CN107814880A - The preparation method of tapioca microballoon - Google Patents
The preparation method of tapioca microballoon Download PDFInfo
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- CN107814880A CN107814880A CN201711015813.8A CN201711015813A CN107814880A CN 107814880 A CN107814880 A CN 107814880A CN 201711015813 A CN201711015813 A CN 201711015813A CN 107814880 A CN107814880 A CN 107814880A
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- tapioca
- microballoon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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Abstract
The present invention discloses a kind of preparation method of tapioca microballoon, comprises the following steps：（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent is added, stirring, is then incubated 2h at 50 DEG C；（2）The preparation of aqueous phase：Tapioca starch is added to the water, stirred, the pH to 10 12 of regulation system, stirring, is subsequently cooled to 35 DEG C, is stood；（3）Under stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, stirring, add initiator and crosslinking agent, stirring, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, spherex is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifugation, sediment is dried in vacuo.Method provided by the invention is simple, and cost is low, and the micro-sphere crosslinked degree of obtained cassava is high, and swellbility can reach more than 500%, and the particle diameter of microballoon microsphere surface rough porous, is adapted to do pharmaceutical carrier between 30 80 microns.
Description
Technical field
The invention belongs to artificial derivatives' manufacturing field, and in particular to a kind of preparation method of tapioca microballoon.
Background technology
Spherex is a kind of one of artificial derivatives of native starch, and not only the property with native starch, also has
Microcellular structure, easily adsorb medicine：There is certain deformability in vivo, can be changed according to the microenvironment of plexus vasculosus
The shape of oneself；When being degraded through enzyme, its Drug loading capacity can be kept for quite a long time before the skeletal disintegration of microballoon, it is thus possible to effectively
Extend the release time of contained medicine, improve medicine the effect of, be expected to turn into preferable targeting drug delivery system (TDDS) medicine carry
Body.A series of researchs on its application performance are also proved as pharmaceutical carrier, spherex have good medicament protection and
Sustained release performance, especially in the chemotherapy of cancer and slow
Good prospect is had shown that in the treatment of property disease such as arterial embolism.
At present, the preparation method of spherex is complicated, and in the preparation, the degree of cross linking of spherex is small, limits its application
Scope.
The content of the invention
The defects of for prior art, the present invention provide a kind of preparation method of tapioca microballoon.
The preparation method of tapioca microballoon, comprises the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent is added, 30-50min is stirred at 60 DEG C, is then incubated at 50 DEG C
2h；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 10-12,2-3h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, then stir
30min, initiator and crosslinking agent are added, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo.
Preferably, step（1）Described in emulsifying agent be Span60.
Preferably, step（1）Described in soybean oil and emulsifying agent mass ratio be 10:1.
Preferably, step（2）The preparation method of middle tapioca starch is：By cassava stripping and slicing, 6h is dried at 105 DEG C, then powder
It is broken, cross 200 mesh sieves.
Preferably, step（3）Middle step（2）Aqueous phase and step（1）Oil phase mass ratio be 2:3.
Preferably, step（3）Described in initiator be potassium peroxydisulfate.
Preferably, step（3）Described in crosslinking agent be N,N methylene bis acrylamide.
Preferably, step（3）Described in vacuum drying condition be at 50 DEG C dry 4-6h.
Advantages of the present invention：
Method provided by the invention, tapioca microballoon being prepared, method is simple, and cost is low, and the micro-sphere crosslinked degree of obtained cassava is high,
Swellbility can reach more than 500%, and the particle diameter of microballoon is between 30-80 microns, microsphere surface rough porous, be adapted to do medicine load
Body.
Embodiment
The preparation of tapioca starch：
By cassava stripping and slicing, 6h is dried at 105 DEG C, is then crushed, cross 200 mesh sieves.
Embodiment 1
The preparation method of tapioca microballoon, comprises the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent Span60 is added, 30min is stirred at 60 DEG C, then at 50 DEG C
2h is incubated, wherein, the mass ratio of soybean oil and emulsifying agent is 10:1；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 10,2h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, wherein, step
Suddenly（2）Aqueous phase and step（1）Oil phase mass ratio be 2:3,30min is then stirred, adds initiator potassium persulfate and friendship
Join agent N, N- methylene-bisacrylamide, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo, wherein, vacuum is done
Dry condition is that 4h is dried at 50 DEG C.
Embodiment 2
The preparation method of tapioca microballoon, comprises the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent Span60 is added, 50min is stirred at 60 DEG C, then at 50 DEG C
2h is incubated, wherein, the mass ratio of soybean oil and emulsifying agent is 10:1；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 10,3h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, wherein, step
Suddenly（2）Aqueous phase and step（1）Oil phase mass ratio be 2:3,30min is then stirred, adds initiator potassium persulfate and friendship
Join agent N, N- methylene-bisacrylamide, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo, wherein, vacuum is done
Dry condition is that 6h is dried at 50 DEG C.
