CN115844806B - Active probiotic membrane material and preparation method thereof - Google Patents
Active probiotic membrane material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an active probiotic membrane material and a preparation method thereof, wherein the active probiotic membrane material comprises a fiber membrane manufactured by an electrostatic spinning process, and the fiber membrane is formed by interweaving core-shell structure fiber filaments encapsulated with active probiotics; the core-shell structured fiber yarn comprises shell fiber and content; the content comprises active probiotics and a probiotic protecting agent, and one or two of functional components and auxiliary materials. The active probiotic membrane material provided by the invention is a dry type pasting membrane material integrated with skin care raw materials, in the use process, the membrane material is firstly taken out from the packaging material and is pasted on the skin, then proper liquid such as purified water, rose water and the like is sprayed on the membrane material, the membrane material can be closely pasted on the skin, the use is convenient, the probiotics are packaged in the shell fiber, and the activity retention rate of the probiotics is high. Meanwhile, the preparation process is simple, continuous high-efficiency production can be realized, the quality is controllable, and the method is suitable for industrial production.
Description
Active probiotic membrane material and preparation method thereof
Technical Field
The invention relates to the technical field of probiotics, in particular to an active probiotic membrane material and a preparation method thereof.
Background
The probiotics mask can regulate skin microecology, and the masks with different effects can enhance the effects through the cooperation of probiotics. At present, the probiotic facial mask mainly comprises two major types, namely a paste facial mask formed by mixing probiotic fermented matters or probiotic bacteria powder with the rest raw materials to form facial mask liquid and then loading the facial mask liquid on a fiber carrier. The other is a powder type facial mask, the probiotics freeze-dried powder and the rest powder raw materials are mixed to form composite powder, and water is added for blending when in use. The mask formed in the first mode has the following problems in the use process: the mask liquid cannot be adsorbed on the mask fibers in general, and a part of the mask liquid remains in the packaging bag, so that the mask liquid is wasted; when the spreading mask is applied to the skin, the risk of dripping mask liquid exists; in the process of application, the mask liquid can be stuck on hands; the activity rate of probiotics is low. The mask formed by the second mode has the following problems: the preparation is needed, and the operation is troublesome; when the dosage of the composite powder and the water is not well controlled, the mixture is too thin or too thick; the skin is easy to be stuck on the skin with uneven thickness; the activity rate of probiotics is low. That is, there are some disadvantages to both of the currently mainstream forms of probiotic masks.
Electrostatic spinning is a special fiber manufacturing process, in which a strong electric field is applied during the manufacturing process to make polymer solution or melt undergo jet spinning. At present, the electrostatic spinning technology is used for manufacturing mask fibers. For example, a document "research (Li Jinian, university of Zhejiang, university of industrial and commercial, 2019) of preparing a polystyrene fiber film as a carrier of a probiotic biological film by electrospinning" reports a technology of preparing a polystyrene fiber film by electrospinning, which is to prepare a fiber film by electrospinning, then put the fiber film into a culture solution of the probiotic bacteria, and attach the probiotic bacteria to the fiber film by utilizing the growth characteristics of the probiotic bacteria, thereby preparing a probiotic film based on the electrospinning technology. However, this technique has the following disadvantages: relates to a probiotic biomembrane loading process, has complex flow, can not realize continuous high-efficiency production, and has lower activity retention rate of probiotics.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide an active probiotic membrane material, which is a dry type and fibrous membrane type adhesive membrane material integrated with skin care raw materials, and has the advantages of convenient use and high active retention rate of probiotics.
The second purpose of the invention is to provide a preparation method of the active probiotic membrane material, which has simple flow and controllable quality and is suitable for industrial production.
One of the purposes of the invention is realized by adopting the following technical scheme:
the active probiotic membrane material comprises a fiber membrane manufactured by an electrostatic spinning process, wherein the fiber membrane is formed by interweaving core-shell structure fiber filaments encapsulated with active probiotics; the core-shell structured fiber yarn comprises shell fibers and contents; the content comprises the active probiotics and a probiotic protecting agent and one or two of functional components and auxiliary materials.
In the invention, the fiber membrane is formed by interweaving fiber filaments of a core-shell structure, which are encapsulated with active probiotics, the interweaving does not refer to textile forming in textile industry, and means that the fiber filaments of the core-shell structure are crisscrossed together, and the fiber filaments are densely staggered with each other to form the fiber membrane.
In the present invention, the core-shell structure fiber includes a sheath fiber and a content, that is, the content is encapsulated in the sheath fiber, and if the preparation raw material of the content includes a polymer raw material, the content may form an inner layer fiber; if the preparation feed of the content does not include a polymer feed, the content is directly supported on the inner walls of the sheath fibers.
As a preferred embodiment of the present invention, the active probiotic membrane material includes, but is not limited to, facial mask, cervical mask, hand mask, foot mask and lip mask. The active probiotics type, the functional components, the auxiliary materials and the like can be selected according to the actual use position and the skin care effect to be achieved, and the film material can be cut according to the use position to form the corresponding shape.
