SU1272067A1 - Method for determining termination of biopreparation freeze drying process - Google Patents

Abstract

The invention relates to biotechnology, in particular, to the control of the removal of moisture from biological preparations weighing 0.05-1 g. The aim of the invention is to increase the accuracy of determining the end of the process of freeze-drying. The biological products drying chamber is evacuated and a high-frequency electric discharge (VER) is excited. The intensity of VER fluorescence varies depending on the content of water vapor released by the biological preparation. At the end of drying, the content of water vapor in the chamber becomes constant. The end of the process is set to achieve a constant intensity of VER glow. 2 tab.

Description

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This invention relates to biotechnology, in particular, to controlling the removal of moisture from 0.05-I g materials in determining the end of the sublimation process.

The aim of the invention is to improve the accuracy of determining the end of the process day.

The accuracy of determining the moment of the end of the cyan process is increased by establishing the specified point and achieving a constant intensity of the high-frequency electric discharge. When freeze-drying biological products in a vacuum. The high-frequency electric discharge is suppressed with water. Its intensity varies with the vapor content. The constant intensity of light indicates that the content of water vapor becomes constant, i.e. about the end of the process of su1nky.

Example. I. In the sublimation chamber of the apparatus, 200 ampoules are loaded containing 0.2 grams of a biological product with sugar-gelatin as a filler. Biopreparation temperature during loading -. After the atom a vacuum is created in the chamber with a residual pressure of 0.01 mm Hg. Art. and start drying. In the volume of the sublimation chamber (in vacuum), a high-frequency electric discharge is excited. With a partial flow of water vapor in the chamber greater than 0.2 m. M. Art. During the drying process, the luminescence of the discharge does not occur. The amount of water vapor released from the preparation decreases, the partial pressure of water vapor in the chamber becomes less than 0.2 mm Hg. Art., there is a glow of high-frequency mexican discharge. Take

Volume of cell loading

as the amount of water vapor in the chamber decreases, the intensity of the glow of the discharge increases.

After 13 m, the intensity of the luminescence reaches a constant level, which indicates that the amount of water vapor R vacuum remains unchanged, i.e. the process is smoked. The chamber is vacuumized, and the dry biological product ampoules are unloaded and packaged.

1Prim, ep 2, Conducted kontrol end of the process of freeze drying of biological material - cattle serum, freeze-dried on a sublimator. The control is carried out in separate cells of the sublimator. Exciting a high-frequency RF discharge, the luminescence is recorded in the cells using a photo sensor followed by recording the luminescence signal on the recorder. The main parameters of the process; loading volume of material is 400 ampoules of 2 ml of serum: in each (amplitudes are placed in 20 cells - in 10 cells of 30 ampoules each and in 10 cells of 10 ampoules each), material freezing temperature is minus 40 ° С, condenser temperature is minus 78 ° С. The pressure in the sublimator chamber is set and maintained at 200 to 20 Pa.

. To obtain comparative data, the end of the process of freeze-drying is monitored in parallel using a tachometer gauge. The end of the drying time is set at the end of the rotational head 1 and the impeller of the sensor.

During the drying process, the residual moisture of the material is controlled.

The data are summarized in table. one.

Table

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24 30 I I As can be seen from the table. 1, the luminescence bandwidth reaches a constant maximum level 5 bh later than the impeller rotation ends. In this case, the achievement of a constant maximum level of luminescence is associated with the end of the sublimation process, since with further sublimation the moisture content of the material does not change. Thus, in comparison with the known method, the proposed method allows more precisely to determine the end of the sublimation process. Example 3. The control of the termination of the process of freeze-drying of human s-stream albumin in a sublimator is carried out. The monitoring is carried out with the help of the low-frequency discharge according to the intensity of the glow of residual gases and vapors in the cells of the sublimator chambers. The main parameters of the sublimation process are: the loading volume of the material is 30 ampoules of I ml in each are placed S two cells x, the freezing temperature of the material is minus 25 ° C, the temperature of the condenser is minus 78 ° C. The pressure in the sublimator chamber is from 5 to 1 Pa. These control using the proposed method in comparison with tachiometric are presented in table. 2, Table 2 Yes. (..1 women of Table 2. From the data presented in examples 2 and 3, it can be seen that the proposed method can be implemented by controlling the amount of water vapor in a vacuum of 200 to 1 Pa. In depth. Thus, the invention allows increasing TOHHocTt: determine the moment of termination of the process of freeze-drying of biological products by controlling the amount of water vapor in a vacuum by determining the end of the process to achieve a constant intensity of the high-frequency electrical discharge, generated in a vacuum. of the invention. The method of determining the end of the process of freeze-drying biological products by controlling the amount of water vapor in a vacuum, characterized in that, in order to improve the accuracy of determining the end of the drying process, a high-frequency electric discharge is excited in vacuum, the number of water ions is controlled by the intensity of the discharge. yes, and the end of the process is set to achieve a constant and 1-intensity of luminescence.

Claims (1)

Claim A method for determining the end of the process of freeze-drying of biological products by controlling the amount of water vapor in a vacuum, characterized in that, in order to improve the accuracy of determining the end of the drying process, a high-frequency electric discharge is excited in a vacuum, the amount of water vapor is controlled by the intensity of the discharge glow, and the moment the process ends set to achieve constant glow intensity. Compose A. Gorbachev