多虑平SPE-HPLC分析方法的建立及其应用

目的　建立尿样和全血中多虑平的固相萃取 高效液相色谱 (SPE HPLC)分析方法。方法　以多沙普仑为内标 ,1ml尿样或 0 5ml全血用Oasis小柱固相萃取后进Lichrospher 10 0RP 18e ( 2 5 0mm× 4mm ,5 μm)分析柱进行分析 ,2 3 0、 2 5 0nm同时进行检测。结果　尿样和全血中的检测限均 2ng/ml,线性相关系数r≥ 0 9992 ,天内和天间精密度均小于 6 75 % ,绝对回收率大于 85 % ,内源性物质不干扰测定。结论　本法快速、简便、准确 ,可用于实际案例的检测。

Analysis of doxepin in urine and whole blood by HPLC after solid-phase extraction

Objective To provide a specific,sensitive,reproducible HPLC method for the determination of doxepin in urine and whole blood with doxapram as the internal standard.Methods The sample preparation was simple and time-saving by using an Oasis pretreatment cartridge.Separations were achieved by a Lichrospher  100 RP-18e (250mm×4.0mm,5μm)column kept at 50 ℃,and the DAD detector was set at 230nm and 250nm.Results The detection limit was 2 ng/ml in urine and whole blood.The results showed excellent linearity.The relative standard deviation of between-day and within-day assay was Less than 6.75%,and absolute recoveries were higher than 85%.Conclusion The method for determination of doxepin in urine and whole blood is effective,simple and reliable,which may be applicable to the practical cases.