Polycaprolactone solution for injection and sterilization process

Abstract

The embodiment of the invention provides a polycaprolactone solution for injection and a sterilization process, and relates to the technical field of medical instrument sterilization. The sterilization process of the polycaprolactone solution for injection provided by the embodiment of the invention comprises the following steps in sequence: S1, pre-pressurizing a chamber in which the polycaprolactone solution is located to a preset pressure, the preset pressure being greater than a saturated vapor pressure of the polycaprolactone solution at a sterilization temperature, and the sterilization temperature being greater than 110 DEG C; s2, heating the chamber to a sterilization temperature, and carrying out sterilization treatment for a period of time; s3, cooling the chamber to a safe temperature, wherein the safe temperature is 60 DEG C or below; and S4, reducing the pressure of the cavity to the environment pressure. According to the polycaprolactone solution for injection and the sterilization process provided by the embodiment of the invention, the product quality and safety of the polycaprolactone solution can be effectively improved.

Description

Technical Field

[0001] The present application relates to the technical field of medical device sterilization, and in particular to a polycaprolactone solution for injection and a sterilization process. Background Art

[0002] As we age, our skin will naturally sag and wrinkle, especially facial contour aging, which will become increasingly severe, including visible skin wrinkles, deep nasolabial folds, frown lines, perioral wrinkles, etc. As people's living standards improve, they pay more and more attention to the pursuit of external beauty. Injectable polycaprolactone solution fillers have the advantages of good cosmetic effects, less painful treatment process, and simple and easy acceptance, and have been widely recognized in the field of beauty. The main component of polycaprolactone solution is the nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in the aqueous phase, and the micelle particle size in the solution is between 160 and 220 nm.

[0003] Before being used as a filler for injection, polycaprolactone solution needs to be sterilized to form an injectable polycaprolactone solution. Currently, the sterilization process of polycaprolactone solution is mostly filtration sterilization, which has a complicated operation process, poor controllability of product quality, and low safety. Summary of the invention

[0004] The purpose of the embodiments of the present application is to provide a polycaprolactone solution for injection and a sterilization process, which can effectively improve the product quality and safety of the polycaprolactone solution.

[0005] In a first aspect, an embodiment of the present application provides a sterilization process for a polycaprolactone solution for injection, which comprises the following steps performed in sequence:

[0006] S1. Pre-pressurizing the chamber where the polycaprolactone solution is located to a preset pressure, wherein the preset pressure is greater than the saturated vapor pressure of the polycaprolactone solution at a sterilization temperature, and the sterilization temperature is greater than 110° C.;

[0007] S2, raising the temperature of the chamber to the sterilization temperature and performing sterilization treatment for a period of time;

[0008] S3, cooling the chamber to a safe temperature, wherein the safe temperature is below 60°C;

[0009] S4. Depressurize the chamber to ambient pressure.

[0010] In the above technical scheme, a pressurized steam sterilization method is adopted, which sequentially passes through the steps of pre-pressurization, heating, sterilization, cooling, and pressure reduction. Under the pressure, the principle of steam-air mixed sterilization is used to achieve rapid heating of the sterilization solution. When the liquid temperature reaches a predetermined temperature, sterilization is carried out so that the sterilized items are fully heated to achieve the purpose of sterilization. Under the pressure maintenance of the present application, the microspheres in the polycaprolactone solution subjected to the high-temperature sterilization process do not expand, and other physical and chemical indicators do not change; the pressure is kept unchanged during the cooling stage, so as to reduce the situation of microspheres bursting due to pressure release during the pressure release process, and inhibit the generation of small bubbles during the sterilization process.

[0011] In order to ensure that the particle size does not change before and after sterilization and maintain the physical and chemical properties of polycaprolactone before and after sterilization, the present invention adopts a sterilization method with pressurization during the entire sterilization process. The specific effects are: temperature increase, temperature maintenance, and temperature drop in three stages. The preset sterilization pressure is maintained throughout the process, and then steam-air mixed sterilization is adopted to achieve sterilization of pressurized air and steam mixture, thereby ensuring that the physical and chemical properties of polycaprolactone do not change before and after sterilization.

[0012] In a possible implementation, in step S1, the preset pressure is 0.2-0.3 MPa.

[0013] In a possible implementation, in step S2, the sterilization temperature is 110-121° C., and the sterilization time is 15-60 minutes.

[0014] In the above technical solution, a sterilization temperature of 110-121° C. is used to ensure that the physical and chemical properties of polycaprolactone remain unchanged before and after sterilization.

[0015] In a possible implementation, in step S3, the safety temperature is 50-60°C.

[0016] In a possible implementation, the polycaprolactone solution includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in an aqueous phase, the particle size of the nano-microsphere micelles is 160-220 nm, and the content of ethylene glycol caprolactone block copolymers in the polycaprolactone solution is 15-25%.

[0017] In a second aspect, an embodiment of the present application provides a polycaprolactone solution for injection, which is prepared by the sterilization process of the polycaprolactone solution provided in the first aspect.

