Evaluation of integrated Raman-DSC technology in early pharmaceutical development: Characterization of polymorphic systems

Huang, Jun; Dali, Manisha M.

doi:10.1016/j.jpba.2013.08.004

Cited by 9 publications

(3 citation statements)

References 7 publications

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“…The search of this relationship is extremely complex because formation of any organic polymorph with molecular packing depends not only on its molecular structure but also on its preparation history ,,,− including a used solvent ,,− or adsorbed gas, crystallization conditions, ,,,, an ability to form solvates, ,, and subsequent thermal treatment of crystallization product. ,,,− Each factor relates to the molecular structure of a target compound in its own way. Consequently, the resulting relationship may be very complicated.…”

Section: Introductionmentioning

confidence: 99%

Smart Polymorphism of Thiacalix[4]arene with Long-Chain Amide Containing Substituents

Gataullina

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Stoikov

et al. 2017

Crystal Growth & Design

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A problem of controlled (smart) formation of polymorphs was solved for a set of tert-butylthiacalix[4]arene derivatives with four N-(2-acetoxyethyl)carbamoylmethoxy substituents at the lower rim with 1,3-alternate, cone, and partial cone conformations. For this, an effective polymorph screening with a reproducible influence of preparation history was achieved using guest vapor inclusion and a standard state of host glass powder. By this procedure with consequent guest release and heating, the ability of the studied calixarenes for polymorphism was investigated and compared as a function of their macrocycle conformation. The data of simultaneous thermogravimetry and differential scanning calorimetry with mass spectrometry of evolved vapors were determined together with the data of powder X-ray diffraction for the initial host samples, intermediate clathrates, and final polymorphs. In addition, single crystal X-ray diffraction data were obtained for four crystalline forms of the studied calixarenes. The results yielded a structure–property relationship, where 1,3-alternate calixarene without an extended H-bonded supramolecular network at least in one crystalline form has a much higher ability for polymorphism than the other two conformations. Thus, 10 polymorphs with essentially different crystal packing were found for this calixarene including a unique tetramorphism with four consecutive melting points of guest-free polymorph and corresponding three crystallization ranges. This ability of 1,3-alternate calixarene is linked with its other smart property: selective crystallization of its compact glass in vapors of binary liquid mixtures, which can be used for visual detection of very small benzene impurities (0.5% (v/v)) in cyclohexane.

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Section: Introductionmentioning

confidence: 99%

Smart Polymorphism of Thiacalix[4]arene with Long-Chain Amide Containing Substituents

Gataullina

Зиганшин

Stoikov

et al. 2017

Crystal Growth & Design

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“…Previous publications on hyphenated analytical techniques involving a DSC or differential thermal analyser (DTA)), and simultaneous optical-based sensing include: (i) Raman spectroscopy [15], [16]; (ii) light intensity-based measurements [17]- [19]; and (iii) DSC/Fourier transform infrared spectroscopy (FTIRS) [20]- [23].…”

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confidence: 99%

Monitoring Cross-Linking, the Evolution of Refractive Index and the Glass Transition Temperature of an Epoxy Resin Using an Optical Fiber Sensor

et al. 2022

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Hyphenated analytical techniques enable the simultaneous measurement of relevant processing and materials parameters under identical environmental conditions. In the current study, a power-compensated differential scanning calorimeter (DSC) was custom-modified to enable the integration of an optical fibre sensor to monitor in situ the progression of the cross-linking reactions by inferring the evolution of the refractive index. A cleaved optical fibre was used and it served as a Fresnel reflection sensor (FRS). The DSC was calibrated with and without the integrated FRS and it was demonstrated that it did not influence the performance of the DSC. The FRS was calibrated using reference refractive index oils within the DSC. An epoxy/amine resin system was cross-linked at 70 o C and the enthalpy of cross-linking and the evolution of the refractive index were monitored simultaneously using the DSC and FRS respectively. After the cross-linking was completed, the DSC was programmed to perform a ramped heating schedule from ambient temperature to 150 o C. The FRS was capable of detecting glass transition temperature (T g ) of the cross-linked resin. An excellent correlation was observed for the T g obtained by the FRS and DSC. The contribution of factors affecting the resolution of the data from the FRS are discussed.

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“…The additional analysis should ideally be noninvasive, so as not to affect the temperature of the sample or to introduce further erroneous heats, and hence spectroscopic probes are often used. For instance, DSC has been hyphenated with Fourier transform-infrared (FT-IR), near-infrared (NIR), and Raman − spectrometers and light microscopy (to make simple optical observations) …”

mentioning

confidence: 99%

Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials

et al. 2016

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We report a powerful new technique: hyphenating synchrotron X-ray powder diffraction (XRD) with differential scanning calorimetry (DSC). This is achieved with a simple modification to a standard laboratory DSC instrument, in contrast to previous reports which have involved extensive and complex modifications to a DSC to mount it in the synchrotron beam. The high-energy X-rays of the synchrotron permit the recording of powder diffraction patterns in as little as 2 s, meaning that thermally induced phase changes can be accurately quantified and additional insight on the nature of phase transitions obtained. Such detailed knowledge cannot be gained from existing laboratory XRD instruments, since much longer collection times are required. We demonstrate the power of our approach with two model systems, glutaric acid and sulfathiazole, both of which show enantiotropic polymorphism. The phase transformations between the low and high temperature polymorphs are revealed to be direct solid-solid processes, and sequential refinement against the diffraction patterns obtained permits phase fractions at each temperature to be calculated and unit cell parameters to be accurately quantified as a function of temperature. The combination of XRD and DSC has further allowed us to identify mixtures of phases which appeared phase-pure by DSC.

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Evaluation of integrated Raman-DSC technology in early pharmaceutical development: Characterization of polymorphic systems

Cited by 9 publications

References 7 publications

Smart Polymorphism of Thiacalix[4]arene with Long-Chain Amide Containing Substituents

Smart Polymorphism of Thiacalix[4]arene with Long-Chain Amide Containing Substituents

Monitoring Cross-Linking, the Evolution of Refractive Index and the Glass Transition Temperature of an Epoxy Resin Using an Optical Fiber Sensor

Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials

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