The analytical problems of dating gypsum speleothems with the U-series technique are reviewed. Gypsum speleothems are, in general, very low in U content, challenging the limits of detection methods. Various approaches to dissolving gypsum and isolation of actinides from the matrix include ion-pairing dissolution with magnesium salts and using nitric acid. The most precise dating technique is Thermal Ionization Mass Spectrometry (TIMS), combined with Fe(OH)3 scavenging and anionic exchange chromatography. Less satisfactory, but much quicker, is direct retention of actinides from HNO3 by means of TRU resin and MC-ICP-MS detection. We have tested these methods on gypsum speleothems from the Sorbas karst in Spain and from the Naica caves in Mexico.