高效液相色譜法檢測菜豆中阿維菌素殘留量

張儒令 安鳳穎 胡德禹 張鈺萍 張侃侃 盧平

摘要? ? 本文建立了反相高效液相色譜法測定菜豆中阿維菌素殘留量的方法，即以乙酸乙酯為提取劑，液液萃取凈化，經N-甲基咪唑和三氟醋酸酐衍生化，采用高效液相色譜法-熒光檢測器（激發波長365 nm，發射波長470 nm）進行測定。同時，為了確定1%阿維菌素水乳劑在菜豆中的施用安全性，通過2年兩地田間試驗和樣品室內檢測試驗，研究了其在菜豆上的消解動態及最終殘留量。結果表明，在0.050～5.000 μg/mL濃度范圍內，阿維菌素的濃度與峰面積線性關系良好，線性相關系數γ=0.999 3。添加濃度在0.004 4～0.440 0 mg/kg時，方法的平均回收率為94.35%～99.42%，相對標準偏差為4.81%～5.84%;以1%阿維菌素水乳劑0.45 g/m2噴藥，阿維菌素在菜豆上的消解半衰期為1.4～1.7 d;施藥7 d后采集的菜豆樣品中阿維菌素含量均低于MRL值0.05 mg/kg。本方法簡便、快速、準確，適用于阿維菌素在菜豆上的殘留量測定。

關鍵詞? ? 阿維菌素;菜豆;殘留;消解動態;高效液相色譜法

中圖分類號? ? S481+.8? ? ? ? 文獻標識碼? ? A

文章編號? ?1007-5739（2020）06-0106-03? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?開放科學（資源服務）標識碼（OSID）

Determination? of? Abamectin? Residue? in? Kidney? Bean? by? HPLC

ZHANG Ru-ling 1? ? AN Feng-ying 1? ? HU De-yu 2 *? ? ZHANG Yu-ping 2? ? ZHANG Kan-kan 2? ? LU Ping 2

（1 Tongren Vocational and Technical College，Tongren Guizhou 554300; 2 Research and Development Cnter for Fine Chemicals，Guizhou University）

Abstract? ? A reversed-phase HPLC method for the determination of avermectin residues in kidney bean was established.The avermectin residues in kidney bean were extracted and purified by liquid-liquid extraction with ethyl acetate as the extractant.After derivatization with N-methylimidazole and trifluoroacetic anhydride，the avermectin residues in kidney bean were determined by HPLC with fluorescence detector（excitation wavelength was 365 nm and emission wavelength was 470 nm）.At the same time，the digestion dynamics and the final residue of abamectin water emulsion in kidney bean were studied through two years of two fields test and sample laboratory test，in order to determine the application safety of 1% abamectin water emulsion in kidney bean.The results showed that in the range of 0.050-5.000 μg/mL，the linear relationship between avermectin concentration and peak area was good，and the linear correlation coefficient was 0.999 3.When the concentration was 0.004 4-0.440 0 mg/kg，the average recovery of the method was 94.35%-99.42%，and the relative standard deviation was 4.81%-5.84%.When the 1% abamectin water emulsion was 0.45 g/m2，the half-life of abamectin digestion on kidney bean was 1.4-1.7 d.The content of abamectin in kidney bean samples collected after 7 days was lower than that of MRL 0.05 mg/kg.This method is simple，rapid and accurate.It is suitable for the determination of avermectin residue in kidney bean.

Key words? ? abamectin;kidney bean;residue;digestion dynamic;HPLC

阿維菌素是一類具有殺蟲、殺螨、殺線蟲活性的十六元環內酯雙糖類化合物，是經過微生物發酵、提取的新型抗生素類殺蟲殺螨劑[1-7]，對多種作物的害蟲和螨類具有觸殺和胃毒作用，同時具有微弱的熏蒸作用，無內吸作用[8-10]，具有廣譜、高效、低殘留等特點，不易對土壤各種微生物和各種酶產生較大危害[11]，是當前農業害蟲綜合防治中理想的生物農藥[12]。

關于阿維菌素的檢測方法國內外有大量報道，張少華等[13]建立了以乙腈為提取溶劑，測定蔥中阿維菌素殘留。……