氟比洛芬对映异构体的手性衍生化反相高效液相色谱拆分及质谱鉴定

Separation and Identification of Flurbiprofen Enantiomers by Reversed-phase HPLC and Mass Spectrometry with Chiral Pre-column Derivatization

以二氯亚砜和R-(+)-1-(1-萘基)乙胺为手性衍生化试剂,建立了一种柱前衍生化反相高效液相色谱法分析氟比洛芬对映异构体的方法。选用C18柱,以乙腈-50 mmol/L磷酸二氢钾溶液(体积比75∶25)为流动相,在254 nm检测,非对映异构体色谱峰的保留时间分别为5.6和6.2 min,分离度为2.0,检出限为12μg/L(S/N=3)。并经液相色谱-电喷雾离子阱质谱实现了衍生物的分离与鉴定。其衍生化产物稳定,方法灵敏度高,重复性好,可用于氟比洛芬及其对映异构体的药理学立体选择性研究和药品质量控制。

The enantiomers of flurbiprofen were separated by reversed-phase high performance liquid chromatography via pre-column derivatization with thionyl chloride and R-（＋）-1-（1-naphthyl） ethylamine. The retention times of the R-（-）-and S-（＋）-flurbiprofen diastereomeric amides were 5.6 and 6.2 rain respectively using a mobile phase of CH3CN -50 mmol/L KH2PO4 （75 ： 25, by volume） at a flow rate of 1.0 mL/min and a resolution factor was 2.0. The detection limit of the method was 12μg/L（S/N=3）. The identification of flurbiprofen derivatives was carried out by LC -MS. It was a suitable, reproducible and sensitive method for study on enantioselective pharmacodynamic and pharmacokinetic. The quality evaluation of flurbiprofen enantiomers was provided.