[0018] In a possible implementation, it comprises nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in an aqueous phase, the particle size of the nano-microsphere micelles is 160-220 nm, and the content of ethylene glycol caprolactone block copolymers in the polycaprolactone solution for injection is 15-25%.

[0019] In the above technical scheme, the solution is a nano-microsphere micelle formed by self-assembly of ethylene glycol caprolactone block copolymer in an aqueous phase, and the micelle particle size in the solution is between 160 and 220 nm; the sterilization solution is an ethylene glycol caprolactone block copolymer, and a pressure sterilization method is adopted, and the properties of the sterilized solution do not change before and after sterilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 This is a diagram of the sterilization process of a polycaprolactone solution at a sterilization temperature of 110° C. in Example 1 of the present application;

[0022] Figure 2 A diagram of the sterilization process of a polycaprolactone solution at a sterilization temperature of 115° C. according to Example 2 of the present application;

[0023] Figure 3 This is a diagram of the sterilization process of a polycaprolactone solution at a sterilization temperature of 121°C in Example 3 of the present application. DETAILED DESCRIPTION

[0024] When studying the sterilization process of polycaprolactone solution, the applicant found that: in conventional steam sterilization, the sterilization pressure increases with the increase of temperature. When it is higher than 100°C, the sterilization pressure will be close to the saturated steam pressure, causing the polycaprolactone solution to produce fine bubbles after boiling and cooling; in the cooling stage, the sterilization pressure will decrease with the decrease of temperature. When the temperature is greater than 100°C, the pressure release will cause the microspheres to burst, affecting the product quality; the polycaprolactone solution will self-assemble into nano-microspheres at room temperature, and the microspheres will expand with the increase of temperature, and the expansion is irreversible, resulting in inconsistent particle size before and after sterilization.

[0025] In order to solve the above problems, a sterilization process that does not change the particle size of microspheres is needed.

[0026] In order to make the purpose, technical scheme and advantages of the embodiments of the present application clearer, the technical scheme in the embodiments of the present application will be described clearly and completely below. Specific conditions are not specified in the embodiments, and the conditions recommended by the manufacturer are carried out according to conventional conditions. The reagents or instruments used without indicating the manufacturer are all conventional products that can be purchased commercially.

[0027] The polycaprolactone solution for injection and the sterilization process of the embodiment of the present application are described in detail below.

[0028] The present application embodiment provides a sterilization process of a polycaprolactone solution for injection, which comprises the following steps performed in sequence:

[0029] S1. Pre-pressurization: pre-pressurize the chamber containing the polycaprolactone solution (hereinafter referred to as "sterilization solution") to a preset pressure, wherein the preset pressure is greater than the saturated vapor pressure of the polycaprolactone solution at the sterilization temperature, and the sterilization temperature is greater than 110°C;

[0030] In a possible implementation, the polycaprolactone solution includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in an aqueous phase, the particle size of the nano-microsphere micelles is 160-220 nm, and the content of the ethylene glycol caprolactone block copolymers in the polycaprolactone solution is 15-25%.

[0031] In a possible implementation, in step S1, the preset pressure is 0.2-0.3 MPa.

[0032] In a possible implementation, the chamber may be a sterilization chamber.

[0033] S2, heating: heating the chamber to the sterilization temperature and performing sterilization for a period of time;

[0034] In a possible implementation, in step S2, the sterilization temperature is 110-121° C., and the sterilization time is 15-60 minutes.

[0035] S3, cooling: cool the chamber to a safe temperature, which is below 60°C;

[0036] In a possible implementation, in step S3, the safety temperature is 50-60°C.

[0037] S4, depressurization: depressurize the chamber to ambient pressure, that is, depressurize it to be consistent with the ambient pressure, and sterilization is completed to obtain the polycaprolactone solution for injection.

[0038] In addition, an embodiment of the present application further provides a polycaprolactone solution for injection, which is prepared by the sterilization process of the polycaprolactone solution of the aforementioned embodiment.

[0039] The physical and chemical properties of the polycaprolactone solution before and after the sterilization process of the embodiment of the present application remain unchanged, and the composition and content do not change, and the pH does not change. In a possible implementation, the polycaprolactone solution for injection includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in an aqueous phase, the particle size of the nano-microsphere micelles is 160 to 220 nm, and the content of ethylene glycol caprolactone block copolymers in the polycaprolactone solution for injection is 15 to 25%.

[0040] The features and performance of the present application are further described in detail below in conjunction with the embodiments.

[0041] Example 1

[0042] This embodiment provides a sterilization process for a polycaprolactone solution for injection, the process is as follows: Figure 1 , which includes the following steps performed in sequence:

[0043] S1. Pre-pressurization: pre-pressurize the sterilization chamber where the polycaprolactone solution is located to a preset pressure, and the preset pressure (relative pressure) is 0.2Mpa;

[0044] In this embodiment, the polycaprolactone solution includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymer in an aqueous phase. The average particle size of the nano-microsphere micelles is 200 nm. The content of ethylene glycol caprolactone block copolymer in the polycaprolactone solution is 20%.

