CN1748717A - Method for prparing bee glue-ethyl cellulose microcapsule - Google Patents
Method for prparing bee glue-ethyl cellulose microcapsule Download PDFInfo
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- CN1748717A CN1748717A CNA2005100842284A CN200510084228A CN1748717A CN 1748717 A CN1748717 A CN 1748717A CN A2005100842284 A CNA2005100842284 A CN A2005100842284A CN 200510084228 A CN200510084228 A CN 200510084228A CN 1748717 A CN1748717 A CN 1748717A
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Abstract
The present invention belongs to the field of medicine and health food technology, and combines bee glue and microcapsule technology. The preparation process of bee glue-ethyl cellulose microcapsule includes the following steps: crushing bee glue extractum to 20-120 mesh and ethyl cellulose to 60-120 mesh; dissolving ethyl cellulose or chitosan in acetone or ethyl acetate solution to obtain solution A; dissolving crushed bee glue in solution A to obtain solution B; heating liquid paraffin in water bath at 20-55 deg c and adding emulsifier Span-80 via stirring to obtain solution C; adding solution B into solution C; stirring to form microcapsule, decompression suction filtering, washing, and drying at 25-35 deg c to obtain the bee glue-ethyl cellulose microcapsule of size 400-800 microns.
Description
Technical field
Propolis-ethyl cellulose microcapsule, its product is applicable to medicine, field of health care food.
Background technology
Propolis is the material that a class contains flavone compound, alcohol, aldehyde, phenol, and that acidic materials and part flavone have is antibiotic, antiinflammatory, antisepsis.Still isolate enzyme and aminoacid and multivitamin from propolis, wherein vitamin B1, vitamin PP, vitamin C, provitamin A and content of vitamin E are abundanter.
To be the forties in 20th century invented by professor D.E.Wuster of Univ Wisconsin-Madison USA microcapsule technology at first, and As time goes on, the microencapsulation technology is also ripe gradually.But the structure of microcapsule is variant along with the difference of process conditions.Particle diameter is also all influential to targeting of distributing in bioavailability and the body etc.Therefore, to the influential technological factor of the preparation of microcapsule, as the size of core-clad material, the consumption of capsule material, preparation method, preparation temperature when 20-55 ℃ of preparation stir speed (S.S.) and the concentration of additives all to be optimized screening.
And propolis is combined with microcapsule technology, make the propolis microcapsule and do not see bibliographical information at home and abroad as yet.Propolis is made the microcapsule product, both improved the stability of effective ingredient in the propolis, the factors such as air, moisture, light that prevent cause the variation of active component, be beneficial to absorption of human body, can reduce propolis product again directly stimulates gastrointestinal, is more convenient for further making food or the medicine being convenient to transport, have health care.Simultaneously, we can control the slow release degree and the Targeting Performance of propolis as required, bring more bigger facilities to life.
Summary of the invention
The present invention obtains that encystation is effective, the microcapsule rounding property is good, the surface is very smooth, the adhesion smaller or equal to 10%, average microcapsule diameter are arranged is 400-800 μ m.
The preparation method of propolis provided by the invention-ethyl cellulose microcapsule adopts intra-liquid desiccation method, it is characterized in that, may further comprise the steps:
(1) respectively the propolis extract powder is broken to the 20-120 order, ethyl cellulose or chitosan powder are broken to the 60-120 order; Propolis and ethyl cellulose mass ratio are 2.5: 1-4: 1, and propolis is 1 with the chitosan mass ratio: 1-1: 2;
(2) be under the 200rpm-500rpm ethyl cellulose or chitosan to be joined in acetone or the ethyl acetate solution dissolving fully with flow velocity 8-15ml/s at rotating speed, obtaining solution is A solution;
(3) the propolis extractum of pulverizing is added in the A solution under rotating speed 200-500rpm stirs and dissolve, obtaining solution is B solution, and B solution is stirred at rotating speed 80-120rpm;
(4) with the liquid paraffin water-bath, the control bath temperature adds purity and is 99.5% emulsifying agent Si Pan-80 while stirring between the 20-55 degree, make emulsifying agent be the dispersity of homogeneous in solution, and obtaining solution is C solution; Emulsifying agent Si Pan-80 volume is 3-10 with the ratio of liquid paraffin volume: 800;
(5) B solution is added in the C solution; Speed with 200-500rpm is stirred to microcapsule formation, decompress filter, and with petroleum ether or Ketohexamethylene washing, 25-35 ℃ of drying obtains propolis-ethyl cellulose microcapsule.
