高效液相色谱-荧光法同时检测水产品中阿维菌素和伊维菌素

Determination of abamectin and ivermectin in aquatic product by HPLC-FD

目的建立了水产品中阿维菌素(abamectin, ABA)和伊维菌素(ivermectin, IVM)的高效液相色谱-荧光检测方法。方法样品经乙腈提取,正己烷除脂后,氮气吹至近干,加入衍生化试剂三氟乙酸酐和N-甲基咪唑室温衍生15 min,甲醇定容。采用甲醇/乙腈/0.4%乙酸溶液三元梯度洗脱,基质工作曲线法定量检测。结果在23 min色谱保留时间内阿维菌素和伊维菌素得到有效的分离。添加水平为4μg/kg、8μg/kg和20μg/kg的平均回收率为88.2%～107.5%,相对标准偏差(RSD)为1.4%～9.6%,阿维菌素和伊维菌素的定量限均为3μg/kg。应用该方法对水产品中的阿维菌素和伊维菌素进行测定,5批次样品均未检出。结论本法前处理过程简便高效,方法灵敏度和准确度均满足实际样品的检测需求,适用于大批量水产品中阿维菌素和伊维菌素残留量的检测。

Objective To develop a sensitive method for the determination of abamectin(ABA)and ivermectin(IVM)in aquatic products by high performance liquid chromatography(HPLC)coupled with fluorescence detection(FD).Methods The extraction was performed by acetonitrile,defatted with n-hexane,and then raw extract was evaporated to dryness under a nitrogen flow and the residue was derived with N-methylimidazole and trifluoroacetic anhydride at room temperature for 15 minutes and dissolved in methanol.The detection was performed on HPLC-FD by a gradient elution with a mobile phase consisted of acetonitrile,methanol and 0.4% acetic acid.The matrix matched calibration curve was used for the quantification.Results The method was able to separate ABA and IVM in 23 min.The mean recoveries ranged from 88.2% to 107.5% at the spiked level of 4 μg/kg,8 μgg/kg and 20 μg/kg,and the relative standard derivations(RSD)were within 1.4%-9.6%.The quantification limit was 3 μg/kg.The developed method was applied for analysis of 5 batch samples,no detectable residues of the target analytes were found in any of the samples.Conclusion The proposed method is simple,accurate,sensitive and efficient.It is suitable for the determination of abamectin and ivermectin in aquatic products.