RESUMO
A simple, sensitive, reliable method was developed for the simultaneous determination of organochlorine and pyrethriod pesticide residues in Chinese patent medicines Six ingredient rehmannia pills and Xiaoyao pills. These pesticides were extracted by ethyl acetate. The extraction time and volume of ethyl acetate were optimized. Cleanup of extracts was performed with dispersive-solid phase extraction using graphitized carbon black as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography-tandem mass spectrometry in multiple reaction monitoring mode (GC-MS/MS, MRM). The linearity of the calibration curves is good in matrix-matched standard and yields the coefficients of determination (R2) ≥0.99 for all of the target analytes. Under optimized conditions, the average recoveries (five replicates) for most pesticides range from 75.5% to 114.6%, and RSDs are less than 10.0%. The LODs of 18 pesticides in Six ingredient rehmannia pill and Xiaoyao pills are in the range of 0.01-8.82 µg kg-1. The developed method meets the requirements of pesticide residue analysis and could be effectively used for routine analysis of the organochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pills and Xiaoyao pills.
Assuntos
Medicamentos de Ervas Chinesas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Resíduos de Praguicidas/análise , Piretrinas/análise , Espectrometria de Massas em Tandem/métodos , Calibragem , Medicamentos de Ervas Chinesas/química , Hidrocarbonetos Clorados/análise , Hidrocarbonetos Clorados/química , Limite de Detecção , Medicamentos sem Prescrição , Piretrinas/química , Extração em Fase Sólida/métodosRESUMO
Gas chromatography with nitrogen phosphorus detector (GC-NPD) was applied to the simultaneous determination of 15 organophosphorus and 6 organonitrogen pesticides residues in Angelica sinensis. The pesticides were extracted by microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE) techniques, respectively. The experimental variables were optimized through orthogonal array experimental design. Cleanup of extracts was performed with column chromatography using florisil and neutral aluminum as the sorbents. The determination of pesticides in the final extracts was carried out by GC-NPD. Under optimized conditions, the average recoveries obtained from MAE and UAE are in the range of 75.1-129% and 70.6-129%, respectively, and the relative standard deviations of MAE and UAE were 3.1-10.6% and 1.0-17.8%, respectively.