title: Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry.
abstract: A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d(2)-pyrroline (2AP-d(2)), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n=10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r(2)=0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g(-1) of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars.
authors.affiliation: UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5, France.
authors.forename: Isabelle
authors.initials: I
authors.lastname: Maraval
authors.forename: Kemal
authors.initials: K
authors.lastname: Sen
authors.forename: Abdelhamid
authors.initials: A
authors.lastname: Agrebi
authors.forename: Chantal
authors.initials: C
authors.lastname: Menut
authors.forename: Alain
authors.initials: A
authors.lastname: Morere
authors.forename: Renaud
authors.initials: R
authors.lastname: Boulanger
authors.forename: Frédéric
authors.initials: F
authors.lastname: Gay
authors.forename: Christian
authors.initials: C
authors.lastname: Mestres
authors.forename: Ziya
authors.initials: Z
authors.lastname: Gunata
mesh_terms: D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D012275:Oryza / Q000737:chemistry*; D011758:Pyrroles / Q000032:analysis* / Q000138:chemical synthesis / Q000302:isolation & purification; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D011758:Pyrroles; C426303:2-acetyl-1-pyrroline