色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定红小豆中残留的6种咪唑啉酮类除草剂

李成1,锁然1,王凤池2,马宏颖1   

  1. 1.College of Food Science, Agricultural University of Hebei, Baoding 071000, China; 2.Hebei Entry &Exit Inspection and Quarantine Bureau, Shijiazhuang 050071, China
  • 收稿日期:2008-05-21 修回日期:2008-08-21 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 李成
  • 基金资助:

Simultaneous determination of residues of six imidazolinone herbicides in adzuki beans by high performance liquid chromatography-electrospray ion trap tandem mass spectrometry

LI Cheng1, SUO Ran1, WANG Fengchi2, MA Hongying1   

  1. 1.College of Food Science, Agricultural University of Hebei, Baoding 071000, China; 2.Hebei Entry &Exit Inspection and Quarantine Bureau, Shijiazhuang 050071, China
  • Received:2008-05-21 Revised:2008-08-21 Online:2008-11-30 Published:1983-06-25
  • Contact: LI Cheng

PDF

664

摘要： 建立了同时测定红小豆中6种咪唑啉酮类除草剂残留的高效液相色谱-串联质谱分析方法。样品经0.1 mol/L NH4HCO3(pH 5)-甲醇(体积比为70∶30)溶液提取,二氯甲烷液-液萃取和凝胶渗透色谱净化后,采用Inertsil ODS-3色谱柱(2.1 mm×150 mm, 5 μm)分离，以甲醇-0.1%乙酸为流动相梯度洗脱,离子阱质谱在选择离子模式下测定。咪唑啉酮类除草剂在10～200 μg/L(灭草喹在5～100 μg/L)内线性关系良好,相关系数为0.9987～0.9997;方法的检出限为0.2～0.5 μg/kg;在红小豆中3个加标水平的平均加标回收率为81.6%～99.4%,相对标准偏差为3.1%～7.8%。该方法简便、灵敏度高、精密度好,适用于红小豆中多种咪唑啉酮类除草剂残留的测定。

关键词: 多残留分析, 高效液相色谱-串联质谱法, 红小豆 , 咪唑啉酮类除草剂, 凝胶渗透色谱

Abstract: A method for the simultaneous determination of six pesticides in adzuki beans by high performance liquid chromatography-electrospray ion trap tandem mass spectrometry was developed and evaluated. The sample was extracted with 0.1 mol/L NH4HCO3 (pH 5)-methanol (70∶30, v/v). The extract was partitioned with dichloromethane, and cleaned up with gel permeation chromatography. The separation was performed on an Inertsil ODS-3 column (150 mm×2.1 mm, 5 μm) with the gradient elution of methanol and 1% acetic acid as mobile phase. The identification and quantification were performed by electrospray ion trap mass spectrometry with selected ion monitoring mode. The calibration curves of imidazolinone herbicides showed good linearities in the range of 10-200 μg/L (5-100 μg/L for imazaquin) with the correlation coefficients between 0.9987 and0.9997. The limits of detection ranged between 0.2 μg/kg and 0.5 μg/kg (S/N=3). The average recoveries of six imidazolinone herbicides spiked in adzuki beans ranged between 81.6% and 99.4%(n=6) with the relative standard deviations of 3.1%-7.8%. The method has been used for the determination of 6 imidazolinone herbicides simultaneously in adzuki beans with easy operation, high accuracy and good precision.

Key words: adzuki beans , imidazolinone herbicides, liquid chromatography-tandem mass spectrometry （LC-MS/MS）, multiresidue determination, gel permeation chromatography