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建立了微波辅助柱前衍生化-HPLC法检测普瑞巴林中的(R)-对映体。含(R)-对映体的普瑞巴林与手性衍生化试剂Nα-(5-氟-2,4二硝基苯基)-D-缬氨酰胺在DMSO中,于微波辅助条件下进行快速衍生化反应,生成具有紫外吸收的一对非对映体衍生化产物。采用Hypersil BDS C18色谱柱,以0.1 mol/L甲酸铵溶液(用甲酸调至pH 3.0)-乙腈(49︰51)为流动相,检测波长340 nm。(R)-对映体在2~20μg/ml浓度范围内与其衍生物峰面积线性关系良好。定量限为0.24μg/ml。
The (R) -enantiomer of pregabalin was detected by microwave assisted pre-column derivatization-HPLC. Pregabalin containing the (R) -enantiomer and the chiral derivatizing agent Nα- (5-fluoro-2,4-dinitrophenyl) -D-valinamide are carried out in DMSO under microwave assisted conditions Rapid derivatization to produce a pair of diastereomer derivatized products with UV absorption. A Hypersil BDS C18 column was used with 0.1 mol / L ammonium formate (adjusted to pH 3.0 with formic acid) -acetonitrile (49:51) as mobile phase and the detection wavelength was 340 nm. The (R) -enantiomer had a good linear relationship with the peak area of its derivative in the concentration range of 2 ~ 20μg / ml. The limit of quantification was 0.24 μg / ml.