Ionic cross-linking of sodium carboxymethyl guar gum as a mild method for microencapsulation of sensitive drugs, like proteins, is presented. When a solution of sodium salt of carboxymethyl guar gum, containing BSA as a model drug, is added, as droplets, to different multivalent metal ion solutions, they get cross-linked to form insoluble microbeads. The amount of protein retained, morphology of the resulting beads and the subsequent release of the retained protein is simulated intestinal fluids varied with the type of metal ion as well as it's concentration. Trivalent metal ions like Al +++ and Fe +++ were found to be superior to divalent metal ions like Ba ++, Ca ++, Cu ++ and Cd ++ . The optimum concentration around which these ions provide maximum drug retention was found to be much lower for trivalent ions. Beads cross-linked with them released the protein over a longer duration in enzyme free simulated intestinal fluid, than those cross-linked with divalent ions. Mg ++, Sr ++, Co ++ and Zn ++ failed to form isolable beads.