Design, construction, and validation of a 1-mm triple-resonance high-temperature-superconducting probe for NMR

Brey, Wallace S.; Edison, Arthur S.; Nast, Robert E.; Rocca, James R.; Saha, Saikat; Withers, R.S.

doi:10.1016/j.jmr.2005.12.008

Cited by 117 publications

(83 citation statements)

References 12 publications

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“…Initial sample preparation of soldier head solvent extracts utilized vapor phase extraction at 80ºC on polymeric adsorbent traps, followed by dichloromethane elution to remove less volatile contaminants (Schmelz et al, 2004). Micropreparative gas chromatography (GC) was accomplished using an Agilent (Santa Clara CA) 6890 gas chromatograph (He carrier gas; 5.7 ml min 1-Dimensional and 2-dimensional NMR spectra were acquired at 20ºC with standard techniques using TopSpin ® (version 2.1) software on a Bruker Avance-II-600 spectrometer equipped with a 1 mm high-temperature superconducting (HTS) CryoProbe (Brey et al 2006). Solutions of the SHE γ-cadinene, ~ 10 µg/15 µl, the authentic γ-cadinene, ~ 25 µg/17 µl and of the SHE γ-cadinene aldehyde, ~ 50 µg/10 µl, were prepared in CDCl 3 (99.96 atom % D).…”

Section: Nuclear Magnetic Resonance (Nmr) Analysis Nmr Analyses Werementioning

confidence: 99%

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Effects of Soldier-Derived Terpenes on Soldier Caste Differentiation in the Termite Reticulitermes flavipes

et al. 2009

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-Primer pheromones play key roles in regulating division of labor, which is one of the most fundamental and defining aspects of insect sociality. Primer pheromones are chemical messengers that transmit hormone-like messages among colony members; in recipients these messages can either induce or suppress phenotypic caste differentiation. Here, we investigated soldier-caste-derived chemicals as possible primer pheromones in the lower termite Reticulitermes flavipes, a species for which no primer pheromones have yet been identified. We determined that soldier head extracts (SHE), when provided to totipotent workers along with the insect morphogenetic juvenile hormone (JH), significantly enhanced soldier caste differentiation. When applied alone, however, SHE had no impacts on caste differentiation, survivorship, or any other aspect of worker biology. These findings support that soldier-derived chemicals serve as primer pheromones which enhance the action of the endogenous morphogenetic hormone JH.Thus, SHE chemicals apparently have no effect when received under natural conditions by non-receptive individuals with presumably low JH titers. Gas chromatography-mass spectrometry analysis identified two terpenes as the most plentiful components of R.flavipes SHE. Through GC-MS and NMR analyses, these terpenes were identified as γ-cadinene and its corresponding aldehyde, γ-cadinenal. Validative bioassays with commercially available cadinene confirmed its activity. However, several other previously identified terpenes were also significantly active. These findings reveal a novel primer pheromone-like function for soldier-derived terpenes in termites, and further suggest convergent evolution of terpene functions in enhancing JH-dependent soldier caste differentiation.

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Section: Nuclear Magnetic Resonance (Nmr) Analysis Nmr Analyses Werementioning

confidence: 99%

“…BioSpin, and that development was funded by a National Institutes of Health grant (P41RR016105) (Brey et al 2006). This work was supported by USDA-CSREES-NRI grant no.…”

Section: Acknowledgements -mentioning

confidence: 99%

Effects of Soldier-Derived Terpenes on Soldier Caste Differentiation in the Termite Reticulitermes flavipes

et al. 2009

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“…23 We thank the staff of the Keys Marine Lab and M. Becerro and R. Ritson-Williams (both Smithsonian Marine Station) for assistance with collections. K.A.A.…”

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Total Structure Determination of Grassypeptolide, a New Marine Cyanobacterial Cytotoxin

