Abstract: A rapid screening method was developed to determine sibutramine and five derivatives in health food by high performance liquid chromatography-quadrupole/electrostatic orbitrap high-resolution mass spectrometry (HPLC-Q/Orbitrap HRMS). The sample was extracted with methanol via ultrasonic-assisted extraction coupled with high-speed centrifugation. Separation was performed on a Hypersil Gold column (100 mm×2.1 mm, 3 μm) by gradient elution with methanol/water (containing 0.15%(v/v) formic acid) as the mobile phase. The positive full mass scan/date-dependent MS² (Full MS/dd-MS²) mode was used during MS detection, and quantification was achieved by resolution of the precursor mass. The analytes in the sample were separated, and accurate mass and MS² fragment ions were simultaneously attained within 8 min. The results indicated that the obtained mass accuracy errors of the six analytes were less than 1×10^-6. Good linearities were obtained in the range of 0.5-20.0 μg/L, and all correlation coefficients were higher than 0.999. The limits of quantification were 25 μg/kg and the recoveries were in the range of 93.5%-103.5% with relative standard deviations of 1.5%-7.7%. This simple-pretreatment, rapid, accurate, high-sensitivity, and high-selectivity method can be used in the rapid screening and quantitative analysis of sibutramine and its derivatives in health food.

Key words: high performance liquid chromatography (HPLC), quadrupole/electrostatic orbitrap high-resolution mass spectrometry (Q/Orbitrap HRMS), sibutramine, derivatives, health food