Determination of anabolic androgenic steroids in dietary supplements and external drugs by magnetic solid‐phase extraction combined with high‐performance liquid chromatography–tandem mass spectrometry

Abstract

The widespread abuse of anabolic androgenic steroids by healthy people leads to the risk of major mood disorders and heart failure; thus, the determination of anabolic androgenic steroids is vital. In this study, 17 anabolic androgenic steroids in dietary supplements and external drugs were identified, and their concentration was determined. For this purpose, polyaniline-coated magnetic nanoparticles were prepared and then subjected to magnetic solid-phase extraction combined with high-performance liquid chromatography-tandem mass spectrometry. The experimental parameters of magnetic solid-phase extraction were studied in detail, and the optimal conditions were established. Under the optimal conditions, the limits of detection were in the range of 0.001-0.02 μg/L, with relative standard deviations of 5.52-11.6% (n = 7) for all the steroids, and the enrichment factors were in the range of 20.0-24.8. The developed method was then successfully applied for the determination of 17 anabolic androgenic steroids in real samples, and dehydroepiandrosterone (prasterone) was detected in a commercially available external drug.

Creatine@SiO2@Fe3O4 nanocomposite as an efficient sorbent for magnetic solid‐phase extraction of escitalopram and chlordiazepoxide from urine samples through quantitation via HPLC–UV

“…Three different concentrations (2, 5, and 10 μgL −1 ) were spiked. Moreover, relative recovery of the procedure was calculated [33]. The results are shown in Table 2.…”

“…Creatine@SiO 2 @Fe 3 O 4 nanoparticles were synthesized according to the previously‐reported methods via modification [27–34]. In summary, FeCl 3 .6H 2 O (21.3 mmol) and FeCl 2 .4H 2 O (10.5 mmol) were dissolved in 145 mL of DI water under constant magnetic stirring and refluxing under N 2 atmosphere at 90°C.…”

“…Synthesis of the Creatine@SiO 2 @Fe 3 O 4 magnetic nanoparticles Creatine@SiO 2 @Fe 3 O 4 nanoparticles were synthesized according to the previously-reported methods via modification [27][28][29][30][31][32][33][34]. In summary, FeCl 3 .6H 2 O (21.3 mmol) and FeCl 2 .4H 2 O (10.5 mmol) were dissolved in 145 mL of DI water under constant magnetic stirring and refluxing under N 2 atmosphere at 90 • C. Then, 12 mL of NH 3 ⋅H 2 O (25%, w/w) was added dropwise (3 min).…”

“…After about 2 h of stirring, the resulting black magnetic precipitate was separated with an external magnet and washed with ethanol and DI water three times. Finally, the obtained Fe 3 O 4 particles were dried at 50 • C in a vacuum for 12 h. In the next step, SiO 2 @Fe 3 O 4 was synthesized according to the reported procedure [33]. Briefly, the prepared Fe 3 O 4 (1 g) was dispersed in a mixture of ethanol (65 mL) and DI water (45 mL), then the mixture was sonicated for 1 h at 25 • C. Afterward, NH 4 OH (2.2 mL) was added to the mixture.…”