普瑞巴林中(R)-对映体的微波辅助柱前衍生化-HPLC法测定  

Determination of(R)-Enantiomer in Pregabalin by HPLC with Microwave-assisted Pre-column Derivatization

作　　者：李硕 刘浩[1,2,3] 林梅[1,2,3] 杜狄峰 

机构地区：[1]中国医药工业研究总院 [2]上海医药工业研究院,上海200040 [3]上海市食品药品检验所 [4]上海秀新臣邦医药科技有限公司,上海201203

出　　处：《中国医药工业杂志》2011年第5期362-364,377,共4页Chinese Journal of Pharmaceuticals

摘　　要：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。A microwave-assisted pre-column derivatization-HPLC method was established for the determination of(R)-enantiomer in pregabalin.With microwave-assistance,pregabalin was derivatized with Nα-(5-fluoro-2,4-dinitrophenyl)-D-valine amide as chiral derivatization agent in DMSO.A Hypersil BDS C18 column was used with the mobile phase of 0.1 mol/L ammonium formate solution(adjusted to pH 3.0 with formic acid)-acetonitrile(49︰51) at the detection wavelength of 340 nm.The calibration curve of(R)-enantiomer was linear in the range of 2-20 μg/ml.The LLOQ was 0.24 μg/ml.

关 键 词：普瑞巴林 Nα-(5-氟-2 4二硝基苯基)-D-缬氨酰胺 对映体 微波辅助 柱前衍生化 高效液相色谱 测定 

分 类 号：R9[医药卫生—药学]