Development and validation of a high-performance thin-layer chromatography method for detection of sibutramine in dietary supplements

Abstract

Introduction: In the period between 1997 and 2010, sibutramine-containing drugs were widely prescribed for obesity and over-weight management. Due to safety concerns, in 2010 all medicines containing sibutramine were urgently withdrawn from the USA and European pharmaceutical market. Although sibutramine is no longer available in pharmaceutical products, there have been numerous reports of mislabeled weight-loss dietary supplements containing sibutramine. Aim: This work aimed to develop and validate an accurate and sensitive high-performance thin-layer chromatographic method for the detection of sibutramine. Materials and methods: The method was developed using a CAMAG HPTLC system. Silica gel 60 F254 aluminum HPTLC plates were used as stationary phase and toluene:ethyl acetate:methanol (7:2:1 v/v/v) as mobile phase. Results: The calibration curve was built in the range of 0.250–1.250 μg/band. The method provided satisfactory linearity, specificity, precision, and accuracy. The LOD and the LOQ were 0.0765 μg/band and 0.2318 μg/band, respectively. Conclusions: The method allows for the simultaneous analysis of multiple samples as well as the rapid and sensitive monitoring of sibutramine levels in dietary supplements.