文献类型：期刊文献

中文题名：2,4-二硝基氟苯柱前衍生化法测定普瑞巴林

英文题名：Determination of Pregabalin by HPLC with Precolumn Derivatization Using 1-Fluoro-2,4-dinitrobenzene

作者：巫婷[1];景秋芳[2];叶波[3];沈永嘉[1]

机构：[1]华东理工大学精细化工研究所结构可控先进功能材料及其制备教育部重点实验室,上海200237;[2]华东理工大学药学院,上海200237;[3]浙江三门腾龙化工有限公司,浙江三门317100

年份：2010

卷号：24

期号：2

起止页码：350

中文期刊名：高校化学工程学报

外文期刊名：Journal of Chemical Engineering of Chinese Universities

收录：CSTPCD;;EI(收录号：20102112958480);Scopus;北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；

语种：中文

中文关键词：普瑞巴林;2,4-二硝基氟苯;高效液相色谱;柱前衍生化

外文关键词：Pregabalin; 1-fluoro-2; 4-dinitrobenzene; HPLC; precolumn derivatization

摘要：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。
A high performance liquid chromatographic （HPLC） method with UV detection was developed to determine the content of Pregabalin （PGB） by using 1-fluoro-2,4-dinitrobenzene （DNFB） as the precolumn derivatization reagent. The effects of light, reaction temperature, molar ratio of DNFB to PGB and reaction time on the derivatization reaction were investigated. Chromatographic separation was achieved on a C18 column with a mixture of phosphate buffer and acetonitrile as the mobile phase. The relationship between the PGB concentration and the PGB-DNFB peak area on the chromatograph is linear over the PGB concentration range of 8～48 μg·mL-1 （r = 0.9998）. The recover ratio is （100.03 ± 1.10）% （n = 9）. The within-day precisions are 0.82%, 0.77% and 1.87% for three different PGB concentrations （n = 6）, respectively. The derivative solution is stable within 8 hours （RSD = 1.92%）. The LOD is as low as 0.8 ng·mL-1. The proposed PGB content determination method is simple, rapid, accurate and reliable.