Thick-film capillary column gas chromatography—field ionization mass spectrometry : A complementary technique for the rapid analysis of volatiles

✍ Scribed by John M. Halket; Hans-Rolf Schulten

• Publisher: Elsevier Science
• Year: 1985
• Tongue: English
• Weight: 380 KB
• Volume: 322
• Category: Article
• ISSN: 1873-3778
• DOI: 10.1016/s0021-9673(01)97672-1

✦ Synopsis

The properties of field ionization (FI) mass spectrometry (MS) in providing molecular ion spectra and strongly reduced fragmentation have been known for many years'. Damico and Barron first demonstrated the utility of gas chromatography (GCEFIMS in the analysis of volatile natural products in spite of the sensitivity disadvantages over electron impact (EI)MS. Several years later, Milberg and Cook3 reported the packed column GC-FI mass spectra of pesticides and drugs.

Recent studies have shown pyrolysis (By) capillary column GC-FIMS4 to be a powerful technique in complementing the direct characterization of tobacco by Py-FIMS and factor analysi@. The present paper demonstrates for the first time the combined capillary column GC-FIMS technique. The method is illustrated by injection of essential oils on to a thick-film capillary column connected directly to a commercially available mass spectrometer ion source.

MATERIALS AND METHODS

Essential oils

Orange oil samples (Florida and California) were obtained from Orissa Drebing, Hamburg, F.R.G. A perfume sample from the desert flower purple sage was purchased from commercial sources in Albuquerque, NM, U.S.A.

Gas chromatography

A Varian 3700 gas chromatograph was employed equipped with a Gerstel (Labormechanik Gerstel, Miilheim/Ruhr, F.R.G.) split/splitless injector. The fusedsilica capillary column, chemically bonded with CpSil5 phase (1.25 m film thickness; Chrompack, Middelburg, The Netherlands) had dimensions 26 m x 0.32 mm I.D. and was programmed from 100°C to 250°C at lO"C/min. The helium carrier gas pressure was 1 bar, the split vent was set at 20 ml/mm and 0.5 ~1 of each oil was