Two sensitive methods have been proposed For spectrophotometric determination pure form of Doxycycline (Dox) and in its pharmaceutical preparation. The procedures based on the oxidation of the Doxycycline in acidic media by Fe(III). The results Fe(II) reacted with 1,10- phenanthroline in Method A, and the ferroin complex can measure at 510 nm versus the blank of reagent. While method B depends on the reaction of 2,2'-bipyridyl with the resulted Fe(II) to form a stable coloured complex with maximum 522 nm absorption against reagent blank. Beer's law is applicable in the range of 0.1-9.00 μg/ml and 0.15-4.50 μg/ml concentration with molar absorption of 8.25×104 and 7.53×104 l.mol-1.cm-1 for method A and B, respectively. For both processes, the mean percentage of recoveries is 99.9 per cent and 98.5% respectively. The suggested methods are free from interferences from common excipients. The proposed methods compared favourably with the official and other spectrophotometric methods.