Crystallization speed of salbutamol as a function of relative humidity and temperature

Zellnitz, Sarah; Narygina, Olga; Resch, Christian; Schroettner, Hartmuth; Urbanetz, Nora Anne

doi:10.1016/j.ijpharm.2015.04.079

Cited by 21 publications

(20 citation statements)

References 13 publications

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“…Humidity variation and XRPD data collection. In situ XRPD data were collected using a laboratory Empyrean diffractometer (Malvern Panalytical) equipped with a built-in transmission temperature humidity chamber (MHC-trans Anton Paar) (Zellnitz et al, 2015). An elliptical focusing X-ray mirror for Cu radiation ( = 1.540598 Å ) was used on the incident-beam side with 0.25 entrance slit, 0.5 anti-scatter slit and 0.04 rad Soller slits.…”

Section: Crystallizationmentioning

confidence: 99%

In situdetection of a novel lysozyme monoclinic crystal form upon controlled relative humidity variation

et al. 2018

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The effect of relative humidity (rH) on protein crystal structures, an area that has attracted high scientific interest during the past decade, is investigated in this study on hen egg‐white lysozyme (HEWL) polycrystalline precipitates via in situ laboratory X‐ray powder diffraction (XRPD) measurements. For this purpose, HEWL was crystallized at room temperature and pH 4.5, leading to a novel monoclinic HEWL phase which, to our knowledge, has not been reported before. Analysis of XRPD data collected upon rH variation revealed several structural modifications. These observations, on a well‐studied molecule like HEWL, underline not only the high impact of humidity levels on biological crystal structures, but also the significance of in‐house XRPD as an analytical tool in industrial drug development and its potential to provide information for enhancing manufacturing of pharmaceuticals.

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Section: Crystallizationmentioning

confidence: 99%

In situdetection of a novel lysozyme monoclinic crystal form upon controlled relative humidity variation

et al. 2018

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“…In-situ XRPD data were collected upon controlled rH variation using a laboratory Empyrean diffractometer (Malvern Panalytical) equipped with a built-in transmission temperature humidity chamber (MHC-trans Anton Paar) [178]. Polycrystalline specimens were loaded into thin Kapton-foil holders in order to reduce background contribution and were placed on a multiple position sample holder inside the chamber.…”

Section: In Situ Xrpd Measurements Upon Variation Of the Physicochemimentioning

confidence: 99%

Applications of X-ray Powder Diffraction in Protein Crystallography and Drug Screening

et al. 2020

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Providing fundamental information on intra/intermolecular interactions and physicochemical properties, the three-dimensional structural characterization of biological macromolecules is of extreme importance towards understanding their mechanism of action. Among other methods, X-ray powder diffraction (XRPD) has proved its applicability and efficiency in numerous studies of different materials. Owing to recent methodological advances, this method is now considered a respectable tool for identifying macromolecular phase transitions, quantitative analysis, and determining structural modifications of samples ranging from small organics to full-length proteins. An overview of the XRPD applications and recent improvements related to the study of challenging macromolecules and peptides toward structure-based drug design is discussed. This review congregates recent studies in the field of drug formulation and delivery processes, as well as in polymorph identification and the effect of ligands and environmental conditions upon crystal characteristics. These studies further manifest the efficiency of protein XRPD for quick and accurate preliminary structural characterization.

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“…In situ XRPD data were collected upon controlled rH variation using a laboratory Empyrean diffractometer (Malvern Panalytical) equipped with a built-in transmission temperature humidity chamber (MHC-trans Anton Paar) (Zellnitz et al, 2015). On the incident beam side are an elliptical focusing X-ray mirror for Cu radiation [ = 1.540585 (3) Å ] (Hö lzer et al, 1997), a 0.25 entrance slit and a 0.5 anti-scatter slit, and 0.04 rad Soller slits.…”

Section: Data Collection Using Laboratory and Synchrotron Sourcesmentioning

confidence: 99%

“…An MHC-trans humidity chamber (multi-sample humidity chamber transmission), compatible with the Empyrean X-ray powder diffractometer by Malvern Panalytical, is now commercially available for in situ experiments and observation of structural modifications under controlled temperature and humidity conditions. The sample temperature and rH level are regulated by two control units which are interdependent in order to have precise control of the temperature and humidity while avoiding condensation (Zellnitz et al, 2015).…”

Section: Introductionmentioning

confidence: 99%

Unit-cell response of tetragonal hen egg white lysozyme upon controlled relative humidity variation

et al. 2019

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Variation of relative humidity (rH) greatly affects the internal order of solventbased protein crystals, and the rearrangement of molecules can be efficiently recorded in distinct diffraction patterns. This study focuses on this topic, reporting the effect of rH variation experiments on hen egg white lysozyme (HEWL) polycrystalline precipitates of tetragonal symmetry using X-ray powder diffraction (XRPD). In situ XRPD data were collected on HEWL specimens during dehydration and rehydration processes using laboratory instrumentation. A known polymorph [space group P4 3 2 1 2, a = 79.07181 (1), c = 38.0776 (1) Å ] was identified during gradual dehydration from 95 to 63% rH and vice versa. Pawley analysis of collected data sets and accurate extraction of unitcell parameters indicated a characteristic evolution of the tetragonal axes with rH. In addition, there is a low humidity level below which samples do not retain their crystallinity. This work illustrates the accuracy of laboratory XRPD as a probe for time-resolved studies of proteins and in situ investigations of gradual structural modifications upon rH variation. These experiments provide essential information for improving production and post-production practices of microcrystalline protein-based pharmaceuticals. research papers J. Appl. Cryst. (2019). 52, 816-827 S. Logotheti et al. Effects of relative humidity on HEWL 817

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Crystallization speed of salbutamol as a function of relative humidity and temperature

Cited by 21 publications

References 13 publications

In situdetection of a novel lysozyme monoclinic crystal form upon controlled relative humidity variation

In situdetection of a novel lysozyme monoclinic crystal form upon controlled relative humidity variation

Applications of X-ray Powder Diffraction in Protein Crystallography and Drug Screening

Unit-cell response of tetragonal hen egg white lysozyme upon controlled relative humidity variation

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