砜嘧磺隆、喹禾糠酯、精喹禾灵及其代谢物在马铃薯植株、土壤及块茎中的残留分析方法

Analysis of Rimsulfuron, Quizalofop-p-tefuryl, Quizalofop-ethyl and Its Metabolites Residues in Potato Plant, Soil and Tuber

[目的]建立超高效液相色谱串联质谱法检测马铃薯植株、土壤和块茎中砜嘧磺隆、喹禾糠酯、精喹禾灵及其代谢物残留的方法。[方法]马铃薯植株、土壤和块茎中的砜嘧磺隆、喹禾糠酯和精喹禾灵及其代谢物精喹禾灵酸经乙腈提取,Qu ECh ERS法净化,利用超高效液相色谱-串联质谱(UPLC-MS/MS)多反应监测(MRM)模式测定,精喹禾灵酸采用电喷雾负离子模式(ESI^-),其他采用电喷雾正离子模式(ESI^+),基质匹配外标法定量。[结果]砜嘧磺隆、喹禾糠酯、精喹禾灵及其代谢物精喹禾灵酸在0.001~1.0 mg/L质量浓度范围内线性关系良好,相关系数为0.9989~0.9998;在0.01~1.0 mg/kg添加水平范围内,植株、土壤和马铃薯块茎中的平均回收率为74.4%~106.5%,相对标准偏差为0.9%~13.6%。在上述检测条件下,砜嘧磺隆、喹禾糠酯、精喹禾灵及其代谢物精喹禾灵酸的最小检出量分别为6.9×10^(-4)、6.3×10^(-4)、3.4×10^(-4)、5.6×10^(-4)ng。[结论]本方法灵敏度、准确度和精确度均符合农药残留分析的要求,适用于马铃薯植株、土壤和块茎中砜嘧磺隆、喹禾糠酯、精喹禾灵及其代谢物精喹禾灵酸的残留检测。

[Aims] A new method was developed for analysis of rimsulfuron, quizalofop-p-tefuryl, quizalofop-ethyl and its metabolites residues in potato plant, soil and tuber by ultra performance liquid chromatography-mass spectrum.[Methods] The rimsulfuron, quizalofop-p-tefuryl, quizalofop-ethyl and its metabolite of quizalofop-acid in potato plant, soil and tuber were extracted with acetonitrile and purified by Qu ECh ERS method, detected by UPLC-MS/MS under multiple reaction monitoring modes as well as negative electrospray ionation（ESI^-） for quizalofop-acid and positive electrospray ionation（ESI~＋） for others, with matrix matching and quantification of external standard method. [Results] When the concentration ranged from 0.001 to 1.0 mg/L, the method for rimsulfuron,quizalofop-p-tefuryl, quizalofop-ethyl and its metabolites of quizalofop-acid displayed good linearity with the correlation coefficient of 0.9989-0.9998. When the spiked levels ranged from 0.01 to 1.0 mg/L, the average recoveries were in the range of 74.4 to 106.5% and the relative standard deviations were in the range of 0.9 to 13.6%.Under these conditions, the limits of detection for rimsulfuron, quizalofop-p-tefuryl, quizalofop-ethyl and its metabolites of quizalofop-acid were 6.9×10^（-4）、6.3×10^（-4）、3.4×10^（-4）、5.6×10^（-4） ng, respectively. [Conclusions] The method is simple and reliable, met with the requirement for pesticide residue analysis, which is suitable for determination of rimsulfuron, quizalofop-p-tefuryl, quizalofop-ethyl and its metabolites of quizalofop-acid in potato plant, soil and tuber.