Capillary HPLC−NMR Coupling: High-Resolution 1H NMR Spectroscopy in the Nanoliter Scale

Autor:	Götz Schlotterbeck, Tony Keller, Ernst Bayer, Li-Hong Tseng, Beate Behnke, Klaus Albert, Sabine Strohschein, Ulrich Tallarek
Rok vydání:	1996
Předmět:	NMR spectra database Detection limit Chromatography Resolution (mass spectrometry) Deuterium Chemistry Capillary action Analytical chemistry Proton NMR Transverse relaxation-optimized spectroscopy High-performance liquid chromatography Analytical Chemistry
Zdroj:	Analytical Chemistry. 68:1110-1115
ISSN:	1520-6882 0003-2700
DOI:	10.1021/ac950925a
Popis:	Coupling HPLC and NMR is one of the most powerful techniques for simultaneous separation and structural elucidation of unknown compounds in mixtures. To date, however, minimizing the detection volume, as is required when coupling NMR with miniaturized separation techniques, has been accompanied by a dramatic loss in resolution of the NMR spectra. Here, we report on the coupling of gradient capillary HPLC with on-column, high-resolution NMR detection. On-line stopped-flow and static (1)H NMR spectra were acquired with capillary columns of 75-315 μm i.d. With detection over a length of 1.2 cm, cell volumes cover a range of 50-900 nL. An on-line-detected NMR separation of dansylated amino acids was carried out in a 315 μm i.d. fused silica capillary packed to a length of 12 cm with C(18) stationary phase. The low solvent consumption makes the use of fully deuterated solvents economically feasible. NMR spectra with resolution on the order of 3 Hz were obtained using a 50 nL detection cell to measure 1.1 nmol of dansylated γ-aminobutyric acid under static conditions in a 75 μm i.d. capillary.
Databáze:	OpenAIRE
Externí odkaz:	https://explore.openaire.eu/search/publication?articleId=doi_dedup___::cc8eeb7d555378c3562121f83717fff0 https://doi.org/10.1021/ac950925a Zobrazit plný text záznamu