CN106916230B - A method of microcapsule embedded wall material is prepared using electronic irradiation technique - Google Patents
A method of microcapsule embedded wall material is prepared using electronic irradiation technique Download PDFInfo
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- CN106916230B CN106916230B CN201710205398.6A CN201710205398A CN106916230B CN 106916230 B CN106916230 B CN 106916230B CN 201710205398 A CN201710205398 A CN 201710205398A CN 106916230 B CN106916230 B CN 106916230B
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Abstract
The present invention discloses a kind of method for preparing microcapsule embedded wall material using electronic irradiation technique, the following steps are included: after galactooligosaccharide premix is added in (1) methylcellulose, it is dissolved in sterile water, it is uniformly mixed, measure index of refraction, make index of refraction control between 1.35-1.44, magnetic agitation；(2) solution for obtaining step (1) is fitted into preservation and packaging in radiotolerant PE polybag, utilizes electron accelerator irradiation, after irradiation, hyperfiltration treatment is carried out, unreacted methylcellulose and galactooligosaccharide are removed, freeze-drying to get.Preparation method technology controlling and process of the present invention is simple, effectively prevent the introducing of chemical substance, safety is higher, and radiation treatment reaction is fast, it is easy to be operated continuously, is suitable for industrialized production, obtained methylcellulose-galactooligosaccharide graft copolymer purity is high, with good gelation, caking property and film forming, can be applied in food industry.
Description
Technical field
The present invention relates to microcapsules fields.It is prepared more particularly, to a kind of utilization electronic irradiation technique microcapsule embedded
The method of wall material.
Background technique
Electron irradiation (Electron irradiation) is exactly to use high-power electron beam to irradiate material, to improve material
A kind of technology of performance.It is the activated atom and anakmetomeres generated using the effect between ray and substance, ionization and excitation,
It is allowed to that a series of physical, the biochemical changes such as chemistry occur with substance, leads to the degradation of substance, polymerization, crosslinking and changes
Property.Radiation processing technology has formed a new industry, and irradiation processing has energy saving, acyclic compared with Conventional processing methods
The features such as border is polluted, can carry out room temperature processing.High-energy ray not only can handle machined object surface, while can go deep into it
Portion, and technology controlling and process is simple.Since irradiation technique is to the form of material, irradiation temperature not harsh requirement, and reacts fast, produces
Product purity is high, easy to control, practicable continuous operation, therefore be considered as a kind of high financial profit, it is energy saving, save manpower,
The new processing technology of nuisanceless or few public hazards.
Applying electronic beam irradiation exploitation new product is one of industrial means most with prospects.Radiation source include electron beam,
Gamma-rays, ultraviolet light, microwave etc..
Methylcellulose (MC) is a kind of long-chain substituted cellulose, wherein about 27%~32% hydroxyl is with the shape of methoxyl group
Formula exists.The methylcellulose of different stage has the different degree of polymerization, in the range of 50~1000；And its molecular weight is (average
Number) range between 10000~220000Da.
MC is almost insoluble in dehydrated alcohol, ether, acetone.Aqueous solution is quite stable at normal temperature, has excellent profit
Moist, dispersed, cementability, thickening property, emulsibility, water-retaining property, acid resistance and film forming, form a film with excellent toughness,
Flexibility and transparency.Cellulosic structure is regular, has fine and close crystal structure, and a large amount of hydroxyl is closed, so that reaction examination
Agent is difficult to and fibrin reaction, limits the application of cellulose.Special processing is carried out to it by using electronic irradiation technique,
Associative key in cellulose molecular chain is opened, introduces new functional group, so that it may change its intrinsic characteristic, it is acidproof to enhance its
Property, water-retaining property, gelation, caking property and film forming.
MC is more applied to as adhesive as a kind of state approval and the food additives that allow to use as needed
Building trade, and be applied to food direction microcapsule wall material using rarely seen.
Accordingly, it is desirable to provide a kind of MC is applied to the microcapsule embedded wall material preparation method in food industry.
