色谱

色谱 ›› 2012, Vol. 30 ›› Issue (04): 414-418.DOI: 10.3724/SP.J.1123.2011.12070

• 特别策划 • 上一篇    下一篇

离子色谱积分脉冲安培法同时测定血浆中阿仑膦酸钠、帕米膦酸钠、伊班膦酸钠和利塞膦酸钠

陈郁1, 刘玉秀2, 陈智栋2, 陈梅兰3*, 朱岩4   

  1. 1. 杭州职业技术学院 2. 常州大学石油化工学院 3. 浙江树人大学生物与环境工程学院 4. 浙江大学化学系
  • 收稿日期:2011-12-19 修回日期:2012-02-15 出版日期:2012-04-28 发布日期:2012-04-28
  • 通讯作者: 陈梅兰,教授,研究方向为环境化学. Tel: (0571)88297103,
  • 基金资助:

    浙江省自然科学基金一般项目(Y2110945)和浙江省科技计划项目(2011C37065).

Simultaneous determination of alendronate, pamidronate, ibandronate and risedronate using ion chromatography with integrated pulsed amperometric detection

CHEN Yu1, LIU Yuxiu2, CHEN Zhidong2, CHEN Meilan3*, ZHU Yan4   

  1. 1. Hangzhou Vocational and Technical College, Hangzhou 310018, China; 2. School of Chemistry and Chemical Engineering, Changzhou University, Changzhou 213164, China; 3. College of Biology and Environment Engineering, Zhejiang Shuren University, Hangzhou 310015, China; 4. Department of Chemistry, Zhejiang University, Hangzhou 310028, China
  • Received:2011-12-19 Revised:2012-02-15 Online:2012-04-28 Published:2012-04-28

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摘要： 建立了离子色谱积分脉冲安培检测器(IPAD)同时检测血浆中阿仑膦酸钠、帕米膦酸钠、伊班膦酸钠和利塞膦酸钠的方法。采用Dionex AS18 (250 mm×2 mm)和AG18 (50 mm×2 mm)色谱柱在24 mmol/L NaOH溶液中进行分离;对多电位波形参数优化以达到最大信噪比;采用优化后的波形方法对4种双膦酸盐类药物进行检测,具有良好的线性(r2为0.9972～0.9995)和重现性(峰面积的相对标准偏差(RSD)为0.84%～1.37%)及较高的灵敏度(检出限为0.061～0.18 μg/mL)。4种双膦酸盐在该方法中有很好的保留且有较好的分离度,与之前报道的衍生后检测方法相比,该方法不用衍生,更简单而易于操作。将该方法成功地用于人体血浆中双膦酸盐类的检测,其回收率为80.81%～97.32%, RSD为1.46%～3.02%。

关键词: 阿仑膦酸钠, 积分脉冲安培检测, 离子色谱, 利塞膦酸钠, 帕米膦酸钠, 血浆, 伊班膦酸钠

Abstract: A method for the simultaneous determination of alendronate, pamidronate, ibandronate and risedronate using ion chromatography with integrated pulsed amperometric detection (IPAD) has been developed. The electrochemical behavior showed the catalytic currents of these bisphosphonates are based on the oxidation of amines in their structures. Because the bisphosphonates are polar compounds and present as anions under alkaline condition, therefore, they can be separated by anion exchange chromatography. A Dionex AS18 column (250 mm×2 mm) and an AG18 column (50 mm×2 mm) and 24 mmol/L NaOH solution were used for the separation. Multi-step potential waveform parameters were optimized to maximize the signal-to-noise ratio (S/N), which exhibited adsorption/desorption catalytic features at the gold electrode surface in alkaline solution. Utilizing the optimized waveform, the method showed good linearity (r2=0.9972~0.9995), satisfactory repeatability (relative standard deviations (RSDs) of the peak areas in the range of 0.84%~1.37%) and sufficient sensitivity (limits of detection of 0.061~0.18 μg/mL) for the identification of the four bisphosphonates. The recoveries were 80.81%~97.32% with the RSDs of 1.46%~3.02%. It is demonstrated that this method is a rapid and simple one for the determination of the four bisphosphonates in human plasma.

Key words: alendronate, integrated pulsed amperometric detection (IPAD), pamidronate&mu, ibandronate&mu, ion chromatography (IC), plasma, risedronate&mu