Abstract

In this work, we developed an analytical method for determining 11 illicit compounds in dietary supplements using high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry. Eleven target compounds, including those meant for weight loss (7-keto-dihydroepiandrosterone, buformin, metformin, phenformin, salbutamol, and tolbutamide), sexual enhancement (dihydroepiandrosterone), and relaxation (asarone, kavain, magnoflorine, and picamilon) were screened and confirmed in dietary supplements. Method validation was performed by evaluating the selectivity, linearity, limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was > 0.993 for all analytes. The LOQs were ranged in 2.1-9.9 μg/mL (HPLC-DAD) and 0.002-0.008 μg/mL (LC-MS/MS). The accuracies (expressed as recovery) were 90.0-106% (HPLC-DAD) and 83.0-114% (LC-MS/MS). The precision (expressed as the relative standard deviation) was below 10% using HPLC and LC-MS/MS. The proposed method can be used for the surveillance of illicit compounds in dietary supplements.

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