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[Determination of doxepin in whole blood by SPE-LC-MS/MS].

Fa yi xue za zhi (2012-01-21)
Fei-Jun Gong, Song-Mao Yan, Zhong-Ping Wu, Run-Sheng Zhang
ABSTRAKT

To develop a method of SPE-LC-MS/MS for the determination of doxepin in whole blood. 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. The calibration curve was linear among the concentration of doxepin range from 0.005 to 1.00 microg/mL. The linear correlation equation was y = 3.2047x + 0.0339, the correlation coefficient was 0.9996. The detection limit of doxepin was 0.001 microg/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. The method is effective, simple, reliable and can be used in the determination of doxepin in whole blood.

MATERIAŁY
Numer produktu
Marka
Opis produktu

Doxepin for system suitability, European Pharmacopoeia (EP) Reference Standard
Supelco
Doxepin hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®
Sigma-Aldrich
Doxepin hydrochloride, ~85% E-isomer basis, ≥98% (GC), 15% Z-isomer basis, powder