A stable isotope dilution assay was developed for the quantitation of the hazelnut odorant 5-methyl-(E)-2-hepten-4-one by mass chromatography using synthesized [(2)H](2)-5-methyl-(E)-2-hepten-4-one as the internal standard. Application of the method on two batches of commercial hazelnut oils, processed from either roasted or unroasted nuts, revealed 6.4 microg 5-methyl-(E)-2-hepten-4-one per kg of unroasted oil whereas 315.8 microg per kg was determined in the roasted nut oil. The about 50-fold higher amount of 5-methyl-(E)-2-hepten-4-one in roasted hazelnut oil suggested the necessity of a thermal treatment to generate the flavor compound. Pan frying of raw hazelnuts (9 to 15 min) or boiling of the crushed nut material for 1 h in water led to an increase of 5-methyl-(E)-2-hepten-4-one by factors of 600 and 800, respectively, thereby corroborating that the major part of the nut flavorant is formed during heat treatment from a yet unknown precursor in hazelnuts.
A low-energy, high-repetition-rate picosecond laser (40 μJ, 20 kHz, 258 nm) was used for multiphoton ionization (MPI) in gas chromatography/time-of-flight mass spectrometry to quantitatively determine dioxins (DXNs) and polycyclic aromatic hydrocarbons (PAHs). The sensitivity of the technique was compared with that obtained using a high-energy, low-repetition-rate femtosecond laser (86 μJ, 1 kHz, 261 nm). The limits of detection (LODs) for the picosecond laser were several femtograms for chlorinated DXNs with low numbers of chloro substituents, and were several times lower than values obtained using a femtosecond laser, although the LODs were increased, reaching values that were nearly identical to those for the femtosecond laser for octachlorodibenzo-p-dioxin (octaCDD) and octachlorodibenzofuran (octaCDF). The LODs were also measured for 16 PAHs specified by the United States Environmental Protection Agency; the values for half of these compounds were at sub-femtogram levels. The procedure was used to analyze a surface-water sample collected from a river.
Particulate matter 2.5 (PM2.5), collected from ambient air in Fukuoka City, was analyzed by gas chromatography combined with multiphoton ionization mass spectrometry using an ultraviolet femtosecond laser (267 nm) as the ionization source. Numerous parent polycyclic aromatic hydrocarbons (PPAHs) were observed in a sample extracted from PM2.5, and their concentrations were determined to be in the range from 30 to 190 pg/m(3) for heavy PPAHs. Standard samples of nitrated polycyclic aromatic hydrocarbons (NPAHs) were examined, and the limits of detection were determined to be in the picogram range. The concentration of NPAH adsorbed on PM2.5 in the air was less than 900-1300 pg/m(3). Graphical Abstract ᅟ.
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