Size Exclusion Chromatography: An Indispensable Tool for the Isolation of Monodisperse Gold Nanomolecules
Size Exclusion Chromatography: An Indispensable Tool for the Isolation of Monodisperse Gold Nanomolecules
复制标题
尺寸排阻色谱：分离单分散金纳米分子不可或缺的工具
DOI：
10.1021/acs.analchem.0c04961
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发表时间：
2021
影响因子：
7.4
通讯作者：
Dass, Amala
中科院分区：
文献类型：
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作者：
Sakthivel, Naga Arjun;Jupally, Vijay Reddy;Eswaramoorthy, Senthil Kumar;Wijesinghe, Kalpani Hirunika;Nimmala, Praneeth Reddy;Kumara, Chanaka;Rambukwella, Milan;Jones, Tanya;Dass, Amala
高度单分散和纯净的原子精确金纳米分子（aunm）样品对于了解其性质和开发使用它们的应用至关重要。不幸的是，在一步反应中产生单尺寸纳米分子的合成方案是不可用的。相反，我们观察到一个多分散产品与芯尺寸的混合物。该产品需要合成后反应和分离技术来分离纯纳米分子。基于不同粒径溶解度的溶剂分馏在分离纯化合物方面有一定的效果。在分离大小非常相似的aunm时，它变得单调乏味，并且提供的控制较少。在这里，我们报告了使用尺寸排除色谱（SEC）作为分离纳米分子和纳米颗粒的工具的通用性和不可或缺的性质。我们已经证明了以下几点：(1)SEC比溶剂分馏更容易分离；(2)更宽尺寸范围的分离（~ 5-200 kDa或~ 1-3 nm）和更大规模的分离（20-100 mg /负载）；(3)从Au329(SR)84、Au144(SR)60、Au137(SR)56和Au130(SR)50的混合物中提纯Au137(SR)56，证明了Au137(SR)56可以分离出紧密粒径的aunm，这是溶剂分馏无法实现的；(4)由不同硫酸盐配体（脂肪族、芳香族和大体积）保护的aunm的分离；(5)增加柱长可提高分离效果。质谱法分析SEC组分。
Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) theease of separationoffered by SEC over solvent fractionation; (2) the separation of awider size range(∼5–200 kDa or ∼1–3 nm) andlarger-scaleseparation (20–100 mg per load); (3) the separation ofclosely sized AuNMs, demonstrated by purifying Au137(SR)56from a mixture of Au329(SR)84, Au144(SR)60, Au137(SR)56, and Au130(SR)50, which could not be achieved using solvent fractionation; (4) the separation ofAuNMs protected by different thiolate ligands(aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.