Determination of doxepin in whole blood by SPE-LC-MS/MS.
- Author:
Fei-Jun GONG
1
;
Song-Mao YAN
;
Zhong-Ping WU
;
Run-Sheng ZHANG
Author Information
1. Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science, Shanghai Public Security Bureau, Shanghai 200083, China.
- Publication Type:Journal Article
- MeSH:
Amitriptyline/blood*;
Antidepressive Agents, Tricyclic/poisoning*;
Biomarkers/blood*;
Chromatography, Liquid/methods*;
Doxepin/poisoning*;
Drug Overdose;
Forensic Toxicology;
Humans;
Reproducibility of Results;
Sensitivity and Specificity;
Solid Phase Extraction/methods*;
Spectrometry, Mass, Electrospray Ionization;
Tandem Mass Spectrometry/methods*
- From:
Journal of Forensic Medicine
2011;27(5):350-352
- CountryChina
- Language:Chinese
-
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 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.
CONCLUSION:The method is effective, simple, reliable and can be used in the determination of doxepin in whole blood.