Simultaneous determination of sibutramine and N-Di-desmethylsibutramine in dietary supplements for weight control by HPLC-ESI-MS.
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.
Huang
Ziqiang
Z
State Key Laboratory of Chemo/Biological Sensing & Chemometrics, Hunan University, Changsha 410082, PR China.
Xiao
Song
S
Luo
Dan
D
Chen
Bo
B
Yao
Shouzhuo
S
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003503:Cyclobutanes / Q000032:analysis*; D019587:Dietary Supplements / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet
D003503:Cyclobutanes; C058254:sibutramine