Summary of the invention
The purpose of the present invention is to provide a kind of method for preparing microcapsule embedded wall material using electronic irradiation technique, the party
Method is modified methylcellulose by using electronic irradiation technique, by itself and oligosaccharide graft copolymerization, as microcapsules packet
Wall material is buried applied in food industry.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
A kind of method for preparing microcapsule embedded wall material using electronic irradiation technique of the present invention, comprising the following steps:
(1) it after galactooligosaccharide premix is added in methylcellulose, is dissolved in sterile water, is uniformly mixed, measure index of refraction, make
Index of refraction controls the magnetic agitation between 1.35-1.44；
(2) solution for obtaining step (1) is fitted into preservation and packaging in radiotolerant PE polybag, utilizes electron accelerator
Irradiation, carries out hyperfiltration treatment after irradiation, removes unreacted methylcellulose and galactooligosaccharide, freeze-drying to get
Methylcellulose-galactooligosaccharide graft copolymer, i.e., microcapsule embedded wall material.
Preferably, the mass ratio of the methylcellulose and galactooligosaccharide is 1:(2-8)；
Preferably, the relative molecular weight of the methylcellulose is 40kDa-60kDa；
Preferably, the time of the magnetic agitation is 15-20min；
Preferably, the parameter of the electron accelerator is set as electron beam 4.5-18MeV, line 30-60mA, rated power
90-120kW；
Preferably, the dosage of the irradiation is 20-200kGy, dosage rate 5-500kGy/hr；
Preferably, the molecule interception of the ultrafiltration is 80kDa, collects the component for being greater than 80kDa.
Methylcellulose hydrogen bond itself is destroyed, and accessibility and reactivity are higher than the cellulose of underivatized, by adopting
Methylcellulose and galactooligosaccharide are handled with electronic irradiation technique, accessibility is allowed to and reactivity further enhances,
Ether bond rupture in the methoxyl group of methylcellulose exposure, the R base (such as methyl) to fall off are easy to the hydroxyl being broken with galactooligosaccharide
Base junction is closed, and galactooligosaccharide associative key is grafted on methylcellulose side chain again and is crosslinked in the form of ether.
By electron irradiation treated new wall material, first, the application field and range of methylcellulose itself have been widened,
More exploitations for being applied to food technology；Second, it is handled by electron irradiation, adjusting methylcellulose that can be more wide in range
The random coil structure of interfacial property, polysaccharide graft effectively improves the physical stability of methylcellulose, reduces it to low
The sensibility of pH and pepsin increase the functional characters such as its gelation, film forming, emulsibility, acid resistance；Third is led to
The length for crossing increase side chain is conducive to increase the crosslink density of internal layer wall material, reduces gel pore, improves microcapsules to gastric acid
Buffer function, its additional good film forming can enhance microcapsules to the water holding capacity for the object that is embedded, strengthen holding for the object that is embedded
It is aqueous, preferably protect the substance that is embedded.
The microcapsule embedded wall material of the present invention is suitable for poor storage stability, orally, the life destroyed vulnerable to degradations such as gastric acids
The embedding of active substances；It is good based on the methylcellulose-galactooligosaccharide graft copolymer obtained after electron irradiation processing
Gelation, caking property and film forming, can be applied to jam, in beverage products, be equally applicable for the fresh-keeping of vegetable and fruit, may be used also
To be used to prepare plastics and sustained release preparation.
Beneficial effects of the present invention are as follows:
(1) electronic irradiation technique is applied to the preparation of the microcapsule embedded wall material in food industry by the present invention for the first time；
(2) methylcellulose-galactooligosaccharide graft copolymer that the present invention selects electron radiation technology to obtain, by mentioning
High-cellulose acid resistance, water-retaining property, gelation, caking property, film forming, enteric solubility make the graft copolymer conduct finally obtained
A kind of New Wall Material is applied among microcapsule embedded technology, improves the acid resistance and enteron aisle releasability of the object that is embedded, together
When improve be embedded object storage, transport and it is edible during stability, such as water retention property, and wall material is released in enteron aisle
It puts rear oligosaccharide and is also used as prebiotics, to promote the proliferation of probiotics.
(3) electronic irradiation technique is applied to the preparation of microcapsule embedded wall material by the present invention, and technology controlling and process is simple, effectively keeps away
Exempted from the introducing of chemical substance, safety is higher, and radiation treatment reaction is fast, and higher product purity can be obtained, be easy into
Row continuous operation, is suitable for industrialized production, while having expanded the application of methylcellulose.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1, which is shown, prepares microcapsule embedded wall material mechanism schematic diagram using electronic irradiation technique.
