2,4-二硝基氟苯柱前衍生化法测定普瑞巴林Determination of Pregabalin by HPLC with Precolumn Derivatization Using 1-Fluoro-2,4-dinitrobenzene
巫婷,景秋芳,叶波,沈永嘉
摘要(Abstract):
利用2,4-二硝基氟苯为柱前衍生剂,建立了用高效液相色谱法测定普瑞巴林的方法。考察了光、反应温度、摩尔比和反应时间对衍生化反应的影响,确定了最佳衍生反应条件:在65℃水浴中避光反应75min。色谱柱为C18,流动相为50mmol·L-1KH2PO4(pH=3.0)/乙腈(30/70,v/v),检测波长为360nm,流速为1.0mL·min-1,柱温为35℃。实验结果:在8~48μg·mL-1范围内呈较好的线性关系(r=0.9998),回收率(100.03±1.10)%(n=9),不同浓度下日内精密度0.82%、0.77%和1.87%,8h内稳定性良好(RSD=1.92%),检测限低至0.8ng·mL-1。实验表明该方法简便、快速、准确、灵敏。通过对该方法的实际应用,三批样品测定值的RSD分别为0.59%、0.68%和1.04%,表明该方法能够用于测定普瑞巴林的含量。
关键词(KeyWords): 普瑞巴林;2,4-二硝基氟苯;高效液相色谱;柱前衍生化
基金项目(Foundation):
作者(Author): 巫婷,景秋芳,叶波,沈永嘉
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