Freeze-drying method of collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder
阅读说明：本技术 含胶原蛋白的美白抗皱护肤冻干粉的冻干方法 (Freeze-drying method of collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder ) 是由 陶海 赵健烽 王磊 缪溢 于 2020-07-03 设计创作，主要内容包括：本发明公开了一种含胶原蛋白的美白抗皱护肤冻干粉的冻干方法。本发明通过调控冷冻干燥过程中预冻、一次升华和解析干燥阶段的升温速度、温度、真空度和保持时间,控制最终产品的水分含量为5～8％,得到的冻干粉具有性状稳定、外观美观、且胶原蛋白活性保持在较高水平等优点。(The invention discloses a freeze-drying method of collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder. According to the invention, the water content of the final product is controlled to be 5-8% by regulating and controlling the heating speed, temperature, vacuum degree and holding time of the pre-freezing, primary sublimation and analytic drying stages in the freeze drying process, and the obtained freeze-dried powder has the advantages of stable properties, attractive appearance, high collagen activity and the like.)
1. The freeze-drying method of the collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder is characterized by comprising the following steps:
placing the whitening anti-wrinkle skin care stock solution containing the collagen into a freeze-drying device, and carrying out the following procedures:
step 1, pre-freezing:
the temperature of the heat conducting oil reaches-5 to-10 ℃ in 2 to 10 minutes at the first stage, and is kept for 0.5 to 1 hour;
the temperature of the heat conducting oil in the second stage reaches-35 to-45 ℃ in 20 to 40 minutes, and is kept for 2 to 3 hours;
step 2, primary sublimation:
the temperature of the heat conducting oil in the first stage reaches-30 to-20 ℃ in 0.5 to 1 hour, the vacuum degree is kept at the limit vacuum, and the vacuum degree is kept for 5 to 10 hours;
The temperature of the second stage heat conducting oil reaches-20 to-10 ℃ within 0.5 to 1 hour, the vacuum degree is 20 to 30 Pa, and the second stage heat conducting oil is kept for 5 to 10 hours;
in the third stage, the temperature of the heat conducting oil reaches-10 ℃ to 0 ℃ in 0.5 to 1 hour, the vacuum degree is 30 Pa to 40 Pa, and the heat conducting oil is kept for 5 hours to 10 hours;
the temperature of the heat conducting oil at the fourth stage reaches 0-5 ℃ in 0.5-1 hour, the vacuum degree is 40-50 Pa, and the heat conducting oil is kept for 2-3 hours;
and 3, resolving and drying:
the temperature of the heat conducting oil in the first stage reaches 5-20 ℃ in 0.5-1 hour, the vacuum degree is 40-50 Pa, and the heat conducting oil is kept for 3-4 hours;
the temperature of the second stage heat conducting oil reaches 20-35 ℃ in 0.5-1 hour, the vacuum degree is 30-40 Pa, and the second stage heat conducting oil is kept for 2-3 hours;
step 4, pressure rise test: setting pressure rise to be 3 Pa/min, wherein the pressure rise is qualified, and the freeze-drying is finished, wherein the water content of the freeze-dried powder is 5-8%.
2. The freeze-drying method according to claim 1, wherein the collagen-containing skin whitening and anti-wrinkle skin care stock solution comprises the following components in percentage by mass:
。
Technical Field
The invention belongs to the technical field of cosmetics, and relates to a freeze-drying method of collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder.
Background
The vacuum freeze drying technology is to sublimate water from ice directly at relatively low temperature (-10 deg.c to-50 deg.c) to dry without surface tension and deformation, and to dewater material. Because the vacuum freeze-drying technology is carried out in a low-temperature and low-pressure environment, most biological reactions are stopped, liquid water does not exist in the treatment process, and the water is directly sublimated in a solid state, so that the original structure and shape of the material are protected to the greatest extent, a high-quality dried product with both appearance and internal quality is finally obtained, and the activity of active substances (such as collagen) in the freeze-dried product can be fully reserved due to the biological reaction stop. The vacuum freeze drying technology is applied to the cosmetic industry to obtain high-quality skin care products.
Because the collagen has bioactivity, the bioactivity needs to be maintained to the maximum extent, and the freeze-dried product has compact internal crystallization, beautiful appearance and no obvious phenomena of collapse, atrophy, bubble formation and the like, the freeze-drying process has extremely strict requirements. In the existing freeze-drying process of products containing collagen, the drying and sublimation temperature is controlled to be higher (higher than 40 ℃), collagen is easy to inactivate, meanwhile, the water control is not strict, and the conditions of product collapse, atrophy or large crystal particles and loose product appearance often occur, so that the products are not beautiful, and the bioactivity does not reach the standard. Therefore, the development of a freeze-drying process is urgently needed, and the quality requirements of the collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder can be met.
