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为制定烟叶中三唑酮及代谢产物的农药残留限量,研究了合理使用条件下,三唑酮及其代谢物三唑醇在烟叶中残留降解规律和残留水平。采用气相色谱电子捕获检测器(GC-ECD)建立了同时测定烟叶中三唑酮和代谢产物三唑醇农药残留的检测方法,结果表明:三唑酮在鲜烟叶和烤后烟叶中的最低检出量(LOQ)分别为0.01、0.05 mg/kg。三唑酮、三唑醇在鲜烟叶和干烟叶样品中添加水平为0.01~5 mg/kg时,平均添加回收率为79.8%~97.3%,RSD为1.5%~9.0%,符合农药残留检测方法要求。对2011-2012年山东、湖南两地三唑酮残留试验的烟叶样品进行了检测。结果表明,三唑酮在自然生长条件下半衰期为3.8~5.6d,在储存条件下的半衰期分别为157~315 d。最终残留试验结果表明,施药剂量和采收安全间隔期与烟叶中农药残留量显著相关,末次施药后7、14、21 d,烤后烟叶中三唑酮及代谢物的残留量分别为0.33~6.44 mg/kg、0.15~2.77 mg/kg、0.18~2.53 mg/kg。建议三唑酮及代谢产物在烟叶中MRL为5mg/kg,安全间隔期(PHI)为14 d。
In order to establish the limit of pesticide residues of triadimefon and its metabolites in tobacco leaves, the degradation and residual levels of triadimenone and its triadimenol residues in tobacco leaves under reasonable conditions were studied. A gas chromatographic electron capture detector (GC-ECD) was established for the simultaneous determination of triadimefon and triadimenol pesticide residues in tobacco leaves. The results showed that triadimefon was the lowest in fresh tobacco leaves and roasted tobacco leaves Output (LOQ) were 0.01,0.05 mg / kg. The average recoveries of triadimefon and triadimenol at the concentration of 0.01-5 mg / kg in fresh and dried tobacco leaves were 79.8% -97.3% and RSD was 1.5% -9.0%, respectively, which accorded with the pesticide residue detection method Claim. Tobacco leaf samples of triadimefon residue test in Shandong and Hunan from 2011 to 2012 were tested. The results showed that the half-life of triadimefon in the natural growth conditions was 3.8 ~ 5.6d, and the half-lives in the storage conditions were 157 ~ 315d. The final residue test results showed that the application dose and harvest safety interval was significantly correlated with the pesticide residues in tobacco leaves. The residues of triadimefon and metabolites in the leaves after 7, 14 and 21 days after the last application were 0.33 ~ 6.44 mg / kg, 0.15 ~ 2.77 mg / kg, 0.18 ~ 2.53 mg / kg. It is suggested that the MRL of triadimefon and its metabolites in tobacco leaves should be 5mg / kg with a safety interval (PHI) of 14 days.