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 |
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Authors: | Isabelle Maraval Kemal Sen Chantal Menut Renaud Boulanger Christian Mestres |
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Affiliation: | a UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5, France b UMR Qualisud, Université Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5, France c UMR 5247, Institut des Biomolécules Max Mousseron (IBMM), CNRS, Universités Montpellier 2 et 1, Ecole Nationale Supérieure de Chimie de Montpellier, 8 Rue de l’Ecole Normale, 34296 Montpellier Cedex 5, France d CIRAD, DORAS Centre, Research and Development Building, Kasetsart University, Bangkok 10900, Thailand e Department of Food Engineering, Faculty of Agriculture, University of Çukurova, 01330 Adana, Turkey |
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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-d2-pyrroline (2AP-d2), 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 (r2 = 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. |
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Keywords: | 2-Acetyl-1-pyrroline Convenient synthesis SIDA HS-SPME GC-MS-MS Rice |
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