CN102860996B - Method for preparing lycoypene microcapsule - Google Patents

Method for preparing lycoypene microcapsule Download PDF

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CN102860996B
CN102860996B CN 201210397726 CN201210397726A CN102860996B CN 102860996 B CN102860996 B CN 102860996B CN 201210397726 CN201210397726 CN 201210397726 CN 201210397726 A CN201210397726 A CN 201210397726A CN 102860996 B CN102860996 B CN 102860996B
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lycopene
wall material
core
oil phase
weight ratio
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CN102860996A (en
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冯鹏
沈建
钱一帆
刘诚
冯敏
王连安
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NANJING ZHONGKE PHARMACEUTICAL CO Ltd
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Abstract

The invention discloses a method for preparing a lycoypene microcapsule. The method includes that lycoypene is prepared to be core materials and the core materials and wall materials are subjected to homogeneous emulsifying and spray drying. The wall materials are prepared by gelatins, sporoderm-broken ganoderma lucidum spore powders, cane sugars and skim milk powders, the weight ratio of the gelatins, the sporoderm-broken ganoderma lucidum spore powders, the cane sugars and the skim milk powders is 1:1:1:(1.2-1.6), and the core materials are prepared by the lycopene, salad oil and sucrose esters. According to the method for preparing the lycoypene microcapsule, a specific microcapsule technology is utilized to embed the lycoypene, the stability of the lycoypene microcapsule is improved, simultaneously the water solubility is improved, and the application field is widened.

