CN102204940B - Evening primrose oil microcapsule and pulverization method - Google Patents
Evening primrose oil microcapsule and pulverization method Download PDFInfo
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- CN102204940B CN102204940B CN201110127596.8A CN201110127596A CN102204940B CN 102204940 B CN102204940 B CN 102204940B CN 201110127596 A CN201110127596 A CN 201110127596A CN 102204940 B CN102204940 B CN 102204940B
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- oenotherae erythrosepalae
- erythrosepalae oil
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Abstract
The invention relates to an evening primrose oil microcapsule and a pulverization method. Evening primrose oil is difficult to dissolve in water and ethanol, is easy to be oxidized by oxygen and has a special grease taste; currently, crude evening primrose oil and evening primrose oil soft microcapsule are mainly products in a market, thereby greatly limiting the application range of the evening primrose oil as a functional health care product and a food additive. The evening primrose oil microcapsule is characterized by comprising the following components in parts by weight: 1 part of evening primrose oil core material, 0.6-8.5 parts of acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III and 0.05-0.5 part of polyoxyethylene hydrogenated castor oil RH40. The evening primrose oil microcapsule is applied to the field of medicaments.
Description
technical field:
invention relates to a kind of for field of medicaments; Be specifically related to a kind of Radix Oenotherae erythrosepalae oil microcapsule and powdered method.
background technology:
radix Oenotherae erythrosepalae is the wild plant of the Northeast of China, and reserves are abundant, wide material sources, and its seed oil is called Radix Oenotherae erythrosepalae oil, has multiple physiologically active.In Radix Oenotherae erythrosepalae oil, contain various human bulk-growth must, can not be synthetic in body unsaturated fatty acid, gamma-Linolenic acid as rare in linolenic acid, linoleic acid, arachidonic acid and plant kingdom.Human body also can be changed various fatty acid, to meet the demand of Human Physiology, but for the specific fatty acid of minority as gamma-Linolenic acid, linoleic acid plus linolenic acid, human body but cannot synthesize voluntarily, must be obtained by food intake.Modern pharmacological research proves: Radix Oenotherae erythrosepalae oil has the blood fat of reduction, atherosclerosis, fat-reducing, antiinflammatory, anticoagulation and antidotal effect.Expand the clinical practice of Radix Oenotherae erythrosepalae oil and the novel form of exploitation Radix Oenotherae erythrosepalae oil, to making full use of Radix Oenotherae erythrosepalae oil, open up its new advantage in disease treatment and health care significant.
radix Oenotherae erythrosepalae oil is insoluble in water and ethanol, is easily oxidized by oxygen, and has special oils and fats abnormal smells from the patient, and the product that goes on the market at present, also only take Radix Oenotherae erythrosepalae oil crude oil and soft capsule as main, has limited the range of application of Radix Oenotherae erythrosepalae oil as functional health product and food additive greatly.Improving the antioxygenic property of Radix Oenotherae erythrosepalae oil, and be prepared into and have good mobility, dispersibility and palatability, and be difficult for the powder of the moisture absorption, is the key addressing the above problem.
document " research of a Mictoencapsulation of Evening Primrose Oil " literary composition has been reported take arabic gum and gelatin as wall material, adopt complex coacervation to carry out micro encapsulation to Radix Oenotherae erythrosepalae oil, and in preparation process, need to use formaldehyde to be cured processing, this brings very large impact to product quality.In addition, this product water content in preparation process is very high, be difficult to be dried, and complex process, poor reproducibility, cost is high, and the cycle is long, and product is after long-time placement, and mobility variation, is prone to caking in various degree.
in document " micro encapsulation of starch octenyl succinate anhydride to Radix Oenotherae erythrosepalae oil ", report that use starch sodium octenyl succinate, as wall material, prepares Radix Oenotherae erythrosepalae oil microcapsule by spray drying method.In preparation process, need to use spray drying device to be prepared, and the parameter of equipment is larger on properties of microcapsules impact; In addition, the substitution value of starch sodium octenyl succinate also has larger impact to properties of product.This legal system is high for the power consumption of Radix Oenotherae erythrosepalae oil microcapsule, and the specification requirement of wall material is high, and complicated operation is wayward, and production cost is higher, and the softgel shell compactness forming is poor, causes oxidation resistance poor, and shelf life of products is short.
