Rantanen J, Räsänen E, Tenhunen J, Känsäkoski M, Mannermaa J, Yliruusi J
Department of Pharmacy, Pharmaceutical Technology Division, University of Helsinki, Helsinki, Finland.
Eur J Pharm Biopharm. 2000 Sep;50(2):271-6. doi: 10.1016/s0939-6411(00)00096-5.
Factors affecting in-line near infrared (NIR) moisture measurement with a four-wavelength sensor were evaluated (choice of binder used in granulation liquid and the increase in particle size). An entire NIR spectrum is not necessary for the measurement of water, and often the use of only a few NIR wavelengths around the water band enables reliable and high-speed detection of moisture. Glass ballotini and microcrystalline cellulose (MCC) were used as model test materials. The binders studied were poly[1-(2-oxo-1-pyrrolidinyl)ethylene] (PVP) and gelatin. Full off-line NIR spectra of test materials at different levels of binder solutions were measured. The major spectral features for both the binders were bands around 1700 nm (first overtones CH related stretches) and 2200 nm (combination bands). Gelatin also had an NH band around 1500 nm (first overtones of NH stretches) and combination bands at about 2050 nm. Particle size effects were observed as an increase in spectra baseline. All these factors should be considered when choosing NIR wavelengths used for detection of water with a fixed wavelength set-up. A robust calibration model enables the development of in-process control of wet granulation processes.
评估了影响使用四波长传感器进行在线近红外(NIR)水分测量的因素(制粒液中所用粘合剂的选择以及粒径的增加)。测量水分并不需要完整的近红外光谱,通常仅使用水吸收带周围的少数几个近红外波长就能实现可靠且高速的水分检测。玻璃珠和微晶纤维素(MCC)用作模型测试材料。所研究的粘合剂为聚[1-(2-氧代-1-吡咯烷基)乙烯](PVP)和明胶。测量了不同粘合剂溶液水平下测试材料的完整离线近红外光谱。两种粘合剂的主要光谱特征是在1700 nm左右的谱带(与CH相关拉伸的一级倍频)和2200 nm处的谱带(组合带)。明胶在1500 nm左右还有一个NH谱带(NH拉伸的一级倍频)以及在约2050 nm处的组合带。观察到粒径效应表现为光谱基线升高。在选择用于固定波长设置的水检测的近红外波长时,应考虑所有这些因素。一个稳健的校准模型有助于开发湿法制粒过程的过程控制。