Rapid determination of illegal addition of new high-risk weight loss drugs such as oxyphenisatin dipropionate in enzyme jelly by UPLC-MS/MS
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the rapid determination of weight loss drugs including oxyphenisatin dipropionate,diaotyldiphenolisatinum and bisoxatin in enzyme jellies. Enzyme jellies samples were extracted using an ultrasonic extraction method with an aqueous methanol solution containing 0.1％ formic acid,Chromatographic separation was achieved on a BEH C18 column (100 mm × 2.1 mm,1.7 μm) with a mobile phase of acetonitrile and 0.1％ formic acid in water via gradient elution. Samples were then detected by UPLC-MS/MS multi-reaction monitoring (MRM) mode and quantification was carried out using external standards. The chromatographic separation conditions,mass spectrometry fragmentation voltage and collision energy were optimized,and effects of extraction time and solvent on recovery were investigated. Results indicated that the three compounds showed good linear relationships within the range of 1～100 ng/mL,with correlation coefficients exceeding 0.999. The limit of detection (LOD) was 20 μg/kg and the limit of quantitation (LOQ) was 50 μg/kg. The recoveries of the three compounds ranged from 82.6％ to 94.2％,with relative standard deviations between 1.3％～7.8％. This method was simple,rapid,sensitive,and provides accurate qualitative and quantitative results,making it suitable for detecting novel high-risk weight-loss drugs such as oxyphenisatin dipropionate in enzyme jellies.
oxyphenisatin dipropionateultra performance liquid chromatography-tandem mass spectrometryenzyme jellyrapid determinationweight-loss drugs
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