色谱 ›› 2014, Vol. 32 ›› Issue (4): 407-412.DOI: 10.3724/SP.J.1123.2013.11011

• 庆祝《色谱》创刊三十周年暨卢佩章院士九十华诞专刊-研究论文 • 上一篇    下一篇

整体柱固相萃取-高效液相色谱法在线分析水果中的氯吡脲

罗伟强1,2, 肖小华1, 杜卓1, 李攻科1   

  1. 1. 中山大学化学与化学工程学院, 广东 广州 510275;
    2. 广西民族大学化学化工学院, 广西 南宁 530006
  • 收稿日期:2013-11-05 修回日期:2013-12-12 出版日期:2014-04-08 发布日期:2014-03-28
  • 通讯作者: 肖小华, 李攻科
  • 基金资助:

    国家自然科学基金项目(21127008);高等学校博士学科点专项(20120171110001);广州市科技计划项目(12A102051514).

Monolith column solid-phase extraction coupled with high performance liquid chromatography in online mode for the determination of forchlorfenuron in fruits

LUO Weiqiang1,2, XIAO Xiaohua1, DU Zhuo1, LI Gongke1   

  1. 1. School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China;
    2. College of Chemistry and Chemical Engineering, Guangxi University for Nationalities, Nanning 530006, China
  • Received:2013-11-05 Revised:2013-12-12 Online:2014-04-08 Published:2014-03-28

摘要:

建立了整体柱固相萃取-高效液相色谱/紫外检测在线联用方法并用于水果中氯吡脲的分析测定。考察了萃取溶剂的pH值及其流速、溶剂解吸时间及其流速等因素对氯吡脲萃取率的影响。在优化的条件下,该方法对氯吡脲的富集倍数为214倍,方法的线性范围为0.01~50.00 μg/L,检出限为25 ng/L,相对标准偏差(RSD)为3.9%。黑葡萄、猕猴桃和西瓜等水果中氯吡脲的加标回收率为87.0%~120.7%,RSD为0.6%~9.2%。结果表明该方法快速、灵敏,能满足水果中痕量氯吡脲残留分析的要求。

关键词: 高效液相色谱, 固相萃取, 氯吡脲, 水果, 在线分析, 整体柱

Abstract:

A novel method based on the monolithic column solid-phase extraction (SPE) coupled with high performance liquid chromatography in online mode was developed for the determination of trace forchlorfenuron in fruits. The enrichment factor of SPE for forchlorfenuron was 214. The method was fully validated. It showed a linear range of 0.01-50.00 μg/L and a limit of detection of 25 ng/L, with the relative standard deviation (RSD) of 3.9%. The proposed method was successfully applied for the determination of forchlorfenuron in grape, kiwifruit and watermelon samples, with the recoveries of 87.0%-120.7% and the RSDs of 0.6%-9.2%. This online method was proved to be selective, sensitive and convenient for the determination of trace forchlorfenuron in complex samples.

Key words: forchlorfenuron, fruits, high performance liquid chromatography (HPLC), monolith column, online analysis, solid-phase extraction

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