Embodiment 3
The preparation method of tapioca microballoon, comprises the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent Span60 is added, 40min is stirred at 60 DEG C, then at 50 DEG C
2h is incubated, wherein, the mass ratio of soybean oil and emulsifying agent is 10:1；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 11,2.5h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, wherein, step
Suddenly（2）Aqueous phase and step（1）Oil phase mass ratio be 2:3,30min is then stirred, adds initiator potassium persulfate and friendship
Join agent N, N- methylene-bisacrylamide, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo, wherein, vacuum is done
Dry condition is that 5h is dried at 50 DEG C.
Embodiment 4
The preparation method of tapioca microballoon, comprises the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent Span60 is added, 46min is stirred at 60 DEG C, then at 50 DEG C
2h is incubated, wherein, the mass ratio of soybean oil and emulsifying agent is 10:1；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 12,2.6h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, wherein, step
Suddenly（2）Aqueous phase and step（1）Oil phase mass ratio be 2:3,30min is then stirred, adds initiator potassium persulfate and friendship
Join agent N, N- methylene-bisacrylamide, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo, wherein, vacuum is done
Dry condition is that 5.2h is dried at 50 DEG C.
By the tapioca microballoon that above-described embodiment is prepared by scanning electron microscopic observation, its rough surface, there is depression,
More, regular shape is adhered, particle diameter is between 30-80 microns.
Claims (8)
1. the preparation method of tapioca microballoon, it is characterised in that：Comprise the following steps：
（1）The preparation of oil phase：Soybean oil is weighed, emulsifying agent is added, 30-50min is stirred at 60 DEG C, is then incubated at 50 DEG C
2h；
（2）The preparation of aqueous phase：According to solid-liquid ratio 3:10, tapioca starch is added to the water, stirred, is adjusted with 2mol/L NaOH solution
The pH of system to 10-12,2-3h is stirred at 70 DEG C, be subsequently cooled to 35 DEG C, stand 30min；
（3）Under 600r/min stirring, by step（2）Aqueous phase step is added dropwise（1）Oil phase in, then stir
30min, initiator and crosslinking agent are added, stir 6h, centrifuge the oil phase for removing upper strata, lower floor obtains spherex, will formed sediment
Powder microballoon is washed with ethyl acetate, acetone, absolute ethyl alcohol successively, centrifuges, sediment is dried in vacuo.
2. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（1）Described in breast
Agent is Span60.
3. the preparation method of tapioca microballoon according to claim 2, it is characterised in that：Step（1）Described in it is big
The mass ratio of soya-bean oil and emulsifying agent is 10:1.
4. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（2）Middle tapioca starch
Preparation method is：By cassava stripping and slicing, 6h is dried at 105 DEG C, is then crushed, cross 200 mesh sieves.
5. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（3）Middle step（2）'s
Aqueous phase and step（1）Oil phase mass ratio be 2:3.
6. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（3）Described in draw
Hair agent is potassium peroxydisulfate.
7. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（3）Described in friendship
Connection agent is N,N methylene bis acrylamide.
8. the preparation method of tapioca microballoon according to claim 1, it is characterised in that：Step（3）Described in vacuum
Dry condition is that 4-6h is dried at 50 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711015813.8A CN107814880A (en) | 2017-10-25 | 2017-10-25 | The preparation method of tapioca microballoon |
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| CN201711015813.8A CN107814880A (en) | 2017-10-25 | 2017-10-25 | The preparation method of tapioca microballoon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111961235A (en) * | 2020-08-26 | 2020-11-20 | 吉林农业大学 | Preparation method of quinoa starch microspheres |
| CN112472866A (en) * | 2020-12-16 | 2021-03-12 | 山西省生物研究院有限公司 | Preparation method of starch microsphere and human recombinant tissue factor lipidated compound hemostatic material |
| CN113480693A (en) * | 2021-06-25 | 2021-10-08 | 广西大学 | Preparation method of cassava residue/polyvinyl alcohol semi-through network super-absorbent microspheres |
| CN114867365A (en) * | 2019-12-23 | 2022-08-05 | 嘉吉公司 | Soluble tapioca flour composition |
-
2017
- 2017-10-25 CN CN201711015813.8A patent/CN107814880A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114867365A (en) * | 2019-12-23 | 2022-08-05 | 嘉吉公司 | Soluble tapioca flour composition |
| CN111961235A (en) * | 2020-08-26 | 2020-11-20 | 吉林农业大学 | Preparation method of quinoa starch microspheres |
| CN112472866A (en) * | 2020-12-16 | 2021-03-12 | 山西省生物研究院有限公司 | Preparation method of starch microsphere and human recombinant tissue factor lipidated compound hemostatic material |
| CN113480693A (en) * | 2021-06-25 | 2021-10-08 | 广西大学 | Preparation method of cassava residue/polyvinyl alcohol semi-through network super-absorbent microspheres |
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Application publication date: 20180320 |