Fig. 2 shows probiotic microcapsule acid resisting test result figures.
Fig. 3 shows probiotic microcapsule enteric solubility test result figure.
Fig. 4 shows probiotic microcapsule storage stability test result figure.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
It is first to cause to live in cellulosic backbone that the present invention, which prepares microcapsule embedded wall material mechanism using electronic irradiation technique,
Property polymerization site, then polymerize with monomer, side chain increases (specific polymerized form such as Fig. 1).
A kind of method for preparing microcapsule embedded wall material using electronic irradiation technique of embodiment 1
A method of microcapsule embedded wall material is prepared using electronic irradiation technique, comprising the following steps:
It (1) be 40kDa methylcellulose according to mass ratio by relative molecular mass is that galactooligosaccharide premix is added in 1:2
Afterwards, it is dissolved in sterile water, is uniformly mixed it, index of refraction is measured using abbe's refractometer, index of refraction is finally controlled 1.35, adopted
With magnetic stirrer 15min.
(2) solution for mixing step (1) is fitted into preservation and packaging in radiotolerant PE polybag, utilizes 4.5MeV electricity
Beamlet, 30mA line, the electron accelerator irradiation of 90kW rated power, irradiation dose 20kGy, radiation dose rate 5kGy/
Sample after irradiation is carried out hyperfiltration treatment (molecule interception is 80kDa) after irradiation, it is fine to remove unreacted methyl by hr
Dimension element and galactooligosaccharide, component of the collection greater than 80kDa is freeze-dried to be connect to get methylcellulose-galactooligosaccharide
Graft copolymer.
A kind of method for preparing microcapsule embedded wall material using electronic irradiation technique of embodiment 2
A method of microcapsule embedded wall material is prepared using electronic irradiation technique, comprising the following steps:
It (1) be 60kDa methylcellulose according to mass ratio by relative molecular mass is that galactooligosaccharide premix is added in 1:8
Afterwards, it is dissolved in sterile water, is uniformly mixed it, index of refraction is measured using abbe's refractometer, index of refraction is finally controlled 1.44, adopted
With magnetic stirrer 20min.
(2) solution for mixing step (1) is fitted into preservation and packaging in radiotolerant PE polybag, utilizes 18MeV electronics
Beam, 60mA line, the electron accelerator irradiation of 120kW rated power, irradiation dose 200kGy, radiation dose rate are
Sample after irradiation is carried out hyperfiltration treatment (molecule interception is 80kDa) after irradiation, removes unreacted by 500kGy/hr
Methylcellulose and galactooligosaccharide, collect greater than 80kDa component be freeze-dried it is oligomeric to get methylcellulose-
Galactolipin graft copolymer.
A kind of method for preparing microcapsule embedded wall material using electronic irradiation technique of embodiment 3
A method of microcapsule embedded wall material is prepared using electronic irradiation technique, comprising the following steps:
It (1) be 50kDa methylcellulose according to mass ratio by relative molecular mass is that galactooligosaccharide premix is added in 1:5
Afterwards, it is dissolved in sterile water, is uniformly mixed it, index of refraction is measured using abbe's refractometer, index of refraction is finally controlled 1.40, adopted
With magnetic stirrer 18min.
(2) solution for mixing step (1) is fitted into preservation and packaging in radiotolerant PE polybag, utilizes 10MeV electronics
Beam, 45mA line, the electron accelerator irradiation of 115kW rated power, irradiation dose 110kGy, radiation dose rate are
Sample after irradiation is carried out hyperfiltration treatment (molecule interception is 80kDa) after irradiation, removes unreacted by 250kGy/hr
Methylcellulose and galactooligosaccharide, collect greater than 80kDa component be freeze-dried it is oligomeric to get methylcellulose-
Galactolipin graft copolymer.
