Simultaneous Determination of 10 2C-series Phenethylamines in Blood and Urine by UPLC-MS/MS
  
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KeyWord:ultra-high performance liquid chromatography-tandem mass spectrometry  blood  urine  2C-series phenethylamines
  
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LI Jin-chang,HE Hong-yuan,ZHANG Yun-feng,WANG Rui-hua 1. School of Criminal Investigation,People’s Public Security University of China,Beijing ,China; 2. Institute of Forensic Science,Ministry of Public Security,Beijing ,China
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Abstract:
      An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was established for the simultaneous detection of 10 2C-series phenethylamines,i.e.2C-H,2C-D,2C-P,2C-T-2,2C-T-4,2C-T-7,25D-NBOMe,25C-NBOMe,25B-NBOMe and 25I-NBOMe in blood and urine samples.Comparing three preparation methods respectively,including precipitated protein(PPT),liquid-liquid extraction(LLE) and solid phase extraction(SPE),blood and urine samples were finally extracted by precipitated protein method with methanol.The chromatographic column and mobile phase were also optimized in this experiment.ACQUITY UPLC? BEH C18(100 mm × 2.1 mm,1.7 μm) was finally used as the analytical column to separate the targeted analytes with methanol-water(0.1% formic acid) solution as the mobile phase.The ion source of the tandem mass spectrometer was electrospray ionization(ESI),which was performed in multiple reaction monitoring(MRM) mode.There were good linear relationships for 10 target compounds in the range of 0.005-50 ng/mL,with the correlation coefficients(r2) of 0.995 8-0.999 9.The limits of detection(LODs) for 10 2C-series phenethylamines in blood and urine were in the range of 0.01-2 ng/mL and 0.002-5 ng/mL,respectively.At three spiked concentration levels of 1,5 and 20 ng/mL,the matrix effects for 10 target compounds in blood and urine were in the range of 71.9%-112%,and the recoveries ranged from 78.8% to 99.3%,with the intra-day and inter-day relative standard deviations(RSDs) both not more than 15%.This method is characterized by rapid analysis,simple operation,high detection sensitivity,small sampling amount,accurate results and good repeatability,and is suitable for the rapid determination of 2C-series phenethylamines in blood and urine.
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