As a preferable scheme of the invention, the preparation raw materials of the shell fiber comprise one or any combination of gum arabic, pullulan, silk fibroin, poly epsilon-caprolactone, polylactic acid, polyethylene glycol, polylactic acid-glycolic acid copolymer, hyaluronic acid and guar gum; preferably, the shell fiber is prepared from one or two of gum arabic and pullulan; more preferably, the shell fiber is prepared from a combination of gum arabic and pullulan, and the mass ratio of the gum arabic to the pullulan is preferably 1: (0.2-5), more preferably 1: (0.5-2), preferably 1:2.
As a preferred embodiment of the present invention, the active probiotics include one or any combination of lactobacillus plantarum (lactobacillus plantarum), lactobacillus paracasei (lactobacillus plantarum), bifidobacterium animalis subspecies lactis (bifidobacterium lactis), lactobacillus fermentum (lactobacillus fermentum), lactobacillus salivarius (lactobacillus salivarius), lactobacillus acidophilus (lactobacillus acidophilus), pediococcus pentosaceus (pediococcus pentosaceus), manella coagulans (bacillus coagulans), bifidobacterium adolescentis (bifidobacterium adolescentis), bifidobacterium animalis subspecies animalis (bifidobacterium animalis), lactobacillus reuteri (lactobacillus reuteri), bifidobacterium longum subspecies (bifidobacterium longum) and bifidobacterium bifidum (bifidobacterium bifidum). More preferably, the active probiotic is a combination of M.Weizhenhancescens, M.paracasei, B.adolescentis and L.acidophilus.
In the invention, the naming of the active probiotics is named according to the bulletins (2022, no. 4) which are issued by the national health and wellness Committee of 8 th month of 2022 and are updated by the edible bacterial strain list and the infant food bacterial strain list.
As a preferred embodiment of the present invention, the probiotic protecting agent includes one or any combination of glycerin, trehalose, hyaluronic acid, mannitol, tween, casein and polyethylene oxide.
As a preferred embodiment of the present invention, the functional component includes one or any combination of whitening active, moisturizing active, anti-aging active, anti-inflammatory active, anti-acne active, anti-allergic active, anti-photoactive active and anti-glycation active; preferably, the functional component is a plant extract, such as tea extract, rose extract, etc.
As a preferred scheme of the invention, the auxiliary materials comprise one or any combination of humectant, emollient, thickener, emulsifier and surfactant; preferably, the auxiliary material is one or any combination of carbomer, hydroxyethyl cellulose, butanediol and glycerol.
In selecting the starting materials for the preparation of the sheath fibers, water-soluble materials such as gum arabic, pullulan, silk fibroin, water-soluble nanofiber polymers (e.g., polyethylene glycol), hyaluronic acid, guar gum, or other water-soluble polymers are preferably selected. In selecting the probiotic protectant and adjuvants, water-soluble materials are preferably selected, for example the probiotic protectant may be selected from glycerol, trehalose, hyaluronic acid, mannitol, tween and polyethylene oxide. The adjuvants may be selected from carbomers, hydroxyethylcellulose, butylene glycol and glycerol. The fiber membrane prepared from the water-soluble raw materials is selected, and after water is sprayed on the fiber membrane in the use process, the membrane material can be dissolved, so that a user does not need to clean after the application, and the use convenience is improved. And the fiber membrane can be used as a skin care component after being dissolved, so as to nourish the skin.
As a preferable mode of the invention, the thickness of the fiber film is 60-120 μm, preferably 80-100 μm.
As a preferred embodiment of the present invention, the water activity of the fiber film is 0.20 or less.
As a preferable mode of the present invention, the fiber film is encapsulated in a package material filled with carbon dioxide and/or nitrogen, preferably, nitrogen.
The second purpose of the invention is realized by adopting the following technical scheme:
the preparation method of the active probiotic membrane material comprises the following steps:
the preparation method of the core spinning liquid comprises the following steps: placing raw materials containing active probiotics, a probiotic protective agent and functional components and/or auxiliary materials into a first blending tank, uniformly mixing, vacuumizing, discharging gas in the first blending tank, and refrigerating to obtain core spinning liquid;
and (3) preparing a shell spinning liquid: placing the preparation raw materials of the shell fibers in a second blending tank, uniformly stirring at normal temperature or heating and uniformly stirring, vacuumizing and discharging gas in the second blending tank, and heating and preserving heat to maintain the preparation raw materials of the shell fibers in a liquid state to obtain shell spinning liquid;
the liquid adding step comprises the following steps: adding the core spinning liquid into a first pump body; adding the shell spinning liquid into a second pump body, and heating and preserving heat to the second pump body so as to maintain the preparation raw materials of the shell fibers in a liquid state;
and (3) electrostatic spinning: adopting coaxial electrostatic spinning equipment to spin, and setting environmental parameters of the coaxial electrostatic spinning equipment and operation parameters of a spinneret of the coaxial electrostatic spinning equipment; starting an electrostatic spinning program, wherein the core spinning liquid and the shell spinning liquid are sprayed out of the spinneret at the same time, and a fiber film formed by interweaving core-shell structure fiber yarns is formed on a receiving roller; the core-shell structured fiber yarn comprises a sheath fiber formed from the core spinning liquid and a content formed from the sheath spinning liquid;
and (3) drying treatment: drying the fiber membrane;
cutting and packaging: cutting and punching the dried fiber membrane, and then filling the fiber membrane into a packing material.
