A complete 3D-printed tool kit for Solid-State NMR sample and rotor handling

IF 2 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS Journal of magnetic resonance Pub Date : 2024-08-06 DOI:10.1016/j.jmr.2024.107748
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Abstract

Solid state NMR (SSNMR) is a highly versatile and broadly applicable method for studying the structure and dynamics of biomolecules and materials. For scientists entering the field of SSNMR, the many quotidian activities required in the workflow to prepare samples for data collection can present a significant barrier to adoption. These steps include transfer of samples into rotors, marking the reflective surfaces for high sensitivity tachometer signal detection, inserting rotors into the magic-angle spinning (MAS) stator, achieving stable spinning, and removing and storing rotors to ensure reproducibility of data collection conditions. Even experienced spectroscopists experience occasional problems with these operations, and the cumulative probability of a delay to successful data collection is high enough to cause frequent disruptions to instrument schedules, particularly in the context of large facilities serving a diverse community of users. These problems are all amplified when utilizing rotors smaller than about 4 mm in diameter. Therefore, to improve the reliability and robustness of SSNMR sample preparation workflows, here we describe a set of tools for rotor packing, unpacking, tachometer marking, extraction and storage. Stereolithography 3D printing was employed as a cost-effective and convenient method for prototyping and manufacturing a full range of designs suitable for several types of probes and rotor geometries.

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用于固态 NMR 样品和转子处理的全套 3D 打印工具包
固态核磁共振(SSNMR)是一种用途广泛的方法,可用于研究生物分子和材料的结构与动力学。对于初涉 SSNMR 领域的科学家来说,工作流程中为数据采集准备样品所需的许多日常活动可能会成为采用该方法的重大障碍。这些步骤包括将样品转移到转子中、标记反射表面以进行高灵敏度转速计信号检测、将转子插入魔角旋转(MAS)定子中、实现稳定旋转以及移除和储存转子以确保数据采集条件的可重复性。即使是经验丰富的光谱分析人员在这些操作过程中也会偶尔遇到问题,而延迟成功采集数据的累积概率很高,足以导致仪器计划经常被打乱,尤其是在大型设施为不同用户群体提供服务的情况下。当使用直径小于 4 毫米的转子时,这些问题都会加剧。因此,为了提高 SSNMR 样品制备工作流程的可靠性和稳健性,我们在此介绍一套用于转子包装、拆包、转速计标记、提取和存储的工具。我们采用了立体光刻 3D 打印技术,这种方法既经济又方便,可用于原型设计和制造适合多种类型探针和转子几何形状的全套设计。
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来源期刊
CiteScore
3.80
自引率
13.60%
发文量
150
审稿时长
69 days
期刊介绍: The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.
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