of temperature Degree dries 1-12h to the drier, finally closes the hot water circulating pump and the rabbling mechanism, takes out Amifostine finished product.
2. a kind of processing method for Amifostine according to claim 1, it is characterised in that:In the step(1)In, After in Amifostine raw material press filtration to the crystallizing tank that will be dissolved, then to adding 0.1-0.6 parts of water in the dissolving tank The activated carbon and the dissolving tank are cleaned, after the Amifostine dissolution of raw material that will be remained in press filtration to the crystallizing tank.
3. a kind of processing method for Amifostine according to claim 1, it is characterised in that:In the step(2)In, After obtained Amifostine is crystallized in press filtration to the drier, then to 95% of 0.1-0.5 parts of addition in the crystallizing tank The ethanol of concentration, after being cleaned to the inside of the crystallizing tank, then in press filtration to the drier.
4. a kind of processing method for Amifostine according to claim 1, it is characterised in that:In the step(2)In, The crystallizing tank is being cooled to 0-15 DEG C afterwards in 2.5-6.5h, the crystallizing tank is maintained 0-15 DEG C, and continue 1- 8h, then again by obtained Amifostine crystallization press filtration to the drier.
5. a kind of processing method for Amifostine according to claim 1, it is characterised in that:In the step(3)In, The drier is single cone vacuum desiccator of the shape in back taper.
6. a kind of processing method for Amifostine according to claim 1, it is characterised in that:In the step(3)It Afterwards, Amifostine finished product is slowly fitted into sterile bag, the sterile bag is entered by weighing mechanism in Aluminum Bottle to the Aluminum Bottle Row is weighed, and when weight reaches setting value, ties the sterile bag, and cover aluminium lid.
7. a kind of processing method for Amifostine according to claim 6, it is characterised in that:Will be described by Cover-rolling machine Aluminium lid is tightened on the Aluminum Bottle.
CN201611223892.7A 2016-12-27 2016-12-27 Processing method for amifostine CN106674272A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101412732A (en) * 2008-09-02 2009-04-22 大连美罗药业股份有限公司 Trihydrate 3-amino propyl amine ethyl phosphorothioic acid high purity stable crystal and preparation thereof
CN102260288A (en) * 2010-06-08 2011-11-30 成都大有得药业有限公司 Synthesis method of 3-amino-propyl aminoethyl thiophosphate trihydrate
CN102445058A (en) * 2010-10-08 2012-05-09 沈善明 Non-sealing single-cone vacuum dryer
CN103509046A (en) * 2013-07-22 2014-01-15 衡阳师范学院 Bis(tri(2-methyl-2-phenyl propyl)tin) dicarboxylic ester and preparation method and application thereof
CN103727753A (en) * 2012-10-12 2014-04-16 沈善明 Wedge-shaped plate internal heating pyramid vacuum dryer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101412732A (en) * 2008-09-02 2009-04-22 大连美罗药业股份有限公司 Trihydrate 3-amino propyl amine ethyl phosphorothioic acid high purity stable crystal and preparation thereof
CN102260288A (en) * 2010-06-08 2011-11-30 成都大有得药业有限公司 Synthesis method of 3-amino-propyl aminoethyl thiophosphate trihydrate
CN102445058A (en) * 2010-10-08 2012-05-09 沈善明 Non-sealing single-cone vacuum dryer
CN103727753A (en) * 2012-10-12 2014-04-16 沈善明 Wedge-shaped plate internal heating pyramid vacuum dryer
CN103509046A (en) * 2013-07-22 2014-01-15 衡阳师范学院 Bis(tri(2-methyl-2-phenyl propyl)tin) dicarboxylic ester and preparation method and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
沈善明: "介绍小型无密封单锥药品真空干燥机", 《医药工程设计》 *
沈善明: "热敏性药品的干燥", 《医药工程设计》 *
沈善明等: "提高中药粉粒体蒸汽灭菌的效率和节能探讨", 《医药工程设计》 *
沈善明等: "用作特殊性物料干燥的单锥真空干燥机", 《医药工程设计》 *

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