色谱

色谱

• 研究论文 • 上一篇    下一篇

柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂

支建梁,牟仁祥,陈铭学,朱智伟

  

  1. Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, China National Rice
    Research Institute, Hangzhou 310006, China
  • 收稿日期:2007-07-03 修回日期:2007-09-17 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 牟仁祥

Multi-residue determination of 15 phenylurea herbicides in vegetables using solid phase extraction and online post-column ultraviolet decomposition-fluorescent derivatization-high performance liquid chromatography

ZHI Jianliang, MOU Renxiang, CHEN Mingxue, ZHU Zhiwei

  

  1. Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, China National Rice
    Research Institute, Hangzhou 310006, China
  • Received:2007-07-03 Revised:2007-09-17 Online:2008-01-30 Published:1984-09-25

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摘要：

建立了蔬菜中15种苯脲除草剂残留的固相萃取-在线柱后紫外光分解和衍生化的高效液相色谱荧光检测分析方法。样品用乙腈提取,弗罗里硅土固相萃取柱净化,目标化合物由反相C18柱分离,经柱后紫外光分解和衍生化后进行荧光检测。对样品的前处理条件、液相色谱分离、柱后紫外光分解和衍生条件等进行了详细的研究。15种苯脲除草剂的高效液相色谱分离在乙腈-水梯度洗脱下完成,目标物的保留时间为9～31 min,线性范围内线性关系良好,相关系数为0.9986~1.0000;在洋葱、菠菜、黄瓜等样品中3个加标水平的平均回收率(n=3)为75.3%～121.6%,相对标准偏差为0.4%-11.6%;15种苯脲除草剂在蔬菜中的检出限为0.005～0.05 mg/kg。该方法操作简便、灵敏度高、选择性好,符合多种农药残留分析的要求。

关键词: 苯脲除草剂, 高效液相色谱, 固相萃取, 蔬菜 , 荧光衍生, 在线柱后紫外光解

Abstract:

A high performance liquid chromatographic (HPLC) method for multi-residue analysis of phenylurea herbicides in vegetables was developed. The sample was extracted with acetonitrile and cleaned up by solid phase extraction (SPE) using a Florisil cartridge. The target compounds were separated on a C18 column (250 mm×4.6 mm, 5 μm) and detected by a fluorescence detector (FLD) after online post-column ultraviolet (UV) decomposition with a UV lamp with 254 nm wavelength and fluorescent derivatization. The elution gradient, sample pretreatment and conditions of decomposition and derivatization were also studied. The elution gradient was as follows: the mobile phase started with 70%A （water） and 30%B （acetonitrile）, which was increased linearly to 50%B in 15 min, and increased 90%B in the next 15 min and held for 2 min, then returned to the initial conditions in 0.5 min. The column was equilibrated for 10 min at 25 ℃. The flow rate was 0.75 mL/min for HPLC and 0.2 mL/min for derivatization reagent. In the linear ranges of concentrations, the correlation coefficients were between 0.9986 and 1.0000. The 15 herbicides were measured in fortified onion, spinach and cucumber samples at three spiked levels, the average recoveries (n=3) were in the range of 75.3%-121.6% with relative standard deviations of 0.4%-11.6%. The limits of detection (LOD) were 0.005-0.05 mg/kg. The method is simple, sensitive, selective and qualified for phenylurea herbicide multi-residue analysis.

Key words: fluorescent derivatization, online post-column ultraviolet decomposition, phenylurea herbicides, solid phase extraction, vegetables , high performance liquid chromatography (HPLC)