›› 2011, Vol. 27 ›› Issue (5): 350-352.DOI: 10.3969/j.issn.1004-5619.2011.05.009

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Determination of Doxepin in Whole Blood by SPE-LC-MS/MS

GONG FEI-JUN, YAN SONG-MAO, WU ZHONG-PING, ZHANG RUN-SHENG   

  1. (Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science, Shanghai Public Security Bureau, Shanghai 200083, China)
  • Online:2011-10-25 Published:2011-10-28

Abstract: Objective To develop a method of SPE-LC-MS/MS for the determination of doxepin in whole blood. Methods After solid phase extraction, the samples were identified by LC-MS/MS. Positive ion electrospray ionization mode and multiple reaction monitoring(MRM) mode was selected. Amitriptyline was used as internal standard. The m/z of doxepin: 280→107, 280→235 and 280→220. The m/z of amitriptyline: 278→233. The retaining time of doxepin and amitriptyline were 15.15 and 16.94 min, respectively. Results The calibration curve was linear among the concentration of doxepin range from 0.005 to 1.00 μg/mL. The linear correlation equation was y=3.204 7 x+0.033 9, the correlation coefficient was 0.999 6. The detection limit of doxepin was 0.001 μg/mL and average recovery rate was 78.0%-82.9%. The relative standard precision for within-day and between-day were less than 2.55% and 5.90%, respectively. Conclusion The method is effective, simple, reliable and can be used in the determination of doxepin in whole blood.

Key words: forensic toxicology, solid phase extraction, LC-MS/MS, doxepin, blood

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