et al. 2008

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A collection of the cyanobacterium Lyngbya confervoides off Grassy Key in Florida yielded grassypeptolide (1), a 31-membered macrocyclic depsipeptide with unusually high D-amino acid content, two thiazolines, and one -amino acid. We report the rigorous 3D structure determination and conformational analysis in solution and solid state by NMR, MS, X-ray crystallography, chemical degradation, and molecular modeling involving distance geometry and restrained molecular dynamics. Grassypeptolide (1) inhibited cancer cell growth with IC 50 values from 1.0 to 4.2 µM.Marine cyanobacteria continue to be a rich source of novel bioactive metabolites, including many cytotoxins predominantly originating from Lyngbya majuscula. 1 Other Lyngbya species are less explored. Recently, we have focused our efforts on marine cyanobacteria in Florida waters and reported several potent elastase inhibitors from Lyngbya conferVoides. 2 Here, we describe the cytotoxicity-guided isolation of a new cytotoxic depsipeptide, grassypeptolide (1), from an extract of another L. conferVoides collected in the Florida Keys. This cyanobacterium was of interest because it inhibited settlement of coral larvae (Porites asteroides) and reduced survival of coral recruits. 3 Grassypeptolide (1) contains some unusual residues, such as the -amino acid 2-methyl-3-aminobutyric acid (Maba, C1-5) and 2-aminobutyric acid (Aba, C20-23). Until now, the Aba unit had precedence only in sponge metabolites, 4 whereas the Maba unit was found in one other cyanobacterial compound, guineamide B. 5 Additionally, compound 1 consists of an unusually high number of D-amino acid units.

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“…Furthermore, it has been difficult to obtain adequate amounts of proteins with high molecular weight, many protein complexes, and especially membrane proteins for structural analysis because they can form insoluble aggregates (14). We here report design and fabrication of a microdevice that can analyze nanomole quantities of proteins (15)(16)(17)(18)(19), and that can be integrated in microfabricated systems.The ultimate sensitivity limit is a single spin. Single-electron spins have been detected by using mechanical oscillations (20) and by single nuclear spins using optical methods (21,22).…”

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Ultra-small-sample molecular structure detection using microslot waveguide nuclear spin resonance

Maguire

Chuang

Zhang

et al. 2007

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

102

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We here report on the design of a planar microslot waveguide NMR probe with an induction element that can be fabricated at scales from centimeters to nanometers to allow analysis of biomolecules at nano-or picomole quantities, reducing the required amount of materials by several orders of magnitude. This device demonstrates the highest signal-to-noise ratio for a planar detector to date, measured by using the anomeric proton signal from a 15.6-nmol sample of sucrose. This probe had a linewidth of 1.1 Hz for pure water without susceptibility matching. Analysis of 1.57 nmol of ribonuclease-A shows high sensitivity in one-and twodimensional NMR spectra. Along with reducing required sample volumes, this integrated geometry can be packed in parallel arrays and combined with microfluidic systems. Further development of this device may have broad implications not only for advancing our understanding of many intractable protein structures and their folding, molecular interactions, and dynamic behaviors, but also for high-sensitivity diagnosis of a number of protein conformational diseases.inductive microslot ͉ miniature probe fabrication ͉ nanomole RNAase-A structural detection ͉ nuclear magnetic resonance scaling ͉ ultra-sensitivity N uclear magnetic resonance (NMR) is a powerful analytical tool not only for determining complex biomolecular structures (1-4) but also for monitoring molecular dynamics (5-7). Despite its versatility, NMR protein and large-molecule structural analyses currently require large quantities of protein material at high concentration and purity (8-10), and timeconsuming data gathering (11-13). Furthermore, it has been difficult to obtain adequate amounts of proteins with high molecular weight, many protein complexes, and especially membrane proteins for structural analysis because they can form insoluble aggregates (14). We here report design and fabrication of a microdevice that can analyze nanomole quantities of proteins (15)(16)(17)(18)(19), and that can be integrated in microfabricated systems.The ultimate sensitivity limit is a single spin. Single-electron spins have been detected by using mechanical oscillations (20) and by single nuclear spins using optical methods (21,22). For a volume on the order of Ϸ10 8 spins, a report of a novel semiconductor detection mechanism shows electronic detection of small quantities of spin 3/2 nuclei at the nanoscale (23). However, all of these techniques require low temperatures. For liquid samples at room temperature, pioneering work on fabrication of solenoids around capillary tubes (16, 24) and microfabrication techniques to create planar coils on semiconductor substrates (1, 25) demonstrates that miniaturization of probes is possible and substantially reduces sample quantity while retaining signal sensitivity (15). Solenoidal microcoils detect nanomole quantities with high sensitivity but have not been successfully fabricated below Ϸ300 m inner diameter (26), whereas planar coils on semiconductor substrates are scalable but show lower signal sensitivit...

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Design, construction, and validation of a 1-mm triple-resonance high-temperature-superconducting probe for NMR

Cited by 117 publications

References 12 publications

Effects of Soldier-Derived Terpenes on Soldier Caste Differentiation in the Termite Reticulitermes flavipes

Effects of Soldier-Derived Terpenes on Soldier Caste Differentiation in the Termite Reticulitermes flavipes

Total Structure Determination of Grassypeptolide, a New Marine Cyanobacterial Cytotoxin

Ultra-small-sample molecular structure detection using microslot waveguide nuclear spin resonance

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