Pharmaceutical cocrystals, salts and polymorphs: Advanced characterization techniques

Pindelska, Edyta; Sokal, Agnieszka; Kołodziejski, Wacław

doi:10.1016/j.addr.2017.09.014

Cited by 118 publications

(89 citation statements)

References 331 publications

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“…By using PXRD, crystalline phases of material can be distinguished by its unique diffraction pattern which is a fingerprint of crystal structures. These phases may represent different materials or different crystalline form of related materials [22]. The overlay of PXRD patterns of atorvastatin calcium, succinic acid, and atorvastatin calcium-succinic acid cocrystal is shown in Fig.…”

Section: ■ Results and Discussion Powder X-ray Diffractionmentioning

confidence: 99%

“…DSC is the most commonly used thermal analysis method, especially since its implementation is relatively quick and easy. This technique is a powerful tool for the detection of new crystalline formation of materials and also for stability studies of crystalline materials as a function of temperature [22]. The cocrystal has a different melting point from initial materials which was suspected due to the influence of differences in the crystal lattice and packing arrangement [18,26].…”

Section: Differential Scanning Calorimetrymentioning

confidence: 99%

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Preparation and Characterization of a Novel Cocrystal of Atorvastatin Calcium with Succinic Acid Coformer

et al. 2019

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Preparation and characterization of a novel cocrystal of atorvastatin calcium with succinic acid coformer were successfully performed. This research aims to modify the crystalline form of atorvastatin calcium through cocrystallization with succinic acid coformer. The cocrystal was prepared by a solvent evaporation method and characterized by Powder X-Ray Diffraction (PXRD), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). The atorvastatin calcium-succinic acid cocrystal has new crystalline peaks at 2θ of 12.9, 18.2 and 26.7° indicating the formation of a new crystalline phase. The cocrystal showed the melting point at 205.7 °C with an enthalpy of fusion 30.2 J/g which is different from the initial components. The FTIR spectra of cocrystal showed the shifting of absorption peaks of groups of initial components indicating of formation of atorvastatin calcium-succinic acid cocrystal through acid–amide intermolecular hydrogen bond interactions. The solubility and dissolution test showed that the cocrystal has solubility and dissolution rate significantly higher than the solubility and dissolution rate of pure atorvastatin calcium.

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Section: ■ Results and Discussion Powder X-ray Diffractionmentioning

confidence: 99%

Section: Differential Scanning Calorimetrymentioning

confidence: 99%

Preparation and Characterization of a Novel Cocrystal of Atorvastatin Calcium with Succinic Acid Coformer

et al. 2019

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“…Solid‐state NMR spectroscopy is now an established method for the characterization of pure, multicomponent (i.e., cocrystals and ASDs), and formulated APIs. Many excellent reviews and books describe the established applications of solid‐state NMR spectroscopy to APIs . One key application of solid‐state NMR spectroscopy to APIs is the identification and differentiation of polymorphs.…”

Section: Introductionmentioning

confidence: 99%

DNP‐enhanced solid‐state NMR spectroscopy of active pharmaceutical ingredients

Zhao

Pinon

Emsley

et al. 2018

Magnetic Reson in Chemistry

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Solid-state NMR spectroscopy has become a valuable tool for the characterization of both pure and formulated active pharmaceutical ingredients (APIs). However, NMR generally suffers from poor sensitivity that often restricts NMR experiments to nuclei with favorable properties, concentrated samples, and acquisition of one-dimensional (1D) NMR spectra. Here, we review how dynamic nuclear polarization (DNP) can be applied to routinely enhance the sensitivity of solid-state NMR experiments by one to two orders of magnitude for both pure and formulated APIs. Sample preparation protocols for relayed DNP experiments and experiments on directly doped APIs are detailed. Numerical spin diffusion models illustrate the dependence of relayed DNP enhancements on the relaxation properties and particle size of the solids and can be used for particle size determination when the other factors are known. We then describe the advanced solid-state NMR experiments that have been enabled by DNP and how they provide unique insight into the molecular and macroscopic structure of APIs. For example, with large sensitivity gains provided by DNP, natural isotopic abundance, C- C double-quantum single-quantum homonuclear correlation NMR spectra of pure APIs can be routinely acquired. DNP also enables solid-state NMR experiments with unreceptive quadrupolar nuclei such as H, N, and Cl that are commonly found in APIs. Applications of DNP-enhanced solid-state NMR spectroscopy for the molecular level characterization of low API load formulations such as commercial tablets and amorphous solid dispersions are described. Future perspectives for DNP-enhanced solid-state NMR experiments on APIs are briefly discussed.

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“…Therefore, bioavailability is a combination of solubility, dissolution and permeability profile of an API. [28] In order to elucidate the pharmacokinetic characteristicsthe prepared fisetin cocrystals were administered in rats. The results showed that all the cocrystals had higher Cmax and AUC, and a shorter Tmax as compared to that of pure fisetin ( figure 11).…”

Section: Bioavailabilitymentioning

confidence: 99%

Crystal engineering of fisetin: a step towards improved biopharmaceutical parameters

Chadha¹,

Bhalla²,

Chadha³

et al. 2019

SDRP-JFST

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Pharmaceutical cocrystals, salts and polymorphs: Advanced characterization techniques

Cited by 118 publications

References 331 publications

Preparation and Characterization of a Novel Cocrystal of Atorvastatin Calcium with Succinic Acid Coformer

Preparation and Characterization of a Novel Cocrystal of Atorvastatin Calcium with Succinic Acid Coformer

DNP‐enhanced solid‐state NMR spectroscopy of active pharmaceutical ingredients

Crystal engineering of fisetin: a step towards improved biopharmaceutical parameters

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