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A high-performance liquid chromatographic method, coupled with UV detection and electrospray ionization mass spectrometry (HPLC—UV-ESI-MS), is developed for the simultaneous determination of the illegal additives sibutramine and its metabolite  N -di-desmethylsibutramine in dietary supplements for weight control. The separation is achieved on a Spherisorb C8 reversedphase column, employing acetonitrile and an aqueous 0.2% formic acid solution containing 20mM ammonium acetate as mobile phases in a gradient mode. UV detection is used for quantitation at a wavelength of 223 nm. Identification of target compounds is completed by ESI-MS using selected ion recording at  m/z  280 for sibutramine and  m/z  252 for  N -di-desmethylsibutramine. Calibration curves are linear over the range of 0.025–1.0 mg/mL for sibutramine and  N -di-desmethylsibutramine. Correlation coefficients are better than 0.9990. The intra- and inter-day precision and accuracy for sibutramine and  N -didesmethylsibutramine are acceptable. The method is successfully applied to the analysis of natural dietary supplement samples.

Simultaneous Determination of Sibutramine and N -Di-desmethylsibutramine in Dietary Supplements for Weight Control by HPLC—ESI-MS