A kind of preparation of the probiotic microcapsule of embodiment 4
1, a kind of bifidobacterium lactis microcapsules preparation
A kind of bifidobacterium lactis microcapsule preparation process, strain purchase is in the management of Chinese industrial Microbiological Culture Collection
The heart comprises the following specific steps that:
(1) composite frozen drying protectant is prepared: glycerol 0.2%, glycine 0.5%, lactose 2%, sorbierite 0.5%,
Bovine serum albumin(BSA) 2% is used after cooling with distilled water constant volume using the preceding 20min that sterilizes under the conditions of 115 DEG C.
(2) methylcellulose of any preparation of embodiment 1-3-galactooligosaccharide graft copolymer is configured to 8mg/mL's
Solution.
(3) culture and activation of bifidobacterium lactis
Bifidobacterium lactis is seeded on the slant medium containing agar that pH is 6.8 Anaerobic culturel under the conditions of 37 DEG C
For 24 hours, it activates 3 times, is then moved into fluid nutrient medium respectively by 1% inoculum concentration and expand culture for 24 hours under the conditions of 37 DEG C.
(4) bacterium solution after culture is placed in a centrifuge and 6min, microorganism collection is centrifuged with the revolving speed of 6000rpm.Every gram of bacterium
1.5mL is added in body to have cooled down and sterilized composite frozen drying protectant.
(5) bacterium solution is prepared, adjustment cell density is 1010cfu/mL.The Methyl cellulose that bacterium solution, step (2) are prepared
Element-galactooligosaccharide graft copolymer solution and 3.5% sodium alginate soln are uniformly mixed according to 1: 5: 2 ratio, under room temperature,
120r/min stirs 25min, then drips in 1% calcium chloride solution bacterium solution mixed liquor, solidify 30min at normal temperature, finally
With sterile water washing and filter.
(6) microcapsules of above-mentioned preparation are freeze-dried to get probiotic microcapsule product.
2, the measurement of probiotic microcapsule strain acid resistance, embedding rate, enteric solubility and storage stability
Solubility property and storage in simulate the gastric juice and simulated intestinal fluid have been carried out to the above-mentioned probiotic microcapsule being prepared
Hide the measurement of stability.
(1) simulate the gastric juice is prepared: taking 2.0g sodium chloride and 3.2g pepsin, (mark should be in every mg containing 800~2500
A unit of activity), add 7.0mL hydrochloric acid and water to make to be dissolved to 1000mL, adjusts pH value to 1.2, finally with 0.22 μm of membrane filtration
Degerming.
(2) simulated intestinal fluid is prepared: taking potassium dihydrogen phosphate 6.8g, water 250mL is added to make to dissolve, add 0.2mol/L sodium hydroxide molten
Liquid 77mL and 500mL water, then plus after pancreatin 10g makes dissolution, with 0.2mol/L sodium hydroxide solution or 0.2mol/L hydrochloric acid solution
PH value is adjusted to 6.8 ± 0.1, dilution is added water and is settled to 1000mL, with 0.22 μm of membrane filtration degerming.
(3) acid resistance is tested: accurately being weighed the bifidobacterium lactis microcapsule formulation 0.5g prepared, is placed it in and fill
In the conical flask of 49.5mL simulate the gastric juice, at 37 DEG C of temperature, 120rpm/min shake culture 2.5h, 0.5mL is drawn every 30min
Sample solution is placed in simulated intestinal fluid, and shake culture 2h discharges thallus completely, and is therefrom drawn 0.5mL sample liquid and buffered with PBS
Liquid makees gradient dilution, measures viable count, and calculate thallus survival rate.Blank is made with the bifidobacterium lactis preparation without embedding simultaneously
Control, method are same as above.
Viable count × 100% before the viable count/embedding measured after thallus survival rate=external condition processing
Test results are shown in figure 2 for acid resistance, as can be seen from Figure 2: viable count decline of the probiotics in simulate the gastric juice
Amplitude is smaller, can almost ignore, and embedded samples survival rate drops to 87.85% by 90.28% after 2.5h, and does not embed sample
Product survival rate then drops to 2.15% by 92.75%, this illustrates that the microcapsules acid-fast ability after embedding is very strong, being capable of effective protection
Prebiotic thallus.
