固相萃取反相高效液相色谱法测定人血浆中多奈哌齐浓度

RP-HPLC determination of donepezil in human plasma by solid-phase extraction

目的：建立固相萃取反相高效液相色谱法测定人血浆中多奈哌齐浓度的方法。方法：血浆经碱化后，用OASIS固相萃取小柱提取血浆中多奈哌齐，紫外检测器检测，检测波长316nm。色谱柱：shim—Pack C18柱（150mm×4．6mm，5μm），保护柱：Shim—Pack C18柱，流动相：0．5％三乙胺溶液（磷酸调pH3．0）．乙腈（65：35），流速为1．0mL·min6-1。结果：标准曲线线性范围为5～100mg·L^-1（r=0．9993），萃取回收率在81．9％～90．7％之间。日内、日间RSD在5．4％～10．2％之间，最低检测浓度为2mg·L^-1。结论：本测定．方法快速、灵敏、准确，适用于临床治疗药物浓度检测的要求。

OBJECTIVE To develop a simple, sensitive and rapid RP-HPLC with ultraviolet detection method for the determination of donepezil in serum. METHODS The donepezil in plasma samples（ 1 mL） was processed by Waters OASIS solid-phase extractor, the separation was conducted by using a reversed-phase Shim-Pack C18 column with isoeratic mobile phase consisting of 0.5% triethylamine solution （adjust pH to 3.0 with H3PO4 ）-acetonitrile （65：35）, the flow rate was 1.0 mL· min^-1, the detective wavelength was 316 nm. RESULTS A linearity was obtained in the range of 5 - 100 mg- L - ~ （ r = 0. 999 3 ） , the detection limit of the plasma was 2 μg·L^-1. The extraction recovery was between 81.9% -90.7%. The relative standard deviations of intra-day and inter-day assay were within 5.4% - 10.2%. CONCLUSION The established method was showen to be sensitive, accurate and simple for the determination of donepezil levels in human plasma. It was suitable for the pharmacokinetics and TDM study of donepezil.