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Pharmaceutical characterization of solid and dispersed carbon nanotubes as nanoexcipients.

International journal of nanomedicine (2012-02-16)
Marina V Ivanova, Constanze Lamprecht, M Jimena Loureiro, J Torin Huzil, Marianna Foldvari
ABSTRACT

Carbon nanotubes (CNTs) are novel materials with considerable potential in many areas related to nanomedicine. However, a major limitation in the development of CNT-based therapeutic nanomaterials is a lack of reliable and reproducible data describing their chemical and structural composition. Knowledge of properties including purity, structural quality, dispersion state, and concentration are essential before CNTs see widespread use in in vitro and in vivo experiments. In this work, we describe the characterization of several commercially available and two in-house-produced CNT samples and discuss the physicochemical profiles that will support their use in nanomedicine. Eighteen single-walled and multi-walled CNT raw materials were characterized using established analytical techniques. Solid CNT powders were analyzed for purity and structural quality using thermogravimetric analysis and Raman spectroscopy. Extinction coefficients for each CNT sample were determined by ultraviolet-visible near infrared absorption spectroscopy. Standard curves for each CNT sample were generated in the 0-5 μg/mL concentration range for dispersions prepared in 1,2-dichlorobenzene. Raman spectroscopy and thermogravimetric analysis results demonstrated that CNT purity and overall quality differed substantially between samples and manufacturer sources, and were not always in agreement with purity levels claimed by suppliers. Absorbance values for individual dispersions were found to have significant variation between individual single-walled CNTs and multi-walled CNTs and sources supplying the same type of CNT. Significant differences (P < 0.01) in extinction coefficients were observed between and within single-walled CNTs (24.9-53.1 mL·cm(-1)·mg(-1)) and multi-walled CNTs (49.0-68.3 mL·cm(-1)·mg(-1)). The results described here suggest a considerable role for impurities and structural inhomogeneities within individual CNT preparations and the resulting spectroscopic properties of their dispersions. Raw CNT materials require thorough analytical workup before they can be used as nanoexcipients. This applies especially to the determination of CNT purity, structure, and concentration. The results presented here clearly demonstrate that extinction coefficients must be determined for individual CNT preparations prior to their use.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
1,2-Dichlorobenzene, anhydrous, 99%
Sigma-Aldrich
1,2-Dichlorobenzene, ReagentPlus®, 99%
Sigma-Aldrich
1,2-Dichlorobenzene, suitable for HPLC, 99%
Supelco
1,2-Dichlorobenzene, PESTANAL®, analytical standard
Supelco
1,2-Dichlorobenzene solution, certified reference material, 200 μg/mL in methanol
Sigma-Aldrich
1,2-Dichlorobenzene solution, NMR reference standard, 5% in acetone-d6 (99.9 atom % D), NMR tube size 5 mm × 8 in.

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