A sensitive fluorometric method using 9-fluorenylmethyl pentafluorophenyl carbonate (FMPC) as the fluorescent labeling agent was developed to determine D-penicillamine (D-PA). The fluorophore had excitation and emission wavelengths of 260 nm and 313 nm, respectively. After derivatization, the fluorescent product was separated, and quantified by spectrofluorometry. The derivative was highly fluorescent and stable. Optimum condition for the reaction was investigated. A linear response was obtained over the range of $4.0{ imes}10^{-7}-5.0{ imes}10{-6};M$ with the correlation coefficient of 0.999 (n=6). The procedure described was successfully applied to the determination of the dosage forms of capsule with the recovery of $98.62{pm}0.57%$ (150 mg), $98.36{pm}0.57%$, (250 mg).