华南农业大学学报2017，Vol.38Issue(4)：41-47,7.DOI:10.7671/j.issn.1001-411X.2017.04.007
印楝素水解动力学研究及水解产物结构解析
Study on hydrolysis kinetics of azadirachtin and structure analysis of hydrolysate
摘要
Abstract
[Objective] To study hydrolysis of azadirachtin in water systematically.[Method]Azadirachtin A from the 44.56% azadirachtin TC was isolated and purified by silica column chromatography and semi-preparative high performance liquid chromatography (HPLC).The chemical structure and content of isolated azadirachtin A were identified by nulear magnetic resonance (NMR) and HPLC.A method for determining azaditachtin residue in water by HPLC was established.[Result]The mass fractions of azadirachtin A were 90.37% and 91.82% detected by NMR and HPLC respectively.When azadirachtin was added with the concentrations of 0.1, 1.0 and 5.0 mg·kg-1, the average recovery rates of azadirachtin from water samples ranged from 92.53% to 94.12%, the variation coefficients ranged from 0.35% to 0.84%, and the minimum detection limit was 0.012 mg·L-1.Azadirachtin was stable in buffer solutions with pH varying from 4.0 to 6.0.When pH was above 8.0, hydrolysis of azadirachtin was accelerated, and the degradation half-life was 14.856 h at pH 8.0 and declined to 0.033 h at pH 10.0.The degration half-lives of azadirachtin in buffer solutions at pH 6.0 were 24.68, 13.69 and 2.36 d under 25, 35 and 45 ℃ temperature respectively, while were 9.35, 6.51 and 0.94 d at pH 7.0.A lactone derivative of azadirachtin was obtained by isolating and purifing hydrolysate in buffer solution at pH 2.0.[Conclusion]Azadirachtin is extremely unstable in alkaline environment while relatively stable in weak acid environment.Temperature has a great effect on the degradation of azadirachtin and the degradation accelerates as temperature increases.关键词
印楝素/残留/水解动力学/水解产物/硅胶柱层析法/高效液相色谱/核磁共振Key words
azadirachtin/residue/hydrolysis kinetics/hydrolysate/silica column chromatography/HPLC/nuclear magnetic resonance分类
农业科技引用本文复制引用
杨晓云,江腾辉,黄其亮,徐汉虹..印楝素水解动力学研究及水解产物结构解析[J].华南农业大学学报,2017,38(4):41-47,7.基金项目
国家自然科学基金(20377015) （20377015）
