US 12,313,613 B2
Method of testing crystallinity in amorphous pharmaceutical compositions
Andreas Berghaus, Berlin (DE); and Angela Spangenberg, Georgetown, TX (US)
Assigned to COLVISTEC AG, Berlin (DE)
Appl. No. 17/426,451
Filed by ColVisTec AG, Berlin (DE)
PCT Filed Jan. 29, 2020, PCT No. PCT/EP2020/052175
§ 371(c)(1), (2) Date Jul. 28, 2021,
PCT Pub. No. WO2020/160980, PCT Pub. Date Aug. 13, 2020.
Claims priority of application No. 1901579 (GB), filed on Feb. 5, 2019.
Prior Publication US 2022/0120726 A1, Apr. 21, 2022
Int. Cl. G01N 33/15 (2006.01); G01N 21/31 (2006.01); G01N 21/3563 (2014.01); G01N 21/47 (2006.01); G01N 21/55 (2014.01); G01N 21/59 (2006.01)
CPC G01N 33/15 (2013.01) [G01N 21/4738 (2013.01); G01N 21/55 (2013.01); G01N 21/59 (2013.01); G01N 2021/3155 (2013.01); G01N 2021/3572 (2013.01); G01N 2021/558 (2013.01); G01N 2201/129 (2013.01)] 16 Claims
OG exemplary drawing
 
1. A method of generating a predictive model for determining an amount of crystallinity of an active pharmaceutical ingredient (API) in an amorphous solid dispersion or solid-state solution, the method comprising:
(i) subjecting a plurality of reference samples of dispersions or solutions spanning a range of API crystallinity to UV/vis spectroscopy using a UV/vis spectrometer;
(ii) measuring a reflectance and/or transmission spectrum of each reference sample using the UV/vis spectrometer wherein the reflectance and/or transmission is produced from subjecting the plurality of reference samples to UV/vis spectroscopy according to step (i); and
(iii) generating a predictive crystallinity model using principle component analysis (PCA) of the spectra from step (ii).