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Mesoporous magnesium carbonate: Synthesis, characterization and biocompatibility
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Nanotechnology and Functional Materials.
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Mesoporous materials constitute a promising class of nanomaterials for a number of applications due to their tunable pore structure. The synthesis of most mesoporous materials involves a surfactant liquid crystal structure to form the pores. As well as the many advantages associated with this method of synthesis, there are disadvantages such as high production costs and a substantial environmental impact which limit the possibilities for large scale production. Therefore there is a need for other synthesis routes.

The aim of the work described herein was to contribute to this field by developing a synthesis route that does not rely on surfactants for pore formation. A mesoporous magnesium carbonate material was therefore formed by self-assemblage of the particles around carbon dioxide gas bubbles, which functioned as pore templates. It was also possible to vary the pore diameter between 3 and 20 nm.

The biocompatibility of the formed magnesium carbonate material was evaluated in terms of in vitro cytotoxicity and hemocompatibility, in vivo skin irritation and acute systemic toxicity. The results from the in vitro cytotoxicity, in vivo skin irritation and acute systemic toxicity test using a polar extraction vehicle showed that the material was non-toxic. While signs of toxicity were observed in the acute systemic toxicity test using a non-polar solvent, this was attributed to injection of particles rather than toxic leachables. In the in vitro hemocompatibility test, no hemolytic activity was found with material concentrations of up to 1 mg/ml. It was further shown that the material had anticoagulant properties and induced moderate activation of the complement system. The anticoagulant properties were ascribed to uptake of Ca2+.

Finally, the ability of the material to increase the dissolution rate of the poorly soluble drug itraconazole was analyzed.  Itraconazole was dissolved up to 23 times faster from the magnesium carbonate pores than when the free drug was used. The release rate from the delivery vehicle was dependent on the pore diameter.

The work presented herein is expected to be useful for the development of alternative synthesis routes for mesoporous materials and also for encouraging the development of biomedical applications for these materials.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2016. , 75 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1363
Keyword [en]
mesoporous, magnesium carbonate, pore size control, cytotoxicity, in vivo, skin irritation, acute systemic toxicity, hemocompatibility, Ca2+ uptake, solubility enhancement
National Category
Nano Technology
Research subject
Engineering Science with specialization in Nanotechnology and Functional Materials
Identifiers
URN: urn:nbn:se:uu:diva-281522ISBN: 978-91-554-9540-4 (print)OAI: oai:DiVA.org:uu-281522DiVA: diva2:916230
Public defence
2016-05-20, Polhemssalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:30 (English)
Opponent
Supervisors
Available from: 2016-04-27 Created: 2016-03-24 Last updated: 2016-04-29
List of papers
1. A Template-Free, Ultra-Adsorbing, High Surface Area Carbonate Nanostructure
Open this publication in new window or tab >>A Template-Free, Ultra-Adsorbing, High Surface Area Carbonate Nanostructure
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2013 (English)In: PLoS ONE, ISSN 1932-6203, E-ISSN 1932-6203, Vol. 8, no 7, e68486- p.Article in journal (Refereed) Published
Abstract [en]

We report the template-free, low-temperature synthesis of a stable, amorphous, and anhydrous magnesium carbonate nanostructure with pore sizes below 6 nm and a specific surface area of ~ 800 m2 g−1, substantially surpassing the surface area of all previously described alkali earth metal carbonates. The moisture sorption of the novel nanostructure is featured by a unique set of properties including an adsorption capacity ~50% larger than that of the hygroscopic zeolite-Y at low relative humidities and with the ability to retain more than 75% of the adsorbed water when the humidity is decreased from 95% to 5% at room temperature. These properties can be regenerated by heat treatment at temperatures below 100°C.The structure is foreseen to become useful in applications such as humidity control, as industrial adsorbents and filters, in drug delivery and catalysis.

National Category
Nano Technology
Research subject
Engineering Science with specialization in Nanotechnology and Functional Materials; Engineering Science with specialization in Materials Science
Identifiers
urn:nbn:se:uu:diva-203772 (URN)10.1371/journal.pone.0068486 (DOI)000322000600009 ()
Note

De två (2) första författarna delar förstaförfattarskapet.

