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Figure 7.16. Schematic illustration of the automated ow-through setup for multiple-sample NMR analysis using a robotic liquid handler, which is controlled by a PC computer and able to communicate with the NMR spectrometer.
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cient as a fully automated method. To realize the complete automatic sample changing, recent experiments using a robotic liquid handler (Gilson, Inc.) as the sample delivering system have recently been reprinted.113 A schematic diagram for the automated multiplex NMR analysis is shown in Figure 7.16.The liquid handler is controlled by a PC computer, and the communication between the liquid handler and the NMR spectrometer is established through TTL signals. In this system the delivery of samples of small volumes (~25 mL) into the multiplex NMR probe with high precision was investigated, and total computer control is straightforward to realize. NMR experiments using the setup of Figure 7.16 show that the NMR analysis of multiple sample chemical libraries can be achieved at a rate of two samples a minute.113
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Serial NMR analysis methodologies with high-throughput capabilities have been studied extensively, and are becoming routine. However, the highthroughput requirements for the analysis of chemical libraries by NMR dictate that alternative approaches need to be formulated. The development of different techniques for parallel NMR data acquisition has occurred only over the past few years, but this is clearly a rapidly evolving
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area of research. Currently most of the development in parallel NMR detection has been in the area of probe hardware design, and in the optimization of different pulse sequences and data processing techniques. Although one is ultimately limited by the extent of the homogeneous region of the magnet, a major thrust is to increase the number of coils. This may well involve the incorporation of microfabrication methods, as have already been prototyped for coil production.96,114 The ultimate aim of parallel NMR probe technologies will likely be to optimize the interface with widely accepted sample formats such as the 96-well plate. However, the number of NMR sample coils that will optimize the throughput is yet to be determined. Hand in hand with an increase in the number of coils, is the requirement for the maintenance of high spectral resolution. This requirement may involve the development of zero-susceptibility materials for very small coils, as the shimming of a small number of sample coils is already challenging. Besides combinatorial library analysis and drug screening there are a number of applications for parallel high-throughput NMR. Clearly, the tremendous advances in hyphenated microseparation/NMR detection can bene t from the incorporation of parallelism. The incorporation of capillary separation with a multicoil NMR probe and the associated capillary uidics to deliver the samples to and from the coils is the next step in probe development.115 We anticipate further advances along these lines. Also exciting will be the interface of such intelligent NMR probe and uidic systems to other integrated detection modalities such as uorescence, absorbance, and even mass spectrometry to provide an integrated system capable of delivering unprecedented structural information from complex samples.
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ACKNOWLEDGMENTS
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The authors would like to thank Greg Fisher, Ernie MacNamara, Megan Macnaughtan, Chris Petucci, Jay Smith, and Jun Xu for their contribution to the work presented here. Financial support from the National Science Foundation, the Alfred P. Sloan Foundation, the Purdue Research Foundation, and the Lemelson Foundation is gratefully acknowledged.
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