高效液相色谱法测定果蔬中松脂酸铜残留

Determination of copper abietate in fruits and vegetables by high-performance liquid chromatography

建立了基于高效液相色谱法-紫外检测器(high-performance liquid chromatography-ultraviolet detector,HPLC-UVD)检测松脂酸铜在火龙果、豇豆和杧果3种果蔬中的农药残留的分析方法。果蔬样品在加入盐酸衍生后,使用石油醚超声提取,提取液蒸干后使用乙腈定容,通过HPLC-UVD对样品进行定量测定,选择静电场轨道阱高分辨质谱仪对松脂酸铜转化为松脂酸进行确证分析。结果表明,松脂酸铜的相关系数R^(2)为0.9996,平均回收率在77%~108%,相对标准偏差均小于5%,线性关系良好,该方法的检出限为0.03 mg/kg,定量限为0.1 mg/kg。该方法简便、准确、快速,可满足果蔬中松脂酸铜残留检测灵敏度和准确度的要求,其他果蔬样品中的松脂酸铜残留也可参照该方法进行分析。

An analytical method based on high-performance liquid chromatography-ultraviolet detector(HPLC-UVD)was established to determine the residues of copper abietate in mango,pitaya,and cowpea.The sample was extracted with hydrochloric acid and petroleum ether,which was ultrasonicated.The extracted supernatant was evaporated to dryness,and then dissolved with acetonitrile,the HPLC-UVD was used to quantitatively determine the sample.The copper abietate in the samples was acidified with hydrochloric acid and changed to abietic acid and the abietic acid was the target for the quantitation of copper abietate.Another high-resolution mass spectrometer was used to qualitatively analyze the copper abietate derivative.Results showed that the correlation coefficient R^(2)was 0.9996 for copper abietate,the recovery of copper abietate in the selected fruit and vegetable samples was in the range of 77%-108%,and the relative standard deviations of copper abietate in the three fruits and vegetables,pitaya,cowpea,and mango were less than 5%.These results indicated that the accuracy of the copper rosin acid analysis method in fruits and vegetables met the requirements of detection and analysis.The limit of detection(LOD)for copper abietate was 0.03 mg/kg and the limit of quantitation(LOQ)was 0.1 mg/kg.The method is simple,accurate,and fast for the determination of residue of copper abietate in fruits and vegetables,where the sensitivity and accuracy can meet the requirements of copper abietate residue detection in fruits and vegetables.