In the core spinning liquid preparation step, the core spinning liquid is refrigerated at a temperature of 2-10 ℃ for 0-4 hours, and the refrigerating time is preferably 0 hours (i.e., the electrospinning operation is performed immediately after the core spinning liquid is prepared).
In the core spinning liquid preparation step, the raw material containing active probiotics is probiotic freeze-dried powder or probiotic mud, and preferably is probiotic freeze-dried powder. The active probiotics comprise one or any combination of lactobacillus plantarum, lactobacillus paracasei, bifidobacterium animalis subspecies lactis, lactobacillus fermentum, lactobacillus salivarius, lactobacillus acidophilus, pediococcus pentosaceus, manella coagulans, bifidobacterium adolescentis, bifidobacterium animalis subspecies animalis, lactobacillus reuteri, bifidobacterium longum subspecies longum and bifidobacterium bifidum; the active probiotic is preferably a combination of M.Weizhengi, B.paracasei, B.adolescentis and Lactobacillus acidophilus.
The probiotic protective agent comprises one or any combination of glycerol, trehalose, hyaluronic acid, mannitol, tween, casein and polyethylene oxide; the functional components comprise one or any combination of whitening active, moisturizing active, anti-aging active, anti-inflammatory active, anti-acne active, antiallergic active, anti-photoactive active and anti-saccharification active; the auxiliary materials comprise one or any combination of humectant, emollient, thickener, emulsifier and surfactant.
In the preparation step of the shell spinning liquid, the shell fiber comprises one or any combination of gum arabic, pullulan, silk fibroin, poly epsilon-caprolactone, polylactic acid, polyethylene glycol, polylactic acid-glycolic acid copolymer, hyaluronic acid and guar gum. Preferably, the shell fiber is prepared from one or two of gum arabic and pullulan, preferably a combination of gum arabic and pullulan, and the mass ratio of the gum arabic to the pullulan is preferably 1: (0.2-5), more preferably 1: (0.5-2), preferably 1:2.
As a preferable scheme of the invention, in the electrostatic spinning step, the environmental parameters comprise environmental temperature, environmental humidity and gas environment, the environmental temperature is set to be 20+/-5 ℃, the environmental humidity is less than 40%, and the gas environment is N 2 And/or CO 2 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the ambient temperature is set to be 20+/-5 ℃, the ambient humidity is less than 30 percent, and the gas environment is N 2 . The thickness of the fiber film formed by electrospinning is 60-120 mu m, preferably 80-100 mu m. The spinning head maintains the same spinning speed in the spinning process, and the receiving roller is covered with a receiving carrier, and the receiving carrier is preferably non-woven fabric, aluminum foil or tencel fiber cloth.
As a preferable scheme of the invention, in the drying treatment step, a low-temperature vacuum drying mode is adopted, and the drying temperature is-30-5 ℃ so that the water activity of the fiber membrane is less than or equal to 0.20.
In a preferred embodiment of the present invention, in the cutting and packaging step, the fibrous film is encapsulated in a packaging material filled with carbon dioxide and/or nitrogen, preferably, nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
(1) The active probiotic membrane material provided by the invention is a dry type and fibrous membrane type adhesive membrane material integrated with skin care raw materials, in the use process, the membrane material is firstly taken out from a packaging material and is adhered to the skin of a face, then proper liquid, such as purified water, rose water and the like, is sprayed on the membrane material, the membrane material can be tightly adhered to the skin, the use is convenient, the probiotics are packaged in the fibers of a shell, and the active retention rate of the probiotics is high.
(2) The preparation method of the active probiotic membrane material provided by the invention has the advantages that the loading mode of the probiotics on the membrane material is novel, the probiotic loading process does not involve the culture of bacteria and the formation of a biological membrane, the flow is simple, the continuous high-efficiency production can be realized, the quality is controllable, and the preparation method is suitable for industrial production and has good commercial prospect.
Drawings
Fig. 1 is a graph showing the change of the stability of probiotics in the mask provided in the embodiment 1 of the present invention;
fig. 2 is a graph showing the change of the stability of probiotics in the mask provided in embodiment 2 of the present invention;
FIG. 3 is a graph showing the result of the survival rate of probiotics in mask provided in examples 19-37 of the present invention;
FIG. 4 is a graph showing the results of the storage stability of the probiotics provided in examples 19-37 of the present invention;
fig. 5 is a physical display diagram of the active probiotic facial mask provided in embodiment 1 of the present invention;
fig. 6 is a physical display diagram of the active probiotic facial mask provided in embodiment 2 of the present invention;
fig. 7 is a display of the active probiotic facial mask according to example 2 of the present invention after being torn apart from the carrier;
fig. 8 is a device diagram of an electrostatic spinning apparatus according to an embodiment of the present invention.
