摘要
【目的】为检测水稻中戊唑醇残留及评价其在水稻上使用的安全性,建立了戊唑醇在水稻植株、稻壳、糙米和土壤中的残留分析方法。【方法】水稻样品采用乙腈提取,FlorisiVb柱净化,GC-NPD测定。同时,于浙江、山东和湖南3地进行了田间试验。【结果】戊唑醇在水稻植株和稻壳中的添加质量分数为0.05~5.0mg/kg时,平均回收率为88.80%一103.86%,相对标准偏差(RSD)为4.25%一14.36%。戊唑醇在糙米和土壤中的添加质量分数为0.02—2.0mg/kg时,平均回收率为89.19%~102.27%,相对标准偏差(RSD)为2.26%~8.58%。戊唑醇在水稻植株和稻壳的最低检测质量分数(LOQ)为0.05mg,kg,在糙米和土壤中最低检测质量分数(LOQ)为0.02mg/kg。田间试验表明:戊唑醇在水稻植株中的消解动态符合一级动力学方程,在浙江、山东和湖南3地水稻植株中的半衰期分别为0.60、11.48、3.14d;最后用药距收期21d时,戊唑醇在植株中的残留量为0.30mg/kg、稻壳中的残留量为0.22mg/kg、糙米中的残留量为〈0.02mg/kg、土壤中的残留量为〈0.02mg/kg。【结论】该方法的灵敏度、精密度和回收率等均符合农药残留分析的要求。戊唑醇在水稻植株中属于易降解农药,降解半衰期为0.60~11.48d。
[Aims] The method for the determination of tebuconazole residues in rice plant, rice hull, rice and soil were estimated for evaluating the safety of tebuconazole in paddy field. [Methods] The samples were extracted with aeetonitrile, clean-up using a Florisil solid phase extraction cartridge, and subsequent determination by GC-NPD. And the field experiments were investigated in Zhejiang, Shandong and Hunan. [Results] Average recoveries of tebueonazole in rice plant and rice hull were found in the range of 88.80-103.86% at the three spiking levels from 0.05 to 5.0 mg/kg with relative standard deviations of 4.25-14.36%. Average recoveries of tebuconazole in rice and soil were found in the range of 89.19-102.27% at the three spiking levels from 0.02 to 2.0 mg/kgwith relative standard deviations of 2.26-8.58%. The limits of quantification (LOQ) in rice plant and rice hull were 0.05 mg/kg. The limits of quantification (LOQ) in rice and soil were 0.02 mg/kg. The field experiments demonstrated that the decline curves of tebuconazole in rice plant were accorded with the first-order kinetics equation, and the half-lives were 0.60 d in Zhejiang, 11.48 d in Shandong, and 3.14 d in Hunan, respectively. The residue of tebuconazole was 0.30 mg/kg in rice plant, 0.22 mg/kg in rice hull, 〈0.02 mg/kg in rice and 〈0.02 mg/kg in soil, respectively, after 21 d of spray. [Conclusions] The method was suitable for the determination of tebuconazole residues in rice. Tebuconazole was easily degradable pesticides in rice plant, and the half-lives were 0.60-11.48 d.
出处
《农药》
CAS
北大核心
2012年第9期675-677,共3页
Agrochemicals