http://jcps.bjmu.edu.cn

• 研究论文 • 上一篇    下一篇

兔血浆中地非三唑(DL111-IT)高效液相色谱荧光检测方法

何敏, 姚彤炜*   

  1. 浙江大学药学院药物分析与药物代谢研究室, 浙江 杭州 310031
  • 收稿日期:2004-12-22 修回日期:2005-02-10 出版日期:2005-03-15 发布日期:2005-03-15
  • 通讯作者: 姚彤炜*

Determination of Diphenytriazol (DL111-IT) in Rabbit Plasma by High-Performance Liquid Chromatography with Fluorescence Detection

HE Min, YAO Tong-wei*   

  1. Department of Pharmaceutical Analysis and Drug Metabolism, College of Pharmac eutical Sciences, Zhejiang University, Hangzhou 310031, China
  • Received:2004-12-22 Revised:2005-02-10 Online:2005-03-15 Published:2005-03-15
  • Contact: YAO Tong-wei*

摘要: 目的 建立兔血浆中DL111-IT的高效液相色谱荧光检测法。方法 血浆样品和内标格列本脲经氯仿提取后, 选用Diamonsil ODS-C18(150 mm ×4.6 mm, 5 μm), 乙腈-0.025 mol·L-1磷酸氢二铵缓冲溶液(磷酸调pH 5.0)(60:40, V/V)为流动相, 流速1.0 mL·min-1,荧光检测ex = 250 nm, λem = 332 nm)结果 DL111-IT在浓度1.00~20.00 ng·mL-1范围内呈良好线性, r = 0.9996, n = 5。高(20.00 ng·mL-1)、中(10.00 ng·mL-1)、低(1.00 ng·mL-1)3个质控样本平均提取回收率分别为85.3%±1.3%, 84.9%±2.7%, 85.8%±1.8%, 方法回收率分别为99.5%±0.4%, 102.1%±1.8%, 101.3%±2.4%; 日内(n = 5)和日间(n = 5)RSD分别低于3.0%7.0%.血浆样品检测限为0.3 ng·mL-1 (S/N = 3), 定量限为1 ng·mL-1 (S/N = 10, RSD<7.0%)结论 本法准确、灵敏、操作简便, DL111-IT药代动力学研究提供了方法学基础.

关键词: 地非三唑, 地非三唑, 地非三唑, 抗孕唑, 抗孕唑, 抗孕唑, DL111-IT, DL111-IT, DL111-IT, HPLC, HPLC, HPLC, 荧光检测, 荧光检测, 荧光检测, 药代动力学, 药代动力学, 药代动力学, 格列本脲, 格列本脲, 格列本脲

Abstract: Aim To develop an HPLC method with fluorescence detection for the assay of DL111-IT in rabbit plasma. Methods DL111-IT and internal standard glybenzcyclamide in rabbit plasma were extracted with chloroform. The determination was performed on a Diamonsil ODS-C18 column (150 mm×4.6 mm, 5 μm) with a mobile phase of acetonitrile and 0.025 mol·L-1 diammonium hydrogen phosphate buffer (pH 5.0, adjusted by phosphoric acid) (60:40, V/V) at a flow-rate of 1.0 mL·min-1. Fluorescence detector was operated at excitation wavelength of 250 nm and emission wavelength of 332 nm. Results The calibration curve in plasma was linear from 1.00-20.00 ng·mL-1 (r = 0.9996, n = 5).The method afforded average extracting recoveries of 85.3%±1.3%, 84.9%±2.7% and 85.8%±1.8%, and the average method recoveries were 99.5%±0.4%, 102.1%±1.8% and 101.3%±2.4% for the high (20.00 ng·mL-1), middle (10.00 ng·mL-1) and low (1.00 ng·mL-1) check samples, respectively. The intra-day (n = 5) and inter-day (n = 5) precisions (RSD) were less than 3.0% and 7.0%, respectively. The limit of detection and quantitation for the method were 0.3 ng·mL-1 (S/N = 3) and 1 ng·mL-1 (S/N = 10, RSD<7.0%) plasma sample, respectively. Conclusion The developed method was accurate, sensitive, simple and could be used for pharmacokinetic study of DL111-IT.

Key words: diphenytriazol, diphenytriazol, contragestazol, contragestazol, DL111-IT, DL111-IT, HPLC, HPLC, fluorescence detection, fluorescence detection, pharmacokinetics, pharmacokinetics, glybenzcyclamide, glybenzcyclamide

中图分类号: 

Supporting: *Corresponding author. Tel.: 86-571-87217203; fax: 0571-87217203