色谱2012，Vol.30Issue(9)：889-895,7.DOI:10.3724/SP.J.1123.2012.04024
茶叶中氟虫腈等8种农药残留的液相色谱-串联质谱法测定及不确定度评定
Determination of eight pesticide residues in tea by liquid chromatography-tandem mass spectrometry and its uncertainty evaluation
摘要
Abstract
A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1= 1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C18 column (150 mm x 2.1 mm, 5 (xm) and with the gradient elu-tion of acetonitrile and 0.1% formic acid. The eight pesticides were determined in the modes of electrospray ionization ( ESI) and multiple reaction monitoring ( MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 -100 jig/L for fipronil, and in 5 -200 jig/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 jig/kg for fipronil and 10 fig/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115. 0% with the relative standard deviations of 2.7% - 7. 7% at the spiked levels of 2, 5, 50 kg/kg for fipronil and 10, 50, 100jjLg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea.关键词
液相色谱-串联质谱/不确定度评定/农药残留/茶叶Key words
liquid chromatography-tandem mass spectrometry (LC-MS/MS)/ uncertainty evaluation/ pesticide residues/ tea分类
化学化工引用本文复制引用
胡贝贞,蔡海江,宋伟华..茶叶中氟虫腈等8种农药残留的液相色谱-串联质谱法测定及不确定度评定[J].色谱,2012,30(9):889-895,7.基金项目
浙江出入境检验检疫局项目(ZK200993X). （ZK200993X）
