高效液相色谱-荧光法同时检测蔬菜中阿维菌素、甲氨基阿维菌素苯甲酸盐和伊维菌素的多残留量

【目的】建立同时测定蔬菜中阿维菌素(abamectin,ABA)、甲氨基阿维菌素苯甲酸盐(emamectin benzoate,EMA)和伊维菌素(ivermectin,IVM)多残留量的高效液相色谱-荧光(HPLC-FD)检测方法。【方法】蔬菜样品经乙腈提取后,以三氟乙酸酐(TFAA)-N-甲基咪唑(NMIM)-乙腈(ACN)法进行柱前荧光衍生化,采用乙腈/甲醇/水三元梯度洗脱程序在高效液相色谱-荧光检测器(HPLC-FD)上完成ABA、EMA和IVM的多残留分析。【结果】研究结果表明,在12min色谱保留时间内ABA、EMA和IVM能有效地得到分离检测。添加浓度为10-1000μg·L-1时,蔬菜中ABA、EMA和IVM的添加回收率分别为90.5%-114.1%、96.7%-118%和92.8%-108.1%,变异系数(C.V.%)分别为0.85%-12.11%、1.38%-9.36%和0.95%-11.52%,在蔬菜样品中最低检出浓度分别为1.2、2.1和1.7μg·kg-1。【结论】高效液相色谱-荧光检测法前处理简便,方法准确可靠,灵敏度和准确度均达到了农药残留检测的要求。

Multi-Residues Determination of Abamectin,Emamectin Benzoate and Ivermectin in Vegetables by HPLC-FD

【Objective】 The aim of the study is to build a sensitive high-performance liquid chromatography with fluorescence detection (HPLC-FD) method for determinating multi-residues of abamectin(ABA), emamectin benzoate (EMA) and ivermectin (IVM) in vegetables. 【Method】 After being extracted by acetonitrile, the avermectins residues in vegetables were directly derivatised by N-methylimidazole (N-NMIM) and trifluoroacetic anhydride (TFAA) and then analyzed on HPLC-FLD using gradient elution program with acetonitrile/methanol/water. 【Result】 Results showed that the developed method had good sensitivity and selectivity for determining the ABA, EMA and IVM residues in vegetables within 12 min. When spiked at 10-1 000 μg?L-1, the fortified recoveries of ABA, EMA and IVM, respectively, were 90.5%-114.1%, 96.7%-118%, and 92.8%-108.1%, and their variation coefficients (C.V. %) were 0.85%-12.11%, 1.38%-9.36%, and 0.95%-11.52%, respectively. The limited detection levels of ABA, EMA and IVM residues in vegetables were 1.2, 2.1, and 1.7 μg?kg-1, respectively. 【Conclusion】 The HPLC-FD method is simple, fast and easy to perform, all validated parameters of this method are sufficient for analysis of pesticide residue.