With the continuous renewal of new psychoactive substances (NPS), the abuse of NPS has seriously harmed social security and public safety. The number of deaths from the abuse of NPS is increasing year by year. Therefore, it is urgent to develop an effective method for detecting NPS. Direct analysis in real time-tandem mass spectrometry (DART-MS/MS) was used to detect 11 NPS in blood and urine. The temperature of ion source was optimized and set to 400°C. The mixture solvent of acetonitrile/methanol (4:1, v/v) was used as precipitant. SKF-525 was selected as the internal standard for quantification. After pretreatment of the analytes in blood or urine, the supernatant was prepared for instrumental analysis. The results indicated that the correlation coefficients (r2 ) of all analytes were ranging from 0.99 to 1 in the linear range. The recoveries of 11 analytes at three spiked levels ranged between 83.4% and 110.4% in blood and between 81.7% and 108.5% in urine. The matrix effects of 11 analytes ranged between 79.5% and 109.5% in blood and between 85.0% and 109.4% in urine. The relative standard deviations (RSDs) of intra-day, inter-day precisions and repeatability were lower than 12.4%, 14.1%, and 14.3% in blood and lower than 11.4%, 13.9%, and 14.3% in urine, respectively. The method established for the detection of 11 NPS could meet the needs of rapid screening of NPS samples. The DART-MS/MS method has the advantages of being efficient, fast, and green. Therefore, it may become a promising technology for the detection of NPS in the future.
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