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CN106344510B - The industrialized preparing process of lycopene microemulsion - Google Patents

The industrialized preparing process of lycopene microemulsion Download PDF

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Publication number
CN106344510B
CN106344510B CN201610731056.3A CN201610731056A CN106344510B CN 106344510 B CN106344510 B CN 106344510B CN 201610731056 A CN201610731056 A CN 201610731056A CN 106344510 B CN106344510 B CN 106344510B
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lycopene
water
microemulsion
preparing process
oil
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CN106344510A (en
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张志明
安晓东
杨丽微
李乾丽
温盼来
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Chenguang Biotech Group Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions
    • A61K9/107Emulsions ; Emulsion preconcentrates; Micelles
    • A61K9/1075Microemulsions or submicron emulsions; Preconcentrates or solids thereof; Micelles, e.g. made of phospholipids or block copolymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/01Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/10Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/22Heterocyclic compounds, e.g. ascorbic acid, tocopherol or pyrrolidones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/46Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
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Abstract

The invention discloses a kind of industrialized preparing process of lycopene microemulsion, first mix lycopene crystal, assistant for emulsifying agent, oil soluble emulsifier and antioxidant, obtain suspension;Suspension is carried out again nano-milled, obtains oily phase;Water and water soluble emulsifier are mixed into water phase;Water phase is mutually mixed with oil finally, the lycopene microemulsion can be obtained.This method is using lycopene crystal as raw material, addition assistant for emulsifying agent, oil soluble emulsifier obtain nanoscale oil suspension by nano-milled, then lycopene microemulsion is mixed to get with water and water soluble emulsifier, lycopene is dissolved without using vegetable oil or organic solvent, and the mode that only oil is mutually ground, material handling capacity is increased, industrial production efficiency is improved.This method simple process, Product Safety is high, can prepare the lycopene microemulsion of high-content, is suitble to industrialization continuous production, remarkable in economical benefits.

