A specific and sensitive approach using magnetic nanoparticle solid-phase extraction combined with gas chromatography-mass spectrometry (GC-MS) was carried out and applied in the simultaneous determination of 16 kinds of synthetic cathinones in human urine. The functionalized extraction material (Fe3O4/NH2-MWCNTs) was synthesized and factors affecting the extraction efficiency were all tested. Under the optimized conditions of magnetic nanoparticle solid-phase extraction, the determination of synthetic cathinones in human urine was carried out with GCMS. Good linear relationships of 16 kinds of synthetic cathinones were obtained in the range of 0.005–5.00 g/mL with the correlation coefficients (r) ranging from 0.9901 to 0.9979, the limits of detection were in the range between 0.005 and 0.01 g/mL, and the limits of quantitation were between 0.01 and 0.02 g/mL. Furthermore, the average intra-day precisions were below 8.90%, the average inter-day precisions were less than 9.52%, and the average recoveries were between 87.03% and 99.13%, respectively. The results show the advantages of the approach in the determination of trace synthetic cathinones in complex matrixes, such as environmentally friendly, fast detection, high efficiency and sensitivity. The practical application indicated that this method could provide scientific basis for the determination of drugs of abuse in forensic laboratories.
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