In the figure, 1, a first pump body; 2. a spinneret; 3. a second pump body; 4. a heat preservation heating device; 5. a receiving roller; 6. and a power supply.
Description of the embodiments
The present invention will be further described with reference to the accompanying drawings and detailed description, wherein it is to be understood that, on the premise of no conflict, the following embodiments or technical features may be arbitrarily combined to form new embodiments. The raw materials, equipment, etc. used in the following examples are available in a purchase manner except for special restrictions.
Examples
The active probiotic membrane material is prepared according to the following method:
the preparation method of the core spinning liquid comprises the following steps: mixing 20 g of protective agent (glycerol 4 parts, trehalose 2 parts, mannitol 0.5 parts) and 29 g of mask raw material (carbomer 1 parts, hydroxyethyl cellulose 1 parts, 1, 3-butanediol 1 parts), heating to 85deg.C, stirring to dissolve uniformly to obtain solution A, maintaining the temperature for 30min, cooling to 30deg.C, mixing 1 g of probiotic lyophilized powder (Lactobacillus plantarum 1 parts, bifidobacterium animalis subspecies 1 part, lactobacillus reuteri 1 part, bifidobacterium bifidum 0.5 parts, and viable count of probiotic lyophilized powder not less than 1.0X10% 11 cfu/g) and the solution A are uniformly mixed, the mixture is rapidly cooled to 5+/-2 ℃ after being vacuumized and discharged, the mixture is refrigerated for standby, and electrostatic spinning is carried out after 4 hours of refrigeration.
And (3) preparing a shell spinning liquid: 50g of shell fiber preparation raw materials (1 part of gum arabic, 2 parts of pullulan, 0.02 part of silk fibroin, 0.5 part of polylactic acid-glycolic acid and 0.2 part of guar gum) are taken, mixed, heated, stirred and melted, and then vacuumized to remove internal gas, so as to obtain liquid B (shell spinning liquid), and the liquid B is kept in a liquid state by sealing and heat preservation.
The liquid adding step comprises the following steps: as shown in fig. 8, core spinning liquid and shell spinning liquid are pumped into a first pump body 1 and a second pump body 3 respectively, and the second pump body is insulated by a heat insulation heating device 4 at 65 ℃ so that the shell spinning liquid is in a liquid state;
and (3) electrostatic spinning: as shown in FIG. 8, the spinning was performed by using a coaxial electrostatic spinning apparatus, and the environmental parameters (temperature 20.+ -. 5 ℃ C., humidity < 30% and gas atmosphere N) of the coaxial electrostatic spinning apparatus were set 2 ) And the operating parameters of the spinneret 2 of the coaxial electrospinning apparatus; starting an electrostatic spinning procedure, spraying core spinning liquid and shell spinning liquid from a spinneret 2 at the same time, keeping the same spinning speed of the spinneret 2 in the spinning process, and finally forming a fiber film with the thickness of 100 mu m formed by interweaving core-shell structure fiber yarns on a receiving roller 5 (the core-shell structure fiber yarns are densely staggered with each other); the core-shell structured fiber yarn comprises shell fiber and content, wherein the content is formed by core spinning liquid, and the shell fiber is formed by shell spinning liquid; wherein the receiving carrier covered on the receiving roller 5 is aluminum foil. The coaxial electrostatic spinning device is connected with a power supply 6.
And (3) drying treatment: carrying out low-temperature vacuum drying treatment on the fiber membrane of the active probiotics obtained by electrostatic spinning, wherein the drying temperature is-5 ℃, so that the water activity of the fiber membrane is less than 0.20;
cutting and packaging: cutting and punching the dried fiber membrane according to the set size (cutting according to a mask mode), then filling nitrogen for packaging, and storing at the temperature of 2-10 ℃.
The mask obtained in example 1 (as shown in FIG. 5) had a live bacterial count of 4.5X10 of probiotics immediately after completion of the preparation 7 cfu/cm 2 . Calculating the survival rate of probiotics after being stored for 1-4 weeks by taking the live bacterial amount of the probiotics of the prepared facial mask as a reference, and accelerating the test stability change condition at 37 DEG CThe condition is shown in figure 1, and after 1 week of preservation, the survival rate of the probiotics is 83.5%; after 2 weeks of storage, the survival rate of the probiotics was 60.7%, after 3 weeks of storage, the survival rate of the probiotics was 36.3%, after 4 weeks of storage, the survival rate of the probiotics was 16.4%.
