HPLC测定氯虫苯甲酰胺在烟草和土壤中的残留与消解动态  

Residue Detection and Digestion Dynamics of Chlorantraniliprole in Tobacco Plants and Soil by HPLC

作　　者：黄丽 邓毅书 浦恩堂[2] 代雪芳[2] 李文希[2] 王静[1] 刘朝敏 张雪燕[2] HUANG Li;DENG Yi-shul;PU En-tang;DAI Xue-fang;LI Wen-xi;WANG Jing;LIU Zhao-min;ZHANG Xue-yan(College of Resources and Environment,Yunnan Agricultural University,Yunnan Kunming 650201,China;Institute of Agricultural Environment and Resources,Yunnan Academy of Agricultural Science,Yunnan Kunming 650205,China;Plant Protection and Inspection Station,Yunnan Zhaoyang 657000,China)

机构地区：[1]云南农业大学资源与环境学院,云南昆明650201 [2]云南省农业科学院农业环境资源研究所,云南昆明650205 [3]昭阳区植保植检站,云南昭阳区657000

出　　处：《西南农业学报》2020年第2期395-400,共6页Southwest China Journal of Agricultural Sciences

基　　金：农业农村部农药检定所(CL17617006)。

摘　　要：【目的】建立烟草和土壤中氯虫苯甲酰胺残留分析方法,探究氯虫苯甲酰胺在烟草和土壤中的残留动态,为其合理使用及其安全性评价提供科学依据。【方法】采用田间小区试验进行氯虫苯甲酰胺在烟草和土壤中的消解动态和最终残留量研究。田间试验采集的样品用乙腈提取、硅胶柱和氨基固相萃取柱净化,高效液相色谱测定。【结果】干烟叶、烟草植株和土壤中添加氯虫苯甲酰胺0.05~10 mg/kg,其平均回收率为80.8%~95.8%,相对标准偏差(RSD)为2.6%~7.6%,氯虫苯甲酰胺在烟草中的定量限(LOQ)为0.1 mg/kg,在土壤中的定量限(LOQ)为0.05 mg/kg。氯虫苯甲酰胺在烟草植株和土壤中的消解动态符合一级动力学反应模型,在烟草植株中的半衰期为12~13.3 d,在土壤中的半衰期为24.8~27.7 d。云南和山东最终残留试验表明,距最后一次施药14 d,干烟叶中氯虫苯甲酰胺平均残留量在2.1~7.7 mg/kg。【结论】该分析方法操作简便,精密度、准确度和灵敏度都符合农药残留标准要求,适用于烟草和土壤中的氯虫苯甲酰胺残留测定;建议5%氯虫苯甲酰胺悬浮剂防治烟草害虫,按推荐剂量41.25 g a.i./hm^2最多施药2次,安全间隔期为14 d。【Objective】In order to provide scientific basis for scientific and rational use of chlorantraniliprole and evaluate its risk after application, an analytical method was developed for the determination of chlorantraniliprole in tobacco plant and soil, and its residual dynamics in tobacco plant and soil were investigated through field trials. 【Method】 Residue and degradation dynamics of chlorantraniliprole were examined after its application to tobacco field. Chlorantraniliprole in tobacco plant and soil samples was extracted by acetonitrile, cleaned by Silica gel column and NH2 SPE-column, determined by HPLC. 【Result】 The results indicated that the average recovery of chlorantraniliprole at spiked levels of 0.05 to 10.00 mg/kg ranged from 80.8 % to 95.8 %, with relative standard deviations(RSD) from 2.4 % to 7.6 %.The limits of quantification(LOQ) were 0.10 mg/kg in tobacco plant and 0.05 mg/kg in soil. The degradation of chlorantraniliprole in tobacco plant and soil was proved to follow the first order kinetic equation, and the half-life of chlorantraniliprole in tobacco plant was 12-13.3 days, in soil was 24.8-27.7 days. Terminal residue studies in Yunnan and Shandong showed that the average residual amount of chlorfenamide in tobacco leaves was between 2.1 and 7.7 mg/kg 14 days after the last application. 【Conclusion】 The precision, accuracy and sensitivity of this method are consistent with the pesticide residue detection requirements. This method is easy to operate and is suitable for the determination of chlorantraniliprole in tobacco plants and soil. Based on the results of risk assessment, it is recommended that 5 % chlorantraniliprole SC used at a dose of 41.25 g(a.i)/hm2 in tobacco field up to 2 times with pre-harvest interval of 14 days.

关 键 词：氯虫苯甲酰胺 烟草 土壤 残留 消解 

分 类 号：S572[农业科学—烟草工业]