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[目的]建立柑橘和土壤中螺虫乙酯及代谢产物BYI08330-enol-glucoside、BYI08330-ketohydroxy、BYI08330-enol和BYI08330-mono-hydroxy的残留分析方法。[方法]前处理方法利用乙腈为提取剂,N-丙基乙二胺(PSA)和石墨化炭黑(GCB)为分散净化剂的Qu ECh ERS方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式(MRM)下进行检测,外标法定量。[结果]螺虫乙酯及4种代谢产物在0.002~0.500 mg/L质量浓度范围内均具有良好的线性关系(r2≥0.994);在0.01~1.00 mg/kg添加水平范围内平均回收率为70.7%~96.0%;相对标准偏差为1.2%~6.4%;方法检出限(LOD)在0.12~1.4μg/kg范围内;定量限(LOQ)在0.4~4.9μg/kg范围内。[结论]该方法分析速度快、灵敏度高、重现性好,适用于柑橘和土壤中螺虫乙酯及其代谢产物残留的快速检测和确证。
[Objective] The study aimed to establish a method for the determination of ethyl spirotetramat and residues BYI08330-enol-glucoside, BYI08330-ketohydroxy, BYI08330-enol and BYI08330-mono-hydroxy in citrus and soil. [Method] The pretreatment method was Qu ECh ERS method using acetonitrile as extractant, N-propyl ethylenediamine (PSA) and graphitized carbon black (GCB) as dispersing and purifying agent. The supercritical fluid chromatography- tandem mass spectrometry (UPLC-MS / MS) in multi-reactive ion monitoring mode (MRM), external standard method. [Result] There was a good linear relationship between spirotetramat and four metabolites in the concentration range of 0.002-0.500 mg / L (r2 ≥ 0.944). The average recoveries of spirotetramate and four metabolites in the range of 0.01-1.00 mg / kg were The relative standard deviations were 1.2% ~ 6.4%. The limits of detection (LOD) were within the range of 0.12-1.4μg / kg. The limits of quantification (LOQ) were within the range of 0.4-4.9μg / kg. [Conclusion] The method was rapid, sensitive and reproducible. It was suitable for rapid detection and confirmation of spirotetramat and its metabolite residues in citrus and soil.