Examples
The active probiotic membrane material is prepared according to the following method:
the preparation method of the core spinning liquid comprises the following steps: mixing 20 g of protective agent (2 parts of glycerin, 0.5 part of trehalose, 2 parts of hyaluronic acid, 0.5 part of mannitol and 2 parts of polyethylene oxide solution), 29 g of mask raw and auxiliary materials (2 parts of 1, 3-butanediol, 0.5 part of carbomer, 0.5 part of hydroxyethyl cellulose, 0.01 part of tea extract and 0.005 part of small-rain bird's nest extract), heating to 85 ℃, stirring and dissolving uniformly to obtain solution A, and cooling to 30 ℃ after heat preservation for 30 min; then 1 g of probiotics freeze-dried powder (1 part of condensed Wittman's bacteria, 1 part of cheese bacillus, 1 part of bifidobacterium adolescentis and 1 part of lactobacillus acidophilus, wherein the viable count of the probiotics freeze-dried powder is more than or equal to 1.0x10) 11 cfu/g) and the solution A are uniformly mixed, the core spinning liquid is obtained by rapidly cooling to 5+/-2 ℃ after vacuumizing and discharging internal gas, and then is immediately added into a pump body, and electrostatic spinning is carried out (namely, the refrigerating time is 0 hour).
And (3) preparing a shell spinning liquid: mixing 50g of shell fiber preparation raw materials (1 part of gum arabic and 2 parts of pullulan), heating, stirring and melting, vacuumizing to remove internal gas to obtain solution B (shell spinning liquid), and sealing and preserving heat to maintain the solution B in a liquid state.
The liquid adding step comprises the following steps: pumping core spinning liquid and shell spinning liquid into a first pump body and a second pump body respectively, and keeping the temperature of the second pump body at 65 ℃ to enable the shell spinning liquid to be in a liquid state;
and (3) electrostatic spinning: adopting coaxial electrostatic spinning equipment to spin, setting environmental parameters (temperature 20+ -5 deg.C, humidity less than 30%, gas environment N) of the coaxial electrostatic spinning equipment 2 ) And operating parameters of a spinneret of the coaxial electrospinning apparatus; starting an electrostatic spinning procedure, and simultaneously spraying core spinning liquid and shell spinning liquid from a spinneret, wherein the spinneret is kept in the spinning processAt the same spinning speed, finally forming a fiber membrane with the thickness of 80 mu m, which is formed by interweaving core-shell structure fiber filaments, on a receiving roller (the core-shell structure fiber filaments are densely staggered with each other); the core-shell structured fiber yarn comprises shell fiber and content, wherein the content is formed by core spinning liquid, and the shell fiber is formed by shell spinning liquid; wherein the receiving carrier covered on the receiving roller is non-woven fabric.
And (3) drying treatment: and carrying out low-temperature vacuum drying treatment on the fiber membrane of the active probiotics obtained by electrostatic spinning, wherein the drying temperature is-5 ℃, so that the water activity of the fiber membrane is less than 0.20.
Cutting and packaging: cutting and punching the dried fiber membrane according to the set size (cutting according to a mask mode), then filling nitrogen for packaging, and storing at the temperature of 2-10 ℃.
The mask obtained in example 2 (as shown in FIGS. 6-7) had a live bacteria count of 6.3X10% of probiotics immediately after completion of preparation 7 cfu/cm 2 . Calculating the survival rate of the probiotics after 1-4 weeks of storage by taking the live bacterial amount of the probiotics of the prepared facial mask as a reference, wherein the change condition of the stability of the 37 ℃ accelerated test is shown in a figure 2, and the survival rate of the probiotics after 1 week of storage is 88.5%; after 2 weeks of storage, the survival rate of the probiotics was 70.2%, after 3 weeks of storage, the survival rate of the probiotics was 55.7%, after 4 weeks of storage, the survival rate of the probiotics was 46.5%.
Examples 3 to 5
Examples 3-5 differ from example 2 in that: in the core dope preparation step, the core dope was cooled for 4 hours in example 3, 8 hours in example 4, and 12 hours in example 5.
The probiotic viable count of the mask product just after the preparation was detected, and the viable count of example 2 was the largest, calculated as 100%. The specific results are shown in Table 1 below.
TABLE 1 Table of results of influences of core spinning liquid refrigerating time on live bacteria amount
| Example 2 | Example 3 | Example 4 | Example 5 | |
| Liquid cooling time (hours) | 0 | 4 | 8 | 12 |
| The number of viable bacteria of the finished mask (x 10) 7 cfu/cm 2 ） | 6.30 | 6.03 | 4.48 | 3.90 |
| Survival (%) | 100 | 95.69 | 71.11 | 61.90 |
As can be seen from the records in table 1 above, the core spinning liquid containing active probiotics, the cold storage time prolonged, the number of living bacteria reduced, and the number of living bacteria loaded on the finished mask product correspondingly reduced. Therefore, the core spinning liquid is preferably added into the pump body for spinning without refrigeration; and the refrigerating time after the preparation of the core spinning liquid is not more than 4 hours.
Examples 6 to 18
Examples 6-18 differ from example 2 in that: in the sheath spinning liquid preparation step, the sheath fibers are prepared from different raw materials, and the details are shown in table 2 below. The viable count of the finished mask of each example was measured separately and stability testing was performed. The method for testing the stability comprises the following steps: the active probiotic-loaded masks of examples 2, 6-18 were vacuum packed in aluminum foil bags, respectively, and placed at 25 ℃ for 3 months, the viable bacteria amounts were determined and the probiotic survival rates were calculated.
