离线紫外照射和高效液相色谱荧光法测定人血浆中他莫昔芬的浓度  

Determination of tamoxifen in human plasma by high performance liquid chromatography with offline ultraviolet and fluorescence detection

作　　者：朱余兵[1] 张倩[2] 邹建军[1] 于翠霞[1] 卢弢[2] 肖大伟[1] 

机构地区：[1]南京医科大学附属南京第一医院临床药理室,江苏南京210006 [2]南京医科大学,江苏南京210029

出　　处：《中国新药与临床杂志》2008年第9期691-694,共4页Chinese Journal of New Drugs and Clinical Remedies

基　　金：南京医科大学科技发展基金资助(06NMUM062)

摘　　要：目的建立测定人血浆中他莫昔芬的高效液相色谱荧光法。方法血浆样品经正己烷-正丁醇(98:2,V:V)提取后,以甲醇-1%三乙胺水溶液(82:18,V:V,pH 11.2)为流动相,流速为1 mL·min^(-1),色谱柱为Agilent Extend C_(18)(4.6 mm×150 mm,5μm),柱温为50℃,离线紫外照射(254 nm)10 min,荧光激发波长(λ_(ex))260 nm,发射波长(λ_(em))375 nm。结果血浆内源性杂质不干扰待测物测定,他莫昔芬的线性范围为0.5～200μg·L^(-1),定量下限为0.5μg·L^(-1),日内、日间精密度(RSD)均小于10%。样品反复冻融4次以及在提取后4℃下12 h内稳定性良好。结论该法灵敏、快速、准确、操作简便、线性范围宽,可用于他莫昔芬的药动学研究及临床治疗药物监测。AIM To establish a high performance liquid chromatography with fluorescence method for the determination of tamoxifen in human plasma. METHODS Plasma samples were extracted with n-hexane ： n- butanol （98 ： 2, V ： V）, and exposed to a 254-nm UV lamp offline for 10 min. Chromatography was performed on a column of Agilent Extend C18 （150 mm × 4.6 mm, 5 um） at 50 ℃. The mobile phase consisted of methanol ： 1% triethylamine （82 ： 18, V ： V） at a flow rate of 1 mL·min^-1. The fluorescence detector was operated at an excitation and emission wavelengths 260 and 375 nm, respectively. RESULTS The intrinsic impurity of plasma did not interfere with the determination of analyte. The linear range of tamoxifen was 0.5 - 200 ug· L^-1. Lower limit of quantification was 0.5 ug· L^-1. The precision of intra-day and inter-day were less than 10 %. The stability of unprocessed and processed samples stored at 4℃ was good. After 4 cycles of freeze and thaw processes, the plasma samples were stable. CONCLUSION The established HPLC-Flu method is fast, sensitive and accurate to be used in the clinical pharmacokinetics study and routine therapeutic drug monitoring.

关 键 词：他莫昔芬 色谱法 高压液相 药物监测 

分 类 号：R969.1[医药卫生—药理学]