Development of a pair of differential H/D isotope-coded derivatization reagents d0/d3-4-(1-methyl-1H-phenanthro[9,10-d]imidazol-2-yl) phenlamine and its application for determination of aldehydes in selected aquatic products by liquid chromatography-tandem mass spectrometry.

A new pair of derivatization reagents, d(0)-4-(1-methyl-1H-phenanthro[9,10-dlimidazol-2-yl)phenlamine (d(0)-MPIA) and d(3)-4-(1-methyl-1H-phenanthro[9,10-d]imidazol-2-yl)phenlamine (d(3)-MPIA) have been designed and synthesized. It was successfully used to label aliphatic aldehydes and the aldehyde derivatives were analyzed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The new isotope-coded reagents could easily label aldehydes under acidic conditions in the presence of NaCNBH3. The target derivatives exhibited intense [M+H](+) and regular product ions with electrospray ionization source in positive mode. The d(0)/d(3)-MPIA-aldehydes were monitored by the transitions of [M+H](+) -> m/z 322 and [M+H](+) -> m/z 165, and the obtained detection limits were in the range of 0.18-15.9 pg/mL at signal to noise ratio of 3. The global isotope internal standard technology was employed for quantification analysis with d(3)-MPIA-aldehyde as internal standard for corresponding d(0)-MPIA-aldehyde. Excellent linear responses for relative quantification were observed in the range of 1/10-10/1 with coefficients > 0.998. The developed method has been applied to the quantification of aliphatic aldehydes in selected aquatic products with RSD <3.6% and recoveries > 85.2%. (C) 2013 Elsevier B.V. All rights reserved.