KR-102962339-B1 - Freeze-dried

KR102962339B1KR 102962339 B1KR102962339 B1KR 102962339B1KR-102962339-B1

Abstract

A freeze-dried product that is continuously manufactured by moving under mechanical force in a freeze-drying device (1), wherein the freeze-drying device (1) comprises a freezing section (2) that produces a frozen product by spraying a raw material liquid and a drying section (3) that dries the frozen product, wherein the drying section (3) has a tubular shape and is provided with a vacuum tubular body (3) having a spiral-shaped wall or groove section formed continuously in the longitudinal direction on the inner wall, and as heat is conducted to the inner wall and the wall section or groove section of the tubular body (3) and the tubular body (3) rotates, the freeze-dried product is conveyed in the longitudinal direction of the tubular body and sublimated or dried, and the flow start time is less than 44 degrees or the angle of repose is greater than the flow start time and also less than 55 degrees, and the residual amount for an input amount of 10g is 3g or less when the longitudinal length of the tubular body (3) is 30cm.

Inventors

모리모토슈지
타케하라 마코토
코바야시 마사토

Assignees

카부시키가이샤 엠아이아이

Dates

Publication Date: 20260507
Application Date: 20220802
Priority Date: 20210803

Claims (6)

As a freeze-dried material that is dried while moving under mechanical force in a freeze-drying device, The above freeze-drying device comprises a freezing section that sprays a raw material liquid to produce a frozen product, and a drying section that dries the frozen product while moving it. The above freezing unit generates a frozen product by releasing the raw material liquid from a nozzle into a vacuum or into a cold air environment, and The above drying unit is configured to have a vacuum cylindrical body having a cylindrical shape extending in a straight line in the horizontal direction and having a spiral-shaped wall or groove formed continuously along the length direction on the inner wall, and is divided into at least three sections in the length direction to surround it, and temperature-controlled air or liquid is supplied to each surrounding area of the divided cylindrical body, so that heat is conducted to the inner wall of the cylindrical body and the wall or groove, causing the cylindrical body to rotate, thereby transporting the frozen material or freeze-dried material along the length direction of the cylindrical body by sliding between the wall or groove, while simultaneously contacting the inner wall of the cylindrical body and the wall or groove to conduct heat and sublimate or dry, and is configured to discharge the moisture evaporated according to sublimation or drying to the outside. A freeze-dried product characterized by the flow initiation time being less than 44 degrees, or the angle of repose being greater than the flow initiation time and also less than 55 degrees, and the residual amount being 3g or less for an input amount of 10g when the longitudinal length of the tubular body is 30cm.
In paragraph 1, A freeze-dried product characterized by a flow onset time of 38.0 degrees or less, an angle of repose greater than the flow onset time and 40.5 degrees or less, and a residual amount of 0.4 g or less.
In paragraph 1 or 2, A freeze-dried product characterized by the above-mentioned raw material liquid containing at least one of a sugar alcohol and a disaccharide as an excipient.
In paragraph 3, A freeze-dried product in which the sugar alcohol is erythritol or mannitol and the disaccharide is sucrose or trehalose.
In paragraph 1 or 2, A freeze-dried product characterized in that the above freeze-dried product is an injectable or solid pharmaceutical product.
In paragraph 5, A freeze-dried product characterized in that the above-mentioned injectable or pharmaceutical product is any one of a vaccine preparation including a COVID-19 vaccine, a smallpox vaccine or an influenza vaccine preparation, a biopharmaceutical including a nucleic acid or antibody, an antiviral agent, and liver cells.