Description

The preparation method of lycopene microcapsule
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of preparation method of lycopene microcapsule.
Background technology
Lycopene (Lycopene) is a kind of of carotenoid, extensively is present in the plants such as Fructus Lycopersici esculenti, Citrullus vulgaris, Fructus Vitis viniferae, Radix Dauci Sativae.Because lycopene does not have the physiologically active of vitamin A, its effect is not taken seriously always.But research in recent years shows, lycopene has the performance more more superior than other carotene, as the ability of removing singlet oxygen is 100 times of vitamin E, is that the twice of bata-carotene is many.Lycopene can improve immunity of organisms, and anticancer propagation reduces the DNA loss, prevents LDL oxidation, reduces the cholesterol level in blood, therefore can reduce the incidence rate of various diseases.
Lycopene is generally peony powder or oily liquids, and sterling is needle-like peony crystal, is orange-yellow in lower concentration solutions, and its fusing point is 174 ℃ (trans), incendivity.As aliphatic hydrocarbon, lycopene is water insoluble, is insoluble in methanol, ethanol isopolarity organic solvent, dissolves in ether, petroleum ether, ethane, acetone, is soluble in chloroform, Carbon bisulfide, benzene, oils and fats etc.Lycopene purity is higher, dissolves more difficultly, and the dissolubility in various solvents increases along with the rising of temperature.Lycopene contains a large amount of unsaturations, easily is heated in the period of processing and storing, the factor impact such as light, oxygen, additive and degraded and isomerization occur, thereby reduces physiologically active.
In order to take full advantage of lycopene, can adopt microcapsule technology by the lycopene embedding, avoid lycopene to contact with the direct of external environment, and then improved stability.So-called microcapsule technology, by selecting suitable filmogen (wall material) liquid, solid or even gas (core) to be coated to the technology that forms molecule, after microcapsule is processed, core does not directly contact with the external environment factor, is effectively protected exactly.But the technique of existing On Technique of Microencapsulation of Lycopene is difficult to guarantee the long-time stability of water solublity and the active constituent content thereof of lycopene microcapsule.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method that improves stability and can improve water miscible lycopene microcapsule, and then enlarge the application of lycopene microcapsule.
The objective of the invention is to realize in the following manner:
A kind of preparation method of lycopene microcapsule, after the method mainly is prepared into core by lycopene, again with the process emulsifying of wall material and spray drying step, wherein, described wall material is prepared by following methods: the gelatin that the weight ratio of take is 1:1:1:1.2~1.6, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder are wall material raw material, add 3~5 times of amount distilled water of above-mentioned material, are heated to 40~45 ℃, stirring becomes uniform suspension, is the wall material.Preferably the wall material is prepared by following methods: the gelatin that the weight ratio of take is 1:1:1:1.4, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder are wall material raw material, add 4 times of amount distilled water of above-mentioned material, be heated to 45 ℃, stir and become uniform suspension, be the wall material.
Described core is prepared by following methods: every 0.5~0.8g lycopene is dissolved in the salad oil of 1ml, and adds sucrose ester to make emulsifying agent, stir and be core, the weight ratio of lycopene and sucrose ester is 10~14:1; Preferably core is prepared by following methods: every 0.68g lycopene is dissolved in the salad oil of 1ml, and adds sucrose ester to make emulsifying agent, stir and be core, the weight ratio of lycopene and sucrose ester is 8.5:0.7.
Wherein, described salad oil can be soybean salad oil, rape salad oil, sunflower seed salad oil, Testa oryzae salad wet goods edible salad oil commonly used.The Ganoderma spore powder with cellular wall broken that Ganoderma spore powder with cellular wall broken should select sporoderm-broken rate to be greater than 95%.
Above-mentioned emulsifying comprises the following steps: the mixed liquor of core and wall material of take is oil phase, slowly add while stirring oil phase in water, water and oil phase weight ratio are 3~3.5:5~6, then are placed in colloid mill, under 5000~10000 rev/mins of conditions, grind, milling time is 20~40min.
Preferably emulsifying comprises the following steps: the mixed liquor of core and wall material of take is oil phase, slowly adds while stirring oil phase in water, and water and oil phase weight ratio are 3:5, then are placed in colloid mill, under 6000 rev/mins of conditions, grind, and milling time is 30min.
Described spray drying condition is: the spray drying inlet temperature is 170 ~ 180 ℃, and leaving air temp is 80 ~ 100 ℃, and feeding temperature is 45 ~ 50 ℃, and charging rate is 0.6 ~ 1.0 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.The preferably spray drying condition is: the spray drying inlet temperature is 180 ℃, and leaving air temp is 80 ~ 100 ℃, and feeding temperature is 50 ℃, and charging rate is 0.6 ~ 1.0 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
Beneficial effect of the present invention compared with the prior art:
That the present invention selects is film-formable, meet the requirement of state food additive, nontoxic to human body, meet water and easily discharge the material of core as the wall material; and adopt suitable Microencapsulation Method by lycopene be coated on one small and the sealing film in; make it to change into tractable powder solid; protect responsive lycopene, prevent that it is oxidized.The wall material that particularly the present invention adopts new material to make can be realized the slow release of core, extension function factor action time, the stability of lycopene microcapsule is significantly improved, and the core that adopts formula of the present invention to prepare makes the present invention's wall material used more easily by its coating.The present invention adopts specific microcapsule technology embedding lycopene, in the stability that improves effective ingredient, can also improve the water solublity of lycopene microcapsule, and then enlarges application.
