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作 者:张春燕[1] 李玉珍[1] 陈碧[2] 张海英[1] 李长龄[1]
机构地区:[1]北京大学人民医院药剂科,北京100044 [2]北京大学药学院药理系,北京100083
出 处:《中国现代应用药学》2005年第6期500-502,共3页Chinese Journal of Modern Applied Pharmacy
摘 要:目的建立一种简单、快速测定9-硝基喜树碱血药浓度的反相高效液相色谱法.方法血浆样品加喜树碱作内标,用正己烷-二氯甲烷-异丙醇(100:50:5)提取,氮气吹干,残渣用流动相溶解进样.色谱条件:分析柱为C18反相柱,流动相为3%甲酸溶液-乙腈(体积比65:35),流速为2.0 mL·min-1,在紫外检测波长370 nm处进行检测.结果9-硝基喜树碱及内标在5min内完全分离,检测限为25 ng·mL-1,在25~1600ng·mL-1内线性关系良好,r=0.999 6,低、中、高浓度的回收率、日间及日内精密度均符合方法学要求.结论本法简便、快速、稳定、重现性好,适用于9-硝基喜树碱临床前药动学研究.OBJECTIVE A simple and rapid reversed phase high performance liquid chromatographic method was developed for determination of 9-nitroeamptotheein. METHOD The samples added eamptotheein as an internal standard, were extracted with nhexane-diehloromethane-dimethyl earbionl( 100: 50:5 ), dried by N2, the residue was dissolved in the mobile phase and 50μL of solution was injected into the chromatographic system. The mobile phase was 3% formic acid solution:CH3 CN = 65:35 ( v/v), the detect wavelength was 370 nm. RESULT The retention time of 9-nitroeamptotheein and the internal standard were 4.9 min and 4.2 min respectively, the detect limit was 25 ng ·mL^- 1, the linear range was between 25~1600 ng· mL^- 1, r = 0. 9996 . The average recovery was 102.1%, the intra-day and inter-day RSDs were 5.0% and 5.0%, respectively. CONCLUSION It is a simple, rapid and stable method for determination of 9-nitroeamptotheein in plasma.
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