Detection of 36 Forbidden and Restricted Pesticide Residues in Citri Reticulatae Pericarpium Viride by UPLC-MS/MS
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.
UPLC-MS/MSCitri Reticulatae Pericarpium Virideforbidden and restricted pesticideresidues
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