Abstract
The biogenic amines (BAs) synephrine (SNP), phenylephrine (PEP), tyramine (TYR), and octopamine (OCT) may be present in products widely consumed for weight loss, muscle power, and in energy supplements. Considering the toxicity of these BAs at high levels and their biomarker role in some human pathologies, their monitoring in urine can be of great help in the detection of abusive consumption or disease. In this work, a combination of dispersive liquid–liquid microextraction (DLLME) with ultra-high performance liquid chromatography and quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) for the simultaneous determination of four aromatic BAs in human urine is presented. The sample treatment included a previous derivatization step with dansyl chloride to achieve the highest extraction efficiency in the DLLME procedure for which a mixture of 350 μL of chloroform and 2 mL of ethanol was added to 5 mL of derivatized urine. Limits of detection were in the 0.54–3.6 µg L−1 range. Method precision and trueness were estimated at two concentration levels and were in the 3.4–10.2% and 93.6–114% ranges, respectively. The analysis of nine urine samples showed concentration levels for TYR between 52 and 304 µg L−1. Non-targeted analysis of the samples was undertaken to control the presence of other BAs and related metabolites, and none of these species was detected.
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