CN108409821A - A kind of preparation method and megestrol acetate of megestrol acetate nanocrystal - Google Patents
A kind of preparation method and megestrol acetate of megestrol acetate nanocrystal Download PDFInfo
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- CN108409821A CN108409821A CN201810225669.9A CN201810225669A CN108409821A CN 108409821 A CN108409821 A CN 108409821A CN 201810225669 A CN201810225669 A CN 201810225669A CN 108409821 A CN108409821 A CN 108409821A
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- C—CHEMISTRY; METALLURGY
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- C07J7/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms
- C07J7/0005—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21
- C07J7/001—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group
- C07J7/004—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group substituted in position 17 alfa
- C07J7/0045—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group substituted in position 17 alfa not substituted in position 16
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention provides a kind of preparation method and megestrol acetate of megestrol acetate nanocrystal, crystallization process is accurately controlled by supercritical fluid recrystallization technology first, control the crystal form and size of crystal, it is made that crystal size is uniform and the good megestrol acetate of rounding property, then pass through airflow pulverization, further pulverized particles, it is final that the megestrol acetate that grain diameter is small, particle is uniform, rounding property is good is made, significantly increase its specific surface area, dissolution rate is improved, and then improves its bioavilability.
Description
Specification
Technical field
The invention belongs to field of pharmaceutical technology, and in particular to a kind of preparation method of megestrol acetate nanocrystal.
Background technology
Megestrol acetate (Megestrol Acetate, MA) is a kind of important synthetic progestin class drug, main to use
In the treatment of advanced breast cancer and carcinoma of endometrium, the appetite and cachexia of late tumor patient can be improved, to dysfunctional uterine
Bleeding, irregular menstruation, endometrial hyperplasia, endometriosis and other diseases also have certain curative effect.Megestrol acetate is one
Kind white crystalline powder, 213~220 DEG C of fusing point are soluble in chloroform, acetone or ethyl acetate solution are dissolvable in water, in second
It is slightly molten in alcohol, the slightly soluble in ether.Solubility of the megestrol acetate in 37 DEG C of water is 2mg/ml, dissolving in blood
Degree is 24 μ g/ml leads to its relatively low bioavilability since its solubility is low.
Chinese invention patent CN101671382A (publication number) disclose " ultra-micronized megestrol acetate and containing its
Pharmaceutical composition " is directed to invent a kind of ultra-micronized megestrol acetate that grain size is less than 10 μm, and comprising effective
The suitable pharmaceutical dosage form that the ultra-micronized megestrol acetate of amount and pharmaceutically acceptable excipient are prepared into, wherein including
Dispersible tablet, ordinary tablet and capsule.
105769763 A of Chinese invention patent CN (application publication number) disclose a kind of " megestrol acetate nanometer suspension
Liquid and its preparation method and application " is directed to invent a kind of megestrol acetate nanosuspension, is by tumer pregnant
It is made through nano-level grinder grinding after ketone and stabiliser solution mixing, acetic acid in the megestrol acetate nanosuspension of the invention
The average grain diameter 1000nm of megestrol acetate is hereinafter, significantly improve the dissolution rate of megestrol acetate, and then improve acetic acid
The oral administration biaavailability of megestrol acetate.
But the above method improves the dissolution rate and bioavilability of megestrol acetate well not yet, needs exist for
A kind of method is further to improve the dissolution rate and bioavilability of megestrol acetate.
Invention content
It is an object of the present invention to overcome the prior art deficiency, provide a kind of fine particle grain size prepared it is small,
The preparation method of megestrol acetate nanocrystal uniform in size, rounding property is good.Another object of the present invention is to apply institute
It states preparation method and produces a kind of megestrol acetate that average grain diameter is 0~800nm.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of megestrol acetate nanocrystal is first recrystallized in shooting flow recrystallization machine
Processing, then enters back into airslide disintegrating mill and crushes processing, include the following steps：
1) use pump by CO2Heater is inputted by pipeline, becomes supercritical CO after heating2Into in crystallization kettle；
2) megestrol acetate solution is inputted by pipeline in above-mentioned crystallization kettle with pump；
3) in crystallization kettle, supercritical CO2It mixes in nozzle with megestrol acetate solution and is sprayed by nozzle, is precipitated
Megestrol acetate crystallizes；
4) input for stopping megestrol acetate solution, is continuing with supercritical CO2Above-mentioned crystallization is washed and done
It is dry, pass through CO2Time be 30~45min, you can megestrol acetate crystal is made；
5) megestrol acetate crystal obtained is entered from the feed inlet of airslide disintegrating mill in its crushing chamber；
6) protective gas spurts into crushing chamber after filtration drying by nozzle at high speeds, in the friendship of multiply high pressure draught
At meeting point material by impact several times, friction, shearing and crush, the material after crushing is transported under wind turbine draft effect with ascending air
It moves to graded region, under the powerful centrifugation force effect that high-speed rotating grading wheel generates, makes thickness feed separation, meet granularity and want
The fine grained asked enters cyclone separator by grading wheel and deduster is collected, and coarse granule, which drops to disintegrating area, to be continued to crush, i.e.,
Megestrol acetate can be obtained；
The solvent of the megestrol acetate solution is that acetone, ethyl acetate are one such or two kinds.
