Analysis of Multiple Samples Using Multiplex Sample NMR:  Selective Excitation and Chemical Shift Imaging Approaches

Hou, Ting; Smith, Jay; MacNamara, Ernesto; Macnaughtan, Megan A.; Raftery, Daniel

doi:10.1021/ac0100751

Cited by 41 publications

(42 citation statements)

References 40 publications

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“…Steady progress is being made to incorporate NMR analysis into high-throughput and combinatorial chemistry applications. [13][14][15][16][17][18] Utilization of conventional NMR for high-throughput biosensor applications may be limited by the intrinsically low sensitivity and the complexity of spectra obtained from biomolecules and mixtures. Laser-polarization 19 of 129 Xe offers an increase in signal-tonoise by several orders of magnitude relative to the equilibrium nuclear-spin polarizations measured in normal NMR experiments.…”

Section: Introductionmentioning

confidence: 99%

Development of a Functionalized Xenon Biosensor

et al. 2004

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NMR-based biosensors that utilize laser-polarized xenon offer potential advantages beyond current sensing technologies. These advantages include the capacity to simultaneously detect multiple analytes, the applicability to in vivo spectroscopy and imaging, and the possibility of "remote" amplified detection. Here we present a detailed NMR characterization of the binding of a biotin-derivatized caged-xenon sensor to avidin. Binding of "functionalized" xenon to avidin leads to a change in the chemical shift of the encapsulated xenon in addition to a broadening of the resonance, both of which serve as NMR markers of ligand-target interaction. A control experiment in which the biotin-binding site of avidin was blocked with native biotin showed no such spectral changes, confirming that only specific binding, rather than nonspecific contact, between avidin and functionalized xenon leads to the effects on the xenon NMR spectrum. The exchange rate of xenon (between solution and cage) and the xenon spin-lattice relaxation rate were not changed significantly upon binding. We describe two methods for enhancing the signal from functionalized xenon by exploiting the laser-polarized xenon magnetization reservoir. We also show that the xenon chemical shifts are distinct for xenon encapsulated in different diastereomeric cage molecules. This demonstrates the potential for tuning the encapsulated xenon chemical shift, which is a key requirement for being able to multiplex the biosensor.

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Section: Introductionmentioning

confidence: 99%

Development of a Functionalized Xenon Biosensor

et al. 2004

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“…Several methods are already available that could be easily adapted to measure thousands of MRS samples per day, such as highthroughput NMR spectroscopy and magnetic resonance (MR) imaging. [31][32][33][34] Here, the feasibility of conducting highthroughput screening for enantiomeric impurities was demonstrated by using MR imaging. MR images were obtained for 60 MRS samples simultaneously in a 384-well plate ( Figure 5 …”

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confidence: 99%

Magnetic Relaxation Switch Immunosensors Detect Enantiomeric Impurities

et al. 2004

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“…Microcoils have been used in a variety of NMR experiments such as LC-NMR and capillary electrophoresis CE-NMR because they provide excellent signal-to-noise ratios (S/N ) for mass-limited and volume-limited samples (24). In our laboratory we have previously used microcoils to analyze multiple samples simultaneously (25)(26)(27). The microcoils are attached to the capillary tubes using a cyanoacrylate adhesive (Krazy Glue, Borden Inc., Columbus, OH).…”

Section: Methodsmentioning

confidence: 99%