Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
46, Number 8, September 2008, pp. 707-711
Simultaneous Determination of Sibutramine and
N-Di-desmethylsibutramine in Dietary Supplements for Weight Control
by HPLC–ESI-MS
Ziqiang Huang1,2, Song Xiao2,
Dan Luo2, Bo
Chen2, and Shouzhuo Yao1,2, 1State Key Laboratory of Chemo/Biological Sensing & Chemometrics,
Hunan University, Changsha 410082, PR China; 2Key Laboratory
of Chemical Biology & Traditional Chinese Medicine Research,
Ministry of Education, Hunan Normal University, Changsha 410081,
PR China
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 reversed-phase 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-di-desmethylsibutramine
are acceptable. The method is successfully applied to the analysis
of natural dietary supplement samples.
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