Description

Freeze-dried The present invention relates to a freeze-dried product according to a vacuum freeze-drying apparatus and a vacuum freeze-drying method. Conventionally, a freeze-drying apparatus and a freeze-drying method have been proposed for discharging a liquid from a nozzle and freeze-drying the frozen particles that freeze-solidify the liquid (Patent Document 1). In addition, a freeze-drying device has been proposed in which a tray containing the raw material liquid is mounted on a shelf to freeze-dry (Patent Document 2). In addition, in a vacuum freeze-drying apparatus, it is proposed to release frozen particles into a vacuum to sublimate and dry them (Patent Document 3). FIG. 1 is a cross-sectional front view of a vacuum freeze-drying apparatus used in the implementation of the present invention. Figure 2 is a front view illustrating the drying section of the vacuum freeze-drying device of Figure 1. Figure 3 is a plan view illustrating the drying section of the vacuum freeze-drying device of Figure 1. FIG. 4 is a perspective view (a), a front view (b), a cross-sectional view (c), a longitudinal front view (d), and a partial enlarged view (e) of (d) showing one of a plurality of tubular parts constituting a tubular body provided in a drying part. FIG. 5 is an explanatory diagram of the angle of repose measurement method according to the present invention. FIG. 6 is a perspective view of a measuring device for the flow start time according to the present invention. Figure 7 is a front view illustrating the measurement state of the flow start time. Figure 8 shows the measurement data of the angle of repose and flow initiation time of freeze-dried experimental samples No. 1 to 8, and reference examples 1 to 2. Figure 9 shows the measurement data of the angle of repose and flow initiation time of freeze-dried experimental samples No. 9 to 17 and Reference Example 3. Figure 10 is analysis data of fluidity based on measurement data of the angle of repose and the flow initiation time. Preferred embodiments of the present invention are described below with reference to the drawings. For a vacuum freeze-drying apparatus used for manufacturing freeze-dried products according to the present invention, please refer to the above Patent Document 4 (Japanese Patent Publication No. 6777350). Meanwhile, the freeze-dried products include injectable or solid pharmaceutical products, such as vaccine preparations including, for example, COVID-19 vaccine, smallpox vaccine, or influenza vaccine, biopharmaceuticals including nucleic acids or antibodies, antiviral agents, and liver cells. FIG. 1 is a cross-sectional front view of a vacuum freeze-drying apparatus used in the embodiment of the present invention, FIG. 2 is a front view showing the drying section of the vacuum freeze-drying apparatus of FIG. 1, and FIG. 3 is a plan view showing the drying section of the vacuum freeze-drying apparatus of FIG. 1. The vacuum freeze-drying device (1) is equipped with a freezing section (2), a drying section (3), a connecting section (4), and a collecting section (5). The freezing section (2) discharges raw material liquid into a vacuum container through a nozzle (21), and the discharged raw material liquid is frozen in the vacuum to produce a frozen product. The discharged or dropped raw material liquid self-freezes as water evaporates during the fall, thereby losing latent heat of evaporation, and becomes a frozen product in the form of fine frozen particles through sublimation, which falls toward a collecting section (22) having a tapered shape that narrows at the bottom and is collected by the collecting section (22). The connecting section (4) connects the freezing section (2) and the drying section (3) and is intended to transfer the frozen product generated in the freezing section (2) to the drying section (3). The drying section (3) sublimates and dries the frozen product. The collecting section (5) collects the dried product discharged from the outlet of the drying section (3). In a vacuum freeze-drying device, it is also possible to produce frozen products by releasing the liquid raw material from a nozzle into a cold air environment and freezing it. When using the cold air freezing method, the raw material is exposed to cold air from the side during loading. The drying section (3) is equipped with a tubular body (31) for transporting frozen material or freeze-dried material. The tubular body (31) is a tubular shape extending in a straight line in the horizontal direction, with both ends open, and is equipped with an inlet section (31b) into which frozen material transported by the connecting section (4) enters, and an outlet section (31c) which serves as the outlet for sublimated and dried material. The inlet section (31b) has a receiving port (302) for receiving frozen material. Inside the tubular body (31), a spiral-shaped transport means (31a) is installed near the inner wall of the tubular body (31) and is continuously fo