关键词: 冻干过程, 质谱仪, 生化药品, 硅油

Abstract: In order to find an effective way to test the micro oil leakage and judge the end point of sublimation drying during the biochemical medicine vacuum freeze-drying process, the leakage of silicone oil in the lyophilizer and primary sublimation drying process online were monitored by mass spectrometer. The results showed that the original silicone oil quantity was 1×10^-12 in the freeze-drying chamber tested by mass spectrometer. The mass spectrometer could test the leakage of silicone oil when the concentration was 1×10^-6 in 15 minutes. With the lyophilizer no-load running, N₂、O₂、H₂O、and Ar gas accounted for 82.31%、15.68%、1.37%、0.64% respectively. In the late period of medicine primary sublimation drying process, the four gases accounted for 82.47%、14.9%、1.75%、0.88% respectively. Each gas can be used to judge the end of the medicine sublimation drying progress in a no-load freeze-drying chamber. The present study provides a new method for the judgement of silicone oil leakage and biochemical medicine primary freeze-drying progress.

Key words: freeze-drying process, mass spectrometer, biochemical medicine, silicone oil