色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-离子交换色谱法测定浓缩苹果汁中残留的苯菌灵、多菌灵、噻菌灵

何强1,孔祥虹1,赵洁2,李建华1,乐爱山1,张莹1   

  1. 1.Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi’an 710068, China; 2.College of Science, Xi’an University of Technology, Xi’an 710054, China
  • 收稿日期:2008-10-27 修回日期:2008-10-27 出版日期:2008-10-27 发布日期:1983-09-25
  • 通讯作者: 何强
  • 基金资助:
    国家质量监督检验检疫总局课题(No. 2007IK166)

Determination of benomyl, carbendazim and thiabendazole in apple juice concentrate using solid-phase extraction coupled with ion exchange chromatography

HE Qiang1, KONG Xianghong1, ZHAO Jie2, LI Jianhua1, YUE Aishan1, ZHANG Ying1   

  1. 1.Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi’an 710068, China; 2.College of Science, Xi’an University of Technology, Xi’an 710054, China
  • Received:2008-10-27 Revised:2008-10-27 Online:2008-10-27 Published:1983-09-25
  • Contact: HE Qiang

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摘要： 建立固相萃取-离子交换色谱法测定浓缩苹果汁中苯菌灵、多菌灵和噻菌灵的残留量。样品直接用水稀释后，于80 ℃下将苯菌灵完全转化为多菌灵，再经SCX固相萃取柱富集,采用LC-SCX离子交换色谱柱(25 cm×4.6 mm,5 μm)分离,二极管阵列检测器检测,以0.1 mol/L KH2PO4溶液(pH 2.5)-乙腈(体积比为70 ∶30)为流动相,在1.0 mL/min下等度洗脱,于282 nm波长下检测。在0.02～2.0 mg/L范围内，多菌灵和噻菌灵的峰面积与其浓度呈良好的线性关系,最低检出限均可达到0.004 mg/kg,回收率为94.2%～100.4%,相对标准偏差低于4.2%。该方法简便、快速、灵敏、准确,可用于浓缩苹果汁中苯菌灵、多菌灵和噻菌灵残留量的检测。

关键词: 苯菌灵, 多菌灵, 固相萃取, 离子交换色谱, 浓缩苹果汁 , 噻菌灵

Abstract: A method was developed for the determination of benomyl, carbendazim and thiabendazole in apple juice concentrate by solid-phase extraction coupled with ion exchange chromatography (IEC). The sample was diluted with water, and then benomyl was degradated completely to carbendazim at 80 ℃, and purified by an SCX solid-phase extraction column. Liquid chromatographic analysis was performed on the instrument of Agilent 1200 series equipped with a diode-array detector and autosampler. The column was LC-SCX (25 cm×4.6 mm, 5 μm). The mobile phase was 0.1 mol/L KH2PO4 (pH 2.5)-acetonitrile (70∶30, v/v) with a flow rate of 1.0 mL/min. The presented method showed good linear relationship with good precision and accuracy at the range of 0.02-2.0 mg/L for carbendazim and hiabendazole. The detection limits were 0.004 mg/kg for carbendazim and thiabendazole. The method was characterized with cceptable sensitivity to meet the requirements for monitoring these pesticides in apple juice concentrate.

Key words: apple juice concentrate , benomyl, carbendazim, ion exchange chromatography （IEC）, thiabendazole, solid-phase extraction （SPE）