柱前衍生化反相高效液相色谱法测定狗血清中格列美脲浓度

柱前衍生化反相高效液相色谱法测定狗血清中格列美脲浓度

卢来春, 蒋学华^*, 周静, 杨俊毅

1.第三军医大学新桥医院药局, 重庆 400037;
2.四川大学华西药学院, 成都, 610044

收稿日期:2002-09-17 修回日期:2003-05-10 出版日期:2003-06-15 发布日期:2003-06-15
通讯作者: 蒋学华*

Determination of Sulphonylurea Glimepiride in Dog Serum by RP-HPLC with Pre-column Derivatization

LU Lai-chun, JIANG Xue-hua^*, ZHOU Jing, YANG Jun-yi

1.Pharmacy of Xinqiao Hospital, Third Military Medical University, Chongqing 400037, China;
2.West China College of Pharmacy, Sichuan University, Chengdu 610041, China

Received:2002-09-17 Revised:2003-05-10 Online:2003-06-15 Published:2003-06-15
Contact: JIANG Xue-hua*

摘要/Abstract

摘要： 目的建立测定狗血清中格列美脲浓度的柱前衍生化反相高效液相色谱法. 方法血清样品二氯甲烷萃取后挥干, 以DNBF试剂衍生化, 所得产物氮气挥干, 用流动相(含1%冰醋酸)溶解进样; 色谱柱为Hypersil BDS C18柱(150 mm×4.6 mm, 5μm); 流动相为乙腈-水(75:30, V/V), 流速0.8 mL·min^-1, 检测波长350 nm. 结果血清中格列美脲浓度在0.028-0.648 μg·mL^-1范围内线性关系良好(R = 0.9998); 高、中、低3种浓度萃取回收率分别为75.9%-83.2%; 方法回收率在96.5%-109.3%之间; 高、中、低三种浓度日内浓度日内精密度RSD分别为1.5%、2.3%、6.3%, 日间精密度RSD分别为2.9%、7.4%、14.8%. 结论本法简便易行、灵敏度高, 衍生化反应速度适中, 适用于格列美脲血药浓度测定及药代动力学研究.

关键词: 格列美脲, 柱前衍生化, DNBF, 血药浓度

Abstract:

Aim A simple, sensitive and rapid RP-HPLC method with pre-column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extracted from the dog serun using dichlromethane followed by derivatization with DNBF for 20 min at 100 °C. The solvent was then evaporated at 60 °C under nitrogen, and the residue was taken up in 100 μL of mobile phase consisting of acetonitrile-water (75:30, v/v). The separation was performed on a Hypersil BDS C18 column with a flow rate of 0.8 mL·min^-1, and the ultraviolet detector wavelength was set at 350nm. Results Extraction recovery ranged from 75.9% to83.2%, and methodological recovery was between 96.5% and 109.3%. Within-day RSD ranged from 1.5% to 6.3%, and inter-day RSD was between 2.9% and 14.8%. The method showed good linearity (R = 0.9998). Conclusion The method was simple, convenient and sensitive. reaction of derivatization was reproducible.

Key words: Glimepiride, Glimepiride, pre column derivatization, pre column derivatization, DNBF, DNBF, serum concentration, serum concentration

中图分类号:

R917

Supporting: ^*Corresponding author. Tel.: 028-5501370

卢来春, 蒋学华^*, 周静, 杨俊毅. 柱前衍生化反相高效液相色谱法测定狗血清中格列美脲浓度[J]. .

LU Lai-chun, JIANG Xue-hua^*, ZHOU Jing, YANG Jun-yi . Determination of Sulphonylurea Glimepiride in Dog Serum by RP-HPLC with Pre-column Derivatization[J]. .

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