title: Hyphenation of gas chromatography to microcoil 1H nuclear magnetic resonance spectroscopy.
abstract: 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.
authors.affiliation: Institute of Organic Chemistry, Chemisches Zentral-Institut, University of Tübingen, Auf der Morgenstelle 18, 72076 Tuebingen, Germany.
authors.forename: Marc David
authors.initials: MD
authors.lastname: Grynbaum
authors.forename: Diana
authors.initials: D
authors.lastname: Kreidler
authors.forename: Jens
authors.initials: J
authors.lastname: Rehbein
authors.forename: Armin
authors.initials: A
authors.lastname: Purea
authors.forename: Paul
authors.initials: P
authors.lastname: Schuler
authors.forename: Walter
authors.initials: W
authors.lastname: Schaal
authors.forename: Harri
authors.initials: H
authors.lastname: Czesla
authors.forename: Andrew
authors.initials: A
authors.lastname: Webb
authors.forename: Volker
authors.initials: V
authors.lastname: Schurig
authors.forename: Klaus
authors.initials: K
authors.lastname: Albert
mesh_terms: 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
chemical_list: D005663:Furans; D011522:Protons; D004986:Ether; D000096:Acetone; C018674:tetrahydrofuran; D008752:Methylene Chloride