Nano-mole scale sequential signal assignment by 1H-detected protein solid-state NMR

Songlin Wang; Sudhakar Parthasarathy; Yiling Xiao; Yusuke Nishiyama; Fei Long; Isamu Matsuda; Yuki Endo; Takahiro Nemoto; Kazuo Yamauchi; Tetsuo Asakura; Mitsuhiro Takeda; Tsutomu Terauchi; Masatsune Kainosho; Yoshitaka Ishii

doi:10.1039/C5CC04618A

Nano-mole scale sequential signal assignment by ¹H-detected protein solid-state NMR†

Songlin Wang,^a Sudhakar Parthasarathy,^a Yiling Xiao,^a Yusuke Nishiyama,^bc Fei Long,^a Isamu Matsuda,^a Yuki Endo,^b Takahiro Nemoto,^b Kazuo Yamauchi,^de Tetsuo Asakura,^f Mitsuhiro Takeda,^g Tsutomu Terauchi,^h Masatsune Kainosho^gi and Yoshitaka Ishii*^aj

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* Corresponding authors

^a Department of Chemistry, University of Illinois at Chicago, Chicago, IL 60607, USA

^b JEOL RESONANCE Inc., 3-1-2 Musashino, Akishima, Tokyo 196-8558, Japan

^c RIKEN CLST-JEOL Collaboration Center, Yokohama, Kanagawa 230-0045, Japan

^d Nuclear Magnetic Resonance Core Lab., King Abdullah University of Science and Technology, Thuwal 23955-6900, Saudi Arabia

^e School of Science and Technology, Nazarbayev University, Astana, Kazakhstan

^f Department of Biotechnology, Tokyo University of Agriculture and Technology 2-24-16, Nakacho, Koganei, Tokyo 184-8588, Japan

^g Structure Biology Research Center, Graduate School of Science, Furocho, Chikusa-ku, Nagoya University, Nagoya, Japan

^h SAIL Technologies Inc., 2008-2 Wada, Tama, Tokyo 206-0001, Japan

ⁱ Graduate School of Science and Engineering, Tokyo Metropolitan University, 1-1 Minami-ohsawa, Hachioji, Tokyo 192-0397, Japan

^j Center for Structural Biology, University of Illinois at Chicago, Chicago, IL 60607, USA
E-mail: yishii@uic.edu
Tel: +1-312-413-0076

Abstract

We present a 3D ¹H-detected solid-state NMR (SSNMR) approach for main-chain signal assignments of 10–100 nmol of fully protonated proteins using ultra-fast magic-angle spinning (MAS) at ∼80 kHz by a novel spectral-editing method, which permits drastic spectral simplification. The approach offers ∼110 fold time saving over a traditional 3D ¹³C-detected SSNMR approach.

Chemical Communications

Nano-mole scale sequential signal assignment by ¹H-detected protein solid-state NMR†

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Nano-mole scale sequential signal assignment by ¹H-detected protein solid-state NMR

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