Residues and Contaminants Laboratory - LANAGRO-GO, Ministry of Agriculture, Livestock and Food Supply, Goiânia, Goiás, CEP 74674-025, Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(4):641-56. doi: 10.1080/19440049.2011.606230. Epub 2011 Oct 21.
A within-laboratory validation procedure for a selective and sensitive method for the simultaneous determination of 98 pesticide residues in mango is presented. QuEChERS extraction was adapted to laboratory conditions. Mango samples (10 g) mixed with sodium sulfate (4 g) and sodium acetate (1 g) were extracted with acetonitrile/acetic acid (99/1 v/v), cleaned using dispersive solids, and subsequently identified and quantified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Pesticides were separated on a reversed-phase column using a gradient elution in conjunction with positive-mode electrospray ionisation. The analytical performance of the method was demonstrated by analysis of spiked mango samples at three concentration levels (0.01, 0.05 and 0.1 mg kg(-1)) for 3 different days, and the analysis was performed by three analysts. Calibration curves were statistically acceptable by the ordinary last-square method (OLSM), with a regression coefficient above 0.98 for all analytes. The method accuracy (n = 18) was between 80% and 110%, and precisions were below 20% for 95% of the analytes. The method uncertainty at the LOQ was evaluated considering the uncertainty associated with the calibration curve and the uncertainty associated with the method precision. The validation data for all pesticides were in accordance with Brazilian and European guidelines for pesticide residue analysis.
本文介绍了一种在实验室条件下对芒果中 98 种农药残留进行同时检测的选择性和灵敏性方法的验证程序。QuEChERS 提取方法经过了实验室条件的调整。将芒果样品（10 g）与硫酸钠（4 g）和乙酸钠（1 g）混合，用乙腈/乙酸（99/1 v/v）提取，使用分散固相萃取净化，然后通过液相色谱-串联质谱（LC-MS/MS）进行鉴定和定量分析。采用正离子模式电喷雾离子化，在反相柱上通过梯度洗脱对农药进行分离。通过在 3 个不同天的 3 个浓度水平（0.01、0.05 和 0.1 mg kg(-1))对添加芒果样品进行分析，证明了该方法的分析性能，所有分析物的线性回归系数均大于 0.98。通过普通最小二乘法（OLSM）对校准曲线进行统计评估，方法的准确度（n = 18）在 80%至 110%之间，95%的分析物的精密度低于 20%。在 LOQ 时，通过考虑校准曲线的不确定度和方法精密度的不确定度来评估方法的不确定性。所有农药的验证数据均符合巴西和欧洲农药残留分析指南的要求。
