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Air-Stable Gadolinium Precursors for the Facile Microwave-Assisted Synthesis of Gd2O3 Nanocontrast Agents for Magnetic Resonance Imaging
Crystal Growth & Design ( IF 3.8 ) Pub Date : 2018-01-18 00:00:00 , DOI: 10.1021/acs.cgd.7b00787
Shifaa M. Siribbal 1 , Johannes Schläfer 1 , Shaista Ilyas 1 , Zhangjun Hu 2 , Kajsa Uvdal 2 , Martin Valldor 3 , Sanjay Mathur 1
Affiliation  

Using metal organic precursors in materials synthesis remains a challenge due to their high moisture susceptibility. In this work, we describe a facile methodology for the synthesis of Gd2O3-based contrast agents from two new gadolinium-based complexes. [Gd(PyTFP)4] (PyH) 1 (PyTFP = C8H5NOF3, Py = C5H5N) and [Gd(DMOTFP)3Py] 2 (DMOTFP = C8H7NO2F3) were synthesized via a classical ligand exchange reaction of [Gd{N(SiMe3)2}3] under inert conditions. As a result, X-ray diffraction analysis revealed a distorted square antiprismatic coordination and an augmented triangular prismatic arrangement of ligands around gadolinium atoms in 1 and 2, respectively. It also showed that 1 is an anionic complex of formula [Gd(PyTFP)4](PyH), while a neutral tris-compound, [Gd(DMOTFP)3Py], was obtained as a pyridine adduct in 2. Fast and reproducible microwave-assisted decomposition of 1 and 2 provided homogeneous Gd(OH)3 nanorods at mild temperature without using any surfactant or capping reagent. As-synthesized nanorods were easily transformed into a cubic phase of Gd2O3 nanoparticles by thermal treatment under ambient conditions. The magnetic measurement showed the typical paramagnetic behavior of the Gd2O3 nanoparticles (NPs). The cytotoxicity profile demonstrates the biocompatibility and negligible toxicity of the as-synthesized nanoprobes. The suggested approach provides a new class of gadolinium-based precursors which allows facile synthesis of highly crystalline Gd2O3 NPs.

中文翻译:

空气稳定的Pre前体,用于微波辅助合成的用于磁共振成像的Gd 2 O 3纳米造影剂。

由于金属易受潮性高,在材料合成中使用金属有机前驱物仍然是一个挑战。在这项工作中,我们描述了一种从两种新的based基复合物合成Gd 2 O 3基造影剂的简便方法。[Gd(PyTFP)4 ](PyH)1(PyTFP = C 8 H 5 NOF 3,Py = C 5 H 5 N)和[Gd(DMOTFP)3 Py] 2(DMOTFP = C 8 H 7 NO 2 F 3)是通过[Gd {N(SiMe 32 } 3 ]在惰性条件下。结果,X射线衍射分析显示扭曲的方形反棱柱配位和分别在12中的atoms原子周围的配体增加了三角棱柱形排列。还显示出1是式[Gd(PyTFP)4 ](PyH)的阴离子络合物,而在2中以吡啶加合物的形式获得了中性三元化合物[Gd(DMOTFP)3 Py] 。快速和可重现的微波辅助分解12提供了均一的Gd(OH)3纳米棒在温和的温度下,不使用任何表面活性剂或封端剂。通过在环境条件下进行热处理,可以将合成后的纳米棒轻松转变为Gd 2 O 3纳米颗粒的立方相。磁性测量显示了Gd 2 O 3纳米颗粒(NPs)的典型顺磁行为。细胞毒性概况证明了合成纳米探针的生物相容性和可忽略的毒性。建议的方法提供了新的一类基于lin的前体,它可以轻松合成高度结晶的Gd 2 O 3 NP。
更新日期:2018-01-18
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