食品科学 ›› 2012, Vol. 33 ›› Issue (10): 264-267.doi: 10.7506/spkx1002-6630-201210055

• 分析检测 • 上一篇    下一篇

离子液体萃取- 荧光猝灭法测定富硒保健品和食盐中的硒(Ⅳ)

武玉杰,孙汉文*,夏祥华   

  1. 河北大学化学与环境科学学院,河北省分析科学重点实验室
  • 出版日期:2012-05-25 发布日期:2012-05-07
  • 基金资助:
    河北省自然科学基金项目(B2008000583)

Determination of Se (Ⅳ) in Se-Enriched Health Food and Salt Samples Using Ionic Liquid Extraction Combined with Fluorescence Quenching Method

WU Yu-jie,SUN Han-wen*,XIA Xiang-hua   

  1. (Key Laboratory of Analytical Science of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China)
  • Online:2012-05-25 Published:2012-05-07

摘要: 建立保健品和食盐中硒(Ⅳ)的离子液体萃取-荧光猝灭法。样品经微波消解,在0.2mol/L盐酸介质条件下,硒(Ⅳ)氧化碘化钾,其反应产物I3-与罗丹明B形成离子缔合物。10g/100mL碘化钾1mL,0.005g/100mL罗丹明B 3mL,以0.5mL 1-丁基-3-甲基咪唑六氟磷酸盐将离子缔合物萃取进入离子液体相。结果表明,荧光淬灭值与硒(Ⅳ)的质量浓度呈正比,线性范围2~60μg/L,方法的定量限(RSN=10)为20μg/kg,平均回收率为87.9%~105%。该方法具有操作简易、无污染、灵敏度高等优点,可用于富硒保健品和食盐中微量硒的测定。

关键词: 微波消解, 室温离子液体, 荧光猝灭, 硒, 食品

Abstract: Sample was digested by microwave. Potassium iodide is oxidized by Se (Ⅳ) in medium of 0.2 mol/L hydrochloric acid,the product I3- reacts with rhodamine B to form ion complex. Potassium iodide of 1 mL at 10 g/100mL and rhodamine B of 3 mL at 0.005 g/100mL were used. The formed ion complex was extracted into the 0.5 mL ionic liquid phase (C4MIM)PF6. The quenched fluorescence was observed for rhodamine B in the presence of Se (Ⅳ). The linear determination range of Se (Ⅳ) was between 2 and 60μg/L. The limit of quantification of method (RSN=10) for selenium was 20μg/kg, and the average recoveries were from 87.9% to 105%. The proposed method has the characteristics of easy operation, no pollution and high sensitivity, and it can be used for the analysis of trace selenium in zinc-selenium health food and fortified nutrient salt.

Key words: microwave digestion, room temperature ionic liquid, fluorescence quenching, selenium, food

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