高效液相色谱法测定花生仁中甲咪唑烟酸残留

Determination of Imazapic in Peanut Kernel by High Performance Liquid Chromatography

目前花生仁中甲咪唑烟酸残留量的检测是参考国标中茶叶农残的方法,花生仁基质含有大量的油脂和蛋白质,这与茶叶基质有显著区别,且该方法只能定性。本文建立了一种高效液相色谱法定量检测花生仁中甲咪唑烟酸残留量的方法。花生仁样品采用乙腈溶液提取后再经过除脂净化处理,以乙腈:0.02mol/L磷酸二氢钾缓冲液(加入0.1%的三乙胺,磷酸调pH3.0)体积比1:3作为流动相进行高效液相色谱紫外检测器分析。结果表明:甲咪唑烟酸标准在0~1.2mg/L范围内线性关系良好(R2=0.9999),检出限为7μg/kg;加标回收率为91.1%~98.9%;精密度、重复性、稳定性都较好。该方法操作简便、分离度好、结果准确,能很好地满足花生仁中甲咪唑烟酸残留量检测的要求。

At present, the detection method of imidazolium nicotinic acid residue in peanut kernels refers to the national standard for the determination of tea residue, but there are significant differences between peanut kernels and tea kernels, and this method can only be qualitative.In this paper, a method for the determination of imidazolium nicotinic acid residue in peanut kernels by high performance liquid chromatography was established.A high performance liquid chromatography(HPLC) method was developed for the determination of imazapic in peanut kernel.The sample was extracted with acetonitrile and purified by acetonitrile saturated n-hexane.Quantitative analysis of purified solution was achieved by HPLC and acetonitrile-phosphoricacid salt duffer solution(1:3, V/V) as the mobile phase.The result showed that the calibration curves showed good linearities in the range of 0~1.2 mg/kg (R2=0.9999).The limits of detection (LOD) for the imazapic was 7 μg/kg, the recoveries obtained by standard addition method were between 91.1% and 98.9%.This method provides the advantages of simple operation, high accuracy, so it can be applied inimazapic quality control testing in peanut kernel.