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[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。
[Objective] To establish a method for the determination of residues of rimsulfuron, quizalofop and quizalofop-p-ethyl in potato plants, soil and tubers by ultra performance liquid chromatography-tandem mass spectrometry. [Method] The rimsulfuron, quizofluorescein and quizalofop-p-ethyl and the metabolite quizalofop-pylori in potato plants, soil and tubers were extracted with acetonitrile and purified by QuECh ERS. The contents of the compounds were determined by ultra performance liquid chromatography --quantitative determination of quizalofop-p-quinaity by electrospray negative ion mode (ESI ~ -) with UPLC-MS / MS, and electrospray positive ion mode (ESI ~ +) External standard method. [Result] The results showed that there was a good linear relationship between rimsulfuron, quizalofop and quizalofop-p-ethyl and its metabolite quizalofop-p-ethyl in the concentration range of 0.001 ~ 1.0 mg / L with the correlation coefficient of 0.9989 ~ 0.9998. The average recoveries of plant, soil and potato tubers ranged from 74.4% to 106.5% and the relative standard deviations (RSDs) ranged from 0.9% to 13.6% within the range of ~ 1.0 mg / kg. Under the above conditions, the minimum detectable amounts of rimsulfuron, quizofluofen, quizalofop and quizalofop and their metabolites were 6.9 × 10 -4 and 6.3 × 10 ~ -4), 3.4 × 10 ~ (-4), 5.6 × 10 ~ (-4) ng. [Conclusion] The sensitivity, accuracy and precision of the method were all in accordance with the requirements of pesticide residue analysis. It was suitable for the determination of rimsulfuron, quizalofop, quizalofop-p-ethyl and quizalofop-p-ethyl in the potato plants, Sour acid residue detection.