Mandarin orange fruits were artificially contaminated with an organophosphorus insecticide phenthoate by dipping and the residue level of phenthoate was investigated during the purification steps of dietary fiber or bioflavonoid. The removal rate of phenthoate at 8 and 0.5 ppm levels was 98% in the total dietary fiber, 99% in the insoluble dietary fiber and 99.8% in the soluble dietary fiber preparations. Kuring the preparation of biflavonoid from peels at a 5 ppm pesticide level, the removal rate was 90% in the intermediate extract and 99.9% in the final extract. In conclusion, phenthoate residues in the peels of mandarin orange were mostly removed during the preparation processes of dietary fiber of bioflavonoid and its residue level would not raise any problem in safety aspects of the purified products.