Temperature in the crystallization kettle is 30~60 DEG C.
Pressure in the crystallization kettle is 100~200bar.
The CO2Flow be 15~30g/min, the flow of megestrol acetate solution is 0.5~3.5ml/min.
The protective gas is one or more of inert gas.
The air pressure of the protective gas is 6~12kgf/cm2。
The rotating speed of the grading wheel is 2000~6000rpm.
The present invention operation principle be：Supercritical fluid recrystallization technology is that in the supercritical state, reducing pressure can be with
Lead to oversaturated generation, and high degree of supersaturation can be reached, solid solute can be crystallized out from supercritical solution.
Since this process carries out in uniform dielectric, crystallization process can be more accurately controlled, to control the crystal form of crystal and big
It is small.Airflow pulverization be will dry, purified compression protective gas by nozzle generate high-speed flow, the band in crushing chamber
Dynamic particle high-speed motion, the effects that making particle be impacted, collide, shearing and be crushed；Pulverized particle with air current classifying,
The particle of fineness requirement qualification is collected by trap, and the coarse granule not up to required returns again to crushing chamber and continues to crush, until
Reach required fineness and storage collection of being caught.By the joint of two kinds of technologies so that the megestrol acetate fine powder prepared has more
High dissolution rate.
It is an advantage of the invention that：The megestrol acetate fine particle grain size of preparation is small, particle is uniform, rounding property is good, base
This is in spherical, the dissolution rate of megestrol acetate is substantially increased, so as to improve its bioavilability.
Specific implementation mode
Below by embodiment, technical scheme of the present invention is described in further detail, the embodiment described is
For illustrating the present invention, and it is not considered as limitation of the present invention.
Following embodiments for preparing megestrol acetate are first to be carried out at recrystallization in shooting flow recrystallization machine
Reason, then enters back into airslide disintegrating mill and crushes processing.
Embodiment 1
It weighs megestrol acetate 4g to be dissolved in 86ml acetone, ultrasonic mixing filters to obtain clear solution；It sets overcritical
Recrystallize device systems parameter；Temperature 45 C, pressure 150bar, CO2Flow 30g/min, by CO2It is flat to system to be pumped into crystallization kettle
Weighing apparatus；Above-mentioned megestrol acetate solution is pumped into crystallization kettle by the flow of 2ml/min；Stop the defeated of megestrol acetate solution
Enter, keeps system mode, continue to be passed through CO230~45min, for drying megestrol acetate crystallization and removing residual in crystallization kettle
Stay solvent, you can megestrol acetate fine powder is made.Above-mentioned fine powder obtained is observed by SEM, is as a result shown：Tumer
Progesterone powder particle size rounding is uniform, and average grain diameter is in 800nm or so；It is measured by particles distribution instrument, grain size is less than the powder of 800nm
Grain accounts for 90% or more.Nitrogen after filtration drying is with 6.0kgf/cm2Gas enter in crushing chamber from air-flow crushing machine nozzle, gas
After flowing pulverizer operation 1h, grading wheel is opened, sets the rotating speed of grading wheel as 2000rpm, finally obtained megestrol acetate
Powder particle size rounding is uniform, and average grain diameter is in 600nm or so；It is measured by particles distribution instrument, powder of the grain size less than 600nm accounts for
90% or more.
Embodiment 2
Pressure, temperature, the type of protective gas and flow in preparation method and technological parameter is same as Example 1,
3g megestrol acetates, i.e., be dissolved in 97ml ethyl acetate by the preparation method for only changing megestrol acetate solution.It will system
The above-mentioned fine powder obtained is observed by SEM, is as a result shown：Products obtained therefrom crystal form is same as Example 1, and average grain diameter is on the left sides 650nm
It is right；It is measured by particles distribution instrument, powder of the grain size less than 650nm accounts for 90% or more.Average grain diameter is in 500nm after air-flow crushing
Left and right；It is measured by particles distribution instrument, powder of the grain size less than 500nm accounts for 90% or more.
