Parts per Million Powder X-ray Diffraction

Newman, Justin A.; Schmitt, Paul D.; Toth, Scott J.; Deng, Fengyuan; Zhang, Shijie; Simpson, Garth J.

doi:10.1021/acs.analchem.5b02758

Title: Parts per Million Powder X-ray Diffraction

Journal Article · Wed Oct 14 00:00:00 EDT 2015 · Analytical Chemistry

DOI:https://doi.org/10.1021/acs.analchem.5b02758· OSTI ID:1228102

Newman, Justin A. ^[1]; Schmitt, Paul D. ^[1]; Toth, Scott J. ^[1]; Deng, Fengyuan ^[1]; Zhang, Shijie ^[1]; Simpson, Garth J. ^[1]

Purdue Univ., West Lafayette, IN (United States). Dept. of Chemistry

Here in this paper we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect low crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.

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Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)

Sponsoring Organization:: National Institutes of Health (NIH); USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-06CH11357; SC0000997; NIH-R01GM103401; NIH-R01GM103910

OSTI ID:: 1228102

Journal Information:: Analytical Chemistry, Vol. 87, Issue 21; ISSN 0003-2700

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: ENGLISH

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Cited by: 59 works

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Droplet Microfluidics XRD Identifies Effective Nucleating Agents for Calcium Carbonate Levenstein, Mark A.; Anduix‐Canto, Clara; Kim, Yi‐Yeoun Advanced Functional Materials, Vol. 29, Issue 19 https://doi.org/10.1002/adfm.201808172	journal	March 2019
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