QuEChERS-HPLC法测定植物性食品中氟吗啉的残留量

Detection of Flumorph residue in vegetable foods by using the QuEChERS coupled with HPLC

以苹果、梨、葡萄、橘子、白菜、西兰花、菠菜、胡萝卜、番茄和黄瓜共10种植物性食品为研究对象,建立了植物性食品中氟吗啉残留量的QuEChERS-HPLC检测方法。样品经0.1%冰醋酸乙腈提取,醋酸钠和无水硫酸镁盐析后,取上清液,加入伯仲胺粉分散固相萃取净化,用配有二极管阵列检测器的高效液相色谱测定,外标法定量。氟吗啉在0.1~2mg/L的范围内具有较好的线性关系,氟吗啉在0.1、0.2、0.5mg/kg三个添加水平平均回收率81%～116%,RSD2.3%~12.1%,定量限为0.05mg/kg。本方法前处理简单、快速,适用于多种植物性食品中氟吗啉残留量测定。

A method for determination of flumorph residues in 10 kinds of vegetable foods was established by QuEChERS and HPLC. The proposed method was successfully applied on apple,pear,grape,orange,cabbage, broccoli,spinach,carrot,tomato and cucumber. Flumorph residues were extracted from samples with acetonitrile containing 0.1% acetic acid and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate plus sodium acetate following by a simple cleanup step known by dispersive solid-phase extraction. Mixed powders of primary secondary amine （PSA） were simply mixed with acetonitrile extract. The aliquot was determined by HPLC using external standard method. The average recovery of this method was in the range from 81% to 116% at the spiked level of 0.1,0.2,0.5mg/kg into samples,and the RSDs were in the range from 2.3% to 12.1%. The linearity of method was good from 0.1 to 2mg/L,and LOQ^0.05mg/kg. This method was simple,rapid,and it was applicable for rapid analysis of fiumorph residues in lots of vegetable foods.