Disclosure of Invention
The invention aims to provide a freeze-drying method of collagen-containing skin-whitening anti-wrinkle skin-care freeze-dried powder. According to the method, the pre-freezing temperature, the sublimation temperature and the vacuum degree during drying are regulated, the moisture of the freeze-dried powder is controlled to be 5-8%, the obtained product is stable in property and attractive in appearance, and the activity of the collagen is kept at a high level.
The technical scheme for realizing the purpose of the invention is as follows:
the freeze-drying method of the collagen-containing skin-whitening, anti-wrinkle and skin-care freeze-dried powder comprises the following steps:
Placing the whitening anti-wrinkle skin care stock solution containing the collagen into a freeze-drying device, and carrying out the following procedures:
step 1, pre-freezing:
the temperature of the heat conducting oil reaches-5 to-10 ℃ in 2 to 10 minutes at the first stage, and is kept for 0.5 to 1 hour;
the temperature of the heat conducting oil in the second stage reaches-35 to-45 ℃ in 20 to 40 minutes, and is kept for 2 to 3 hours;
step 2, primary sublimation:
the temperature of the heat conducting oil in the first stage reaches-30 to-20 ℃ in 0.5 to 1 hour, the vacuum degree is kept at the limit vacuum, and the vacuum degree is kept for 5 to 10 hours;
the temperature of the second stage heat conducting oil reaches-20 to-10 ℃ within 0.5 to 1 hour, the vacuum degree is 20 to 30 Pa, and the second stage heat conducting oil is kept for 5 to 10 hours;
in the third stage, the temperature of the heat conducting oil reaches-10 ℃ to 0 ℃ in 0.5 to 1 hour, the vacuum degree is 30 Pa to 40 Pa, and the heat conducting oil is kept for 5 hours to 10 hours;
the temperature of the heat conducting oil at the fourth stage reaches 0-5 ℃ in 0.5-1 hour, the vacuum degree is 40-50 Pa, and the heat conducting oil is kept for 2-3 hours;
and 3, resolving and drying:
the temperature of the heat conducting oil in the first stage reaches 5-20 ℃ in 0.5-1 hour, the vacuum degree is 40-50 Pa, and the heat conducting oil is kept for 3-4 hours;
the temperature of the second stage heat conducting oil reaches 20-35 ℃ in 0.5-1 hour, the vacuum degree is 30-40 Pa, and the second stage heat conducting oil is kept for 2-3 hours;
step 4, pressure rise test: setting pressure rise to be 3 Pa/min, wherein the pressure rise is qualified, and the freeze-drying is finished, wherein the water content of the freeze-dried powder is 5-8%.
The whitening anti-wrinkle skin care stock solution containing collagen comprises the following components in percentage by mass:
collagen protein
0.5％
Hyaluronic acid sodium salt
2.0％
Mannitol
0.3％
Pullulan polysaccharide
0.3％
Trehalose
0.6％
Hydroxypropyl cyclodextrins
0.5％
Nicotinamide
0.15％
Water (W)
Balance of
The inventor finds that in the pre-freezing process, if the vacuum pumping treatment is directly carried out, gas dissolved in water escapes due to reduction of external pressure to form bubbles, so that cavities appear in the interior and on the surface of the raw material, and the appearance of the product is affected. Therefore, the invention keeps normal pressure operation during pre-freezing, and performs stage pre-freezing at different temperatures and time, and the finally obtained product has compact internal crystal and beautiful appearance.
Compared with the prior art, the invention has the following remarkable effects:
vacuum drying is generally divided into 2 stages of sublimation drying (one time sublimation) and resolution drying. Sublimation drying is mainly directed at free water in the material; the desorption drying is mainly to remove the adsorbed water strongly bonded to the solid. The vacuum degree and temperature during the drying process directly influence the drying process and the final moisture of the product, and the moisture in turn influences the biological activity of the collagen. The invention selects reasonable pre-freezing and sublimation temperatures and vacuum degrees, optimizes the freeze-drying curve, improves the product properties, enhances the product stability, keeps the biological activity of the collagen at a higher level, and ensures that the quality standard of the freeze-dried product meets various indexes specified by the national drug standard.
Drawings
FIG. 1 is a diagram of a lyophilized powder prepared in example 1;
FIG. 2 is a diagram of a lyophilized powder prepared in comparative example 1;
fig. 3 is a diagram of a lyophilized powder entity prepared in example 2 and comparative example 2.
Detailed Description
The invention is further illustrated by the following examples and figures.
In the following examples and comparative examples, the adopted collagen-containing whitening anti-wrinkle skin care stock solution consists of the following components in percentage by mass:
collagen protein
0.5％
Hyaluronic acid sodium salt
2.0％
Mannitol
0.3％
Pullulan polysaccharide
0.3％
Trehalose
0.6％
Hydroxypropyl cyclodextrins
0.5％
Nicotinamide
0.15％
Water (W)
Balance of