Monitoring the Crystallization Process of Methylprednisolone Hemisuccinate (MPHS) from Ethanol Solution by Combined ATR-FTIR- FBRM- PVM
writer：Yang-Hui Luo, Yong-Rui Tu, Ji-Long Ge, Bai-Wang Sun*
keywords：ATR-FTIR- FBRM- PVM, crystallization, nucleation, supersaturation
source：期刊
Issue time：2013年
In-situ Attenuated total re?ectance Fourier transform infrared (ATR-FTIR), focused beam re?ectance measurement (FBRM) and particle video microscope (PVM) have been used simultaneously in this work to monitor the concentration, supersaturation, chord length distribution, and crystal habit, respectively, during a cooling crystallization process of Methyprednisolone Hemisuccinate (MPHS) from ethanol system. We developed a new calibration method based on peak ratios for the assessment of the concentration, solubility, and supersaturation in the 20–60C temperature range. The
crystallizations were conducted at two concentrations (7.5 and 9.5%w/w) with three different cooling rates (0.3, 0.5, and 0.7K/min). The lower concentration was chosen within the constructed calibration range while the higher one was outside the calibration range and it was used to examine the extrapolating and predicting ability of the constructed calibration curves. The metastable zone widths (MSZW), supersaturation at nucleation, and the number of ?ne particle chord length of MPHS were all increased with the cooling rate, while the number of the larger chord length decreased with the increasing of the cooling rate.