Guo C, Hu J-Y, Chen X-Y, Li J-Z
Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, People's Republic of China.
Bull Environ Contam Toxicol. 2008 Feb;80(2):173-7. doi: 10.1007/s00128-007-9340-2. Epub 2008 Jan 9.
An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.
建立了一种测定大豆中咪唑喹啉酸残留量的分析方法。所开发的液/液分配和强阴离子交换固相萃取程序可有效净化,去除最多数量的样品基质干扰物。通过用磷酸优化流动相pH值、水/乙腈条件,使用C-18反相色谱柱并采用紫外检测,实现了出色的峰分离度。本文报道的联合净化和色谱方法步骤对于测定大豆样品中的咪唑喹啉酸残留量灵敏且可靠。该方法的特点是回收率>88.4%,精密度<6.7%变异系数,灵敏度为0.005 ppm,符合残留分析方法验证的指令要求。大豆中的咪唑喹啉酸残留量通过高效液相色谱-质谱联用(LC-MS)进一步确证。所提出的方法成功应用于分析经咪唑喹啉酸制剂处理后的试验田中种植的大豆样品中的咪唑喹啉酸残留量。