Description of drawings
Fig. 1 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 1.
Fig. 2 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 2.
Fig. 3 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 3.
Fig. 4 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 5.
Fig. 5 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 6.
Fig. 6 is the sem photograph of propolis-ethyl cellulose microcapsule of embodiment 7.
Fig. 7 is the sem photograph of propolis-chitosan microcapsules of embodiment 12.
The specific embodiment:
Embodiment 1: the propolis extract powder is broken to 80 orders, ethyl cellulose is crushed to 120 orders, propolis and ethyl cellulose amount ratio are 3: 1, at rotating speed is under the 250rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 250rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 20 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 250rpm is stirred to microcapsule formation.Decompress filter is used petroleum ether, and 25 ℃ of dryings obtain that encystation is effective, the microcapsule rounding property is good, the surface is very smooth, adhesion smaller or equal to 10% is arranged, particle size distribution is at the microcapsule of 400-800 μ m.
Embodiment 2: the propolis extract powder is broken to 60 orders, ethyl cellulose is crushed to 120 orders, propolis and ethyl cellulose amount ratio are 3: 1, at rotating speed is under the 250rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 250rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 25 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 5: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 250rpm is stirred to microcapsule formation.Decompress filter is used petroleum ether, and 35 ℃ of dryings obtain that encystation is effective, the microcapsule rounding property is good, the surface is very smooth, the adhesion smaller or equal to 5%, average microcapsule diameter are arranged is the microcapsule of 800 μ m.
Embodiment 3: the propolis extract powder is broken to 60 orders, ethyl cellulose is crushed to 80 orders, propolis and ethyl cellulose amount ratio are 4: 1, at rotating speed is under the 300rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 300rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 55 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 10: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 300rpm is stirred to microcapsule formation.Decompress filter is used petroleum ether, 25 ℃ of dryings, and obtaining that encystation is respond well, the microcapsule rounding property is medium, the adhesion smaller or equal to 10%, average microcapsule diameter are arranged is the microcapsule of 400 μ m.
Embodiment 4: the propolis extract powder is broken to 80 orders, ethyl cellulose is crushed to 60 orders, propolis and ethyl cellulose amount ratio are 4: 1, at rotating speed is under the 500rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 500rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 30 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 500rpm is stirred to microcapsule formation.Decompress filter is used petroleum ether, and 25 ℃ of dryings obtain that the encystation effect is medium, the microcapsule rounding property is relatively poor, adhesion smaller or equal to 10% is arranged, particle size distribution is at the microcapsule of 150-500 μ m.
Embodiment 5: the propolis extract powder is broken to 20 orders, ethyl cellulose is crushed to 120 orders, propolis and ethyl cellulose amount ratio are 4: 1, at rotating speed is under the 230rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 230rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 25 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 230rpm is stirred to microcapsule formation.Decompress filter is used petroleum ether, and 25 ℃ of dryings obtain that encystation is respond well, the microcapsule rounding property is good, smooth surface, the adhesion smaller or equal to 5%, average microcapsule diameter are arranged is the microcapsule of 900 μ m.
Embodiment 6: the propolis extract powder is broken to 80 orders, ethyl cellulose is crushed to 100 orders, propolis and ethyl cellulose amount ratio are 3: 1, at rotating speed is under the 200rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 200rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 30 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 200rpm is stirred to microcapsule formation.Decompress filter with Ketohexamethylene washing, 30 ℃ of dryings, obtains that encystation is respond well, the microcapsule rounding property good, smooth surface, the adhesion smaller or equal to 5%, average microcapsule diameter are arranged is the microcapsule of 1000 μ m.
Embodiment 7: the propolis extract powder is broken to 100 orders, ethyl cellulose is crushed to 100 orders, propolis and ethyl cellulose amount ratio are 2.5: 1, at rotating speed is under the 250rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 250rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 30 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 250rpm is stirred to microcapsule formation.Decompress filter, with Ketohexamethylene washing, 30 ℃ of dryings, obtain that encystation is respond well, the microcapsule rounding property good, smooth surface, size evenly, it is the microcapsule of 700 μ m that the adhesion smaller or equal to 5%, average microcapsule diameter are arranged.
