Portable Microcoil NMR Detection Coupled to Capillary Electrophoresis

Diekmann, J.; Adams, Kristl L.; Klunder, Gregory L.; Evans, Lee; Steele, Paul T.; Vogt, Carsten; Herberg, Julie L.

doi:10.1021/ac102389b

Cited by 22 publications

(17 citation statements)

References 47 publications

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“…5A) 13 C channel consists of a second chip and a separate 13 C coil placed underneath the capillary. The orthogonal orientation of the two coils minimizes mutual interactions.…”

Section: Significancementioning

confidence: 99%

“…Although one doubly tuned coil (24) can be used, we use the two coils for simplicity of their design. The 1D 1 H spectrum without activating the 13 C channel (Fig. 5B) shows two large peaks with a 140-Hz splitting originating from the 1 H- 13 C J coupling (the third smaller peak is from the OH group).…”

Section: Significancementioning

confidence: 99%

“…The 1D 1 H spectrum without activating the 13 C channel (Fig. 5B) shows two large peaks with a 140-Hz splitting originating from the 1 H- 13 C J coupling (the third smaller peak is from the OH group). HSQC and HMQC (Fig.…”

Section: Significancementioning

confidence: 99%

“…5 C and D) use both 13 C and 1 H channels for excitation and magnetization transfer, and only the 1 H channel is used for detection. In each of the resulting spectra, the two peaks separated by 140 Hz along the 1 H spectrum appear at the same 13 C chemical shift, unequivocally identifying the 13 C-1 H single-bond coupling. As the OH proton is uncoupled to a carbon, its signal vanishes in the 2D spectra.…”

Section: Significancementioning

confidence: 99%

“…In this case, portable, affordable, and low-maintenance NMR spectrometers built with a permanent magnet can make the benefits of NMR spectroscopy more broadly available and enable new applications. Bulky superconducting systems have to be permanently placed in dedicated laboratories, but portable systems can enable in-field, on-demand, or online applications such as quality control and chemical reaction monitoring (4), and can greatly facilitate co-use of NMR spectroscopy with other analytical methods such as liquid chromatography (12) and capillary electrophoresis (13). Thus, much effort has been devoted to miniaturizing NMR spectrometers, leading to the critical development of small permanent magnets with high field homogeneity (10,14,15).…”

mentioning

confidence: 99%

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Scalable NMR spectroscopy with semiconductor chips

Paulsen

Sun

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

112

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State-of-the-art NMR spectrometers using superconducting magnets have enabled, with their ultrafine spectral resolution, the determination of the structure of large molecules such as proteins, which is one of the most profound applications of modern NMR spectroscopy. Many chemical and biotechnological applications, however, involve only small-to-medium size molecules, for which the ultrafine resolution of the bulky, expensive, and high-maintenance NMR spectrometers is not required. For these applications, there is a critical need for portable, affordable, and low-maintenance NMR spectrometers to enable in-field, on-demand, or online applications (e.g., quality control, chemical reaction monitoring) and co-use of NMR with other analytical methods (e.g., chromatography, electrophoresis). As a critical step toward NMR spectrometer miniaturization, small permanent magnets with high field homogeneity have been developed. In contrast, NMR spectrometer electronics capable of modern multidimensional spectroscopy have thus far remained bulky. Complementing the magnet miniaturization, here we integrate the NMR spectrometer electronics into 4-mm 2 silicon chips. Furthermore, we perform various multidimensional NMR spectroscopies by operating these spectrometer electronics chips together with a compact permanent magnet. This combination of the spectrometer-electronics-on-a-chip with a permanent magnet represents a useful step toward miniaturization of the overall NMR spectrometer into a portable platform. N MR spectroscopy has been celebrated for its ability to probe molecular structures and dynamics with the atomic resolution (1-9). State-of-the-art NMR spectrometers use large superconducting magnets, whose high and uniform magnetic fields lead to the fine spectral resolution necessary for interrogating large molecules such as proteins. In fact, the structural study of large molecules is one of the most profound applications of modern NMR spectroscopy.However, the spectral resolution of the bulky, expensive, and high-maintenance NMR spectrometers is not necessary for a broad array of studies involving small-to-medium size molecules in chemistry, chemical engineering, and biotechnology (10, 11). In this case, portable, affordable, and low-maintenance NMR spectrometers built with a permanent magnet can make the benefits of NMR spectroscopy more broadly available and enable new applications. Bulky superconducting systems have to be permanently placed in dedicated laboratories, but portable systems can enable in-field, on-demand, or online applications such as quality control and chemical reaction monitoring (4), and can greatly facilitate co-use of NMR spectroscopy with other analytical methods such as liquid chromatography (12) and capillary electrophoresis (13). Thus, much effort has been devoted to miniaturizing NMR spectrometers, leading to the critical development of small permanent magnets with high field homogeneity (10,14,15).Complementing this advance in magnet miniaturization, here we integrate the spectrometer elec...

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“…5A) 13 C channel consists of a second chip and a separate 13 C coil placed underneath the capillary. The orthogonal orientation of the two coils minimizes mutual interactions.…”

Section: Significancementioning

confidence: 99%