summary of the invention:
the object of invention is to provide solvent-non-solvent method that a kind of adopting process is simple, equipment cost is cheap and prepares Radix Oenotherae erythrosepalae oil microcapsule.
above-mentioned object realizes by following technical scheme:
a powdered method for Radix Oenotherae erythrosepalae oil microcapsule, this method adopts solvent-non-solvent method that Radix Oenotherae erythrosepalae oil is overmolding to microcapsule, and described solvent-non-solvent method comprises the following steps:
1) EudragitⅡ or Eudragit Ⅲ or EudragitⅡ and Eudragit Ⅲ mixture are mixed by a certain percentage, with dissolve with ethanol, as wall material solution; The parts by weight of described Radix Oenotherae erythrosepalae oil core are 1, and the parts by weight of described acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III are 0.6 ~ 8.5; The parts by weight of described polyoxyethylene hydrogenated Oleum Ricini RH40 are 0.05 ~ 0.5;
2) add Radix Oenotherae erythrosepalae oil and polyoxyethylene hydrogenated Oleum Ricini RH40, high-shear emulsifying disperses to form stable O/W type Emulsion;
3) stir the while to core, wall material and middle dropping sodium dodecyl sulfate solution, along with the continuous increase of water content in system, the concentration of ethanol is reduced, cause wall material dissolubility to decline and from system, separate out the coated core-clad material Radix Oenotherae erythrosepalae oil microcapsule that forms;
4) after filtering, by 0.2% sodium dodecyl sulfate solution washed twice, refilter, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microscapsule powder.
a kind of Radix Oenotherae erythrosepalae oil microcapsule, its composition comprises: Radix Oenotherae erythrosepalae oil core, acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III, polyoxyethylene hydrogenated Oleum Ricini RH40, it is characterized in that: the parts by weight of described Radix Oenotherae erythrosepalae oil core are 1, the parts by weight of described acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III are 0.6 ~ 8.5; The parts by weight of described polyoxyethylene hydrogenated Oleum Ricini RH40 are 0.05 ~ 0.5.
beneficial effect:
1. prepared by solvent-non-solvent method that adopting process of the present invention is simple, equipment cost is cheap, wall material is selected enteric material acrylic resin, can regulate release position and the properties of product of microcapsule.
the present invention is by carrying out accelerated oxidation experiment contrast with the Radix Oenotherae erythrosepalae oil of micro encapsulation not, and result shows that Radix Oenotherae erythrosepalae oil microcapsule has good antioxygenic property, and microscopic pattern is spheroidal, and dispersibility is fine.
acrylic resin good film-forming property of the present invention, the fine and close flexible of film, moisture resistance, can improve medicine stability; Minimizing oils and fats reacts with external environment (oxygen, illumination); Reduce the volatilization degree of volatile oil; Be convenient to processing and store; Control the release of capsule-core; Cover the abnormal smells from the patient of capsule-core; When capsule-core consumption hour, be convenient to accurately take and make dose comparison accurate.
the present invention is by carrying out accelerated oxidation experiment contrast with the Radix Oenotherae erythrosepalae oil of micro encapsulation not, and result shows that Radix Oenotherae erythrosepalae oil microcapsule has good antioxygenic property; The mean diameter that records microscapsule powder by laser particle analyzer is 0.1 ~ 25 μ m; Be spheroidal, surface compact and good dispersion by the microscopic pattern of sem observation microcapsule.
the present invention at room temperature, makes Radix Oenotherae erythrosepalae oil microscapsule powder by simple process condition, and the ethanol using can reclaim and reuse, and this preparation technology can realize zero-emission substantially.The Radix Oenotherae erythrosepalae oil microscapsule powder of preparing by the present invention, can prevent unsaturated fatty acid oxidative rancidity in Radix Oenotherae erythrosepalae oil effectively, has increased the stability of Radix Oenotherae erythrosepalae oil, keeps the activity of Radix Oenotherae erythrosepalae oil, has covered the offending abnormal smells from the patient of Radix Oenotherae erythrosepalae oil.Radix Oenotherae erythrosepalae oil powder is stored convenient transportation, has good mobility, dispersibility and palatability, and is difficult for the moisture absorption, is easy to add in food and health product.
technological operation of the present invention is simple, and envelop rate is up to more than 95%, and equipment needed thereby is simple, inexpensive, be easy to get, and production cost is low, and the cycle is short.
the present invention can effectively stop contacting of air and Radix Oenotherae erythrosepalae oil, protects its a large amount of unsaturated fatty acids that contain oxidized, effectively extends the holding time.
