| Title: | Nanogram-scale preparation and NMR analysis for mass-limited small volatile compounds |
| Author(s): | Nojima S; Kiemle DJ; Webster FX; Apperson CS; Schal C; |
| Address: | "Department of Entomology and WM Keck Center for Behavioral Biology, North Carolina State University, Raleigh, North Carolina, United States of America" |
| DOI: | 10.1371/journal.pone.0018178 |
| ISSN/ISBN: | 1932-6203 (Electronic) 1932-6203 (Linking) |
| Abstract: | "Semiochemicals are often produced in infinitesimally small quantities, so their isolation requires large amounts of starting material, not only requiring significant effort in sample preparation, but also resulting in a complex mixture of compounds from which the bioactive compound needs to be purified and identified. Often, compounds cannot be unambiguously identified by their mass spectra alone, and NMR analysis is required for absolute chemical identification, further exacerbating the situation because NMR is relatively insensitive and requires large amounts of pure analyte, generally more than several micrograms. We developed an integrated approach for purification and NMR analysis of <1 microg of material. Collections from high performance preparative gas-chromatography are directly eluted with minimal NMR solvent into capillary NMR tubes. With this technique, (1)H-NMR spectra were obtained on 50 ng of geranyl acetate, which served as a model compound, and reasonable H-H COSY NMR spectra were obtained from 250 ng of geranyl acetate. This simple off-line integration of preparative GC and NMR will facilitate the purification and chemical identification of novel volatile compounds, such as insect pheromones and other semiochemicals, which occur in minute (sub-nanogram), and often limited, quantities" |
| Keywords: | Acetates/*analysis/*chemistry Acyclic Monoterpenes Limit of Detection Magnetic Resonance Spectroscopy Molecular Weight Nanotechnology/*methods Terpenes/*analysis/*chemistry Volatile Organic Compounds/*analysis/*chemistry Weights and Measures; |
| Notes: | "MedlineNojima, Satoshi Kiemle, David J Webster, Francis X Apperson, Charles S Schal, Coby eng U01 AI058303/AI/NIAID NIH HHS/ 1 U01 AI058303-01/AI/NIAID NIH HHS/ Research Support, N.I.H., Extramural 2011/04/06 PLoS One. 2011 Mar 28; 6(3):e18178. doi: 10.1371/journal.pone.0018178" |