Description

The industrialized preparing process of lycopene microemulsion
Technical field
The invention belongs to natural pigment applied technical field, especially a kind of industrialized production side of lycopene microemulsion Method.
Background technique
Lycopene is one of carotenoid.Contain many double bonds in lycopene molecule, there is stronger life Manage function.Such as: lycopene has very strong antioxidant activity, can be avoided the anti-oxidative damage of cell, pre- anti-cancer Occur, secondly lycopene can also prevent the functions such as the generation of cardiovascular and cerebrovascular diseases, and anti-aging.
Lycopene is fat-soluble pigment, is soluble in lipid and nonpolar solvent, not soluble in water, is insoluble in highly polar molten Agent such as methanol, ethyl alcohol etc. dissolves in the organic solvents such as aliphatic hydrocarbon, aromatic hydrocarbon and chlorohydrocarbon such as ethane, benzene, chloroform.Due to tomato The water-insoluble of red pigment, the application for causing lycopene are extremely limited.Currently in order to improving the hydrophobic of lycopene Property, the method mainly used has: 1) microcapsules technology: but since its particle size after cracking is inadequate, after wall material dissolution, lycopene is not It can preferably be suspended in aqueous solution, can settle quickly.2) microemulsion technology: in the prior art, lycopene microemulsion Preparation rely primarily on and prepare the mode that lycopene crystal is dissolved in grease or solvent, technique is relatively complicated, is preparing The mode of high-temperature fusion or the mode of solvent dissolution are mostly used in the process, not only result in the loss of lycopene, but also meeting There is the danger of dissolvent residual.Such as the patent of 101991175 A of Publication No. CN provides a kind of high-cis content of isomer Lycopene is dissolved in plant under high temperature (150 DEG C or so) state by lycopene microemulsion formulation product and preparation method In oil, then assistant for emulsifying agent, emulsifier and water is added under the conditions of 100 DEG C, microemulsion is made;Not only technique is cumbersome for this method, but also High temperature is wherein repeatedly used, the loss of lycopene is easily caused.The patent application of Publication No. CN200710024111.6 mentions A kind of water-soluble lycopene Nanodispersion product and preparation method have been supplied, lycopene has been dissolved in organic solvent, Then the mode of assistant for emulsifying agent and emulsifier is added, microemulsion is prepared by high-pressure homogeneous mode, then uses rotary evaporation Mode remove dissolvent residual;The microemulsion not only complex process of this method preparation, and that there are also solvents is residual for obtained microemulsion The danger stayed.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of works of the lycopene microemulsion of simple process, safety and stability Industry production method.
In order to solve the above technical problems, the technical solution used in the present invention is: first by lycopene crystal, help emulsification Agent, oil soluble emulsifier and antioxidant mix, and obtain suspension;Suspension is carried out again nano-milled, obtains oily phase;By water with Water soluble emulsifier is mixed into water phase;Water phase is mutually mixed with oil finally, the lycopene microemulsion can be obtained.
Lycopene crystal of the present invention, assistant for emulsifying agent, oil soluble emulsifier and antioxidant weight ratio be 1:4~ 15:1~3:0.2~1.
Assistant for emulsifying agent of the present invention is glycerine and/or sorbierite;Oil soluble emulsifier is lecithin, pungent capric acid glycerol One or more of ester, sorbester p18.
Antioxidant of the present invention is water soluble antioxidant.The antioxidant is L-AA, tea polyphenols, white One or more of veratryl alcohol, aurantiamarin.
Nano-milled condition of the present invention are as follows: 1500~2500r/min of grinding rate, milling time be 20~ 60min, grinding temperature are 15~30 DEG C.
Water soluble emulsifier of the present invention is TWEEN Series and/or Sucrose Fatty Acid Ester series.The water and water soluble emulsifier Weight ratio be 1:0.2~1.
The weight ratio of water phase of the present invention and oily phase is 1:1~4.
The beneficial effects of adopting the technical scheme are that lycopene crystal is directly used for by (1) present invention The preparation of microemulsion avoids dissolving crystal with organic solvent or prepares microemulsion by the way of high-temperature fusion crystal, causes molten Agent residual or high temperature crystal content loss.(2) time flow of the present invention is shorter, and production technology temperature is lower, can effectively avoid The loss of lycopene content can prepare content in the lycopene microemulsion of the high-content of 1~10wt%, it is more to meet market The demand of kind specification product.(3) microemulsion preparation temperature is low in the present invention, effectively prevents lycopene crystal content loss, The loss late < 1wt% of lycopene in obtained product.(4) present invention using water soluble antioxidant as oil phase in it is anti-oxidant Agent is ground, can protect crystal and addition oil insoluble oxidation agent make emulsifier burden and caused by cream Agent dosage increases.(5) present invention is simple to operation, time-consuming shorter, it is only necessary to which consuming 2~3h can be made into finished product, be suitble to work Industry metaplasia produces.
The present invention using lycopene crystal as raw material, received by nano-milled by addition assistant for emulsifying agent, oil soluble emulsifier Then the oil suspension of meter level is mixed to get lycopene microemulsion with water and water soluble emulsifier, without using vegetable oil or have Solvent dissolves lycopene, and the mode only mutually ground to oil, increases material handling capacity, improves industrial metaplasia Produce efficiency;Especially oily phase grinding when add water-soluble antioxidant, preferably reduce emulsifier burden, reduce emulsifier Dosage.Present invention process is simple, and Product Safety is high, can prepare the lycopene microemulsion of high-content, and industrialization is suitble to connect Continuous production, remarkable in economical benefits.
Specific embodiment
The present invention will be further described in detail with reference to the specific embodiments.
The industrialized preparing process of this lycopene microemulsion uses following processing steps:
(1) lycopene crystal even suspension is suspended in assistant for emulsifying agent, oil soluble emulsifier and antioxidant Liquid;The lycopene crystal: assistant for emulsifying agent: oil soluble emulsifier: antioxidant=1:4~15:1~3:0.2~1(weight);Institute Stating assistant for emulsifying agent is glycerine and/or sorbierite;Oil soluble emulsifier is lecithin, Glycerin, mixed triester with caprylic acid capric acid, sorbester p18 (sorbitol anhydride One or more of monostearate);The antioxidant uses water soluble antioxidant, more selected from L-AA, tea One or more of phenol, resveratrol, aurantiamarin.