it is last that the present invention is prepared into microcapsule powder, and gained powder has good mobility, dispersibility and palatability, can be applicable to food, medicine, health product, cosmetics and food additive, greatly increased the range of application of Radix Oenotherae erythrosepalae oil.
accompanying drawing explanation:
accompanying drawing 1 is the Microcapsules Size scattergram of this product.
accompanying drawing 2 is scanning electron microscope (SEM) photographs of the microcapsule of this product.
accompanying drawing 3 is investigation figure of the antioxygenic property of this product.
the specific embodiment:
embodiment 1:
a powdered method for Radix Oenotherae erythrosepalae oil microcapsule, this method adopts solvent-non-solvent method that Radix Oenotherae erythrosepalae oil is overmolding to microcapsule, and described solvent-non-solvent method comprises the following steps:
1) EudragitⅡ or Eudragit Ⅲ or EudragitⅡ and Eudragit Ⅲ mixture are mixed by a certain percentage, with dissolve with ethanol, as wall material solution.
) add Radix Oenotherae erythrosepalae oil and polyoxyethylene hydrogenated Oleum Ricini RH40, high-shear emulsifying to disperse to form stable O/W type Emulsion.
) stir the while to core, wall material and middle dropping sodium dodecyl sulfate solution, along with the continuous increase of water content in system, the concentration of ethanol is reduced, cause wall material dissolubility to decline and from system, separate out the coated core-clad material Radix Oenotherae erythrosepalae oil microcapsule that forms.
) after filtration, by 0.2% sodium dodecyl sulfate solution washed twice, refilter, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microscapsule powder.
embodiment 2:
a kind of Radix Oenotherae erythrosepalae oil microcapsule, its composition comprises: Radix Oenotherae erythrosepalae oil core, acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III, polyoxyethylene hydrogenated Oleum Ricini RH40, it is characterized in that: the parts by weight of described Radix Oenotherae erythrosepalae oil core are 1, the parts by weight of described acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III are 0.6 ~ 8.5; The parts by weight of described polyoxyethylene hydrogenated Oleum Ricini RH40 are 0.05 ~ 0.5.In accompanying drawing 3, () is Radix Oenotherae erythrosepalae oil; (▲) is Radix Oenotherae erythrosepalae oil microcapsule.
embodiment 3:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ and Eudragit Ⅲ (1: 1) 8 g with after 95% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 2 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.2 g, 10000 rpm emulsifying 2 min, drip 0.2% sodium dodecyl sulfate solution with 50 ml acid burets, 1000 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use again 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microscapsule powder.The last Radix Oenotherae erythrosepalae oil microcapsule the obtaining powder that is white in color, good fluidity, oxidation resistance is fine, and the mean diameter of measuring this microcapsule by laser particle analyzer is 7.66 μ m, and envelop rate is 95.7%.
embodiment 4:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ and Eudragit Ⅲ (1: 1) 6 g with after 90% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 4 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.5 g, 12000 rpm emulsifying 2 min, drip 0.8% sodium dodecyl sulfate solution with 50 ml acid burets, 1000 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use again 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microcapsule.The microcapsule powder that is white in color, powder flowbility is higher, and oxidation resistance is good, and the mean diameter of microcapsule is 5.27 μ m, and envelop rate is 95.3%.
embodiment 5:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ and Eudragit Ⅲ (2: 1) 5 g with after 85% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 5 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.5 g, 18000 rpm emulsifying 3 min, drip 0.6% sodium dodecyl sulfate solution, 1200 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microcapsule again.The microcapsule powder that is creamy white, powder flowbility is higher, and oxidation resistance is better, and the mean diameter of microcapsule is 5.13 μ m, and distribution is narrower, and envelop rate is 96.06%.
embodiment 6:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ and Eudragit Ⅲ (1: 2) 7 g with after 70% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 3 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.35 g, 14000 rpm emulsifying 2 min, drip 5% sodium dodecyl sulfate solution with 50 ml acid burets, 800 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microcapsule again.The microcapsule powder that is creamy white, powder flowbility is good, and envelop rate is 95.5%, and oxidation resistance is good, and the mean diameter of microcapsule is 6.39 μ m, and narrow distribution range.
