甘蓝中阿维菌素残留检测方法研究

摘　要：利用反相高效液相色谱法建立了在甘蓝中阿维菌素残留量的测定方法，并试验了阿维菌素在甘蓝的残留动态及最终残留量。样品采用甲醇提取，二氯甲烷萃取，经弗罗里硅土柱净化后，采取反相HPLC—UVD方法测定。方法的添加回收83.78%-87.13%， 变异系数为1.51%-4.16%，最低检出浓度为0.01mg／kg ，最低检出量为1.0×10-9 g。残留动态试验结果表明，阿维菌素按3倍推荐使用剂量施药，它在甘蓝的半衰期为1.79d。在推荐使用剂量和1.5倍推荐使用剂量施药3次的情况下，最后1次施药距收获间隔期7d，推荐使用剂量处理阿维菌素在甘蓝均未检出，1.5倍推荐使用剂量处理阿维菌素在甘蓝内的残留为0.05 mg／kg。
关键词：阿维菌素；甘蓝；农药残留。

Study on residues analysis of Avermectin in cabbage
Abstract:A reversed-phase high performance liquid chromatography(RP-HPLC) method for determination of avermectin in cabbage was developed and degradation dynamics andfinal residues of avermectin in cabbage were estimated. Samples of cabbage were extracted by methanol,and further extracted with dichloromethane by liquid-liquid extraction,The extract was cleaned-up with florisil cartridge.The analysis was determined by reversed-phase high performance liquid chromatography(RP- HPLC) with UVD.The average recoveries ranged from 83.78%-87.13%.With relative standard deviation 1.51%-4.16%.The lowest detectable concentration of avermectin was 0.01mg／kg．and the detection limit was 1.0 x10 -9 g.The results of residue dynamics showed that the half life of avermectin in cabbage was 1.79d ,respectively,when it was applied on plants of three recommended dosages. Avermectin in cabbage was not detected in 7d after final application. Avermectin in cabbage was 0.05mg／kg, respectively, when it was used at three times by 1.5 recommended dosages．
Key words: Avermectins; cabbage; residues

目    录    7000字
摘要…………………………………………………………………………………………1
关键词………………………………………………………………………………………1
1 前言………………………………………………………………………………………2
1.1 阿维菌素的简介……………………………………………………………………2
1.2 阿维菌素的理化性质………………………………………………………………2
1.3 阿维菌素的研究……………………………………………………………………2
1.4 阿维菌素的作用特点………………………………………………………………3
1.5 阿维菌素的残留及分析方法………………………………………………………3
1.6 选题的目的及意义…………………………………………………………………3
2 实验部分…………………………………………………………………………………3
2.1仪器与实验材料……………………………………………………………………3
2.1.1 仪器……………………………………………………………………………4
2.1.2 试剂……………………………………………………………………………4
2.2 阿维菌素的实验方法………………………………………………………………4
2.2.1 甘蓝样品的制备………………………………………………………………4
2.2.2 甘蓝最终残留田间实验………………………………………………………4
2.2.3 甘蓝消解动态田间试验………………………………………………………4
2.3 阿维菌素方法研究…………………………………………………………………5
2.3.1 提取方法一——活性炭脱色提取及其回收率实验…………………………5
2.3.2 提取方法二——层析柱脱色提取及其回收率实验…………………………5
2.3.3 阿维菌素的分析条件…………………………………………………………5
2.3.4 标准曲线的绘制………………………………………………………………6
2.3.5 阿维菌素的添加回收…………………………………………………………6
2.3.6 阿维菌素的最终残留…………………………………………………………6
2.3.7 阿维菌素的消解动态研究……………………………………………………6
3 结果与讨论………………………………………………………………………………7
3.1 方法的最低检出溶度，准确度于精密度………………………………………7
3.1.1 线性关系的确定……………………………………………………………7
3.1.2 方法的准确度和精密度……………………………………………………7
3.1.3 最低检测浓度………………………………………………………………8
3.2 阿维菌素的消解动态……………………………………………………………9
3.3 阿维菌素的最终残留……………………………………………………………9
4 结论………………………………………………………………………………………10
参考文献……………………………………………………………………………………10
致谢…………………………………………………………………………………………12