Two new derivatives are described that confer electron-capturing properties to hydroxyl-containing steroids. The 9-H-hexadecafluoronanoate (HFN) and 11-H-eicosafluoroundecanoate (EFU) derivative of testosterone have 2.30 and 2.55 times the area response of equimolar amounts of testosterone heptafluorobutyrate, as well as longer retention times on both polar and nonpolar phases. Thin-layer and GLC properties of the 17-mono-derivatives and the 3,17-di-derivatives of estradiol are presented. Using the HFN derivative, a simplified method is presented for the measurement of testosterone in human plasma. © 1969.