TABLE 2 Table of results of the effect of raw materials for preparing sheath fibers on the viable count
As can be seen from the record in table 2, the live bacterial count and the viable bacterial count of the probiotics are higher when the encapsulating wall material (shell fiber) is gum arabic and/or pullulan. In addition, when the shell fiber raw material is combined with the gum arabic and the pullulan, the effect is better. When the mass ratio of the gum arabic to the pullulan is 1: (0.5-2), the synergistic effect (examples 2, 6-7) is achieved. In particular, the synergy is most pronounced when the ratio of gum arabic to pullulan is 1:2, example 2 being the preferred example.
Examples 19 to 37
Examples 19-37 differ from example 2 in that example 19 uses a probiotic bacterial sludge; examples 20-37 employed different probiotics and a differential selection of probiotic freeze-dried powder and probiotic puree was performed. The survival rate and storage stability of the probiotic after processing were recorded and the results are shown in table 3 and figures 3 and 4.
Wherein the survival rate of the probiotics after processing is calculated according to the following method: calculating the number of living bacteria loaded on the theoretical mask by using the addition amount of the bacteria powder/the bacteria mud before processing, and taking the number as a denominator; and taking the actual measured value of the number of the live bacteria carried by the processed mask as a molecule. The ratio of the numerator to the denominator was taken as the survival rate after processing.
The storage stability calculating method comprises the following steps: the finished mask product is packaged in an aluminum foil bag in a sealing way, the speed is increased by 7 days at 37 ℃, and the stability result is obtained by the ratio of the viable count of the 7 th day to the viable count of the 0 th day (namely, the mask is just prepared). The accelerating experiment of the invention is carried out according to the guiding principle of the stability test of biological products in 2020 edition of Chinese pharmacopoeia, the set temperature is 37 ℃ and the time is 7 days.
TABLE 3 results of Probiotics lyophilized powder/sludge effects on Probiotics survival and stability
As can be seen from the records in table 3, the lyophilized powder of different strains has a higher resistance to the outside during the preparation of the probiotic mask, a higher survival rate of the probiotics after processing, and a higher stability in the storage of the simulated finished product, compared with the freshly cultured probiotic centrifugal re-suspension bacterial sludge. That is, the encapsulated active probiotic is preferably a probiotic freeze-dried powder.
The results of example 34 show that when lyophilized powder of coagulated Wittman's bacteria is used as the active probiotic of the mask, the survival rate of the probiotic after processing is high and the storage stability is good. From the results of example 36, it can be obtained that when the bifidobacterium adolescentis freeze-dried powder is used as active probiotics of the facial mask, the survival rate of the probiotics after processing is lower, the survival rate is only 75%, and the stability after 7 days acceleration at 37 ℃ is only 80%. When the bifidobacterium adolescentis is combined with the ' condensation of the Weizhman's bacteria, the cheese bacillus and the lactobacillus acidophilus ', the survival rate after processing reaches 97%, the storage stability reaches 88.5%, and the four can play a role in synergy, so that the survival rate and the storage stability of the probiotics after processing are integrally improved. This is very important for mask preparation, as different probiotics can play different beneficial roles on the skin, and the beneficial effects of different probiotics can be exerted simultaneously by combining different probiotics.
Examples 38 to 43
Examples 38-43 differ from example 2 in the electrospinning environment, as detailed in table 5 below. The evaluation index comprises the survival rate of probiotics and the spinning quality.
The survival rate of the probiotics is that the mask is prepared under the corresponding environment, and the probiotics are stored for 7 days at 25 ℃. Survival levels were divided into 3 classes, wherein: grade A, the survival rate is more than or equal to 70%; b, the survival rate is more than or equal to 50 and less than 70 percent; grade C, survival rate is less than 50%.
The examination index of the spinning quality is shown in Table 4.
TABLE 4 quality score index record of spun fiber film
| Index (I) | Weight (%) |
| Ease of separation from receiving |
20 |
| Flatness of spinning |
20 |
| Skin feel of fitting face | 30 |
| Strength of fiber | 30 |
TABLE 5 results of the effects of the electrospinning environment on the survival rate and spinning quality of probiotics
| Spinning environment (temperature, humidity, gas environment) | Survival rate level (3 grade) | Spinning quality (5 minutes) | |
| Example 2 | 20±5℃，30%，N 2 | A | 4.8 |
| Example 38 | 30±5℃，30%，N 2 | B | 4.2 |
| Example 39 | 40±5℃，30%，N 2 | C | 3.8 |
| Example 40 | 20±5℃，20%，N 2 | A | 4.8 |
| Example 41 | 20±5℃，40%，N 2 | B | 4.2 |
| Example 42 | 20±5℃，30%，CO 2 | B | 4.5 |
| Example 43 | 20±5℃，30%，CO 2 :N 2 =1:1 | B | 4.5 |
As can be seen from the records in Table 5, the environmental temperature of the electrostatic spinning device of the present invention was maintained at 20.+ -. 5 ℃ and the humidity of the environment was < 30% in the spinning equipment, and the gas environment composition was N 2 The survival rate of the probiotics is highest, the spinning quality is optimal, and the spinning environment of the embodiment 2 is a preferable spinning environment.
