色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1230-1235.DOI: 10.3724/SP.J.1123.2011.01230

• 研究论文 • 上一篇    下一篇

胶束电动色谱-激光诱导荧光检测法测定肌松弛药巴氯芬

王宇飞, 杨甲甲, 蔡元丽, 林夏, 李晖*   

  1. 四川大学化学工程学院, 四川 成都 610065
  • 收稿日期:2011-07-12 修回日期:2011-08-21 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 李晖,教授,博士生导师,研究方向为药物分析

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

WANG Yufei, YANG Jiajia, CAI Yuanli, LIN Xia, LI Hui*   

  1. College of Chemical Engineering, Sichuan University, Chengdu 610065, China
  • Received:2011-07-12 Revised:2011-08-21 Online:2011-12-28 Published:2012-01-15

PDF

801

被引次数

9

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0.9999,检出限(S/N=3)和定量限(S/N=10)分别为0.90 μg/L和6.25 μg/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。

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

Abstract: 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 0.9999. 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.

Key words: 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl), baclofen, micellar electrokinetic chromatography-laser induced fluorescence detection (MEKC-LIFD), capillary electrophoresis (CE), derivatization