色谱

色谱 ›› 2015, Vol. 33 ›› Issue (12): 1333-1337.DOI: 10.3724/SP.J.1123.2015.08036

• 技术与应用 • 上一篇    

二维离子色谱法同时测定4种无机阴离子和葡萄糖酸根离子

陈爱连, 丁卉, 方琳美, 施超欧   

  1. 华东理工大学分析测试中心, 上海 200237
  • 收稿日期:2015-08-31 出版日期:2015-12-08 发布日期:2012-06-21
  • 通讯作者: 施超欧

Determination of inorganic anions and gluconate by two-dimensional ion chromatography

CHEN Ailian, DING Hui, FANG Linmei, SHI Chaoou   

  1. Analysis and Testing Center, East China University of Science and Technology, Shanghai 200237, China
  • Received:2015-08-31 Online:2015-12-08 Published:2012-06-21

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摘要：

建立了一种新的二维离子色谱分析模式,应用阀切换技术并联抑制电导和脉冲安培双检测体系,同时测定Cl-、NO2-、SO42-、NO3-和葡萄糖酸根离子。第一维色谱采用Ionpac AG18+Ionpac AS18阴离子分析柱,分别以5和20 mmol/L的NaOH溶液等度淋洗,流速为1.0 mL/min,进样量为25 μL,抑制电导检测Cl-、NO2-、SO42-和NO3-。第二维色谱采用CarboPac PA1+CarboPac PA20两保护柱串联,以90 mmol/L NaOH溶液、0.8 mL/min的流速洗脱,由AG15柱分离富集葡萄糖酸根,脉冲安培检测器检测。结果表明:无机阴离子在0.1~5.0 mg/L、葡萄糖酸根在0.0856~4.2825 mg/L范围内有良好的线性关系,RSD在1.05%~1.94%之间,相关系数(R2)在0.9945以上;无机阴离子的方法检出限为0.615~2.17 μg/L,葡萄糖酸根的方法检出限为24.24 μg/L;回收率在90.3%~102.8%之间。该方法并联两种检测模式,有良好的准确度和精密度,适用于复杂样品的分离分析。

关键词: 电导检测, 二维离子色谱, 脉冲安培检测, 葡萄糖酸根, 无机阴离子

Abstract:

A new two-dimensional ion chromatography method was developed to parallelly analyze two different types of samples with the application of valve switching technology-suppressed conductivity and pulsed amperometric analysis system, for concurrent determination of chloride, nitrite, sulfate, nitrate four inorganic anions and gluconate. The first dimensional chromatography was using Ionpac AG18+Ionpac AS18 anion analysis columns with a suppressed conductivity detector for the separation and detection of Cl-, NO2-, SO42- and NO3-. Respectively, the elution was 5 and 20 mmol/L NaOH at an isocratic flow rate of 1.0 mL/min and sample injection volume of 25 μL. The second dimensional chromatography was utilizing two guard columns, CarboPac PA1 and CarboPac PA20, with 90 mmol/L NaOH solution for the isocratic eluent of 0.8 mL/min. Gluconate was enriched by an AG15 column and switched into the pulsed amperometric detector. The results showed that: each inorganic anion in 0.1-5.0 mg/L and gluconate in 0.0856-4.2825 mg/L had a good linear relationship (R2≥0.9945). The RSDs of the peak areas were between 1.05%-1.94%. The limits of detection were 0.61-2.17 μg/L for the anions and 24.24 μg/L for the gluconate. The recoveries were between 90.3%-102.8%. The two detection modes parallelly have good separation efficiency, detection accuracy and the precision of the separation and are suitable for the analysis of complex samples.

Key words: conductivity, gluconate, inorganic anion, pulsed amperometric, two-dimensional ion chromatography

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