固相萃取-液相色谱-串联质谱法测定全血中多塞平

目的建立固相萃取-液相色谱-串联质谱（SPE-LC-MS/MS）分析全血中多塞平的方法。方法以阿米替林为内标,全血样品经固相萃取处理后,通过液相色谱-串联质谱技术进行检测（电喷雾离子源正离子方式,多反应监测模式）。监测离子对m/z多塞平为280→107、280→235、280→220,阿米替林为278→233。多塞平和阿米替林的保留时间分别为15.15min和16.94min。结果全血中多塞平在0.005～1.00μg/mL质量浓度范围内呈线性关系,线性方程为y=3.2047x＋0.0339,相关系数（r）=0.9996,检出限为0.001μg/mL;平均提取回收率为78.0%～82.9%,日内精密度〈2.55%,日间精密度〈5.90%。结论本方法快速简便、灵敏、重现性好,适用于全血中多塞平的检测。

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

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.