The specific embodiment
Below according to embodiment, the invention will be further described, and the specific embodiments of following examples just is described more specifically the present invention, and the present invention is not limited to the content of following examples.The described lycopene of following examples is the lycopene raw material, and for Israel Le Kangruide (Lycored) company produces, purity is 98%; Salad oil is golden imperial fish soybean salad oil, and manufacturer is grain and oil Industrial Co., Ltd in praise in Shanghai; Sucrose ester (being sucrose fatty acid ester) manufacturer is Liuzhou Ai Gefu food science and technology company limited; Ganoderma spore powder with cellular wall broken (sporoderm-broken rate is greater than 95%) manufacturer is NanJing ZhongKe Pharmacy Co., Ltd; The manufacturer of defatted milk powder is Heilungkiang flying crane dairy industry company limited; Commercial lycopene microcapsule 1 is that India Parry Nutraceutical company produces; Commercial lycopene microcapsule 2 is that Israel Le Kangruide (Lycored) company produces.
Embodiment 1
1, core preparation: the 8.5g lycopene is added in the salad oil of 12.5ml, and add the 0.7g sucrose ester and make emulsifying agent, stir, this is oil phase A.
2, wall material preparation: gelatin, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder (being wall material raw material) that to get part by weight be 1:1:1:1.4, add 4 times of amount distilled water of wall material raw material, be heated to 45 ℃, stir and make it to become uniform suspension, this is oil phase B.
3, emulsifying: the mixed liquor that slowly adds while stirring oil phase A and oil phase B in water, the weight ratio of water and oil phase (being oil phase A and oil phase B sum) is 3:5, be placed in again colloid mill, under 6000 rev/mins of conditions, grind, milling time is 30min, lycopene is scattered in the wall material equably, obtains the emulsion after homogenizing.
Obtain Powdered lycopene microcapsule by the emulsion after homogenizing is spray-dried.Spray-dired controlled condition is: the spray drying inlet temperature is 180 ℃, and leaving air temp is 90 ℃, and feeding temperature is 50 ℃, and charging rate is 0.8 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
Stability test and the testing result of the present embodiment lycopene microcapsule content:
By the lycopene microcapsule for preparing, the lycopene raw material of micro encapsulation and commercial lycopene microcapsule 1, commercial lycopene microcapsule 2 are not loaded on respectively sealing storage in transparent sample bottle, at the lower natural light irradiation that adopts of room temperature (20 ± 5 ℃), the content of lycopene in the sampling and measuring sample, compare to obtain retention rate with the content of lycopene in sample before storage at set intervals.The assay result that table 1 is lycopene in different samples, wherein, the content of lycopene assay method is according to national standard: GB/T22249-2008.
Table 1
Figure 2012103977264A00800011
The present embodiment lycopene microcapsule testing result disintegration is in Table 2, adopt 2010 editions " Chinese pharmacopoeia appendix method is carried out Parallel testing three times:
Table 2
Figure 2012103977264A00800012
Embodiment 2
1, core preparation: the 8g lycopene is added in the salad oil of 12.5ml, and add the 0.7g sucrose ester and make emulsifying agent, stir, this is oil phase A.
2, wall material preparation: gelatin, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder (being wall material raw material) that to get part by weight be 1:1:1:1.2, add 3 times of amount distilled water of wall material raw material, be heated to 45 ℃, stir and make it to become uniform suspension, this is oil phase B.
3, emulsifying: the mixed liquor that slowly adds while stirring oil phase A and oil phase B in water, the weight ratio of water and oil phase is 3:5, be placed in again colloid mill, under 8000 rev/mins of conditions, grind, milling time is 25min, be about to lycopene and be scattered in equably in the wall material, obtain the emulsion after homogenizing.
Emulsion after homogenizing is spray-dried obtains Powdered lycopene product.Spray-dired controlled condition is: the spray drying inlet temperature is 180 ℃, and leaving air temp is 80 ℃, and feeding temperature is 45 ℃, and charging rate is 0.6 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
In the present embodiment lycopene microcapsule, the Detection of Stability of lycopene content the results are shown in Table 3, and detection method is with embodiment 1:
Table 3
Figure 2012103977264A00800013
Detection disintegration of the present embodiment lycopene microcapsule adopts 2010 editions, and " Chinese pharmacopoeia appendix method is carried out, and it is 46min that three Parallel testings obtain average disintegration time.
Embodiment 3
1, core preparation: the 9g lycopene is added in the salad oil of 12.5ml, and add the 0.7g sucrose ester and make emulsifying agent, stir, this is oil phase A.
2, wall material preparation: gelatin, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder (being wall material raw material) that to get part by weight be 1:1:1:1.6, add 5 times of amount distilled water of wall material raw material, be heated to 40 ℃, stir and make it to become uniform suspension, this is oil phase B.
3, emulsifying: the mixed liquor that slowly adds while stirring oil phase A and oil phase B in water, the weight ratio of water and oil phase is 3.5:5, be placed in again colloid mill, under 5000 rev/mins of conditions, grind, milling time is 35min, lycopene is scattered in the wall material equably, obtains the emulsion after homogenizing.
Emulsion after homogenizing is spray-dried obtains Powdered lycopene product.Spray-dired controlled condition is: the spray drying inlet temperature is 170 ℃, and leaving air temp is 100 ℃, and feeding temperature is 50 ℃, and charging rate is 1.0 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
In the present embodiment lycopene microcapsule, the Detection of Stability of lycopene content the results are shown in Table 4, and detection method is with embodiment 1:
Table 4
Figure 2012103977264A00800021
Detection disintegration of the present embodiment lycopene microcapsule adopts 2010 editions, and " Chinese pharmacopoeia appendix method is carried out, and it is 48min that three Parallel testings obtain average disintegration time.

