分散固相萃取-高效液相色谱法测定柑橘中四螨嗪的残留量
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农业部农药残留田间试验项目(2011P107)


HPLC determination of clofentezine in oranges with dispersive solid phase extraction
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    摘要:

    建立了高效液相色谱法快速检测柑橘中四螨嗪残留量的方法。试样经乙腈提取,使用N-丙基乙二胺键合固相吸附材料(PSA)和C18吸附剂净化,在C18柱上以乙腈-水(V∶V=70∶30)为流动相进行分离,在268 nm波长下检测。四螨嗪在0.05~5.00 mg/L时线性关系良好(R2=0.999 3);柑橘果肉和果皮中四螨嗪的最低检测限(LOD)均为0.05 mg/kg;在0.05~1.00 mg/kg添加水平时,果肉和果皮中四螨嗪的回收率分别为77.6%~91.6%、79.3%~105.6%,相对标准偏差(RSD)均低于8.1%。

    Abstract:

    A quick method was developed for determining clofentezine residues in oranges by HPLC with dispersive solid phase extraction.The residues of clofentezine in samples was extracted by acetronitrile,cleaned up by PSA and C18 adsorbent.HPLC was performed on a C18 column with UV detection at 268 nm using acetonitrile-water(70∶30,V/V) as mobile phase.The newly developed method showed a good linear relationship at the range of 0.05-5.00 mg/L with good precision and accuracy for clofentezine(R2=0.999 3).The limit of quantification (LOD) of clofentezine in orange pulp and peel was all 0.05 mg/kg.With RSD lower than 8.1% for pulp and peel,the average recoveries were 77.6%-91.6% and 79.3%-105.6% for pulp and peel samples spiked with 0.05-1.00 mg/kg of clofentezine,respectively.

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杨愿愿,杨晓云,黄其亮,洪海,苗雪雪,徐汉虹.分散固相萃取-高效液相色谱法测定柑橘中四螨嗪的残留量[J].华中农业大学学报,2013,32(4):73-76

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