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当前位置: 首页 > 文章 > 二氯吡啶酸·氨氯吡啶酸·烯草酮及其代谢产物在油菜籽与土壤中的残留分析方法 农药 2017 (7) 499-501+505
Position: Home > Articles > Residual Analysis of Clopyralid·Picloram·Clethodim and Its Metabolites in Rapeseed and Soil Agrochemicals 2017 (7) 499-501+505

二氯吡啶酸·氨氯吡啶酸·烯草酮及其代谢产物在油菜籽与土壤中的残留分析方法

作  者：
刘良月;刘晓旭;李闯;赵晓峰;王鑫宏;逯忠斌;侯志广
单  位：
吉林农业大学资源环境学院;吉林省谱尼测试科技有限公司;松辽流域水资源保护局松辽流域水环境监测中心
关键词：
烯草酮;二氯吡啶酸;氨氯吡啶酸;油菜籽;土壤;残留
摘  要：
[目的]建立一种同时测定油菜籽和土壤中二氯吡啶酸、氨氯吡啶酸、烯草酮及其代谢物烯草酮砜和烯草酮亚砜的高效液相色谱串联质谱法。[方法]油菜籽和土壤中的二氯吡啶酸、氨氯吡啶酸、烯草酮及其代谢物烯草酮砜和烯草酮亚砜用乙腈提取,采用QuEChERS法净化,用Agilent Zorbax RRHD Eclipse Plus C_(18)色谱柱分离,流动相为甲醇-水(0.1%甲酸和5 mmol/L乙酸铵),采用多反应监测模式(MRM),外标法定量。[结果]对样品中的二氯吡啶酸、氨氯吡啶酸、烯草酮、烯草酮砜和烯草酮亚砜进行不同水平的添加回收试验,方法的回收率为70.4%~108.6%,相对标准偏差为0.5%~14.8%。最低检测质量浓度为0.05 mg/L。在上述检测条件下,二氯吡啶酸、氨氯吡啶酸、烯草酮、烯草酮砜、烯草酮亚砜的最小检出量分别为0.08、0.1、0.008、0.004、0.007 ng。[结论]该方法的灵敏度、准确度、精密度符合农药残留分析的要求,适合大批量的油菜样品的检测。
译  名：
Residual Analysis of Clopyralid·Picloram·Clethodim and Its Metabolites in Rapeseed and Soil
作  者：
LIU Liang-yue;LIU Xiao-xu;LI Chuang;ZHAO Xiao-feng;WANG Xin-hong;LU Zhong-bin;HOU Zhi-guang;College of Resource and Environmental Science, Jilin Agricultural University;Songliao River Basin Water Resources Protection Bureau Water Environment Monitoring Center of Songliao Basin;Pony Testing International Group;
关键词：
clethodim;;clopyralid;;picloram;;rapeseed;;soil;;residue
摘  要：
[Aims] A new method for analysis of clopyralid, picloram, clethodim and the metabolites residues in rapeseed and soil by high performance liquid chromatography-tandem mass spectrum was developed. [Methods] The clopyralid, picloram, clethodim and the metabolites clethodim sulfone and clethodim sulfoxide residues in rapeseed and soil were extracted with acetonitrile and purified by QuEChERS method. Then Agilent Zorbax RRHD Eclipse Plus C_(18) chromatographic column was used to separate the residues, the mixture of 0.1% formic acid and 5 mmol/L ammonium acetate aqueous solution and methanol was used as mobile phase in gradient elution. Finally, the samples were detected under multiple reaction mode(MRM). The matrix-matched external standard calibration curves were used for the quantitative analysis. [Results] The average recoveries ranged from 70.4 to 108.6%, the relative standard deviations were 0.5-14.8%. The lowest detectable concentrations for clopyralid, picloram, clethodim and the metabolites clethodim sulfone and clethodim sulfoxide in samples were 0.05 mg/L. Under these conditions, the limits of detection for clopyralid, picloram, clethodim, clethodim sulfone and clethodim sulfoxide were 0.08, 0.1, 0.008, 0.004, 0.007 ng,respectively. [Conclusions] The method is simple, reliable, and met with the requirement for pesticide residue analysis,which can be applied for determining clopyralid, picloram, clethodim and the metabolites residues in rape samples.

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