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A practical analytical method has been developed for the determination of an analog of vitamin D3(Ro 24-2090) in plasma samples. The method employs liquid–liquid extraction, precolumn derivatization, HPLC separation using an automated column-switching system, and particle-beam negative ionization MS determination. An electron-capture derivatization reagent, 4-pentafluorobenzyl-1,2,4-triazoline-3,5-dione,...