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Isolation of cantharidin from Cyaneolytta sapphirina

Free cantharidin Dried beetles (10 g) in the form of a coarse powder were extracted (18 h) with acetone in a soxhlet apparatus. Removal of acetone gave a dark brown residue (1.6 g), which was dissolved in benzene on a silica gel column (Merck) (0.05-0.2 mm). The column was eluted successively with 200 ml each of benzene, benzene-ether (95: 5, v/v), ether, chloroform, acetone and methanol. The residues from the above fractions weighed 0.13, 0.10, 0.5, 0.06,0.3 and 0.4 g respectively. The presence of free cantharidin in each fraction was detected by thin-layer chromatography on silica gel G (Merck), developed by acetone-benzene (1 : 4, v/v) using cantharidin (BDH) as a reference. The plates were sprayed with 50% H,SO, and heated to 150" in an oven: cantharidin (RF, 0.7) was observed in the benzene-ether eluate and was purified by washing with a small volume of light petroleum+thanol (19: 1) when a microcrystalline powder (3.5 mg) (0.035%) m.p. (214-216") was obtained; sublimation gave colourless needles m.p. 217-21 8".