(2) suspension addition nano-level grinder is ground, obtains oily phase;Nano-milled condition are as follows: grinding rate 1500~2500r/min, milling time are 20~60min, and grinding temperature is 15~30 DEG C.
(3) water is mixed with water soluble emulsifier, obtains water phase;Water emulsifier is that TWEEN Series (spit by polysorbas20 Temperature 80), Sucrose Fatty Acid Ester series one or more of (sucrose lauric acid rouge, sucrose stearate rouge);Water: water soluble emulsifier=1: 0.2~1(weight);Hybrid mode: 40~80 DEG C of temperature, mixing speed be 50~100r/min under conditions of stirring 10~ 20min。
(4) water phase and oil are mixed uniformly, water phase: oily phase=1:1~4(weight), the lycopene can be obtained Microemulsion;When mixing, under the conditions of temperature is 30~50 DEG C, mixing speed is 100~200r/min, oil is mutually added slowly to In water phase, mixing speed is adjusted to 500~800r/min high-speed stirred after oil phase addition, stirs 15~30min.
Embodiment 1: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 90wt% lycopene crystal as raw material;By 30g lycopene crystal, 450g the third three Alcohol, 50g lecithin and 9g tea polyphenols after mixing, are ground in nano-level grinder;Grind revolving speed 1700r/min, grinding temperature Degree is 20 DEG C, nano-milled 60min;Obtain uniform, fine and smooth oily phase.It in temperature is 40 DEG C by 234g water, 117g polysorbas20 Under the conditions of, 15min is stirred with the revolving speed of 80r/min, is uniformly mixed and obtains water phase.Above-mentioned water phase: oily phase=1:1.54;It will be oily Mutually 40 DEG C, revolving speed be 100r/min under conditions of, be slowly added into water phase, then revolving speed adjusted to 600r/min, is stirred 20min is mixed, the lycopene microemulsion can be obtained, the content of lycopene is in gained lycopene microemulsion 3.01wt%;Wherein the loss late of lycopene is 0.99%.
Embodiment 2: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 85wt% lycopene crystal as raw material;By 50g lycopene crystal, 500g sorb Alcohol, 150g sorbester p18 and 10g aurantiamarin after mixing, are ground in nano-level grinder;Grind revolving speed 2000r/min, grinding Temperature is 30 DEG C, nano-milled 30min;Obtain uniform, fine and smooth oily phase.It is in temperature by 150g water, 75g sucrose stearate rouge Under conditions of 50 DEG C, 12min is stirred with the revolving speed of 100r/min, is uniformly mixed and obtains water phase.Above-mentioned water phase: oily phase=1: 3.16;By it is oily mutually 30 DEG C, revolving speed be 150r/min under conditions of, be slowly added in water phase, then adjust revolving speed to 700r/ Min stirs 30min, the lycopene microemulsion can be obtained, the content of lycopene in gained lycopene microemulsion For 4.53wt%;Wherein the loss late of lycopene is 0.33%.
Embodiment 3: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 92wt% lycopene crystal as raw material;By 90g lycopene crystal, 500g the third three Alcohol, 90g lecithin and 20g resveratrol after mixing, are ground in nano-level grinder;Grind revolving speed 2500r/min, grinding Temperature is 25 DEG C, nano-milled 20min;Obtain uniform, fine and smooth oily phase.By 300g water, 180g Tween 80 temperature be 45 DEG C Under conditions of, 20min is stirred with the revolving speed of 70r/min, is uniformly mixed and obtains water phase.Above-mentioned water phase: oily phase=1:1.46;It will It is oily mutually 50 DEG C, revolving speed be 120r/min under conditions of, be slowly added in water phase, then revolving speed adjusted to 800r/min, is stirred 25min is mixed, the lycopene microemulsion can be obtained, the content of lycopene is in gained lycopene microemulsion 7.00wt%;Wherein the loss late of lycopene is 0.28%.
Embodiment 4: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 89wt% lycopene crystal as raw material;By 100g lycopene crystal, 400g the third three Alcohol, 100g Glycerin, mixed triester with caprylic acid capric acid, 100g sorbester p18 and 60g L-AA after mixing, ground in nano-level grinder; Revolving speed 1500r/min is ground, grinding temperature is 25 DEG C, nano-milled 50min;Obtain uniform, fine and smooth oily phase.By 110g water, 80g sucrose lauric acid rouge stirs 10min under conditions of temperature is 80 DEG C, with the revolving speed of 90r/min, is uniformly mixed and obtains water Phase.Above-mentioned water phase: oily phase=1:4;By it is oily mutually 35 DEG C, revolving speed be 200r/min under conditions of, be slowly added in water phase, so Revolving speed is adjusted to 650r/min afterwards, 15min is stirred, the lycopene microemulsion can be obtained, gained lycopene is micro- The content of lycopene is 9.35wt% in lotion;Wherein the loss late of lycopene is 0.21%.
Embodiment 5: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 90.6wt% lycopene crystal as raw material;By 40g lycopene crystal, 200g third Triol, 160g sorbierite, 100g Glycerin, mixed triester with caprylic acid capric acid, the L-AA of 20g and 20g resveratrol after mixing, are being received It is ground in rice grinder;Revolving speed 2200r/min is ground, grinding temperature is 15 DEG C, nano-milled 40min;It obtains uniform, fine and smooth Oily phase.By 100g water, 50g polysorbas20 and 50g sucrose lauric acid rouge under conditions of temperature is 65 DEG C, with the revolving speed of 50r/min 18min is stirred, is uniformly mixed and obtains water phase.Above-mentioned water phase: oily phase=1:2.7;By oily mutually in 45 DEG C, revolving speed 170r/min Under conditions of, it is slowly added in water phase, then revolving speed is adjusted to 500r/min, 20min is stirred, the tomato can be obtained Red pigment microemulsion, the content of lycopene is 4.85wt% in gained lycopene microemulsion;Wherein the loss late of lycopene is 0.96%。
Embodiment 6: the concrete technology of the industrialized preparing process of this lycopene microemulsion is as described below.
Using lycopene content for 91.3wt% lycopene crystal as raw material;By 30g lycopene crystal, the mountain 330g Pears alcohol, 60g Glycerin, mixed triester with caprylic acid capric acid and 24g aurantiamarin after mixing, are ground in nano-level grinder;Grind revolving speed 1900r/ Min, grinding temperature are 27 DEG C, nano-milled 35min;Obtain uniform, fine and smooth oily phase.By 370g water, 74g sucrose lauric acid rouge Under conditions of temperature is 60 DEG C, 15min is stirred with the revolving speed of 60r/min, is uniformly mixed and obtains water phase.Above-mentioned water phase: oil Phase=1:1;By it is oily mutually 40 DEG C, revolving speed be 150r/min under conditions of, be slowly added into water phase, then by revolving speed adjust to 750r/min stirs 25min, the lycopene microemulsion, lycopene in gained lycopene microemulsion can be obtained Content be 3.05wt%;Wherein the loss late of lycopene is 0.97%.

