Simultaneous Determination of Clomiphene, Trimetazidine and Meldonium in Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Pass-Through Solid Phase Extraction

Abstract

In this study, we established a method for the determination of three metabolic regulators including clomiphene, trimetazidine and meldonium in foods by pass-through solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The samples were extracted with 5% formic acid in acetonitrile, and the extract was purified on a pass-through solid phase extraction column and chromatographically separated on an amide column (3.0 mm × 100 mm, 1.7 μm). The separated analytes were detected in the multiple reaction monitoring (MRM) mode, and quantitated by an internal standard method. Good linearity was observed for clomiphene and trimetazidine within the concentration range of 1.0-40.0 ng/mL, and 5.0-200.0 ng/mL for meldonium. The average recoveries for spiked samples ranged from 81.3% to 100.7%, and the relative standard deviations (RSD) were between 0.3% and 6.1% (n = 6). The developed method was simple, rapid and practical with low matrix interferences, and was generally suitable for the determination of clomiphene, trimetazidine and meldonium in foods, which could provide effective technical support for the assurance of food safety for sports events.

Keywords

• clomiphene; trimetazidine; meldonium; ultra-high performance liquid chromatography-tandem mass spectrometry; solid phase extraction