人血浆中盐酸多奈哌齐的HPLC-MS测定法

目的:建立人血浆中盐酸多奈哌齐的HPC-MS法.方法:血样经饱和NaHCO3碱化后用乙酸乙酯提取,进行HPLC-MS分析,色谱柱为Hypersil ODS(5μm,250mm×4.6 mm),流动相为甲醇-水-三乙胺-冰醋酸(70:30:0.3:0.3),内标为盐酸非洛普,检测离子为m/z 380(多奈哌齐)、m/z 344(内标),裂解电压为120V.结果:在0.2～20ng/ml范围内多奈哌齐与内标峰面积比值与浓度线性关系良好(r=0.9996),最低可定量浓度为0.1 ng/ml,提取回收率为87.52%～90.91%.结论:本实验建立的分析方法灵敏、准确、简便.

Quantitation of Donepezil in Human Plasma by HPLC-MS

AIM and METHOD:A highly sensitive method for quantitation of donepezil in human plasma was established by using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS),with phenopromlamine hydrochloride as the internal standard (I.S.).After alkalizing with saturated sodium bicarbonate,plasma was extracted with ethyl acetate and the extracts were separated by HPLC on a C18 reversed-phase column with methanol-water-acetic acid-triethylamine (70:30:0.3 :0.3,v/v ) as mobile phase.LC-ESI-MS was performed in the selected ion monitoring (SIM) mode using target ions at m/z 380 for donepezil and m/z 344 for the I.S..RESULT:Calibration curves,which were linear over the range of 0.2 to 20 ng/ ml,were established contemporaneously with the analyses of each batch of samples,along with low (0.2 ng/ml),medium (2 ng/ml) and high (20 rng/ml) quality control samples.The intra and inter-assay variability ranged from 1.25% to 9.84% for the low,medium and high quality control samples.The extraction recovery of donepezil from plasma was in the range of 87.5% ～ 91.9%.CONCLUSION:The method has been used successfully to study donepezil pharmacokinetics in human plasma.