色谱

色谱 ›› 2015, Vol. 33 ›› Issue (7): 753-758.DOI: 10.3724/SP.J.1123.2015.03014

• 研究论文 • 上一篇    下一篇

离子液体均相液液微萃取-高效液相色谱法测定婴儿奶粉中5种三嗪类除草剂

张丽媛1,2, 姚笛2, 李娜1, 张寒琦1, 于爱民1   

  1. 1. 吉林大学化学学院, 吉林 长春 130012;
    2. 黑龙江八一农垦大学食品学院, 黑龙江 大庆 163319
  • 收稿日期:2015-03-17 出版日期:2015-07-08 发布日期:2015-07-27
  • 通讯作者: 于爱民
  • 基金资助:

    国家自然科学基金面上项目(31171657);国家重大科学仪器设备开发专项项目(2011YQ1401500);黑龙江省农垦总局项目(HNK125B-13-03).

Determination of five triazine herbicides in infant milk powder by high performance liquid chromatography coupled with ionic liquid-based homogeneous liquid-liquid microextraction

ZHANG Liyuan1,2, YAO Di2, LI Na1, ZHANG Hanqi1, YU Aimin1   

  1. 1. College of Chemistry, Jilin University, Changchun 130012, China;
    2. College of Food, Heilongjiang Bayi Agricultural University, Daqing 163319, China
  • Received:2015-03-17 Online:2015-07-08 Published:2015-07-27

PDF

122

被引次数

6

摘要：

建立了婴儿配方奶粉中三嗪类除草剂的均相液液微萃取-高效液相色谱分析方法。以离子液体为液液微萃取溶剂,Eclipse XDB-C18为色谱柱,乙腈和水为流动相梯度洗脱分离。详细研究了液液微萃取条件对实验结果的影响。在最优实验条件下,三嗪类除草剂的标准曲线呈良好的线性(r≥0.9992),草净津、敌草净、特丁通、特丁津和异戊乙净的检出限分别是12.1、13.8、11.8、14.6和13.7 μg/kg;婴儿配方奶粉中的加标回收率为92.2%~103.2%,相对标准偏差低于6%。该方法灵敏度高、操作简单,适用于奶粉样品中三嗪类除草剂残留的检测。

关键词: 高效液相色谱法, 均相液液微萃取, 离子液体, 三嗪除草剂, 婴儿奶粉

Abstract:

A high performance liquid chromatography coupled with homogeneous liquid-liquid microextraction was developed for the determination of five triazine herbicides in infant milk powders. The ionic liquid was used as microextraction solvent. The separation of the herbicides was performed on an Eclipse XDB-C18 column using acetonitrile and water as mobile phases in gradient mode. The effects of homogeneous liquid-liquid extraction conditions on the experimental results were investigated in detail. Under the optimized experimental conditions, the calibration curves for determining the analytes were linear and the correlation coefficients were ≥0.9992. The limits of detection for cyanazine, desmetryn, terbumeton, terbuthylazine and dimethametryn were 12.1, 13.8, 11.8, 14.6 and 13.7 μg/kg, respectively. The recoveries of the analytes spiked in four infant milk powders ranged from 92.2% to 103.2% and the relative standard deviations were lower than 6%. This method is sensitive, simple, and suitable for the determination of triazine herbicides in milk powder samples.

Key words: high performance liquid chromatography (HPLC), homogeneous liquid-liquid microextraction, infant milk power, ionic liquid, triazine herbicides

中图分类号: