色谱

色谱

• 技术与应用 • 上一篇    下一篇

整体柱离子对色谱-直接电导检测法快速测定微量碘酸根

刘玉珍,于泓,李偲文   

  1. 哈尔滨师范大学化学化工学院, 黑龙江 哈尔滨 150025
  • 收稿日期:2011-04-19 修回日期:2011-06-03 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 于泓,博士,教授,主要从事离子色谱和液相色谱的分析研究. Tel: (0451)88060570,
  • 基金资助:
    黑龙江省自然科学基金资助项目|哈尔滨师范大学科技发展预研项目

Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection

LIU Yuzhen, YU Hong*, LI Siwen   

  1. College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China
  • Received:2011-04-19 Revised:2011-06-03 Online:2011-10-28 Published:2011-10-13

PDF

395

被引次数

3

摘要： 建立了整体柱离子对色谱-直接电导检测快速测定微量碘酸根的方法。采用反相硅胶整体柱,以氢氧化四丁铵(TBA)-邻苯二甲酸-水-乙腈水溶液为淋洗液,分别讨论了淋洗液、流速及柱温对碘酸根保留的影响,并确定最佳色谱条件为: 以0.25 mmol/L TBA-0.18 mmol/L邻苯二甲酸-3%乙腈(pH 5.5)水溶液为淋洗液,流速4.0 mL/min,柱温30 ℃。在此条件下,碘酸根与其他常见阴离子(Cl~、NO~3、SO2~4和I~)达到基线分离且保留时间在0.5 min之内,检出限(S/N=3)为0.36 mg/L,峰面积和保留时间的相对标准偏差(n=5)分别为0.35%和0.28%。方法应用于加碘药品中微量碘酸根的测定,加标回收率为96.4%。本方法快速、简单、准确、可靠,具有良好的实用性。

关键词: 碘酸根, 电导检测, 离子对色谱, 整体柱

Abstract: A method was developed on a monolithic column for the fast determination of trace iodate (IO~3) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0.25 mmol/L TBA-0.18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 ℃. Under the optimal conditions, retention time of iodate was less than 0.5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl~, NO~3, SO2~4, I~). The detection limit (S/N=3) was 0.36 mg/L for IO~3. Relative standard deviation (RSD, n=5) of chromatographic peak area and retention time were 0.35% and 0.28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96.4%. The method is rapid, simple, accurate, reliable, and practical.

Key words: ion-pair chromatography, conductivity detection, iodate, monolithic column