Hyphenation of gas chromatography to microcoil 1H nuclear magnetic resonance spectroscopy.
Whereas the hyphenation of gas chromatography (GC) with mass spectrometry is of great importance, little is known about the coupling to nuclear magnetic resonance spectroscopy (NMR). The investigation of this technique is an attractive proposition because of the valuable information given by NMR on molecular structure. The experiments shown here are to our knowledge the first hyphenating capillary GC to microcoil NMR. In contrast to liquids, gases have rarely been investigated by NMR, mainly due to the experimental difficulties in handling gases and the low signal-to-noise-ratio (SNR) of the NMR signal obtained at atmospheric pressure. With advances in NMR sensitivity (higher magnetic fields and solenoidal microprobes), this limitation can be largely overcome. In this paper, we describe the use of a custom-built solenoidal NMR microprobe with an active volume of 2 microL for the NMR detection of several compounds at 400 MHz, first in a mixture, and then with full coupling to capillary GC to identify them separately. The injected amounts of each analyte in the hyphenated experiments are in the range of 15-50 micromol, resulting in reasonable SNR for sample masses of 1-2 microg.
Grynbaum
Marc David
MD
Institute of Organic Chemistry, Chemisches Zentral-Institut, University of Tübingen, Auf der Morgenstelle 18, 72076 Tuebingen, Germany.
Kreidler
Diana
D
Rehbein
Jens
J
Purea
Armin
A
Schuler
Paul
P
Schaal
Walter
W
Czesla
Harri
H
Webb
Andrew
A
Schurig
Volker
V
Albert
Klaus
K
D000096:Acetone / Q000032:analysis; D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods; D004986:Ether / Q000032:analysis; D005663:Furans / Q000032:analysis; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation* / Q000379:methods*; D008752:Methylene Chloride / Q000032:analysis; D011522:Protons; D012680:Sensitivity and Specificity
D005663:Furans; D011522:Protons; D004986:Ether; D000096:Acetone; C018674:tetrahydrofuran; D008752:Methylene Chloride