Available from: 2013-07-19 Created: 2013-07-19 Last updated: 2017-12-06Bibliographically approved
2. On the pore forming mechanism of Upsalite, a micro- and mesoporous magnesium carbonate
Open this publication in new window or tab >>On the pore forming mechanism of Upsalite, a micro- and mesoporous magnesium carbonate
2014 (English)In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 190, 99-104 p.Article in journal (Refereed) Published
Abstract [en]

This work analyzes the pore forming mechanism and stability of Upsalite; an extraordinary moisture absorbing, high-surface area magnesium carbonate powder synthesised without the use of surfactants as pore forming agents. The pores in Upsalite were found to be created in a two-step process where the first step includes the formation of micropores by solvent evaporation and release of physically bound carbon dioxide, acting as an in-situ pore-forming template. In the second step, the micropores expand to mesopores due to partial decomposition of organic groups on the surface of the pore walls when the material is stored in air at moderate temperatures (70 °C). The resulting material has a narrow pore size distribution centered at 5 nm, and the amorphous structure is stable upon storage in a humid atmosphere.

It was further shown that calcination at temperatures above 250 °C is required for complete removal of the organic surface groups in Upsalite. Prior to calcination, the organic groups present in the material act as barriers hindering water to induce crystallization of the bulk material. After calcination, however, Upsalite crystallizes into nesquehonite when stored at 100 % relative humidity for several days. The results presented herein are expected to be useful for the development of novel surfactant-free synthesis routes of porous materials as well as for the understanding of the long-term performance of such materials.

Keyword
pore forming mechanism, surfactant-free, in situ gas template, microporous, mesoporous, magnesium carbonate
National Category
Nano Technology
Research subject
Engineering Science with specialization in Nanotechnology and Functional Materials
Identifiers
urn:nbn:se:uu:diva-212802 (URN)10.1016/j.micromeso.2013.12.011 (DOI)000335102500014 ()
Available from: 2013-12-14 Created: 2013-12-14 Last updated: 2017-12-06Bibliographically approved
3. Nanostructure and pore size control of template-free synthesized mesoporous magnesium carbonate Upsalite
Open this publication in new window or tab >>Nanostructure and pore size control of template-free synthesized mesoporous magnesium carbonate Upsalite
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(English)Manuscript (preprint) (Other academic)
National Category
Nano Technology
Identifiers
urn:nbn:se:uu:diva-281520 (URN)
Available from: 2016-03-24 Created: 2016-03-24 Last updated: 2016-04-29
4. Cytotoxicity, in Vivo Skin Irritation and Acute Systemic Toxicity of the Mesoporous Magnesium Carbonate Upsalite®
Open this publication in new window or tab >>Cytotoxicity, in Vivo Skin Irritation and Acute Systemic Toxicity of the Mesoporous Magnesium Carbonate Upsalite®
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2015 (English)In: Journal of Biomaterials and Nanobiotechnology, ISSN 2158-7027, E-ISSN 2158-7043Article in journal (Refereed) Published
National Category
Nano Technology
Identifiers
urn:nbn:se:uu:diva-264802 (URN)10.4236/jbnb.2015.64024 (DOI)
Available from: 2015-10-19 Created: 2015-10-19 Last updated: 2017-12-01
5. Study of mesoporous magnesium carbonate in contact with whole human blood
Open this publication in new window or tab >>Study of mesoporous magnesium carbonate in contact with whole human blood
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2016 (English)In: RSC Advances, ISSN 2046-2069, E-ISSN 2046-2069, Vol. 6, no 58, 52810-52816 p.Article in journal (Refereed) Published
Abstract [en]

The interaction of mesoporours magnesium carbonate (Upsalite) particles (50-100 mm) with human whole blood was investigated using an in vitro loop model and the effect on the complement system, blood coagulation and red blood cell lysis was assessed. The removal of Ca2+ by Upsalite and the possible exchange with and/or release of Mg2+ were explored as well. Upsalite was found to present anticoagulant properties, most probably due to the uptake of Ca2+ by the particles. No hemolytic activity was detected at Upsalite concentrations up to 1 mg ml(-1). Moderate to high levels of C3a and sC5b-9 were observed for Upsalite, however such levels were statistically different from the negative control only when the particle concentrations were 0.25 mg ml(-1) and 1.0 mg ml(-1), respectively. The presented findings are promising for the future development of mesoporous magnesium carbonate-based materials for biomedical applications.

National Category
Nano Technology
Identifiers
urn:nbn:se:uu:diva-281465 (URN)10.1039/c6ra05679b (DOI)000378563200037 ()2-s2.0-84973390611 (Scopus ID)
Funder
Swedish Research Council
Available from: 2016-03-24 Created: 2016-03-24 Last updated: 2017-11-30Bibliographically approved

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