Embodiment 8: the propolis extract powder is broken to 20 orders, ethyl cellulose is crushed to 80 orders, propolis and ethyl cellulose amount ratio are 4: 1, at rotating speed is under the 500rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 500rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 35 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 500rpm is stirred to microcapsule formation.Decompress filter with Ketohexamethylene washing, 30 ℃ of dryings, obtains that encystation is respond well, the microcapsule rounding property is medium, adhesion smaller or equal to 10% is arranged, particle size distribution is at the microcapsule of 150-500 μ m.
Embodiment 9: the propolis extract powder is broken to 80 orders, ethyl cellulose is crushed to 60 orders, propolis and ethyl cellulose amount ratio are 2.5: 1, at rotating speed is under the 250rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 250rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 55 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 250rpm is stirred to microcapsule formation.Decompress filter, the adhesion that with Ketohexamethylene washing, 30 ℃ of dryings, obtain that the encystation effect is medium, the microcapsule rounding property is relatively poor, 20%-30% is arranged, particle size distribution are at the microcapsule of 400-800 μ m.
Embodiment 10: the propolis extract powder is broken to 80 orders, ethyl cellulose is crushed to 120 orders, propolis and ethyl cellulose amount ratio are 2.5: 1, at rotating speed is under the 200rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 200rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 40 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 200rpm is stirred to microcapsule formation.Decompress filter with Ketohexamethylene washing, 30 ℃ of dryings, obtains that encystation is effective, the microcapsule rounding property is good, adhesion smaller or equal to 5% is arranged, particle size distribution is at the microcapsule of 500-900 μ m.
Embodiment 11: the propolis extract powder is broken to 120 orders, ethyl cellulose is crushed to 80 orders, propolis and ethyl cellulose amount ratio are 2.5: 1, at rotating speed is under the 200rpm 5g ethyl cellulose to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 200rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 30 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 3: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 200rpm is stirred to microcapsule formation.Decompress filter with Ketohexamethylene washing, 30 ℃ of dryings, obtains that encystation is respond well, the microcapsule rounding property good, adhesion smaller or equal to 10% is arranged, particle size distribution is at the microcapsule of 500-900 μ m.
Embodiment 12: the propolis extract powder is broken to 120 orders, chitosan powder is broken to 80 orders, propolis is 1: 1 with the chitosan dosage ratio, earlier with the chitosan glutaraldehyde cross-linking, at rotating speed is under the 300rpm 40g chitosan to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 300rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 35 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 5: 800 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 300rpm is stirred to microcapsule formation.Decompress filter, with Ketohexamethylene washing, 30 ℃ of dryings, obtaining that encystation is effective, the microcapsule rounding property is good, adhesion, microcapsule mean diameter smaller or equal to 5% are arranged is the microcapsule of 300 μ m.
Embodiment 13: the propolis extract powder is broken to 80 orders, chitosan powder is broken to 120 orders, propolis is 1: 2 with the chitosan dosage ratio, earlier with the chitosan glutaraldehyde cross-linking, at rotating speed is under the 250rpm 40g chitosan to be joined in 200ml-300ml acetone or the ethyl acetate solution with flow velocity 8-15ml/s to dissolve, and obtaining solution is A solution.The propolis extractum of pulverizing added in the A solution under rotating speed 250rpm stirs dissolve, obtaining solution is B solution, and B solution is left standstill under rotating speed 80-120rpm stirs.As for water-bath in the beaker, the control bath temperature adds emulsifying agent Si Pan-80 while stirring at 30 ℃ with the 800ml liquid paraffin, and emulsifying agent Si Pan-80 volume is 1: 200 with the ratio of liquid paraffin volume, and B solution is added in the C solution.Speed with 250rpm is stirred to microcapsule formation.Decompress filter with Ketohexamethylene washing, 30 ℃ of dryings, obtains that encystation is effective, the microcapsule rounding property is good, adhesion smaller or equal to 5% is arranged, particle size distribution is at the microcapsule of 80-250 μ m.
