【摘要】 [目的]建立超高效液相色谱串联质谱法检测花生植株、土壤、花生籽粒和花生壳中扑草净、乙草胺残留的方法。[方法]花生植株、土壤、花生籽粒和花生壳中扑草净、乙草胺用乙腈提取采用QuEChERS法净化,用Agilent Zorbax RRHD Eclipse Plus C₁₈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0.3 mL/min,采用正离子电喷雾电离模式测定,外标法定量。[结果]扑草净方法的线性范围为0.002⁰.2 mg/kg,相关系数为0.9911,乙草胺方法的线性范围为0.002¹.0 mg/kg,相关系数为0.9991;在0.02、0.1、1.0mg/kg,3个添加水平下,花生植株中2种农药的平均回收率为83.5%⁹1.6%,相对标准偏差为0₃%⁷.8%;在花生土壤中平均回收率为77.7%⁹8.9%,相对标准偏差为1.0%⁵.9%;在花生籽粒中平均回收率为82.6%⁹5.6%,相对标准偏差为0.7%³.2%;在花生壳中平均回收率为71.6%⁹6.4%,相对标准偏差为1.1%⁵.5%。在上述检测条件下,扑草净和乙草胺的最小检出量分别为2.0×10^-5、4.0×10^-4ng。[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,适合大批量花生样品的检测。更多还原

【Abstract】 [Aims] A new method was developed for residual analysis of prometryne and acetochlor in peanut plant,kernel, shell and soil by ultra performance liquid chromatography- tandem mass spectrum. [Methods] Prometryne and acetochlor residues in peanut plant, kernel, shell and soil were extracted with acetonitrile and purified by Qu ECh ERS method. Then Agilent Zorbax RRHD Eclipse Plus C18 chromatographic column was used to separate the residues, the mixture of 0.1% formic acid aqueous solution and acetonitrile was used as mobile phase in gradient elution with the flow rate of 0.3 m L/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 linearity range of calibration curve for prometryne was 0.002-0.2 mg/kg and the linear correlation coefficient was 0.9911, the linearity range of calibration curve for acetochlor was 0.002-1.0 mg/kg and the linear correlation coefficient was 0.9991. When the spiked levels were 0.02, 0.1 and 1.0 mg/kg, the average recoveries of the two pesticides in peanut plant were 83.5-91.6%, and relative standard deviations were 0.3-7.8%. The average recoveries of the two pesticides in soil were 77.7-98.9%, and relative standard deviations were 1.0-5.9%. The average recoveries of the two pesticides in kernel were 82.6-95.6%, and relative standard deviations were 0.7-3.2%,The average recoveries of the two pesticides in shell were 71.6-96.4%, and relative standard deviations were 1.1-5.5%.Under these condition, the limits of detection for prometryne and acetochlor were 2.0 ×10^-5 and 4.0 ×10^-4ng,respectively. [Conclusions] The method is simple and reliable, met with the requirement for pesticide residue analysis,which can be applied for determining prometryne and acetochlor residues in peanut samples.更多还原