An effective method for preparing Maillard reaction intermediate (MRI) derived from xylose (Xyl) and phenylalanine (Phe) in aqueous medium was proposed in this study.

The synergistic effect of a thermal reaction and vacuum dehydration on the conversion of xylose (Xyl) and phenylalanine (Phe) to a Maillard-reaction intermediate (MRI) was researched. The yield of N-(1-deoxy-α-d-xylulos-1-yl)-phenylalanine was successfully improved and increased from 13.62 to 47.23% through the method combining a thermal reaction and vacuum dehydration. A dynamic process was involved in the transformation of Xyl and Phe (Xyl-Phe) to N-substituted d-xylosamine and in the transformation of N-substituted d-xylosamine to N-(1-deoxy-α-d-xylulos-1-yl)-phenylalanine during the initial stage of dehydration; then, only the transformation of N-substituted d-xylosamine to N-(1-deoxy-α-d-xylulos-1-yl)-phenylalanine occurred during the final stage. Furthermore, the MRI was prepared under optimized conditions (90 °C and pH 7.4), and the obtained MRI was characterized and confirmed by ESI mass spectrometry and NMR.

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