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Luo Y.-H.,Nanjing Southeast University | Tu Y.-R.,Changzhou Siyao Pharmacy Ltd Company | Ge J.-L.,Changzhou Siyao Pharmacy Ltd Company | Sun B.-W.,Nanjing Southeast University
Separation Science and Technology (Philadelphia) | Year: 2013

In-situ Attenuated total reflectance Fourier transform infrared (ATR-FTIR), focused beam reflectance 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 20-60°C 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 0.7 K/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 fine 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. © 2013 Copyright Taylor and Francis Group, LLC.


Shen Z.,Changzhou Siyao Pharmacy Ltd Company | Mao Q.-X.,Changzhou Siyao Pharmacy Ltd Company | Ge J.-L.,Changzhou Siyao Pharmacy Ltd Company | Tu Y.-R.,Changzhou Siyao Pharmacy Ltd Company | Wang Y.,Changzhou Siyao Pharmacy Ltd Company
Acta Crystallographica Section E: Structure Reports Online | Year: 2014

In the title molecule, C11H10ClFO2, the benzene ring, the F atom and the O atom of the dihydropyran ring are essentially coplanar, with an r.m.s. deviation of 0.007Å. The dihydropyran ring is in a half-chair conformation. In the crystal, molecules are linked by pairs of weak C-H⋯π hydrogen bonds, forming inversion dimers.

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