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Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. I. Method development and optimization.
J Chromatogr A. 2007 Apr 20; 1147(2):213-23.JC

Abstract

An analytical method for the determination of volatile and semi-volatile compounds representing various chemical groups in ice wines was developed and optimized in the presented study. A combination of the fully automated solid-phase microextraction (SPME) sample preparation technique and gas chromatographic-mass spectrometric (GC-MS) system to perform the final chromatographic separation and identification of the analytes of interest was utilized. A time-of-flight mass spectrometric (TOF-MS) analyzer provided very rapid analysis of this relatively complex matrix. Full spectral information in the range of m/z 35-450 was collected across the short GC run (less than 5 min). Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) 50/30 microm fiber performed best during the optimization experiments and it was used in the headspace SPME mode to isolate compounds from ice wine samples, consisting of 3 mL wine with 1g salt addition. After the sample incubation and extraction (both 5 min at 45 degrees C), analytes were thermally desorbed in the GC injector for 2 min (injector maintained at 260 degrees C) and transferred into the column. The MS data acquisition rate of 50 spectra/s was selected as optimal. The optimized analytical method did not exceed 20 min per sample, including both the isolation and pre-concentration of the analytes of interest, the final GC-TOF-MS analysis and the fiber bake-out. Both a linear temperature-programmed retention index (LTPRI) method using C(8)-C(20) alkanes loaded onto the fiber and a mass spectral library search were employed to identify the target compounds. The repeatability of the developed and optimized HS-SPME-GC-TOF-MS method for ice wine analysis, expressed as relative standard deviation (RSD, %, n=7), ranged from 3.2 to 9.0%.

Authors+Show Affiliations

University of Waterloo, 200 University Avenue West, Waterloo, Ontario N2L 3G1, Canada.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

17359985

Citation

Setkova, Lucie, et al. "Rapid Headspace Solid-phase Microextraction-gas Chromatographic-time-of-flight Mass Spectrometric Method for Qualitative Profiling of Ice Wine Volatile Fraction. I. Method Development and Optimization." Journal of Chromatography. A, vol. 1147, no. 2, 2007, pp. 213-23.
Setkova L, Risticevic S, Pawliszyn J. Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. I. Method development and optimization. J Chromatogr A. 2007;1147(2):213-23.
Setkova, L., Risticevic, S., & Pawliszyn, J. (2007). Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. I. Method development and optimization. Journal of Chromatography. A, 1147(2), 213-23.
Setkova L, Risticevic S, Pawliszyn J. Rapid Headspace Solid-phase Microextraction-gas Chromatographic-time-of-flight Mass Spectrometric Method for Qualitative Profiling of Ice Wine Volatile Fraction. I. Method Development and Optimization. J Chromatogr A. 2007 Apr 20;1147(2):213-23. PubMed PMID: 17359985.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. I. Method development and optimization. AU - Setkova,Lucie, AU - Risticevic,Sanja, AU - Pawliszyn,Janusz, Y1 - 2007/02/24/ PY - 2006/10/17/received PY - 2007/01/06/revised PY - 2007/02/15/accepted PY - 2007/3/16/pubmed PY - 2007/6/1/medline PY - 2007/3/16/entrez SP - 213 EP - 23 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1147 IS - 2 N2 - An analytical method for the determination of volatile and semi-volatile compounds representing various chemical groups in ice wines was developed and optimized in the presented study. A combination of the fully automated solid-phase microextraction (SPME) sample preparation technique and gas chromatographic-mass spectrometric (GC-MS) system to perform the final chromatographic separation and identification of the analytes of interest was utilized. A time-of-flight mass spectrometric (TOF-MS) analyzer provided very rapid analysis of this relatively complex matrix. Full spectral information in the range of m/z 35-450 was collected across the short GC run (less than 5 min). Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) 50/30 microm fiber performed best during the optimization experiments and it was used in the headspace SPME mode to isolate compounds from ice wine samples, consisting of 3 mL wine with 1g salt addition. After the sample incubation and extraction (both 5 min at 45 degrees C), analytes were thermally desorbed in the GC injector for 2 min (injector maintained at 260 degrees C) and transferred into the column. The MS data acquisition rate of 50 spectra/s was selected as optimal. The optimized analytical method did not exceed 20 min per sample, including both the isolation and pre-concentration of the analytes of interest, the final GC-TOF-MS analysis and the fiber bake-out. Both a linear temperature-programmed retention index (LTPRI) method using C(8)-C(20) alkanes loaded onto the fiber and a mass spectral library search were employed to identify the target compounds. The repeatability of the developed and optimized HS-SPME-GC-TOF-MS method for ice wine analysis, expressed as relative standard deviation (RSD, %, n=7), ranged from 3.2 to 9.0%. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17359985/Rapid_headspace_solid_phase_microextraction_gas_chromatographic_time_of_flight_mass_spectrometric_method_for_qualitative_profiling_of_ice_wine_volatile_fraction__I__Method_development_and_optimization_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(07)00329-9 DB - PRIME DP - Unbound Medicine ER -