Abstract New, rapid and sensitive spectrophotometric method have been developed for the determination of Hostacycline (HTC) and Doxycycline (DC). The procedure is based on the observation that, HTC and OTC form coloured complexes with Chromium(VI). The absorbance of which is proportional to the amount of tetracycline present. The variables affecting development of the colour have been investigated and conditions are optimized. Beer’s law is obeyed in the range 0.01 to 0.06 mg/ml for HTC and 0.01 to 0.08 mg/ml for DC. The proposed can be employed for the analytical determination of Chromium(VI). The present methods are successfully applied for the determination of HTC and DC in pharmaceutical formulation.