(4) embedding rate measures
The specific method is as follows for embedding rate measurement: accurately weighing the bifidobacterium lactis microcapsule formulation that 0.5g is prepared, is added
In the phosphate buffer preheated to 49.5mL (37 DEG C, 0.1mol/L NaH2PO4, pH8.0), keep it broken by high-shear homogenizer
It is broken, this broken liquid about 30min is then shaken, so that embedding wall material is discharged embedded bifidobacterium lactis completely, finally therefrom draws
0.5mL sample liquid PBS buffer solution makees gradient dilution, measures viable count.
Viable count × 100% before total viable count/embedding in embedding rate/%=microcapsules
Embedding rate is the important indicator for evaluating microcapsules, and microcapsule embedded rate of the invention reaches 95.8% after measured.
(5) enteric solubility is tested: accurately being weighed the bifidobacterium lactis microcapsule formulation 0.5g prepared, is placed it in and fill
In the conical flask of 49.5mL simulated intestinal fluid, at 37 DEG C of temperature, 120rpm/min shake culture 2.5h is therefrom drawn every 20min
0.5mL sample liquid PBS buffer solution makees gradient dilution, measures viable count.As a result as shown in figure 3, from figure 3, it can be seen that small
Enteral, microcapsule embedded prebiotic thallus are substantially completely dissolved in 40min or so, this shows it with preferable intestines solvability.
(6) storage stability is tested: the bifidobacterium lactis microcapsules prepared being taken to be respectively placed in 4 DEG C, in 37 DEG C of insulating boxs
30d is stored, is sampled every 6d, strain survival rate is measured.As a result as shown in figure 4, figure 4, it is seen that probiotic microcapsule
For preparation when storing 30d, 37 DEG C of condition hypothallus survival rates are still greater than 79%, and it is practical that this shows that process program of the invention has
Application value.
The present invention further often replaces methylcellulose-galactooligosaccharide to be grafted with current microcapsules with wall material sodium alginate
Copolymer, referring to a kind of above-mentioned bifidobacterium lactis microcapsule preparation method directly prepare with sodium alginate be embed wall material cream it is double
Discrimination bacillus microcapsules (comparison bifidobacterium lactis microcapsules), wherein bacterium solution and the adding proportion of 3.5% sodium alginate soln are 1:
5.With above-mentioned using methylcellulose-galactooligosaccharide graft copolymer as bifidobacterium lactis microcapsules (this of embedding wall material
Invention bifidobacterium lactis microcapsules) acid resistance carried out according to the method for step 2, embedding rate, enteric solubility and storage stability are surveyed
Examination, test result are shown in Table 1.Methylcellulose-galactooligosaccharide graft copolymer conduct is applied in index in the table of comparisons 1, discovery
It is more preferable in terms of compactness and water-retaining property compared with common wall material sodium alginate when embedding wall material, embedding rate, acid resistance, enteric solubility
The indexs such as energy, storage stability are all greatly improved, be more advantageous to ensure prebiotic thallus in vivo external activity and
Stability.
Performance compares under the conditions of the different embedding wall materials of table 1
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (6)
1. a kind of method for preparing microcapsule embedded wall material using electronic irradiation technique, which comprises the following steps:
(1) it after galactooligosaccharide premix is added in methylcellulose, is dissolved in sterile water, is uniformly mixed, measure index of refraction, make refractive power
Rate controls the magnetic agitation between 1.35-1.44；
(2) solution for obtaining step (1) is fitted into preservation and packaging in radiotolerant PE polybag, using electron accelerator irradiation,
Carry out hyperfiltration treatment after irradiation, remove unreacted methylcellulose and galactooligosaccharide, freeze-drying to get；
The dosage of the irradiation is 20-200kGy, dosage rate 5-500kGy/hr.
2. according to the method described in claim 1, it is characterized by: the mass ratio of the methylcellulose and galactooligosaccharide is
1:(2-8).
3. according to the method described in claim 1, it is characterized by: the relative molecular weight of the methylcellulose is 40 kDa-
60kDa。
4. according to the method described in claim 1, it is characterized by: the time of the magnetic agitation is 15-20min.
5. according to the method described in claim 1, it is characterized by: the parameter of the electron accelerator is set as electron beam 4.5-
18MeV, line 30-60mA, rated power 90-120kW.
6. according to the method described in claim 1, collection is greater than it is characterized by: the molecule interception of the ultrafiltration is 80kDa
The component of 80kDa.
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