Claims (1)
1, the preparation method of propolis-ethyl cellulose microcapsule is characterized in that, may further comprise the steps:
Step 1) is broken to the 20-120 order with the propolis extract powder respectively, and ethyl cellulose or chitosan powder are broken to the 60-120 order; Propolis and ethyl cellulose mass ratio are 2.5: 1-4: 1, and propolis is 1 with the chitosan mass ratio: 1-1: 2;
Step 2) be under the 200rpm-500rpm ethyl cellulose or chitosan to be joined in acetone or the ethyl acetate solution dissolving fully with flow velocity 8-15ml/s at rotating speed, obtaining solution is A solution;
Step 3) adds to the propolis extractum of pulverizing in the A solution under rotating speed 200-500rpm stirs dissolves, and obtaining solution is B solution, and B solution is stirred at rotating speed 80-120rpm;
Step 4) is the liquid paraffin water-bath, and the control bath temperature adds purity and be 99.5% emulsifying agent Si Pan-80 while stirring between the 20-55 degree, make emulsifying agent be the dispersity of homogeneous in solution, and obtaining solution is C solution; Emulsifying agent Si Pan-80 volume is 3-10 with the ratio of liquid paraffin volume: 800;
Step 5) is added to B solution in the C solution; Speed with 200-500rpm is stirred to microcapsule formation, decompress filter, and with petroleum ether or Ketohexamethylene washing, 25-35 ℃ of drying obtains propolis-ethyl cellulose microcapsule.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100842284A CN1303984C (en) | 2005-07-18 | 2005-07-18 | Method for prparing bee glue-ethyl cellulose microcapsule |
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| CNB2005100842284A CN1303984C (en) | 2005-07-18 | 2005-07-18 | Method for prparing bee glue-ethyl cellulose microcapsule |
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| CN1748717A true CN1748717A (en) | 2006-03-22 |
| CN1303984C CN1303984C (en) | 2007-03-14 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101011419B (en) * | 2007-02-06 | 2011-01-19 | 傅金龙 | Propolis preparation and its preparation method |
| CN102174123A (en) * | 2011-02-25 | 2011-09-07 | 重庆大学 | Production method of water soluble flavone-chitosan derivative |
| CN102641256A (en) * | 2012-05-03 | 2012-08-22 | 青岛绿曼生物工程有限公司 | Preparation method for propolis micro-capsules |
| TWI402084B (en) * | 2007-11-30 | 2013-07-21 | Food Industry Res & Dev Inst | Microcapsules and method of preparing the same |
| CN112494456A (en) * | 2020-12-16 | 2021-03-16 | 西南石油大学 | Ethyl cellulose hollow microcapsule |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3614261B2 (en) * | 1996-11-08 | 2005-01-26 | 森川健康堂株式会社 | Method for producing microcapsules |
| JP3081873B2 (en) * | 1997-02-03 | 2000-08-28 | 株式会社シャブロン | Cellulose with propolis |
| JP2003000161A (en) * | 2001-06-20 | 2003-01-07 | Fancl Corp | Power composition of propolis extract and method for producing the same |
| CN1220497C (en) * | 2001-09-18 | 2005-09-28 | 姜德勇 | Antivirus antioxidizing active extract of proplis and its molecular inclusion compound |
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2005
- 2005-07-18 CN CNB2005100842284A patent/CN1303984C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101011419B (en) * | 2007-02-06 | 2011-01-19 | 傅金龙 | Propolis preparation and its preparation method |
| TWI402084B (en) * | 2007-11-30 | 2013-07-21 | Food Industry Res & Dev Inst | Microcapsules and method of preparing the same |
| CN102174123A (en) * | 2011-02-25 | 2011-09-07 | 重庆大学 | Production method of water soluble flavone-chitosan derivative |
| CN102174123B (en) * | 2011-02-25 | 2012-09-26 | 重庆大学 | Production method of water soluble flavone-chitosan derivative |
| CN102641256A (en) * | 2012-05-03 | 2012-08-22 | 青岛绿曼生物工程有限公司 | Preparation method for propolis micro-capsules |
| CN102641256B (en) * | 2012-05-03 | 2014-12-03 | 青岛绿曼生物工程有限公司 | Preparation method for propolis micro-capsules |
| CN112494456A (en) * | 2020-12-16 | 2021-03-16 | 西南石油大学 | Ethyl cellulose hollow microcapsule |
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