色谱

色谱 ›› 2015, Vol. 33 ›› Issue (5): 501-507.DOI: 10.3724/SP.J.1123.2014.12043

• 研究论文 • 上一篇    下一篇

QuEChERS-液相色谱-串联质谱法测定甜玉米及毛豆中32种磺酰脲类除草剂残留

王连珠1, 黄小燕1, 王登飞1, 陈泳1, 徐敦明2, 周昱2   

  1. 1. 漳州出入境检验检疫局, 福建 漳州 363100;
    2. 厦门出入境检验检疫局, 福建 厦门 361012
  • 收稿日期:2014-12-30 发布日期:2015-04-23
  • 通讯作者: 王连珠
  • 基金资助:

    福建省自然科学基金项目(2011J01386).

Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry

WANG Lianzhu1, HUANG Xiaoyan1, WANG Dengfei1, CHEN Yong1, XU Dunming2, ZHOU Yu2   

  1. 1. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363100, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China
  • Received:2014-12-30 Published:2015-04-23

PDF

202

被引次数

30

摘要：

建立了基于QuEChERS方法的液相色谱-串联质谱同时测定甜玉米及毛豆中32种磺酰脲类除草剂残留的方法。以提取液净化前后蒸发残渣质量及回收率为考察指标,评估了C18、氧化锆包覆硅胶(Z-Sep)/C18混合物、C18键合锆胶(Z-Sep+) 3种分散吸附剂对甜玉米的净化效果,结果Z-Sep/C18吸附剂的净化效果最佳。样品采用乙腈提取、无水硫酸镁及氯化钠盐析、Z-Sep/C18分散固相萃取净化;液相色谱以CSH C18色谱柱梯度洗脱分离,质谱分析采用电喷雾负离子电离、按时间表的多反应监测模式(Scheduled MRM),以基质匹配校准曲线外标法进行定量。32种农药在甜玉米及毛豆中3个添加水平(10、20、100 μg/kg)的回收率为80.0%~108.2%,相对标准偏差为1.2%~13.0%, 32种农药的定量限(S/N≥10)为0.2~5.0 μg/kg。方法简便、灵敏、环保,适用于甜玉米及毛豆中32种磺酰类除草剂残留的定性定量分析。

关键词: QuEChERS, 磺酰脲类除草剂, 毛豆, 甜玉米, 氧化锆, 液相色谱-串联质谱

Abstract:

A fast method based on QuEChERS methodology for the simultaneous determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The clean-up effects of three dispersive sorbents were evaluated in terms of the residue mass for extracts after evaporation and recoveries. The three sorbents were C18, a mixture of two sorbents silica coated with zirconium dioxide (Z-Sep) and C18, a bonded C18 zirconia-coated silica (Z-Sep+). As a result, the best effects were obtained from using Z-Sep/C18 sorbents. The samples were extracted with acetonitrile, and salted out with anhydrous magnesium sulphate and sodium chloride. The extracts were cleaned up with dispersive solid phase extraction using Z-Sep/C18 sorbents. Chromatographic analysis was carried out using a CSH C18 column with gradient elution. The pesticides were analyzed by negative electrospray ionization tandem mass spectrometry under scheduled multiple reaction monitoring mode. The quantification was achieved using matrix-matched standard calibrations as the external standard. The recoveries at fortification levels of 10, 20, 100 μg/kg in sweet corns and green beans ranged from 80.0% to 108.2% with the relative standard deviations of 1.2%-13.0%. The limits of quantification (S/N≥10) were 0.2-5.0 μg/kg. The method has been proven to be simple, sensitive, environmental, and thus suitable for the determination of the 32 sulfonylurea herbicide residues in sweet corns and green soybeans.

Key words: green soybean, liquid chromatography-tandem mass spectrometry (LC-MS/MS), QuEChERS, sulfonylurea herbicide, sweet corn, zirconium dioxide

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