A new modified Spectrophotometric procedures are presented for the determination of three pharmaceutical antibiotic compounds through charge-transfere complexation reaction with chloranil. The complex shows an absorption mAxima at 550 nm, having a molar absorptivity coefficient of 5.55×10,7.81×10 and 1.38×10 1. molcm for ampicillin, amoxycillin and neomycin, respectively. Optimization of the reaction conditions has been investigated Obediance to Beer's law (40μg/ml) permitted the assay of thes drugs in its dosage forms A variety of pharmaceutical dosage forms containing ampicillin, amoxycillin and neomycin are successfully analysed by the proposed procedure.