离子液体乳相液液微萃取结合高效液相色谱法测定豆奶中的磺酰脲类除草剂

马铭扬; 徐尉力; 常珊珊; 王林; 梁正基; 李吉龙; 王志兵

doi:10.13386/j.issn1002-0306.2020020268

离子液体乳相液液微萃取结合高效液相色谱法测定豆奶中的磺酰脲类除草剂

长春工业大学化学与生命科学学院, 吉林长春 130012

基金项目:

国家自然科学基金青年科学基金项目（21401011）；吉林省教育厅"十三五"科学技术项目（JJKH20181014K）；2019年度国家级大学生创新创业训练项目（201910190010）。

详细信息

作者简介:
马铭扬(1999-),男,本科,研究方向:食品分析,E-mail:13634443875@163.com。

通讯作者:
王志兵(1982-),男,博士,副教授,研究方向:食品分析,E-mail:wangzhibing@ccut.edu.cn。

中图分类号: TS201.4
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出版历程
- 收稿日期: 2020-02-26
- 网络出版日期: 2021-01-20
- 刊出日期: 2021-01-14

Ionic Liquids Emulsion Phase Liquid-Liquid Microextraction Combined with High Performance Liquid Chromatography for Determination of Sulfonylurea Herbicides in Soy Milk

College of Chemistry and Life Science, Changchun University of Technology, Changchun 130012, China

摘要

摘要: 建立一种绿色、高效的涡旋/超声协同乳化离子液体乳相液液微萃取法，用于提取和富集豆奶中残留的噻吩磺隆、甲磺隆、醚苯磺隆、氯磺隆、苄嘧磺隆和吡嘧磺隆等6种磺酰脲类除草剂，并结合高效液相色谱法对目标分析物进行分离与测定。本方法以离子液体为萃取剂，以改性蒙脱土为固相分散吸附剂，经涡旋和超声协同作用促使离子液体乳化，形成离子液体乳相萃取液，增加离子液体与目标分析物的接触面积，通过改性蒙脱土对结合了目标分析物的离子液体进行吸附，经离心后改性蒙脱土与样液实现相分离，用定量乙腈解析改性蒙脱土中的目标分析物，解析液过滤后进行色谱分析。结果表明，在7.80~500.00 μg/L的线性范围内各目标分析物具有良好的线性关系（r>0.9990），其检出限（LODs）与定量限（LOQs）分别为1.60~3.15和5.34~10.12 μg/L。各目标分析物的日内精密度和日间精密度（RSD）分别为1.31%~5.07%和1.12%~6.63%，加标回收率在81.55%~116.44%之间，相对标准偏差在0.05%~8.91%之间。本法以离子液体为萃取剂，将涡旋/超声协同乳化与离子液体液液微萃取相结合，集样品提取、分离、净化于一体，具有萃取效率高、操作简单和绿色环保等优点。
- 离子液体乳相液液微萃取 /
- 涡旋-超声协同乳化 /
- 分散固相萃取 /
- 改性蒙脱土 /
- 磺酰脲类除草剂 /
- 高效液相色谱
Abstract: A green and efficient vortex-ultrasonic co-emulsification combined with ionic liquids emulsion phase liquid-liquid microextraction method was developed for extraction and enrichment of six sulfonylurea herbicides such as thifensulfuron,metsulfuron,sulfensulfuron,chlorsulfuron,benzsulfuron and pyrimisulfuron in soybean milk. High performance liquid chromatography was used for the separation and determination of target analytes. In the proposed method,ionic liquid was used as an extractant and modified montmorillonite was used as solid phase adsorbent. The synergism of vortex and ultrasound promoted the emulsification of the ionic liquid and increased the contact area between the ionic liquid and the target analyte. After dispersive liquid-liquid microextraction,the ionic liquids combined with the target analytes were adsorbed by modified montmorillonite. Subsequently,the modified montmorillonite was separated from sample solution through centrifugation. The quantitative acetonitrile solution was used to desorb the target analytes from modified montmorillonite. The desorption solution was used for chromatographic analysis after passing through the 0.22 μm filter membrane. The experimental results showed that good linearities with the correlation coefficients higher than 0.9990 were obtained under the optimum conditions. The limits of detection(LODs)and quantification(LOQs)were in the range of 1.60~3.15 and 5.34~10.12 μg/L,respectively. The intra-day precision and inter-day precision of each target analyte were 1.31%~5.07% and 1.12%~6.63%,respectively. The spiked recovery was between 81.55%~116.44% and the relative standard deviation was between 0.05%~8.91%,respectively. In the proposed method,ionic liquid was used as extraction solvent instead of organic solvent. This method combined vortex and ultrasound-assisted dispersive liquid-liquid microextraction with dispersive solid-phase extraction based on modified montmorillonite,and integrated sample extraction,separation,and purification into one step. The present method has the advantages of high extraction efficiency,simple operation and low cost,and can be used for the separation and detection of sulfonylurea herbicides in commercially available packaged soy milk.

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