阅读说明：本技术 一种天然抗菌保水面膜的制备方法 (Preparation method of natural antibacterial water-retention mask ) 是由 汤佳鹏 葛彦 朱俐 于 2019-09-20 设计创作，主要内容包括：本发明公开了一种天然抗菌保水面膜的制备方法,包括(1)将一定量聚谷氨酸和聚赖氨酸完全溶解于5v/v％三氟乙酸溶液,搅拌均匀,得到纺丝液；(2)采用纺丝液进行静电纺丝,得到PGA/PL纳米纤维膜；(3)将PGA/PL纳米纤维膜经等离子处理器处理活化；(4)活化的纳米纤维浸泡在二十八烷醇脂酶溶液中进行负压闪爆,之后进行酯化接枝反应,离心冻干。本发明制备的面膜环保可降解,且对皮肤具有高效的吸水保湿激活的作用,能够用于高级化妆品和面膜中。(The invention discloses a preparation method of a natural antibacterial water-retention mask, which comprises the following steps of (1) completely dissolving a certain amount of polyglutamic acid and polylysine in 5 v/v% trifluoroacetic acid solution, and uniformly stirring to obtain spinning solution; (2) carrying out electrostatic spinning by adopting the spinning solution to obtain a PGA/PL nano fiber membrane; (3) activating the PGA/PL nano fiber membrane by a plasma processor; (4) soaking the activated nano-fiber in octacosanol lipase solution for negative pressure flash explosion, then carrying out esterification graft reaction, centrifuging and freeze-drying. The mask prepared by the invention is environment-friendly and degradable, has efficient water absorption, moisture retention and activation effects on skin, and can be used in advanced cosmetics and masks.)

1. A preparation method of a natural antibacterial water-retention mask is characterized by comprising the following steps:

s1: dissolving polyglutamic acid and polylysine in trifluoroacetic acid solution, and uniformly stirring to obtain spinning solution;

s2: performing electrostatic spinning by using the spinning solution to obtain a PGA/PL nano fiber membrane;

s3: activating the PGA/PL nano fiber membrane through plasma treatment to obtain an activated nano fiber membrane;

s4: and (4) soaking the nanofiber membrane obtained in the step (S3) in a octacosanol lipase solution for negative pressure flash explosion, performing esterification grafting reaction, and performing centrifugal freeze-drying to obtain the natural antibacterial water-retention mask.

2. The method for preparing a natural antibacterial water-retention mask as claimed in claim 1, wherein in step S1, the polyglutamic acid has an average molecular weight of 200-1000kDa, and the polylysine has an average molecular weight of 3000-4000 Da.

3. The preparation method of the natural antibacterial water-retention mask as claimed in claim 1, wherein in step S1, the concentration of polyglutamic acid in the spinning solution is 5-20 g/L, and the concentration of polylysine is 4-10 g/L.

4. The preparation method of the natural antibacterial water-retention mask as claimed in claim 1, wherein in the step S2, in the electrostatic spinning process, the specification of an injector is 10ml, the specification of a needle head is a flat head, a 7-gauge needle is adopted, the voltage is 12-20 KV, the distance is 7-10 cm, the sample injection rate is 0.3-1.0 ml/h, and the temperature is 25-35 ℃.

5. The method for preparing a natural antibacterial water-retaining mask as claimed in claim 1, wherein in step S3, the plasma treatment conditions are as follows: the gas is nitrogen or oxygen, the treatment power is 250-300W, the pressure is 50-60 Pa, and the treatment time is 10-15 min.

6. The method for preparing a natural antibacterial water-retention mask as claimed in claim 1, wherein in step S4, the solvent in the octacosanol lipase solution is ethanol, the octacosanol concentration is 4-8 g/L, and the lipase concentration is 20-50 g/L.

7. The method for preparing a natural antibacterial water-retention mask as claimed in claim 1 or 6, wherein in step S4, the lipase activity is 30-80U/mg.

8. The preparation method of the natural antibacterial water-retention mask as claimed in claim 1, wherein in step S4, the vacuum degree of negative pressure flash explosion is 0.100-0.024 mBar.

9. The preparation method of the natural antibacterial water-retention mask as claimed in claim 1, wherein in the step S4, the immersion bath ratio of the esterification grafting reaction is 1: 100-1: 300, the reaction temperature is 35-40 ℃, and the reaction time is 12-24 hours.

10. The preparation method of the natural antibacterial water-retention mask as claimed in claim 1, wherein in step S4, the freeze-drying temperature is-30 to-20 ℃, the vacuum degree is 0.100 to 0.024mBar, and the freeze-drying time is 3 to 5 days.

Technical Field

The invention relates to the fields of biochemical engineering and cosmetics, in particular to a preparation method of a natural antibacterial water-retention mask.

Background

At present, the beauty and skin care facial mask on the market is basically manufactured by adopting chemical synthetic fiber non-woven fabrics or artificial fiber non-woven fabrics through the working procedures of folding, bagging, injecting soak solution, sealing and the like, but the synthetic fiber non-woven fabrics or the artificial fiber non-woven fabrics generally have the degradation problem, can not be recycled, and easily cause environmental pollution after being used by consumers. The fiber and the adhesive of the non-woven fabric can be partially dissolved after being soaked in the soaking solution for a long time, so that the using effect of the mask is reduced, and even the phenomenon of consumer allergy can be caused. In addition, the soak solution of the common mask is thickened by using high molecular synthetic resin, so that a consumer feels tight after using the mask and feels uncomfortable when using the mask. The mask with the synthetic fiber non-woven fabric or artificial fiber non-woven fabric substrate has the advantages that nutrient substances and a large amount of moisture exist in the soak solution, and microorganisms and bacteria are easily generated, so the shelf life of the mask is directly influenced, and particularly the effective period of bioactivity is directly influenced.

Disclosure of Invention

In view of the above, the invention aims to provide a preparation method of a natural antibacterial water-retaining facial mask, and the facial mask prepared by the invention has a better water-retaining and skin cell activating function.

In order to solve the technical problems, the invention provides a preparation method of a natural antibacterial water-retention mask, which comprises the following steps:

s1: dissolving polyglutamic acid and polylysine in trifluoroacetic acid solution, and uniformly stirring to obtain spinning solution;

s2: performing electrostatic spinning by using the spinning solution to obtain a PGA/PL nano fiber membrane;

s3: activating the PGA/PL nano fiber membrane through plasma treatment to obtain an activated nano fiber membrane;

s4: and (4) soaking the nanofiber membrane obtained in the step (S3) in a octacosanol lipase solution for negative pressure flash explosion, performing esterification grafting reaction, and performing centrifugal freeze-drying to obtain the natural antibacterial water-retention mask.

Preferably, in step S1, the polyglutamic acid has an average molecular weight of 200 to 1000kDa, and the polylysine has an average molecular weight of 3000 to 4000 Da.

Preferably, in step S1, the concentration of polyglutamic acid in the spinning solution is 5-20 g/L, and the concentration of polylysine is 4-10 g/L.

Preferably, in the step S2, in the electrostatic spinning process, the specification of the injector is 10ml, the specification of the needle head is a flat head, the needle is a 7-gauge needle, the voltage is 12-20 KV, the distance is 7-10 cm, the sample injection rate is 0.3-1.0 ml/h, and the temperature is 25-35 ℃.

Preferably, in step S3, the plasma processing conditions are: the gas is nitrogen or oxygen, the treatment power is 250-300W, the pressure is 50-60 Pa, and the treatment time is 10-15 min.

Preferably, in step S4, the solvent in the octacosanol lipase solution is ethanol, the octacosanol concentration is 4-8 g/L, and the lipase concentration is 20-50 g/L.

Preferably, in step S4, the lipase activity is 30-80U/mg.

Preferably, in step S4, the vacuum degree of the negative pressure flash explosion is 0.100 to 0.024 mBar.

Preferably, in step S4, the bath ratio of the esterification grafting reaction is 1:100 to 1:300, the reaction temperature is 35 to 40 ℃, and the reaction time is 12 to 24 hours.

Preferably, in step S4, the temperature of the freeze-drying is-30 to-20 ℃, the vacuum degree is 0.100 to 0.024mBar, and the freeze-drying time is 3 to 5 days.

Compared with the prior art, the preparation method provided by the invention utilizes a plurality of technologies, including an electrostatic spinning technology, a low-temperature plasma treatment technology, a negative pressure flash explosion technology and the like, the esterification grafting efficiency of octacosanol on polyglutamic acid is greatly improved by using the technologies, the loading capacity is larger, and the prepared mask can better play a role of octacosanol in activating skin cells:

1) the active carboxyl of the polyglutamic acid and the active amino of the polylysine are amidated to adjust the water solubility and the mechanical property of the mask. Meanwhile, the carboxyl is more than the amino in a proper proportion, and the residual carboxyl can be subjected to esterification reaction with octacosanol, so that the mask has strong skin-friendly property and does not have a hard feeling.

2) The antibacterial and antiseptic properties of the polylysine are utilized, so that the mask has antibacterial property.

3) The octacosanol lipase solution is permeated into a fiber structure by a negative pressure flash explosion technology, and the octacosanol can reach the periphery of a carboxyl group more efficiently by the technology because the octacosanol is insoluble in water, so that the bioavailability of the octacosanol is improved.

4) The invention adopts the low-temperature plasma treatment technology to treat the nano-fibers, so that the carboxyl of polyglutamic acid molecules is activated, the esterification reaction is easier to occur, more octacosanol can be combined, and the abundance of the octacosanol is greatly improved.

Drawings

FIG. 1 shows the proliferation rate of mouse L929 fibroblasts treated by the examples of the present invention and the comparative examples;

FIG. 2 shows the results of the moisture retention test of nanofibers according to the examples of the present invention and comparative examples.

Detailed Description

For a further understanding of the invention, reference will now be made to the preferred embodiments of the present invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the present invention and is not intended to limit the scope of the claims which follow.

All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.