embodiment 7:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ and Eudragit Ⅲ (1: 1) 9 g with after 70% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 1 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.1 g, 10000 rpm emulsifying 3 min, drip 8% sodium dodecyl sulfate solution, 900 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microcapsule again.The microcapsule powder that is white in color, powder flowbility is good, and the mean diameter of microcapsule is 8.24 μ m, and distribution is wider, and oxidation resistance is fine, and envelop rate is 97.02%.
embodiment 8:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, take EudragitⅡ 4 g with after 95% dissolve with ethanol, add Radix Oenotherae erythrosepalae oil 6 g, polyoxyethylene hydrogenated Oleum Ricini RH40 0.55 g, 18000 rpm emulsifying 3 min, drip 2% sodium dodecyl sulfate solution with 50 ml acid burets, 1000 rpm constantly stir until separate out a large amount of microcapsule solids in solution simultaneously, after filtration, use 0.2% sodium dodecyl sulfate solution washed twice, after filtering, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microcapsule again.Microcapsule oxidation resistance is better, and envelop rate is 95.7%, and the mean diameter of microcapsule is 6.14 μ m, and distribution is narrower, the powder that is creamy white, and powder flowbility is higher.
embodiment 9:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, the preparation of Radix Oenotherae erythrosepalae oil microcapsule tablet
get the Radix Oenotherae erythrosepalae oil microcapsule that embodiment 3 makes, add starch, lactose, dextrin and make in right amount filler, add carboxymethyl starch sodium and make in right amount disintegrating agent, after mix homogeneously, make in right amount binding agent with 10% starch slurry, soft material processed, cross 18 mesh sieves granulations, dry, granulate, add 1% magnesium stearate and make lubricant, after mix homogeneously, tabletting, obtains tablet of the present invention.
embodiment 10:
radix Oenotherae erythrosepalae oil microcapsule described in above embodiment and powdered method, the preparation of Radix Oenotherae erythrosepalae oil microcapsule hard capsule
the Radix Oenotherae erythrosepalae oil microcapsule more than making, add starch, microcrystalline Cellulose and make in right amount filler, add low-substituted hydroxypropyl cellulose and make in right amount disintegrating agent, after mix homogeneously, make in right amount binding agent with 1% polyvidone alcoholic solution, soft material processed, cross 24 mesh sieves granulations, dry, granulate, add 1% micropowder silica gel and make lubricant, after mix homogeneously, in common gelatine capsule, obtain capsule of the present invention by particles filled.
Claims (2)
1.
a powdered method for Radix Oenotherae erythrosepalae oil microcapsule, is characterized in that: adopt solvent-non-solvent method that Radix Oenotherae erythrosepalae oil is overmolding to microcapsule, described solvent-non-solvent method comprises the following steps:
1) EudragitⅡ or Eudragit Ⅲ or EudragitⅡ and Eudragit Ⅲ mixture are mixed by a certain percentage, with dissolve with ethanol, as wall material solution; The parts by weight of Radix Oenotherae erythrosepalae oil core are 1, and the parts by weight of acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III are 0.6 ~ 8.5; The parts by weight of polyoxyethylene hydrogenated Oleum Ricini RH40 are 0.05 ~ 0.5;
2) add Radix Oenotherae erythrosepalae oil and polyoxyethylene hydrogenated Oleum Ricini RH40,10000 ~ 18000rpm emulsifying, 2 ~ 3min disperses to form stable O/W type Emulsion;
3) stir and in core, wall material, drip 0.2 ~ 8% sodium dodecyl sulfate solution simultaneously, along with the continuous increase of water content in system, the concentration of ethanol is reduced, cause wall material dissolubility to decline and from system, separate out the coated core-clad material Radix Oenotherae erythrosepalae oil microcapsule that forms;
4) after filtering, by 0.2% sodium dodecyl sulfate solution washed twice, refilter, drying under reduced pressure obtains Radix Oenotherae erythrosepalae oil microscapsule powder.
2.
a kind of Radix Oenotherae erythrosepalae oil microcapsule, its composition comprises: the mixture of Radix Oenotherae erythrosepalae oil core, acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III, polyoxyethylene hydrogenated Oleum Ricini RH40, it is characterized in that: the parts by weight of described Radix Oenotherae erythrosepalae oil core are 1, the parts by weight of the mixture of described acrylic resin II or acrylic resin III or acrylic resin II and acrylic resin III are 0.6 ~ 8.5; The parts by weight of described polyoxyethylene hydrogenated Oleum Ricini RH40 are 0.05 ~ 0.5.
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