中国药业2024，Vol.33Issue(11)：75-79,5.DOI:10.3969/j.issn.1006-4931.2024.11.017
超高效液相色谱串联质谱法测定青皮中36种禁限用农药残留量
Detection of 36 Forbidden and Restricted Pesticide Residues in Citri Reticulatae Pericarpium Viride by UPLC-MS/MS
摘要
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.关键词
超高效液相色谱串联质谱法/青皮/禁限用农药/残留量Key words
UPLC-MS/MS/Citri Reticulatae Pericarpium Viride/forbidden and restricted pesticide/residues分类
医药卫生引用本文复制引用
方蓓倩,袁诗晴,徐礼萍,姚建胜,卫欣,宋剑锋..超高效液相色谱串联质谱法测定青皮中36种禁限用农药残留量[J].中国药业,2024,33(11):75-79,5.基金项目
浙江省衢州市衢江区科技计划项目[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]. （）