Claims (5)

1. the preparation method of a lycopene microcapsule, after the method mainly is prepared into core by lycopene, again with the process emulsifying of wall material and spray drying, it is characterized in that described wall material is prepared by following methods: the gelatin that the weight ratio of take is 1:1:1:1.2~1.6, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder are wall material raw material, add 3~5 times of amount distilled water of above-mentioned material, be heated to 40~45 ℃, stir and become uniform suspension, be the wall material; Described core is prepared by following methods: every 0.5~0.8g lycopene is dissolved in the salad oil of 1ml, and adds sucrose ester to make emulsifying agent, the weight ratio of lycopene and sucrose ester is 10~14:1, is core; Described emulsifying comprises the following steps: the mixed liquor of core and wall material of take is oil phase, slowly add while stirring oil phase in water, water and oil phase weight ratio are 3~3.5:5~6, then are placed in colloid mill, under 5000~10000 rev/mins of conditions, grind, milling time is 20~40min; Described spray drying condition is: the spray drying inlet temperature is 170 ~ 180 ℃, and leaving air temp is 80 ~ 100 ℃, and feeding temperature is 45 ~ 50 ℃, and charging rate is 0.6 ~ 1.0 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
2. the preparation method of lycopene microcapsule according to claim 1, it is characterized in that described wall material is prepared by following methods: the gelatin that the weight ratio of take is 1:1:1:1.4, Ganoderma spore powder with cellular wall broken, sucrose, defatted milk powder are wall material raw material, add 4 times of amount distilled water of above-mentioned material, be heated to 45 ℃, stirring becomes uniform suspension, is the wall material.
3. the preparation method of lycopene microcapsule according to claim 1, it is characterized in that described core is prepared by following methods: every 0.68g lycopene is dissolved in the salad oil of 1ml, and add sucrose ester to make emulsifying agent, the weight ratio of lycopene and sucrose ester is 8.5:0.7, is core.
4. the preparation method of lycopene microcapsule according to claim 1, it is characterized in that described emulsifying comprises the following steps: the mixed liquor of core and wall material of take is oil phase, slowly add while stirring oil phase in water, water and oil phase weight ratio are 3:5, be placed in again colloid mill, under 6000 rev/mins of conditions, grind, milling time is 30min.
5. the preparation method of lycopene microcapsule according to claim 1, it is characterized in that described spray drying condition is: the spray drying inlet temperature is 180 ℃, leaving air temp is 80 ~ 100 ℃, feeding temperature is 50 ℃, charging rate is 0.6 ~ 1.0 kg/min, 50 ~ 60 liter/mins of cold air blast velocities.
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CN105853245A (en) * 2016-04-29 2016-08-17 佛山市芊茹化妆品有限公司 Anti-aging composition containing lycopene and microcapsule and preparation method thereof
CN107361363B (en) * 2016-05-12 2020-08-11 山东常青藤生物科技有限公司 Lycopene preparation and preparation method thereof
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CN107821923A (en) * 2017-11-28 2018-03-23 戴凤 The preparation method of microcapsules containing lycopene
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