Examples 44 to 47
Examples 44-47 differ from example 2 in the thickness of the electrospun formed fibrous films, as detailed in Table 6 below. In Table 6, the index of the fiber quality score is the same as that in Table 4, and the viable count of the probiotics is the viable count of the mask product just after the preparation.
TABLE 6 results recording the effect of fiber film thickness on probiotic survival and spinning quality
| Fiber thickness (mum) | Fiber quality score (5 minutes system) | Probiotic viable count (×10) 7 cfu/cm 2 ） | |
| Example 44 | 50 | 2.2 | 0.18 |
| Example 45 | 60 | 3.7 | 1.74 |
| Example 2 | 80 | 4.6 | 6.30 |
| Example 46 | 100 | 4.3 | 8.38 |
| Example 47 | 120 | 3.5 | 13.20 |
From the record of table 6, it can be seen that the thickness of the fibrous membrane affects the quality of the fibers and also directly affects the survival rate of the probiotics. From the standpoint of combining 2 indices, the thickness of the fiber formed by spinning can be selected to be 60 μm to 120 μm, more preferably 80 μm to 100 μm.
Examples 48 to 78
Examples 48-78 differ from example 2 in that the water activity of the fibrous membrane after drying differs during the drying treatment step or the active probiotics selected during the core spinning liquid preparation step, as detailed in table 7 below. The survival rate of the probiotics (survival rate of probiotics when the mask was formed) of the different examples was recorded. The probiotic survival rate was calculated according to the following method: calculating the number of living bacteria loaded on the theoretical mask by using the addition amount of the probiotics freeze-dried powder before processing, and taking the number as a denominator; and taking the actual measured value of the number of the live bacteria carried by the processed mask as a molecule. The ratio of the numerator to the denominator is taken as the survival rate of the probiotics.
TABLE 7 results of the effect of water activity on probiotic survival
As can be seen from the results of table 7, the water activity of the fiber film directly affects the survival rate of the probiotics, and the survival rate of the probiotics is high when the water activity of the fiber film is controlled to be 0.20 or less.
When the probiotics in the mask is a single strain and the water activity is 0.2+/-0.03, the survival rate of lactobacillus plantarum, weizhman's bacteria, lactobacillus paracasei and lactobacillus acidophilus can reach 90% or more. And when the water activity is 0.2+/-0.03, the survival rate of the bifidobacterium adolescentis is only 75%, and the survival rate is lower. When the bifidobacterium adolescentis is combined with the 'condensation of the Weizhman bacteria, the cheese bacillus and the lactobacillus acidophilus', the survival rate after processing reaches 97%, and the four can play a role in synergy, so that the survival rate and the storage stability of the probiotics after processing are integrally improved. This is very important for mask preparation, as different probiotics can play different beneficial roles on the skin, and the beneficial effects of different probiotics can be exerted simultaneously by combining different probiotics.
Examples 79 to 82
Examples 79-82 differ from example 2 in that the mask pack (aluminum foil pouch sealed package) was filled with a gas, as detailed in table 8. The survival rate of probiotics is examined, and the method is as follows: the finished mask product is packaged in an aluminum foil bag in a sealing way, the speed is increased by 7 days at 37 ℃, and the stability result is obtained by the ratio of the viable count of the 7 th day to the viable count of the 0 th day (namely, the mask is just prepared).
TABLE 8 Table of the results of the effect of package aeration on probiotic survival
| Gas composition | Survival rate (37 ℃,7 days,%) | |
| Example 79 | Ordinary air | 48.36 |
| Example 80 | Dehumidified air (humidity less than or equal to 20%) | 57.65 |
| Example 81 | CO 2 | 60.35 |
| Example 2 | N 2 | 88.5 |
| Example 82 | CO 2 :N 2 =1:1（v/v） | 72.68 |
As can be seen from the records in table 8, the mask provided in the embodiment of the present invention can fill carbon dioxide, nitrogen or a mixture of the two into the packaging material. When the gas filled is nitrogen, the survival rate of the probiotics is high.
According to the active probiotic membrane material provided by the embodiment of the invention, probiotics are uniformly mixed in the core spinning liquid, and the core spinning liquid and the shell spinning material are spun simultaneously, so that the coating effect of the probiotics is greatly improved, and the stability of the active probiotics is enhanced.
The embodiment of the invention innovatively provides a set of preparation technical parameters of the active probiotic membrane material, and ensures that the probiotics loaded on the processed mask keep high survival rate and activity.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.
