Abstract:

A confirmative method was developed for determining β-methylphenethylamine (BMPEA) and picamilon in health products by ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UPLC-Q Trap MS). The sample was ultrasonically extracted with methanol. The purification was carried out on a new reversed phase solid-phase extraction column (PRiME HLB). The detection of compounds was in the positive mode. Multiple technologies were applied to solve the identification and quantification for the two compounds, such as multiple reaction monitoring (MRM), online enhanced product ion full scan (EPI) and library search. Methanol and 0.1% (v/v) formic acid aqueous solution were used as the mobile phases with gradient elution. A SHISEIDO CAPCELL MG Ⅱ C₁₈ column was used to separate the analytes. The LODs and LOQs for BMPEA and picamilon in liquid, table and capsule samples were 0. 2-0.5 μg/kg and 0.5-2.0 μg/kg, respectively. The average spiked recoveries of the method varied from 79.5% to 103.8% and the RSDs were between 3.6% and 15.4%. In the range of 0.2-200.0 μg/kg, the peak areas and concentrations of matrix standard solution showed good linear relationship (r≥0.9969). The qualitative confirmation results were required based on the search-match MRM and EPI mass spectra simultaneously. The method is simple and accurate for the determination of BMPEA and picamilon in imported and commercial health products.

Key words: β-methylphenethylamine (BMPEA), enhanced product ion full scan (EPI), health products, picamilon, solid-phase extraction (SPE), ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UPLC-Q Trap MS)