Abstract
The thermal and structural evolutions associated to active pharmaceutical ingredient (API) purity are monitored using a laboratory instrument (S3-MicroCaliX) allowing simultaneous time-resolved X-ray scattering at both wide and small angles (SWAXS) as a function of temperature. This is performed simultaneously with differential scanning calorimetric (DSC) that is carried out in the same apparatus at scanning rate of 2 K/min on the same sample in the range from 20° to 200°C. We have studied simultaneous thermal and structural properties of pentoxifylline, as an active pharmaceutical ingredient (API), for its purity quality control. We have found a satisfying API purity, due to obtained melting temperature and enthalpy values, which are in a well agreement with literature. We have also found that the combination of these techniques allows the thermal monitoring of scanning rates of 2 K/min, continuously without the need for static thermal equilibration, particularly for X-ray spectra. Hence, DSC and SWAXS allowing better identification of the structural thermal events recorded by following of the phase transitions simultaneously. This interpretation is much better possible when X-ray scattering at small and wide angles is coupled with DSC from the same sample. Hence, as a laboratory tool, the method presents a reproducible thermal and crystallographic API purity quality control of non-complex samples, as crucial information for pharmaceutical technology.
Highlights
Analytical quality control of active pharmaceutical ingredient (API) is a key to follow quality of pharmaceutical processes and products
We report about SWAXS/differential scanning calorimetric (DSC) simultaneous laboratory technique application for an API quality control, probing the API structural and the melting behavior whose combination provides information about material quality and purity
DSC-signals have been recorded simultaneously with scattering patterns presented as a three-dimensional plot of l (scattered intensity expressed in arbitrary units (a.u.)) versus q and versus T by small angle X-ray scattering (SAXS) in Fig 2a and versus 2 Ѳ and versus T by wide angle X-ray scattering (WAXS) in Fig 3a and S2 Fig, respectively
Summary
Analytical quality control of APIs is a key to follow quality of pharmaceutical processes and products. A coupling with an X-ray scattering method allows resolving this issue Both methods, SWAXS and DSC, provide relevant information for raw material and product analysis, the combination of both methods into one instrument, and the simultaneous analysis of a single sample provide more analytical advantages. The possibility to resolve ambiguities in the understanding of phase-transition mechanisms by allowing accurate determination of the order of the events occurrence by the different techniques is even more important Combining these two methods, SWAXS and DSC, crystallinity, phase and polymorph identification. The repeatability and time flexible experimental planning are not that much possible at a synchrotron beam-line due to access limitations This was the motivation for such laboratory instrument and we present the first commercially available laboratory SWAXS/DSC system called S3-MICROcaliX (Hecus X-Ray Systems) and its application in the API solid-state purity quality control. First results of this innovative system applied in pharmaceutical quality control applications for non-complex samples are presented in the following
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