| Abstract: | An extremely sensitive method for the analysis of 2‐acetyl‐1‐pyrroline (2AP) in rice, employing stir bar sorptive extraction (Twister) was studied. The Twister stir bar is placed in the headspace of a 20‐mL vial containing 1 g of rice kernels, 7.5 mL of 0.1M KOH, and 2.2 g of NaCl, along with a second Teflon‐coated stir bar for mixing. Analytes are adsorbed onto the Twister for 4 hr at 40°C and then desorbed at 270°C into a GC column while cryofocusing at –80°C. The headspace sorptive extraction (HSSE) method was able to detect <0.1 ppb of 2AP in rice. The precision of the HSSE method (>10%) was not as good as the GC/FID method (≈6%). Using HSSE, 2AP was observed in all samples generally considered to be aromatic and was not observed in any nonaromatic samples. Additionally, a modified method for the synthesis of 2‐acetyl‐1‐pyrroline was studied and the presence of a tautomer of 2‐acetyl‐1‐pyrroline was confirmed. |
