Phosphonosphingolipids from 15 kinds of shellfish were analyzed by fast atom bombardment mass spectrometry to determine the contents of ceramide aminoethylphosphonate (CAEPn) and ceramide N-methylaminoethylphosphonate (CMAEPn). Two pairs of ions, at m/z 126 and 140 in the positive ion mode and at m/z 124 and 138 in the negative ion mode, were used to distinguish between aminoethylphosphonic acid and N-methylaminoethylphosphonic acid in CAEPn and CMAEPn. Interestingly, mollusca in the early stage of evolution have both CAEPn and CMAEPn, while most in the middle stage have only CMAEPn and those in the highest stage have only CAEPn.