仲丁灵在水稻植株、稻田水及糙米中的残留分析方法  

Analysis of Butralin Residues in Rice Plant,Field Water and Rough Rice

作　　者：侯志广[1] 李闯 刘晓旭[3] 刘良月 赵晓峰[1] 王鑫宏[1] 逯忠斌[1] 

机构地区：[1]吉林农业大学资源与环境学院,长春130118 [2]吉林省谱尼测试科技有限公司,长春130012 [3]松辽流域水资源保护局松辽流域水环境监测中心,长春130021

出　　处：《农药》2017年第5期354-356,共3页Agrochemicals

基　　金：吉林省参茸办人参产业发展专项(201501)

摘　　要：[目的]建立超高效液相色谱串联质谱法检测水稻植株、稻田水和糙米中仲丁灵残留的方法。[方法]植株和糙米中的仲丁灵用乙腈提取,采用QuEChERS法净化,稻田水中的仲丁灵用乙酸乙酯萃取,用Agilent Zorbax RRHD Eclipse Plus C_(18)色谱柱分离,以0.1%甲酸水-乙腈为流动相进行梯度洗脱,流速为0.4 mL/min,采用正离子电喷雾电离模式测定,外标法定量。[结果]方法的线性范围为0.001~1.0 mg/L,相关系数为0.9996;在0.01、0.1、1.0 mg/L 3个添加水平下,水稻植株中平均回收率为92.1%~95.2%,相对标准偏差为0.6%~3.9%;稻田水中平均回收率为86.4%~90.9%,相对标准偏差为1.5%~5.5%;糙米中平均回收率为93.9%~97.8%,相对标准偏差为2.2%~2.9%。在上述检测条件下,仲丁灵的最小检出量为2.0×10^(-3)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,适合大批量的水稻样品的检测。[Aims] A new method for analysis of butralin residues in rice plant, field water and rough rice by ultra performance liquid chromatography-tandem mass spectrum was developed. [Methods] The butralin residues in rice plant and rough rice were extracted with acetonitrile and purified by QuEChERS method, and the residues in field water were extracted with ethyl acetate. Then the residues were separated with Agilent Zorbax RRHD Eclipse Plus C18 chromatographic column, meanwhile the mixture of 0.1% formic acid aqueous solution and acetonitrile was used as mobile phase in gradient elution, and the flow rate was 0.4 mL/min. Finally, the samples were detected by UPLC-MS/MS under positive electrospray ionization and multiple reaction monitoring mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. [Results] The linear range of calibration curves was 0.001-1.0 mg/L and linear correlation coefficient was 0.9996. When the spiked levels were 0.01, 0.1 and 1.0 mg/L, the average recoveries of butralin in rice plant were 92.1-95.2% with relative standard deviations of 0.6-3.9%, the average recoveries of butralin in field water were 86.4-90.9% with relative standard deviations of 1.5-5.5%, the average recoveries of butralin in rough rice were 93.9-97.8% with relative standard deviations of 2.2-2.9%. Under these conditions, the limits of detection for butralin were 2.0× 10^-3 ng. [Conclusions] The method is simple and reliable, meets with the requirement for pesticide residue analysis, which can be applied for analysis ofbutralin residues in rice samples.

关 键 词：仲丁灵 超高效液相色谱串联质谱 水稻植株 稻田水 糙米 

分 类 号：O657.63[理学—分析化学] TQ450.263[理学—化学]