食品科学

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温控辅助离子液体分散液液微萃取-高效液相色谱检测果汁中杀菌剂残留

张 琰1,2,赵其阳1,3,4,张耀海1,3,4,5,焦必宁1,2,3,4,5,*   

  1. 1.中国农业科学院柑桔研究所/西南大学柑桔研究所,重庆 400712;2.西南大学园艺园林学院,重庆 400715;
    3.农业部柑橘产品质量安全风险评估实验室,重庆 400712;4.农业部柑桔及苗木质量监督检验测试中心,重庆 400712;
    5.国家柑桔工程技术研究中心,重庆 400712
  • 出版日期:2015-02-25 发布日期:2015-02-16
  • 通讯作者: 焦必宁
  • 基金资助:

    农业部现代农业(柑桔)产业技术体系建设专项(CARS-27);2014年国家农产品质量安全风险评估重大专项(GJFP2014003);
    重庆市自然科学基金(重点)项目(cstc2013jjB80009)

Temperature-Controlled Ionic Liquid Dispersive Liquid-Liquid Microextraction Coupled with High Performance Liquid Chromatography for the Determination of Fungicide Residues in Fruit Juices

ZHANG Yan1,2, ZHAO Qiyang1,3,4, ZHANG Yaohai1,3,4,5, JIAO Bining1,2,3,4,5,*   

  1. 1. Citrus Reserch Institute, Chinese Academy of Agricultural Sciences/Southwest University, Chongqing 400712, China;
    2. College of Horticulture and Landscape Architecture, Southwest University, Chongqing 400715, China;
    3. Laboratory of Quality & Safty Risk Assessment for Citrus Products, Ministry of Agriculture, Chongqing 400712, China;
    4. Quality Supervision and Testing Center for Citrus and Seedling, Ministry of Agriculture, Chongqing 400712, China;
    5. National Center for Citrus Engineering, Chongqing 400712, China
  • Online:2015-02-25 Published:2015-02-16
  • Contact: JIAO Bining

摘要:

建立温控辅助离子液体分散液液微萃取结合高效液相色谱-二极管阵列检测器法检测果汁中7 种杀菌剂农药残留的新方法。对影响萃取效果的因素萃取剂和分散剂类型及体积、溶解温度、萃取时间和离心时间进行优化。在优化后的方法条件下,7 种杀菌剂富集倍数可达64~101;方法检出限在4.3~13.0 μg/L之间;在0.02、0.05 mg/L和0.10 mg/L三个水平下加标,果汁(苹果汁、梨汁、葡萄汁、桃汁和橙汁)的平均加标回收率在70.0%~116.2%范围内,相对标准偏差均小于9.8%,能满足多种果汁中杀菌剂农药多残留检测的要求。

关键词: 离子液体, 分散液液微萃取, 杀菌剂, 果汁

Abstract:

A novel method was developed for the determination of seven fungicide residues in fruit juices using temperaturecontrolled
ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) coupled with high performance liquid
chromatography with photodiode array detection (HPLC-PDA). Parameters affecting the extraction performance such as the
type and volume of extraction and dispersive solvents, temperature, extraction time and centrifugation time were studied and
optimized. Under optimized conditions, the enrichment factors ranged from 64 to 101, and the limits of detection of the established
method were in the range of 4.3–13.0 μg/L. The recoveries from apple, pear, grape, peach and orange juices at three fortified levels
of 0.02, 0.05 and 0.10 mg/L ranged from 70.0% to 116.2% with relative standard deviations (RSDs) less than 9.8%. Therefore, this
method can meet the requirements for the determination of fungicide residues in various fruit juices.

Key words: ionic liquid (IL), dispersive liquid-liquid microextraction (DLLME), fungicide, fruit juice

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