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建立了改进的QuEChERS-超高效液相色谱法,定量检测柑橘(果肉、果皮和全果)样品中残留的吡唑醚菌酯。样品用乙腈提取,经N-丙基乙二胺(PSA)和十八烷基硅烷(C18)净化,采用甲醇和水为流动相,用UPLC-PDA进行检测。试验结果表明,添加水平为0.05~5.0mg/kg时回收率为82.34%~97.44%,相对标准偏差(RSD)为0.40%~5.66%。吡唑醚菌酯在贵州和湖南两地柑橘全果中的半衰期分别为10.34d和9.76d。施药剂量为180mga.i./m2和270mga.i./m2,施药3~4次,距最后1次施药7~28d采样,吡唑醚菌酯在柑橘中的残留量为0.05~0.886mg/kg。
An improved QuEChERS-UPLC method was developed for the quantitative detection of pyraclostrobin residues in citrus (pulp, peel and whole fruit) samples. Samples were extracted with acetonitrile, purified with N-propyl ethylenediamine (PSA) and octadecylsilane (C18) using methanol and water as mobile phases and detected by UPLC-PDA. The test results showed that the recoveries ranged from 82.34% to 97.44% and the relative standard deviations (RSDs) ranged from 0.40% to 5.66% at 0.05-5.0 mg / kg. The half-lives of pyraclostrobin in citrus fruits of Guizhou and Hunan were 10.34d and 9.76d, respectively. Application dose of 180mga.i./m2 and 270mga.i./m2, application 3 to 4 times, from the last application 7 ~ 28d sampling pyraclostrobin residue in citrus is 0.05 ~ 0.886 mg / kg.