作者：张莉1, 李东2, 肖正华1, 张梦军1, 郭嘉伟1, 周娟1, 李滨3, 张惠静1
作者单位：1. 第三军医大学药学院药物分析与分析化学教研室, 重庆 400038;
2. 第三军医大学学员旅, 重庆 400038;
3. 重庆市科学技术研究院, 重庆 401123
关键词：NI221; 阿魏酸; 反相高效液相色谱法; 血药浓度
摘要：
建立一种快速、准确测定大鼠血清中NI221含量的RP-HPLC分析方法。以阿魏酸为内标物,360 L血清样品经冰冻乙腈蛋白沉淀处理后,取20 L上清进样分析;色谱柱为Diamonsil C18柱(200 mm4.6 mm5 m),流动相组成为甲醇:0.05%的磷酸=55:45(用氢氧化钠调节pH=2.5),流速为1.0 mLmin-1,紫外检测波长为302 nm,柱温为室温。血清中NI221浓度在0.15~20 gmL-1范围内呈线性,相关系数r=0.999 6,样品加标回收率为97.36%~112.50%(n=15),日内和日间精密度RSD均15%。所建立的RP-HPLC方法准确可靠,重现性好,可用于临床前药代动力学研究中NI221血药浓度的测定。
Determination of NI221 in rats serum by RP-HPLC
ZHANG Li1, LI Dong2, XIAO Zheng-hua1, ZHANG Meng-jun1, GUO Jia-wei1, ZHOU Juan1, LI Bin3, ZHANG Hui-jing1
1. Department of Analytical Chemistry, College of Pharmacy, Third Military Medical University, Chongqing 400038, China;
2. Cadet Brigade, Third Military Medical University, Chongqing 400038, China;
3. Chongqing Research Institute of Science and Technology, Chongqing 401123, China
Abstract: A rapid and accurate RP-HPLC method for determining NI221 in rats serum was developed. Following deproteinisation by freezing acetonitrile, NI221 and the internal standard ferulic acid were separated on the Diamonsil C18 column (200 mm×4.6 mm× 5 μm) using isocratic elution with methanol-0.05%phosphoric acid (pH 2.5) (V:V=55:45) at a flow rate of 1.0 mL/min. The detection wave length was at 302 nm. The linear range of NI221 was 0.15~20 μg·mL-1,the correlation coefficient was 0.999 6,the recovery of the method was between 97.36% and 112.50% (n=15). The coefficients of variation for inter-day and intra-day precisions were less than 15%. This method can be applied to determine NI221 concentration in rats serum,which was suitable for the preclinical pharmacokinetic investigation of NI221.
Keywords: NI221; ferulic acid; RP-HPLC; serum drug concentration
2013, 39(6): 53-56 收稿日期: 2013-6-5;收到修改稿日期: 2013-9-25
基金项目: 国家科技重大专项(2012ZX09103-101-080)重庆市科技攻关计划项目(CSTC,2010AB5099)
作者简介: 张莉(1971-),女,重庆市人,副教授,博士,主要从事分析化学工作。
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