Liquid–liquid phase separation and crystallization of aspirin polymorphs from a water–acetonitrile mixed solvent medium through a swift cooling process

Muthusamy, Ramya; Karuppannan, Srinivasan

doi:10.1039/d3ce00611e

CrystEngComm

2023

DOI: 10.1039/d3ce00611e

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Liquid–liquid phase separation and crystallization of aspirin polymorphs from a water–acetonitrile mixed solvent medium through a swift cooling process

Ramya Muthusamy,

Srinivasan Karuppannan

Abstract: Screening of form-I and form-II polymorphs of the pharmaceutical solid aspirin in the vicinity of liquid–liquid phase separation in water–acetonitrile solvent mixtures through a novel swift cooling crystallization process is successfully attained.

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2024

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Cited by 2 publications

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Nucleation Control and Isolation of Polymorphic Forms of Aspirin through an Efficient Template‐Assisted Swift Cooling Process

Muthusamy,

Gnanasekar,

Karuppannan

2024

Cryst. Res. Technol.

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Aspirin, a commonly used pharmaceutical therapeutic pharmacological substance, exhibits cross‐nucleation (intergrowth or overgrowth) of stable polymorphic Form‐I over the preferably required metastable polymorphic Form‐II, which creates a bottleneck issue in the solution crystallization of aspirin in most organic solvents and their mixtures. Controlling the overgrowth phenomenon is a key factor for designing the pharmaceutical drug material aspirin with desired properties. Hence, our present work chose a novel template‐assisted swift cooling crystallization with selected templates like copper‐wire and nylon 6/6 polymer, and also N‐N‐Dimethylformamide (DMF) as a solvent. The pure solution in the absence and the presence of a nylon 6/6 template in all the experimental supersaturation ranges achieves only thermodynamically stable polymorphic Form‐I of aspirin with slightly different morphologies. Contrarily, the presence of a copper‐wire template induces both stable and metastable polymorphs of aspirin depending on the level of supersaturation in the mother solution. The effect of templates on the nucleation kinetics of aspirin polymorphs is estimated using classical nucleation theory, and the determined values exactly match with experimental results. The polymorphic nature of the grown crystals is ascertained by powder X‐ray diffraction (PXRD), single crystal X‐ray diffraction (SCXRD), and differential scanning calorimetry (DSC) analyses.

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Nucleation Control and Isolation of Polymorphic Forms of Aspirin through an Efficient Template‐Assisted Swift Cooling Process

Muthusamy,

Gnanasekar,

Karuppannan

2024

Cryst. Res. Technol.

Self Cite

View full text Add to dashboard Cite

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Revealing the intergrowth phenomenon of aspirin polymorphs through a swift cooling crystallization process

Muthusamy,

Karuppannan

2024

CrystEngComm

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Liquid–liquid phase separation and crystallization of aspirin polymorphs from a water–acetonitrile mixed solvent medium through a swift cooling process

Abstract: Screening of form-I and form-II polymorphs of the pharmaceutical solid aspirin in the vicinity of liquid–liquid phase separation in water–acetonitrile solvent mixtures through a novel swift cooling crystallization process is successfully attained.

Cited by 2 publications

References 51 publications

Nucleation Control and Isolation of Polymorphic Forms of Aspirin through an Efficient Template‐Assisted Swift Cooling Process

Nucleation Control and Isolation of Polymorphic Forms of Aspirin through an Efficient Template‐Assisted Swift Cooling Process

Revealing the intergrowth phenomenon of aspirin polymorphs through a swift cooling crystallization process

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