Abstract: Compound preparations of ethinyloestradiol are widely use in contraceptive drugs, but the ethinyloestradiol content in the preparations is less than 35 μg per tablet. The content was too low to be determined directly by the normal methods. A HPLC method has been developed for determination of ethinyloestrodiol norethisterone and norgestrel acetate in the compound preparations after separation by μ-Bodapak ODS columnn with methaqualone as internal standard and MeOH—H₂O (130:100) as a mobile phage using a UV—Fluorescence (FL) combination detector. For the detection of ethinyloestrodiol FL was used and for all other drugs UV was usedThe UV-FL combined detection is favourable to overcome the difficulties of relatively low content in the Preparation and low absorptivity of the minor component.This method is accurate, rapid, sensitive and has a good linearity and suitable to various preparations.