The technical scheme adopted by the invention is as follows:

a preparation method of a natural antibacterial water-retention mask comprises the following steps:

s1: dissolving polyglutamic acid and polylysine in trifluoroacetic acid solution, and uniformly stirring to obtain spinning solution;

s2: performing electrostatic spinning by using the spinning solution to obtain a PGA/PL nano fiber membrane;

s3: activating the PGA/PL nano fiber membrane through plasma treatment to obtain an activated nano fiber membrane;

s4: and (4) soaking the nanofiber membrane obtained in the step (S3) in a octacosanol lipase solution for negative pressure flash explosion, performing esterification grafting reaction, and performing centrifugal freeze-drying to obtain the natural antibacterial water-retention mask.

Firstly, dissolving polyglutamic acid and polylysine in trifluoroacetic acid solution, and uniformly stirring to obtain spinning solution. The sources of polyglutamic acid and polylysine in the present invention are not limited, and commercially available products well known to those of ordinary skill in the art can be used. Polyglutamic acid is an extracellular natural high molecular polymer material synthesized by microorganisms, and is a homopolyamide formed by dehydration condensation between alpha-amino and gamma-carboxyl of L-glutamic acid, and the molecular weight is usually between 100kDa and 1000 kDa. Under proper conditions, polyglutamic acid can be catalyzed and degraded by gamma-glutamyl transpeptidase which is widely existed in organisms, and the product is harmless glutamic acid. A large amount of free active alpha-carboxyl exists in the molecular chain of the polyglutamic acid, so that the polyglutamic acid has negative surface charge under the neutral pH condition, and has excellent water solubility and strong adsorbability. The specification of polyglutamic acid in the present invention is preferably an average molecular weight of 200-1000kDa, more preferably an average molecular weight of 600 kDa. Polylysine is a pale yellow powder, has strong hygroscopicity and slight bitterness, and is a straight-chain polymer of lysine. It is not affected by pH, is stable to heat, and can inhibit thermophilic bacteria, so that it can be heat-treated after being added. However, acidic polysaccharides, hydrochlorides, phosphates, copper ions and the like may be bound to decrease the activity. The composition can be used in combination with hydrochloric acid, citric acid, malic acid, glycine and higher fatty glyceride to achieve synergistic effect. The polylysine with the molecular weight of 3600-4300 has the best bacteriostatic activity, and when the molecular weight is lower than 1300, the polylysine loses the bacteriostatic activity. Therefore, the polylysine of the present invention preferably has an average molecular weight of 3000 to 4000Da, and more preferably has an average molecular weight of 3500 Da. The concentration of the polyglutamic acid in the spinning solution prepared in the step S1 is preferably 5-20 g/L, more preferably 15g/L, and the concentration of the polylysine is preferably 4-10 g/L, more preferably 6 g/L.

And (4) after obtaining the spinning solution, carrying out electrostatic spinning to obtain the PGA/PL nano fiber membrane. In the invention, in the electrostatic spinning process, the specification of the used injector is preferably 10ml, and the specification of the needle head is preferably flat head and 7-gauge needle; the electrostatic spinning condition is preferably 12-20 KV, more preferably 18KV, the distance is preferably 7-10 cm, more preferably 9cm, the sample injection rate is preferably 0.3-1.0 ml/h, more preferably 0.5ml/h, and the temperature is preferably 25-35 ℃, more preferably 30 ℃.

And (3) after obtaining the PGA/PL nano fiber membrane, carrying out treatment and activation by a plasma processor to obtain the activated nano fiber membrane. The plasma treatment conditions were: the gas is preferably nitrogen or oxygen, more preferably oxygen, the treatment power is preferably 250-300W, more preferably 280W, the pressure is preferably 50-60 Pa, more preferably 55Pa, and the treatment time is preferably 10-15 min, more preferably 12 min.

And (3) after the activated nano fibrous membrane is obtained, soaking the activated nano fibrous membrane in octacosanol lipase solution for negative pressure flash explosion, and performing centrifugal freeze-drying after esterification grafting reaction to obtain the natural antibacterial water-retaining facial mask. The octacosanol lipase solution can be obtained by dissolving octacosanol and lipase in ethanol, wherein the octacosanol concentration is preferably 4-8 g/L, more preferably 6g/L, and the lipase concentration is preferably 20-50 g/L, more preferably 40 g/L; the activity of the lipase is preferably 30-80U/mg, and more preferably 50U/mg; the vacuum degree of negative pressure flash explosion is preferably 0.100-0.024 mBar, and more preferably 0.050 mBar; the soaking bath ratio of the esterification grafting reaction is preferably 1: 100-300, more preferably 1:200, the reaction temperature is preferably 35-40 ℃, more preferably 37 ℃, and the reaction time is preferably 12-24 hours, more preferably 18 hours. The freeze-drying temperature is preferably-30 to-20 ℃, more preferably-25 ℃, the vacuum degree is preferably 0.100 to 0.024mBar, more preferably 0.050mBar, and the freeze-drying time is preferably 3 to 5 days, more preferably 4 days.

For further understanding of the present invention, the following examples are provided to illustrate the preparation method of a natural antibacterial water-retaining facial mask, and the scope of the present invention is not limited by the following examples.