摘要
目的 建立同时测定青皮中 36 种禁限用农药残留量的超高效液相色谱串联质谱法.方法 青皮样品采用乙腈均质处理,浓缩后经装有无水硫酸镁、N-丙基乙二胺、十八烷基硅烷键合硅胶的净化管净化,采用正离子多反应监测(MRM)模式测定青皮样品中36 种禁限用农药的残留量.结果 36 种禁限用农药均在各的质量浓度范围内与峰面积积分值线性关系良好(r2≥0.991,n=6);检测限为 0.020 9～8.659 4µg/kg;平均回收率为 73.25%～102.83%,RSD为 1.59%～9.74%(n=6).32 批青皮样品中,毒死蜱、多菌灵、吡虫啉、哒螨灵、螺螨酯的检出率分别为 96.88%,65.63%,46.88%,25.00%,6.25%,残留量分别为 0.002～0.674 mg/kg、0.001～1.535 mg/kg、0.006～0.133 mg/kg、0.002～0.074 mg/kg、0.09 mg/kg,均未超过最大残留量限度,其余溴氰菊酯等 31 种农药化合物均未检出.结论 所建立的方法分析时间短、灵敏度高,可用于同时测定青皮中 36 种禁限用农药的残留量.
Abstract
Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of 36 forbidden and restricted pesticide residues in Citri Reticulatae Pericarpium Viride.Methods The samples of Citri Reticulatae Pericarpium Viride were extracted by acetonitrile homogenization.After concentration,the samples were purified by a purification tube containing anhydrous magnesium sulfate,N-propyl ethylenediamine and octadecylsilane chemically bonded silica.The positive ionization in multi-reaction monitoring(MRM)model was used to determine the 36 forbidden and restricted pesticide residues in Citri Reticulatae Pericarpium Viride samples.Results The 36 forbidden and restricted pesticide residues showed a good linear relationship with peak area within their mass concentrations(r2≥0.991,n=6),the limits of detection was in the range of 0.020 9-8.659 4 µg/kg,the average recovery rate was in the range of 73.25%-102.83%,with an RSD of 1.59%-9.74%(n=6).Among 32 batches of Citri Reticulatae Pericarpium Viride samples,the detection rates of chlorpyrifos,carbendazim,imidacloprid,pyridaben,and spirodiclofen were 96.88%,65.63%,46.88%,25.00%,and 6.25%,respectively.The residual volumes of chlorpyrifos,carbendazim,imidacloprid,pyridaben,and spirodiclofen were in the ranges of 0.002-0.674 mg/kg,0.001-1.535 mg/kg,0.006-0.133 mg/kg,0.002-0.074 mg/kg,and 0.09 mg/kg,all of which did not exceed the maximum residue limit,while and the other 31 kinds of pesticide compounds such as deltamethrin were not detected.Conclusion The established method has a short analysis time,and high sensitivity,which can be used for the simultaneously determination of 36 forbidden and restricted pesticide residues in Citri Reticulatae Pericarpium Viride.
基金项目
浙江省衢州市衢江区科技计划(QJ2021010)
浙江省衢州市"衢六味"质量控制与药理分析科技创新团队项目(衢委人才[2020]3号)
国家科技期刊平台
NSTL
万方数据