Navickiene Sandro, Aquino Adriano, Bezerra Débora Santos Silva
Departamento de Química, Universidade Federal de Sergipe, Av. Marechal Rondon s/n°, Jardim Rosa Elze, 49100-000 São Cristóvão/SE, Brazil.
J Chromatogr Sci. 2010 Oct;48(9):750-4. doi: 10.1093/chromsci/48.9.750.
A simple and effective extraction method based on matrix solid-phase dispersion was developed to determine trichlorfon, pyrimethanil, methyl parathion, tetraconazole, thiabendazole, imazalil, and tebuconazole in papaya and mango using gas chromatography-mass spectrometry with selected ion monitoring. Different parameters of the method were evaluated, such as type of solid-phase (silica-gel, neutral alumina, and Florisil), the amount of solid-phase, and eluent [dichloromethane, ethyl acetate-dichloromethane (4:1, 1:4, 1:1, 2:3, v/v)]. The best results were obtained using 2.0 g of mango or papaya, 3.0 g of silica as dispersant sorbent, and ethyl acetate-dichloromethane (1:1, v/v) as eluting solvent. The method was validated using mango and papaya samples fortified with pesticides at different concentration levels (0.05, 0.10, and 1.0 mg/kg). Average recoveries (4 replicates) ranged from 80% to 146%, with relative standard deviations between 1.0% and 28%. Detection and quantification limits for mango and papaya ranged from 0.01 to 0.03 mg/kg and 0.05 to 0.10 mg/kg, respectively. The proposed method was applied to the analysis of these compounds in commercial fruit samples from a local market (Aracaju/SE, Brazil), and residues of the pesticides were not detected on the samples.
建立了一种基于基质固相分散的简单有效的提取方法，用于使用气相色谱-质谱联用选择离子监测法测定木瓜和芒果中的敌百虫、嘧霉胺、甲基对硫磷、四氟醚唑、噻菌灵、抑霉唑和戊唑醇。对该方法的不同参数进行了评估，如固相类型（硅胶、中性氧化铝和弗罗里硅土）、固相量和洗脱剂[二氯甲烷、乙酸乙酯-二氯甲烷（4:1、1:4、1:1、2:3，v/v）]。使用2.0 g芒果或木瓜、3.0 g硅胶作为分散吸附剂以及乙酸乙酯-二氯甲烷（1:1，v/v）作为洗脱溶剂时获得了最佳结果。该方法通过在不同浓度水平（0.05、0.10和1.0 mg/kg）下添加农药的芒果和木瓜样品进行了验证。平均回收率（4次重复）在80%至146%之间，相对标准偏差在1.0%至28%之间。芒果和木瓜的检测限和定量限分别为0.01至0.03 mg/kg和0.05至0.10 mg/kg。将该方法应用于当地市场（巴西阿拉卡茹/塞尔希培）商业水果样品中这些化合物的分析，样品中未检测到农药残留。
