Abstract: α-cyano-ferulic acid(CFA)and 2,5-dihydroxybenzoic acid (DHB)were used as matrices to determineβ-cyclodextrin, saccharide A from animal, saccharide B from plant an dextrans by MALDI-TOF-MS. The results showed that CAF could make some analytes desorbed and ionized more easliy and getting better reproducibility than DHB.