Embodiment 3
Pressure, temperature, the type of protective gas and flow in preparation method and technological parameter is same as Example 1,
The preparation method for only changing megestrol acetate solution, i.e., be dissolved in 96ml acetoneand ethyl acetates by 4g megestrol acetates
In mixed liquor, wherein the volume ratio of acetoneand ethyl acetate is 6:4.Above-mentioned fine powder obtained is observed by SEM, is as a result shown
Show：Products obtained therefrom crystal form is same as Example 1, and average grain diameter is in 800nm or so；It is measured by particles distribution instrument, grain size is less than
The powder of 800nm accounts for 90% or more.Average grain diameter is in 500nm or so after air-flow crushing；It is measured by particles distribution instrument, grain size is small
90% or more is accounted in the powder of 500nm.
Embodiment 4
The type of the preparation method of megestrol acetate solution and the parameter setting of Jet Mill and protective gas
It is same as Example 2, change shooting flow recrystallization device systems parameter, 30 DEG C of temperature, pressure 100bar, CO2Flow
15g/min, by CO2Crystallization kettle is pumped into system balancing；Above-mentioned megestrol acetate solution is pumped by the flow of 0.5ml/min
In crystallization kettle.Above-mentioned fine powder obtained is observed by SEM, is as a result shown：Products obtained therefrom crystal form is same as Example 1, average
Grain size is in 800nm or so；It is measured by particles distribution instrument, powder of the grain size less than 800nm accounts for 90% or more.It is put down after air-flow crushing
Equal grain size is in 600nm or so；It is measured by particles distribution instrument, powder of the grain size less than 600nm accounts for 90% or more.
Embodiment 5
The type and reality of the preparation method of megestrol acetate solution and the parameter setting of air-flow crushing and protective gas
It is identical to apply example 2, changes shooting flow recrystallization device systems parameter, temperature 45 C, pressure 100bar, CO2Flow 25g/
Min, by CO2Crystallization kettle is pumped into system balancing；Above-mentioned megestrol acetate solution is pumped into crystallization kettle by the flow of 1ml/min
It is interior.Above-mentioned fine powder obtained is observed by SEM, is as a result shown：Products obtained therefrom crystal form is same as Example 1, and average grain diameter exists
600nm or so；It is measured by particles distribution instrument, powder of the grain size less than 600nm accounts for 90% or more.Average grain diameter after air-flow crushing
In 350nm or so；It is measured by particles distribution instrument, powder of the grain size less than 350nm accounts for 90% or more.
Embodiment 6
The type and reality of the preparation method of megestrol acetate solution and the parameter setting of air-flow crushing and protective gas
It is identical to apply example 2, changes overcritical recrystallization device systems parameter, temperature 60 C, pressure 200bar, CO2Flow 30g/min, will
CO2Crystallization kettle is pumped into system balancing；Above-mentioned megestrol acetate solution is pumped into crystallization kettle by the flow of 3.5ml/min.
Above-mentioned fine powder obtained is observed by SEM, is as a result shown：Products obtained therefrom crystal form is same as Example 1, and average grain diameter exists
700nm or so；It is measured by particles distribution instrument, powder of the grain size less than 700nm accounts for 90% or more.Average grain diameter after air-flow crushing
In 450m or so；It is measured by particles distribution instrument, powder of the grain size less than 450nm accounts for 90% or more.
Embodiment 7
Preparation method, shooting flow recrystallization device systems parameter setting and the air-flow powder of megestrol acetate solution
Broken device systems parameter is same as Example 5, only changes the type of protective gas, and protective gas is changed to carbon dioxide and finally obtains
Megestrol acetate powder particle size rounding it is uniform.Product crystal form and size after crystallization is identical as after the crystallization of embodiment 5.
Average grain diameter is in 500nm or so after air-flow crushing；Measured by particles distribution instrument, grain size less than 500nm powder account for 90% with
On.
Embodiment 8
Preparation method, shooting flow recrystallization device systems parameter setting and the air-flow powder of megestrol acetate solution
Broken device systems parameter is same as Example 5, only changes the type of protective gas, and protective gas is the mixed of carbon dioxide and nitrogen
Close gas, volume ratio 6:4, finally obtained megestrol acetate powder particle size rounding is uniform.Product crystal form after crystallization with
And size is identical as after the crystallization of embodiment 5.Average grain diameter is in 500nm or so after air-flow crushing.It is measured by particles distribution instrument,
Powder of the grain size less than 500nm accounts for 90% or more.
