高效液相色谱法同时测定大豆中12种酰胺类除草剂的残留量

建立了大豆中12种酰胺类除草剂多残留量同时检测的高效液相色谱方法。样品经丙酮提取、弗罗里硅土柱净化后,用高效液相色谱-二极管阵列检测器检测。在0.05～1.0 mg/kg的添加水平范围内,12种酰胺类药物的回收率为75%～102%,相对标准偏差为1.9%～16.1%；12种酰胺类除草剂的测定低限均能达到国家相关的残留限量要求。对样品的前处理条件进行了研究和优化,经商品化的固相萃取柱净化过的样品干扰杂质较少,有利于后续的检测分析和方法的推广应用。该方法能够在35 min内完成一次分析,具有快速、灵敏、准确、可靠的特点。

Simultaneous Determination of Residues of 12 Amide Herbicides in Soybeans by High Performance Liquid Chromatography

An analytical method was developed for the simultaneous determination of 12 amide herbicide residues in soybeans. The 12 amide herbicides were extracted with acetone from soybean samples. The extract was cleaned up using a Florisil cartridge, and then determined by high performance liquid chromatography. Kromasil 100-5 C18 column (4.6 mm i. d. x 250 mm, 5 microm) as analytical column, pure water-acetonitrile as mobile phase with a flow rate of 1.0 mL/min and gradient elution, and a diode array detector set at 210 nm were used. The recoveries of amide herbicides from soybeans spiked at levels of 0.05, 0.1 and 1.0 mg/kg were in the range of 75% - 102% with relative standard deviations of 1.9% - 16.1%. The method has good linear in the range of 0.05 - 1.0 mg/L for each analyte (nu > 0.999). The detection limit for each amide herbicide was less than 0.05 mg/kg. The method is simple, rapid and accurate. It can be used for the inspection of amide herbicide residues in soybeans.