互为内标法测定患者血浆中氟西汀和西酞普兰的浓度

目的：建立测定人血浆中氟西汀、西酞普兰的高效液相色谱-荧光（HPLC-FLU）法,为临床用药提供参考。方法：氟西汀和西酞普兰互为内标,血浆样品碱化后经液-液萃取,以Ultimate XB-C18反相色谱柱进行分离,流动相为乙腈：0.02 mol·L-1磷酸氢二钠溶液（35∶65,pH 5.0）,流速为1.0 ml·min-1,柱温为30℃。荧光检测氟西汀和西酞普兰的激发波长为230nm,发射波长为305 nm。结果：氟西汀、西酞普兰血药浓度均在15.625～1 000μg.L-1范围内线性关系良好;平均回收率分别为100.72%和100.94%;分析方法的最低定量限均为5μg.L-1;日内、日间RSD均〈3%;冻融稳定性RSD均〈10%。结论：本法快速、简便、灵敏、准确,适用于氟西汀、西酞普兰的血药浓度监测及药动学研究。

Determination of Fluoxetine and Citalopram in Patient Plasma Using Each Internal Standard Method by HPLC

Objective: To establish an HPLC method with fluorescence detection assay for the determination of fluoxetine and citalopram in the patient plasma and provide a scientific basis for the clinical application.Method: Fluoxetine and citalopram were used as the internal standard for each other.The samples were alkalized and extracted by liquid-liquid extraction.Then the samples were separated on an Ultimate XB-C18 column with the mixture of acetonitrile-0.02 mol·L-1 disodium hydrogen phosphate(35∶ 65,pH 5.0) as the mobile phase.The flow rate was 1.0 ml·min-1.The column temperature was set at 30℃.Fluoxetine and citalopram were detected by fluorescence detection(Ex=230 nm,Em=305 nm).Result: Linearity was obtained from 15.625 to 1 000 μg·L-1 for fluoxetine and citalopram.The LOQ was 5 μg·L-1.The average recovery of fluoxetine and citalopram was 100.72% and 100.94%,respectively.Both the inter-day and intra-day RSD were less than 3%.The Freeze-thaw stability RSD was less than 10%.Conclusion: The method is rapid,convenient,sensitive and reliable in the drug determination,adverse reaction control and pharmacokinetic study of fluxetine and citalopram in human plasma.