Embodiment 9
The preparation method and shooting flow recrystallization device systems parameter setting of megestrol acetate solution and embodiment 5
It is identical, change Jet Mill systematic parameter, the nitrogen after filtration drying is with 10.0kgf/cm2Gas from airslide disintegrating mill
Nozzle enters in crushing chamber, after airslide disintegrating mill runs 1h, opens grading wheel, sets the rotating speed of grading wheel as 4000rpm, it is final must
The megestrol acetate powder particle size rounding arrived is uniform.Product crystal form and size after crystallization and the phase after the crystallization of embodiment 5
Together.Equal grain size is in 300nm or so after flat air-flow crushing；It is measured by particles distribution instrument, powder of the grain size less than 300nm accounts for 90%
More than.
Embodiment 10
The preparation method and shooting flow recrystallization device systems parameter setting of megestrol acetate solution and embodiment 5
It is identical, change Jet Mill systematic parameter, the nitrogen after drying is with 12.0kgf/cm2Gas from air-flow crushing machine nozzle
Enter in crushing chamber, after airslide disintegrating mill runs 1h, opens grading wheel, set the rotating speed of grading wheel as 4000rpm, it is finally obtained
Megestrol acetate powder particle size rounding is uniform.Product crystal form and size after crystallization is identical as after the crystallization of embodiment 5.Gas
Average grain diameter after stream crushing is in 200nm or so；Measured by particles distribution instrument, grain size less than 200nm powder account for 90% with
On.
Embodiment 11
The preparation method and shooting flow recrystallization device systems parameter setting of megestrol acetate solution and embodiment 5
It is identical, change Jet Mill systematic parameter, the nitrogen after drying is with 12.0kgf/cm2Gas from air-flow crushing machine nozzle
Enter in crushing chamber, after airslide disintegrating mill runs 1h, opens grading wheel, set the rotating speed of grading wheel as 6000rpm, it is finally obtained
Megestrol acetate powder particle size rounding is uniform.Product crystal form and size after crystallization is identical as after the crystallization of embodiment 5.Gas
Average grain diameter is in 250nm or so after stream crushes；It is measured by particles distribution instrument, powder of the grain size less than 250nm accounts for 90% or more.
Claims (8)
1. a kind of preparation method of megestrol acetate nanocrystal, it is characterized in that, including supercritical fluid re-crystallization step and
Jet milling step, operating procedure are as follows：
1) use pump by CO2Heater is inputted by pipeline, becomes supercritical CO after heating2Into in crystallization kettle；
2) megestrol acetate solution is inputted by pipeline in above-mentioned crystallization kettle with pump；
3) in crystallization kettle, supercritical CO2It mixes in nozzle with megestrol acetate solution and is sprayed by nozzle, acetic acid is precipitated
Megestrol acetate crystallizes；
4) input for stopping megestrol acetate solution, is continuing with supercritical CO2Above-mentioned crystallization is washed and dried, is led to
Cross CO2Time be 30~45min, you can megestrol acetate crystal is made；
5) megestrol acetate crystal obtained is entered from the feed inlet of airslide disintegrating mill in its crushing chamber；
6) protective gas spurts into crushing chamber after filtering, drying by nozzle at high speeds, in the joint of multiply high pressure draught
Place's material by impact several times, friction, shearing and crush, the material after crushing moves under wind turbine draft effect with ascending air
Graded region makes thickness feed separation, meets granularity requirements under the powerful centrifugation force effect that high-speed rotating grading wheel generates
Fine grained enters cyclone separator by grading wheel and deduster is collected, and coarse granule, which drops to disintegrating area, to be continued to crush, you can
Megestrol acetate；
The solvent of the megestrol acetate solution is one or both of acetone, ethyl acetate.
2. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：The knot
Temperature in brilliant kettle is 30~60 DEG C.
3. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：The knot
Pressure in brilliant kettle is 100~200bar.
4. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：The CO2
Flow be 15~30g/min, the flow of megestrol acetate solution is 0.5~3.5ml/min.
5. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：The guarantor
Shield property gas is one or more of inert gas.
6. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：The guarantor
The air pressure of shield property gas is 6~12kgf/cm2。
7. a kind of preparation method of megestrol acetate nanocrystal according to claim 1, it is characterised in that：Described point
The rotating speed of step cone is 2000~6000rpm.
8. a kind of megestrol acetate, it is characterised in that；Have the right what the method described in any one of requirement 1~7 was prepared
Average grain diameter is the megestrol acetate of 0~800nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116444516A (en) * | 2023-03-20 | 2023-07-18 | 济宁学院 | Paliperidone palmitate nanocrystals and preparation method thereof, paliperidone palmitate nanocrystal suspension injection and preparation method thereof |
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Application publication date: 20180817 |