[0045] S2. Heating: Heat the sterilization chamber to the sterilization temperature, the sterilization temperature is 110°C, and the sterilization time is 30 minutes.

[0046] S3, cooling: cool the sterilization chamber to a safe temperature, which is 60°C;

[0047] S4. Depressurization: Reduce the pressure in the sterilization chamber to ambient pressure. Sterilization is completed and the polycaprolactone solution for injection is obtained.

[0048] After testing, the polycaprolactone solution for injection obtained by the above sterilization treatment is sterile, and the physical and chemical properties of the solution before and after the treatment do not change.

[0049] Example 2

[0050] This embodiment provides a sterilization process for a polycaprolactone solution for injection, the process is as follows: Figure 2 , which includes the following steps performed in sequence:

[0051] S1. Pre-pressurization: pre-pressurize the sterilization chamber where the polycaprolactone solution is located to a preset pressure of 0.25 MPa;

[0052] In this embodiment, the polycaprolactone solution includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymer in an aqueous phase. The average particle size of the nano-microsphere micelles is 200 nm. The content of ethylene glycol caprolactone block copolymer in the polycaprolactone solution is 20%.

[0053] S2. Heating: Heat the sterilization chamber to the sterilization temperature, the sterilization temperature is 115°C, and the sterilization time is 30 minutes.

[0054] S3, cooling: cool the sterilization chamber to a safe temperature, which is 60°C;

[0055] S4. Depressurization: Reduce the pressure in the sterilization chamber to ambient pressure. Sterilization is completed and the polycaprolactone solution for injection is obtained.

[0056] After testing, the polycaprolactone solution for injection obtained by the above sterilization treatment is sterile, and the physical and chemical properties of the solution before and after the treatment do not change.

[0057] Example 3

[0058] This embodiment provides a sterilization process for a polycaprolactone solution for injection, the process is as follows: Figure 3 , which includes the following steps performed in sequence:

[0059] S1. Pre-pressurization: pre-pressurize the sterilization chamber where the polycaprolactone solution is located to a preset pressure of 0.28 MPa;

[0060] In this embodiment, the polycaprolactone solution includes nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymer in an aqueous phase, the particle size of the nano-microsphere micelles is 200 nm, and the content of the ethylene glycol caprolactone block copolymer in the polycaprolactone solution is 20%.

[0061] S2. Heating: Heat the sterilization chamber to the sterilization temperature, the sterilization temperature is 121°C, and the sterilization time is 30 minutes.

[0062] S3, cooling: cool the sterilization chamber to a safe temperature, which is 60°C;

[0063] S4. Depressurization: Reduce the pressure in the sterilization chamber to ambient pressure. Sterilization is completed and the polycaprolactone solution for injection is obtained.

[0064] After testing, the polycaprolactone solution for injection obtained by the above sterilization treatment is sterile, and the physical and chemical properties of the solution before and after the treatment do not change.

[0065] In summary, the polycaprolactone solution for injection and the sterilization process of the embodiments of the present application can effectively improve the product quality and safety of the polycaprolactone solution.

[0066] The above description is only an embodiment of the present application and is not intended to limit the scope of protection of the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the scope of protection of the present application.

Claims

1. A sterilization process for a polycaprolactone solution for injection, characterized in that: It includes the following steps performed in sequence: S1. Pre-pressurizing the chamber where the polycaprolactone solution is located to a preset pressure, wherein the preset pressure is greater than the saturated vapor pressure of the polycaprolactone solution at a sterilization temperature, and the sterilization temperature is greater than 110° C.; S2, raising the temperature of the chamber to the sterilization temperature and performing sterilization treatment for a period of time; S3, cooling the chamber to a safe temperature, wherein the safe temperature is below 60°C; S4. Depressurize the chamber to ambient pressure.

2. The sterilization process of the polycaprolactone solution for injection according to claim 1, characterized in that: In step S1, the preset pressure is 0.2-0.3 MPa.

3. The sterilization process of the polycaprolactone solution for injection according to claim 1, characterized in that: In step S2, the sterilization temperature is 110-121°C, and the sterilization time is 15-60 minutes.

4. The sterilization process of the polycaprolactone solution for injection according to claim 1, characterized in that: In step S3, the safety temperature is 50-60°C.

5. The sterilization process of the polycaprolactone solution for injection according to claim 1, characterized in that: The polycaprolactone solution comprises nano-microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in an aqueous phase. The particle size of the nano-microsphere micelles is 160-220 nm. The content of the ethylene glycol caprolactone block copolymers in the polycaprolactone solution is 15-25%.

6. A polycaprolactone solution for injection, characterized in that: The method is prepared by the sterilization process of the polycaprolactone solution as claimed in any one of claims 1 to 5.

7. The polycaprolactone solution for injection according to claim 6, characterized in that: The invention comprises nanometer microsphere micelles formed by self-assembly of ethylene glycol caprolactone block copolymers in water phase, the particle size of the nanometer microsphere micelles is 160-220nm, and the content of the ethylene glycol caprolactone block copolymers in the injection polycaprolactone solution is 15-25%.

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