title: An efficient method and device for transfer of semisolid materials into solid-state NMR spectroscopy rotors.
abstract: The study of mass-limited biological samples by magic angle spinning (MAS) solid-state NMR spectroscopy critically relies upon the high-yield transfer of material from a biological preparation into the MAS rotor. This issue is particularly important for maintaining biological activity and hydration of semi-solid samples such as membrane proteins in lipid bilayers, pharmaceutical formulations, microcrystalline proteins and protein fibrils. Here we present protocols and designs for rotor-packing devices specifically suited for packing hydrated samples into Pencil-style 1.6 mm, 3.2 mm standard, and 3.2 mm limited speed MAS rotors. The devices are modular and therefore readily adaptable to other rotor and/or ultracentrifugation tube geometries.
authors.affiliation: University of Illinois at Urbana-Champaign, Department of Chemistry, 600 South Mathews Avenue, Urbana, IL 61801, USA. Electronic address: hisao2@illinois.edu.
authors.forename: Grant S
authors.initials: GS
authors.lastname: Hisao
authors.affiliation: University of Illinois at Urbana-Champaign, School of Chemical Sciences Machine Shop, 505 South Matthews Ave., Urbana, IL 61801, USA. Electronic address: mharland@illinois.edu.
authors.forename: Michael A
authors.initials: MA
authors.lastname: Harland
authors.affiliation: University of Illinois at Urbana-Champaign, School of Chemical Sciences Machine Shop, 505 South Matthews Ave., Urbana, IL 61801, USA.
authors.forename: Robert A
authors.initials: RA
authors.lastname: Brown
authors.affiliation: University of Illinois at Urbana-Champaign, Department of Chemistry, 600 South Mathews Avenue, Urbana, IL 61801, USA. Electronic address: berthold@illinois.edu.
authors.forename: Deborah A
authors.initials: DA
authors.lastname: Berthold
authors.affiliation: University of Illinois at Urbana-Champaign, School of Chemical Sciences Machine Shop, 505 South Matthews Ave., Urbana, IL 61801, USA. Electronic address: thomew@illinois.edu.
authors.forename: Thomas E
authors.initials: TE
authors.lastname: Wilson
authors.affiliation: University of Illinois at Urbana-Champaign, Department of Chemistry, 600 South Mathews Avenue, Urbana, IL 61801, USA; University of Illinois at Urbana-Champaign, Department of Biochemistry, Center for Biophysics and Quantitative Biology, 600 South Mathews Avenue, Urbana, IL 61801, USA. Electronic address: rienstra@illinois.edu.
authors.forename: Chad M
authors.initials: CM
authors.lastname: Rienstra
mesh_terms: D003460:Crystallization; D004134:Dimyristoylphosphatidylcholine / Q000737:chemistry; D008051:Lipid Bilayers; D008081:Liposomes / Q000737:chemistry; D008565:Membrane Proteins / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000295:instrumentation / Q000379:methods*; D004364:Pharmaceutical Preparations; D011506:Proteins / Q000737:chemistry; D014461:Ultracentrifugation
chemical_list: D008051:Lipid Bilayers; D008081:Liposomes; D008565:Membrane Proteins; D004364:Pharmaceutical Preparations; D011506:Proteins; D004134:Dimyristoylphosphatidylcholine
keywords: Gel phase samples; MAS rotor-packing; Magic angle spinning; Solid-state NMR