Polyethylene Glycol-Assisted Melt Crystallization of Two New Piroxicam Polymorphs Revealed by 3D Electron Diffraction

Jiaoyan Xu; Changlin Yao; Shufang Zhang; Xiaodong Zou; Yue Gui; Lei Wang; Hongyi Xu

doi:10.1021/acs.cgd.4c00951

Polyethylene Glycol-Assisted Melt Crystallization of Two New Piroxicam Polymorphs Revealed by 3D Electron Diffraction

Jiaoyan Xu, Changlin Yao^*, Shufang Zhang, Xiaodong Zou, Yue Gui, Lei Wang^*, Hongyi Xu^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

2 Citations (Scopus)

Abstract

Two new polymorphs (forms VIII and IX) of piroxicam were discovered through poly(ethylene glycol) (PEG)-assisted melt crystallization, and their structures were revealed by 3D electron diffraction (3D ED). This discovery provides insight into the potential of PEG in pharmaceutical polymorph discovery and verifies the significance of 3D ED as an essential technique for structural determination of pharmaceuticals. Furthermore, the direct contribution of intermolecular hydrogen bonding to melting points was discussed based on the structural divergency between the newly solved form VIII and the previously reported form IV. Combining PEG-assisted melt crystallization and 3D ED not only accelerated the discovery of new polymorphs but also provided unique opportunities for understanding structure-property relationships in pharmaceutical crystals.

Original language	English
Pages (from-to)	7298-7305
Number of pages	8
Journal	Crystal Growth and Design
Volume	24
Issue number	17
Early online date	26 Aug 2024
DOIs	https://doi.org/10.1021/acs.cgd.4c00951
Publication status	Published - 4 Sept 2024
Externally published	Yes

Access to Document

10.1021/acs.cgd.4c00951

Cite this

@article{d54a3a8d4c4f4907b9cc0de15deb901b,

title = "Polyethylene Glycol-Assisted Melt Crystallization of Two New Piroxicam Polymorphs Revealed by 3D Electron Diffraction",

abstract = "Two new polymorphs (forms VIII and IX) of piroxicam were discovered through poly(ethylene glycol) (PEG)-assisted melt crystallization, and their structures were revealed by 3D electron diffraction (3D ED). This discovery provides insight into the potential of PEG in pharmaceutical polymorph discovery and verifies the significance of 3D ED as an essential technique for structural determination of pharmaceuticals. Furthermore, the direct contribution of intermolecular hydrogen bonding to melting points was discussed based on the structural divergency between the newly solved form VIII and the previously reported form IV. Combining PEG-assisted melt crystallization and 3D ED not only accelerated the discovery of new polymorphs but also provided unique opportunities for understanding structure-property relationships in pharmaceutical crystals.",

author = "Jiaoyan Xu and Changlin Yao and Shufang Zhang and Xiaodong Zou and Yue Gui and Lei Wang and Hongyi Xu",

note = " {\textcopyright} 2024 The Author(s)",

year = "2024",

month = sep,

day = "4",

doi = "10.1021/acs.cgd.4c00951",

language = "English",

volume = "24",

pages = "7298--7305",

journal = "Crystal Growth and Design",

issn = "1528-7483",

publisher = "American Chemical Society",

number = "17",

}

TY - JOUR

T1 - Polyethylene Glycol-Assisted Melt Crystallization of Two New Piroxicam Polymorphs Revealed by 3D Electron Diffraction

AU - Xu, Jiaoyan

AU - Yao, Changlin

AU - Zhang, Shufang

AU - Zou, Xiaodong

AU - Gui, Yue

AU - Wang, Lei

AU - Xu, Hongyi

PY - 2024/9/4

Y1 - 2024/9/4

N2 - Two new polymorphs (forms VIII and IX) of piroxicam were discovered through poly(ethylene glycol) (PEG)-assisted melt crystallization, and their structures were revealed by 3D electron diffraction (3D ED). This discovery provides insight into the potential of PEG in pharmaceutical polymorph discovery and verifies the significance of 3D ED as an essential technique for structural determination of pharmaceuticals. Furthermore, the direct contribution of intermolecular hydrogen bonding to melting points was discussed based on the structural divergency between the newly solved form VIII and the previously reported form IV. Combining PEG-assisted melt crystallization and 3D ED not only accelerated the discovery of new polymorphs but also provided unique opportunities for understanding structure-property relationships in pharmaceutical crystals.

AB - Two new polymorphs (forms VIII and IX) of piroxicam were discovered through poly(ethylene glycol) (PEG)-assisted melt crystallization, and their structures were revealed by 3D electron diffraction (3D ED). This discovery provides insight into the potential of PEG in pharmaceutical polymorph discovery and verifies the significance of 3D ED as an essential technique for structural determination of pharmaceuticals. Furthermore, the direct contribution of intermolecular hydrogen bonding to melting points was discussed based on the structural divergency between the newly solved form VIII and the previously reported form IV. Combining PEG-assisted melt crystallization and 3D ED not only accelerated the discovery of new polymorphs but also provided unique opportunities for understanding structure-property relationships in pharmaceutical crystals.

UR - https://www.scopus.com/pages/publications/85202500771

U2 - 10.1021/acs.cgd.4c00951

DO - 10.1021/acs.cgd.4c00951

M3 - Article

AN - SCOPUS:85202500771

SN - 1528-7483

VL - 24

SP - 7298

EP - 7305

JO - Crystal Growth and Design

JF - Crystal Growth and Design

IS - 17

ER -

Polyethylene Glycol-Assisted Melt Crystallization of Two New Piroxicam Polymorphs Revealed by 3D Electron Diffraction

Abstract

Access to Document

Other files and links

Fingerprint

Cite this