Moxley-Paquette, Vincent, Lane, Daniel, Steiner, Katrina, Downey, Katelyn, Costa, Peter M., Lysak, Daniel H., Ronda, Kiera, Soong, Ronald, Zverev, Dimitri, De Castro, Peter, Frei, Thomas, Stuessi, Juerg, Al Adwan-Stojilkovic, Danijela, Graf, Stephan, Gloor, Simon, Schmidig, Daniel, Kuemmerle, Rainer, Kuehn, Till, Busse, Falko, Utz, Marcel, Lacerda, Andressa, Nashman, Ben, Albert, Larry, Anders, Jens and Simpson, André J. (2023) Development of low-magnetic susceptibility microcoils via 5-axis machining for analysis of biological and environmental samples. Analytical Chemistry, 95 (37), 13932-13940. (doi:10.1021/acs.analchem.3c02437).
Abstract
In environmental research, it is critical to understand how toxins impact invertebrate eggs and egg banks, which, due to their tiny size, are very challenging to study by conventional nuclear magnetic resonance (NMR) spectroscopy. Microcoil technology has been extensively utilized to enhance the mass-sensitivity of NMR. In a previous study, 5-axis computer numerical control (CNC) micromilling (shown to be a viable alternative to traditional microcoil production methods) was used to create a prototype copper slotted-tube resonator (STR). Despite the excellent limit of detection (LOD) of the resonator, the quality of the line shape was very poor due to the magnetic susceptibility of the copper resonator itself. This is best solved using magnetic susceptibility-matched materials. In this study, approaches are investigated that improve the susceptibility while retaining the versatility of coil milling. One method involves machining STRs from various copper/aluminum alloys, while the other involves machining ones from an aluminum 2011 alloy and electroplating them with copper. In all cases, combining copper and aluminum to produce resonators resulted in improved line shape and SNR compared to pure copper resonators due to their reduced magnetic susceptibility. However, the copper-plated aluminum resonators showed optimal performance from the devices tested. The enhanced LOD of these STRs allowed for the first 1H-13C heteronuclear multiple quantum coherence (HMQC) of a single intact 13C-labeled Daphnia magna egg (∼4 μg total biomass). This is a key step toward future screening programs that aim to elucidate the toxic processes in aquatic eggs.
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