Rapid and sensitive detection of Amadori compounds was achieved by high performance anion exchange chromatography (HPAEC) coupled with a pulse amperometric detector (PAD). Several Amadori compounds were separated, such as fructosyl proline (Fru-Pro), fructosyl glycine (Fru-Gly), fructosyl valine (Fru-Val), fructosyl isoleucine (Fru-Ile), and fructosyl methionine (Fru-Met). The HPAEC–PAD method is suitable for high-throughput routine analysis of Amadori compounds in complex reaction systems such as the Maillard reaction. It was used to monitor the formation of Fru-Pro from glucose and proline in methanol resulting in a continuous increase with about 30 g Fru-Pro/mol glucose after a reaction period of 5 h. Another application included monitoring of Fru-Gly. The rate of Fru-Gly degradation increased with increasing pH. Phosphate accelerated the degradation of Fru-Gly, particularly in the pH range 5–7.