Claims (8)

1. a kind of industrialized preparing process of lycopene microemulsion, it is characterised in that: first by lycopene crystal, help emulsification Agent, oil soluble emulsifier and antioxidant mix, and obtain suspension;Suspension is carried out again nano-milled, obtains oily phase;By water with Water soluble emulsifier is mixed into water phase;Water phase is mutually mixed with oil finally, the lycopene microemulsion can be obtained;It is described Antioxidant is water soluble antioxidant.
2. the industrialized preparing process of lycopene microemulsion according to claim 1, it is characterised in that: the tomato red Cellulose crystal, assistant for emulsifying agent, oil soluble emulsifier and antioxidant weight ratio be 1:4~15:1~3:0.2~1.
3. the industrialized preparing process of lycopene microemulsion according to claim 1, it is characterised in that: described to help emulsification Agent is glycerine and/or sorbierite;Oil soluble emulsifier is one or more of lecithin, Glycerin, mixed triester with caprylic acid capric acid, sorbester p18.
4. the industrialized preparing process of lycopene microemulsion according to claim 1, it is characterised in that: described anti-oxidant Agent is one or more of L-AA, tea polyphenols, resveratrol, aurantiamarin.
5. the industrialized preparing process of lycopene microemulsion according to claim 1, which is characterized in that the nanometer is ground The condition of mill are as follows: 1500~2500r/min of grinding rate, milling time are 20~60min, and grinding temperature is 15~30 DEG C.
6. the industrialized preparing process of lycopene microemulsion according to claim 1, it is characterised in that: the water solubility Emulsifier is TWEEN Series and/or Sucrose Fatty Acid Ester series.
7. the industrialized preparing process of lycopene microemulsion according to claim 1, it is characterised in that: the water and water The weight ratio of soluble emulsification agent is 1:0.2~1.
8. the industrialized preparing process of lycopene microemulsion described in -7 any one, feature exist according to claim 1 In: the weight ratio of the water phase and oily phase is 1:1~4.
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CN107259506A (en) * 2017-06-20 2017-10-20 武汉星辰现代生物工程有限公司 A kind of preparation technology of bata-carotene nanosized emulsion and application
CN107736616A (en) * 2017-09-19 2018-02-27 常州瑞坦商贸有限公司 A kind of preparation method of lycopene micro emulsion
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CN109566973A (en) * 2018-12-14 2019-04-05 晨光生物科技集团股份有限公司 A kind of lycopene composition and its emulsion formulations
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