Development of analytical method for determination of 1,3-dimethylamylamine in sports nutrition and bodybuilding supplements using pH-switchable deep eutectic solvents followed by high-performance liquid chromatography-diode array detector

Abstract

In this work, an easy, safe, simple, and efficient pH-switchable deep eutectic solvents (DESs)-based liquid phase microextraction followed by high-performance liquid chromatography-diode array detector analysis was developed for the determination of 1,3-dimethylamylamine (DMAA). The switchability of the obtained DESs was investigated by changing the pH. Then the best-selected DES was characterized and the application of the selected DES in the extraction of DMAA from sports nutrition and bodybuilding supplements was investigated. The DES synthesized from l-menthol: oleic acid in a molar ratio of 1:2 had the highest efficiency in the extraction of the target compound. Under the optimum conditions, (50 µL of DES, 100 µL of 4 mol/L KOH, 100 µL of 4 mol/L HCl, extraction time of 40 s and without salt addition) the calibration graph was linear in the range of 0.05–100 µg/kg and limit of detection was 0.02 µg/kg. The relative standard deviations including intra-day and inter-day for 10.0 µg/kg of DMAA in real samples were 2.7% (n = 7) and 5.3% (n = 7), respectively. The enrichment factor and percentage extraction recovery of the method were 283 and 85%, respectively. The relative recoveries for DMAA in different samples were in the range of 90%–109%.