色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱法同时测定布洛芬注射液中布洛芬和精氨酸的含量

刘静, 马鹤群, 朱萌, 王欢, 张天虹*   

  1. 沈阳药科大学, 辽宁 沈阳 110016
  • 收稿日期:2011-05-06 修回日期:2011-06-14 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 张天虹,博士,副教授,主要从事药物分析及药物动力学研究. Tel: (024)23984159,

Simultaneous determination of ibuprofen and arginine in ibuprofen injection using ultra performance liquid chromatography

LIU Jing, MA Hequn, ZHU Meng, WANG Huan, ZHANG Tianhong*   

  1. Shenyang Pharmaceutical University, Shenyang 110016, China
  • Received:2011-05-06 Revised:2011-06-14 Online:2011-10-28 Published:2011-10-13

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摘要： 建立了一种同时测定布洛芬注射液中布洛芬和精氨酸含量的超高效液相色谱方法。精氨酸与衍生化试剂2,4-二硝基氟苯(DNFB)反应后,与布洛芬同时在超高效液相色谱-二极管阵列检测器(UPLC-PDA)上检测。采用BEH C18色谱柱(50 mm×2.1 mm, 1.7 μm),以乙腈-0.05 mol/L磷酸二氢钾缓冲液(pH 2.5)为流动相进行梯度洗脱,流速为0.4 mL/min,柱温为30 ℃,检测波长分别为357 nm(精氨酸衍生物)和220 nm(布洛芬)。结果表明,布洛芬与精氨酸分别在2.0～100.5 mg/L和1.7～84.5 mg/L范围内呈良好的线性关系,相关系数(r)均为0.9997;平均回收率分别为99.8%和99.6%,相对标准偏差(RSDs)分别为0.37%和0.25%;定量限(信噪比（S/N）=10)分别为0.1 ng和0.2 ng;检出限(S/N=3)分别为0.03 ng和0.05 ng。本方法快速、准确,重复性好,可较全面地评价布洛芬注射液的质量。

关键词: 布洛芬, 布洛芬注射液, 超高效液相色谱, 精氨酸, 柱前衍生

Abstract: An ultra performance liquid chromatography-photodiode array detector (UPLC-PDA) method was developed for the determination of ibuprofen and the solubilizer arginine in ibuprofen injection. 2,4-Dinitroflurobenzene (DNFB) was used as the precolumn derivatization reagent. The separation of ibuprofen and arginine derivative was performed on a BEH C18 column (50 mm×2.1 mm, 1.7 μm) with the mobile phase consisting of acetonitrile-0.05 mol/L potassium dihydrogen phosphate (pH 2.5) in a gradient elution mode at a flow rate of 0.4 mL/min. Ultraviolet absorption detection wavelengths were set at 357 nm for arginine derivative and 220 nm for ibuprofen. The column temperature was set at 30 ℃. Good linearities were obtained in the ranges of 2.0~100.5 mg/L for ibuprofen and 1.7~84.5 mg/L for arginine, both with the correlation coefficients (r) of 0.9997. The spiked recoveries were 99.8% and 99.6% with the relative standard deviations (RSDs) of 0.37% and 0.25% for ibuprofen and arginine, respectively. Their respective limits of quantification (LOQs) (S/N=10) were 0.1 ng and 0.2 ng, and the limits of detection (LODs) (S/N=3) were 0.03 ng and 0.05 ng. The results demonstrated that the proposed method is simple, accurate, reproducible and suitable for the quality control of ibuprofen injection.

Key words: arginine, ibuprofen, ibuprofen injection, pre-column derivatization, ultra performance liquid chromatography (UPLC)