Claims (7)
1. The active probiotic membrane material is characterized by comprising a fiber membrane manufactured by an electrostatic spinning process, wherein in the electrostatic spinning process, the environment temperature is set to be 20+/-5 ℃, the environment humidity is less than 30%, and the gas environment is N 2 ；
The thickness of the fiber membrane is 80-100 mu m; the fiber membrane is formed by interweaving core-shell structure fiber filaments encapsulated with active probiotics; the core-shell structured fiber yarn comprises shell fibers and contents; the shell fiber is prepared from the raw materials of combination of gum arabic and pullulan, wherein the mass ratio of the gum arabic to the pullulan is 1:2; the content comprises the active probiotics and a probiotic protecting agent and one or two of functional components and auxiliary materials;
the active probiotics comprise one or any combination of lactobacillus plantarum, lactobacillus paracasei, bifidobacterium animalis subspecies lactis, lactobacillus mucilaginosus, lactobacillus salivarius, lactobacillus acidophilus, pediococcus pentosaceus, M.Weizhenhanensis and bifidobacterium adolescentis; the raw materials of the active probiotics are probiotic freeze-dried powder;
the probiotic protective agent comprises one or any combination of glycerol, trehalose, hyaluronic acid, mannitol, tween, casein and polyethylene oxide;
the functional components comprise one or any combination of whitening active, moisturizing active, anti-aging active, anti-inflammatory active, anti-acne active, antiallergic active, anti-photoactive active and anti-saccharification active;
the auxiliary materials comprise one or any combination of humectant, emollient, thickener, emulsifier and surfactant.
2. The active probiotic film of claim 1, wherein the active probiotic is a combination of mansoni coagulans, lactobacillus paracasei, bifidobacterium adolescentis, and lactobacillus acidophilus; the functional component is a plant extract; the auxiliary material is one or any combination of carbomer, hydroxyethyl cellulose, butanediol and glycerol.
3. The active probiotic film material of claim 1, wherein the fiber film has a water activity of 0.20 or less; the fiber membrane is encapsulated in a packing material, and carbon dioxide and/or nitrogen is filled in the packing material.
4. The active probiotic film material of claim 1, wherein the fiber film is encapsulated in a wrapper, the wrapper being filled with nitrogen.
5. A method of preparing an active probiotic film according to any one of claims 1 to 4, comprising the steps of:
the preparation method of the core spinning liquid comprises the following steps: placing the probiotic freeze-dried powder, the probiotic protective agent and the functional components and/or auxiliary materials into a first blending tank, uniformly mixing, vacuumizing, discharging gas in the first blending tank, and refrigerating to obtain core spinning liquid;
and (3) preparing a shell spinning liquid: placing the preparation raw materials of the shell fibers in a second blending tank, uniformly stirring at normal temperature or heating and uniformly stirring, vacuumizing and discharging gas in the second blending tank, and heating and preserving heat to maintain the preparation raw materials of the shell fibers in a liquid state to obtain shell spinning liquid;
the liquid adding step comprises the following steps: adding the core spinning liquid into a first pump body; adding the shell spinning liquid into a second pump body, and heating and preserving heat to the second pump body so as to maintain the preparation raw materials of the shell fibers in a liquid state;
and (3) electrostatic spinning: adopting coaxial electrostatic spinning equipment to spin, and setting environmental parameters of the coaxial electrostatic spinning equipment and operation parameters of a spinneret of the coaxial electrostatic spinning equipment; the environmental parameters comprise environmental temperature, environmental humidity and gas environment, the environmental temperature is set to be 20+/-5 ℃, the environmental humidity is less than 30%, and the gas environment is N 2 The method comprises the steps of carrying out a first treatment on the surface of the Starting an electrostatic spinning program, wherein the core spinning liquid and the shell spinning liquid are sprayed out of the spinneret at the same time, and a fiber film formed by interweaving core-shell structure fiber yarns is formed on a receiving roller; the core-shell structured fiber yarn comprises a sheath fiber formed from the core spinning liquid and a content formed from the sheath spinning liquid;
and (3) drying treatment: drying the fiber membrane;
cutting and packaging: cutting and punching the dried fiber membrane, and then filling the fiber membrane into a packing material.
6. The method for preparing an active probiotic film material according to claim 5, wherein in the core spinning liquid preparation step, the cooling temperature is 2-10 ℃ and the cooling time is 0-4 hours;
in the electrostatic spinning step, the spinning nozzle keeps the same spinning speed in the spinning process, and a receiving carrier is covered on the receiving roller;
in the drying treatment step, a low-temperature vacuum drying mode is adopted, and the drying temperature is-30-5 ℃ so that the water activity of the fiber membrane is less than or equal to 0.20;
in the cutting and packaging step, the fiber film is encapsulated in a packaging material, and the packaging material is filled with carbon dioxide and/or nitrogen.
7. The method for preparing an active probiotic membrane material according to claim 5, wherein in the core spinning liquid preparation step, the raw material containing active probiotics is probiotic freeze-dried powder, and the refrigerating time is 0 hours;
in the electrostatic spinning step, the receiving carrier covered on the receiving roller is non-woven fabric, aluminum foil or tencel fiber cloth;
in the cutting and packaging step, the fiber film is encapsulated in a packaging material, and the packaging material is filled with nitrogen.
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