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分散固相萃取-分散液液微萃取/高效液相色谱法测定西瓜中氟唑菌酰羟胺残留

智沈伟 李兴海 赵尔成 贾春虹 朱晓丹

分析测试学报2017,Vol.36Issue(10):1265-1268,4.
分析测试学报2017,Vol.36Issue(10):1265-1268,4.DOI:10.3969/j.issn.1004-4957.2017.10.018

分散固相萃取-分散液液微萃取/高效液相色谱法测定西瓜中氟唑菌酰羟胺残留

Determination of Pydiflumetofen Residues in Watermelon by High Performance Liquid Chromatography with Dispersive Solid-phase Extraction and Dispersive Liquid-Liquid Microextraction

智沈伟 1李兴海 2赵尔成 1贾春虹 2朱晓丹2

作者信息

  • 1. 沈阳农业大学植物保护学院,辽宁沈阳110866
  • 2. 北京市农林科学院植物保护环境保护研究所,北京 100097
  • 折叠

摘要

Abstract

A high performance liquid chromatography method for the determination of pydiflumetofen residues in watermelon was developed using dispersive solid-phase extraction and dispersive liquid-liquid microextraction as sample preparation methods.The samples were extracted with acetonitrile and water solution,purified with primary secondary amine as sorbents,and concentrated into 1,1,2,2-tetrachloroethane by dispersive liquid-liquid microextraction.The extracts were analyzed by high performance liquid chromatography.The conditions affecting the purification efficiency of the dispersed solid phase extraction,including the extraction solvent and the type of adsorbent were optimized.Factors affecting the extraction efficiency such as type and volume of extraction solvent,volume of dispersive solvent and salt concentration,were investigated.The results indicated that the calibration curves for the analytes were linear in the concentration range of 0.01-5 mg/L with the correlation coefficients of 0.999 9.The limits of quantification(S/N =10) were 0.01 mg/kg.The mean recoveries at three concentration levels of 0.01,0.1,1 mg/kg were in the range of 89.2%-94.5% with the relative standard deviations below 8.7%.With the advantages of simplicity,high efficiency and sensitivity,the proposed method was applicable for the analysis of pydiflumetofen residues in watermelon samples.

关键词

氟唑菌酰羟胺/分散固相萃取/分散液液微萃取/西瓜/高效液相色谱

Key words

pydiflumetofen/dispersive solid-phase extraction/dispersive liquid-liquid microextraction/watermelon/high performance liquid chromatography

分类

化学化工

引用本文复制引用

智沈伟,李兴海,赵尔成,贾春虹,朱晓丹..分散固相萃取-分散液液微萃取/高效液相色谱法测定西瓜中氟唑菌酰羟胺残留[J].分析测试学报,2017,36(10):1265-1268,4.

基金项目

国家自然科学基金项目(31301649) (31301649)

辽宁省自然科学基金(2015020766) (2015020766)

辽宁省教育厅科学研究项目(LSNYB201611) (LSNYB201611)

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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