|
|
|
| Establishment of reverse-phase high-performance liquid chromatography with chiral reagent derivatization for separation of fexofenadine enantiomers |
| YAO Qing-qing, QU Bo-xuan, ZHOU Quan, ZENG Su |
| Laboratory of Pharmaceutical Analysis and Drug Metabolism, College of Pharmaceutical Sciences, Zhejiang Provincial Key Laboratory of Anti-Cancer Drug Research，Zhejiang University, Hangzhou 310058, China |
|
|
|
Abstract Objective： To establish a precolumn chiral derivatization method for determination of fexofenadine enantiomers, a chiral substrate of OATP1B1, in cellular model. Methods： R-(+)-phenylethylisocyanate was selected as chiral derivatization reagent, which was reacted with fexofenadine to form carbamate derivatives. Enantiomers were identified by LC/MS and separated by RP-HPLC.Results： Under the experimental conditions, the fexofenadine enantiomers were separated completely. The standard curve was linear over the concentration range of 25-100 ng/ml (R2=0.9992, 0.9989). Accuracy was 101.1% and 98.3%, intra-precision was 2.4% and 3.1%, inter-precision was 3.1% and 4.0% for D1 and D2, respectively. Conclusion： The method established is sensitive and accurate for determination of fexofenadine enantiomers in cells.
|
|
Received: 11 October 2013
|
|
Corresponding Authors:
ZHOU Quan, E-mail: zhouquan142602 @zju.edu.cn
|
非索非那定对映体柱前手性衍生化反相高效液相色谱分析方法的建立
目的：建立适用于体外细胞模型的OATP1B1手性底物非索非那定柱前手性衍生化分析方法，为测定细胞中非索非那定对映体提供分析手段。方法：选择R-(+)-苯乙基异氰酸酯作为手性衍生化试剂，与非索非那定生成氨基甲酸酯衍生物，应用液相色谱-串联质谱法确定对映体衍生物色谱峰，通过反相高效液相色谱法实现对映体的分离分析。结果：在建立的手性分离条件下，成功实现非索非那定对映体分离分析，非索非那定两个对映体衍生物在25 ~100 ng/ml浓度范围内线性关系良好 (R2=0.9992, 0.9989)，日内、日间精密度均小于10%。结论：本实验建立的非索非那定对映体柱前手性衍生化反相高效液相色谱分析方法灵敏、准确，可用于体外细胞模型中盐酸非索非那定立体选择性分析。
关键词：
特非那定/化学,
异氰酸盐类,
立体异构现象,
色谱法,
高压液相/方法,
指示剂和试剂
|
Viewed |
|
|
|
Full text
|
|
|
|
|
Abstract
|
|
|
|
|
Cited |
|
|
|
|
| |
Shared |
|
|
|
|
| |
Discussed |
|
|
|
|
