胶束电动色谱-激光诱导荧光检测法测定肌松弛药巴氯芬  

Determination of baclofen using micellar electrokinetic chromatography with laser induced fluorescence detection

作　　者：王宇飞[1] 杨甲甲[1] 蔡元丽[1] 林夏[1] 李晖[1] 

机构地区：[1]四川大学化学工程学院,四川成都610065

出　　处：《色谱》2011年第12期1230-1235,共6页Chinese Journal of Chromatography

摘　　要：以4-氯-7-硝基苯并-2-氧杂-1,3-二唑(NBD-Cl)为柱前衍生试剂,建立了胶束电动色谱-激光诱导荧光检测法测定肌松弛药巴氯芬(BAL)的新方法。经过实验条件的优化,采用15 mmol/L硼砂、20 mmol/L十二烷基硫酸钠、10%(v/v)乙腈、pH 9.75的缓冲体系,在分离电压为17.5 kV、柱温为25℃的条件下,压力进样3.45 kPa(0.5 psi)×3 s,巴氯芬及其内标物的衍生产物在7 min内实现较好的基线分离,线性范围为0.025～25 mg/L,相关系数为0.999 9,检出限(S/N=3)和定量限(S/N=10)分别为0.90μg/L和6.25μg/L。该方法被应用于巴氯芬制剂及加入巴氯芬对照品的尿液样品分析,回收率范围分别为101.6%～107.9%和107.0%～109.6%。该方法有望应用于巴氯芬药物制剂的质量监控以及为巴氯芬药物代谢的研究提供辅助手段。A novel micellar electrokinetic chromatographic method with laser induced fluorescence detection after derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole（NBD-Cl） was developed for the determination of muscle relaxant drug baclofen（BAL）.After optimization,baseline separation of the derivatives of BAL and gabapentin（internal standard） was obtained within 7 min in a running buffer（pH 9.75） composed of 15 mmol/L sodium borate,20 mmol/L sodium dodecyl sulfate and 10%（v/v） acetonitrile.The separation voltage was 17.5 kV.The column temperature was 25 ℃.The samples were injected by a pressure of 3.45 kPa（0.5 psi） for 3 s.The method has a linear range of 0.025-25 mg/L for BAL with the correlation coefficient of 0.999 9.The limit of detection（LOD,S/N=3） and the limit of quantification（LOQ,S/N=10） were 0.90 μg/L and 6.25 μg/L,respectively.The developed method was used for the analysis of BAL pharmaceutical preparation and urine samples spiked with BAL standard.The ranges of recovery were 101.6%-107.9% for BAL preparation and 107.0%-109.6% for urine samples.This method can be applied to the quality assessment of baclofen drug products,and provide supplementary means for the drug metabolism research of baclofen.

关 键 词：毛细管电泳 胶束电动色谱-激光诱导荧光检测 衍生化 巴氯芬 4-氯-7-硝基苯并-2-氧杂-1 3-二唑 

分 类 号：O658[理学—分析化学]