Viana E, Moltó J C, Font G
Laboratory of Food Chemistry and Toxicology, Faculty of Pharmacy, University of València, Spain.
J Chromatogr A. 1996 Nov 22;754(1-2):437-44. doi: 10.1016/s0021-9673(96)00538-9.
A multiresidue method based on matrix solid-phase dispersion (MSPD) is studied to determine chlorfenvinfos, chlorpyrifos, fenarimol, iprodione, procimydone, propiconazole, tetradifon, triadimefon and vinclozolin in artichokes, green beans, lettuces and tomatoes. Alumina, silica and Florisil were assessed as extracting phases, and the extracts from Florisil were the cleanest. To facilitate manual extraction, sand was added to the sample together with the dispersing phase. Three eluting systems were then studied, and dichloromethane proved to be the best. Further purification can be performed using solid-phase cleanup after diluting extracts with aqueous solutions. Octyl- and octadecyl-silica, modifications of the aqueous diluted extracts and several eluting solvents were studied. Determination was done by capillary gas chromatography (GC) with electron-capture detection, and confirmed by GC-MS using the electron impact mode and the selected ion monitoring. The proposed MSPD method was used to analyze 48 samples taken in the course of a year. Procymidone, vinclozolin, chlorpyrifos and chlorfenvinfos were identified in 10 samples at levels below the maximum residue levels allowed by the Spanish Government.
研究了一种基于基质固相分散（MSPD）的多残留方法，用于测定洋蓟、四季豆、生菜和西红柿中的毒虫畏、毒死蜱、氯苯嘧啶醇、异菌脲、腐霉利、丙环唑、三氯杀螨砜、三唑酮和乙烯菌核利。评估了氧化铝、硅胶和弗罗里硅土作为萃取相，结果表明弗罗里硅土的提取物最纯净。为便于手动萃取，将沙子与分散相一起加入样品中。随后研究了三种洗脱系统，结果表明二氯甲烷是最佳选择。在用水溶液稀释提取物后，可使用固相净化进行进一步纯化。研究了辛基硅烷和十八烷基硅烷对水稀释提取物的改性以及几种洗脱溶剂。采用带电子捕获检测的毛细管气相色谱（GC）进行测定，并通过GC-MS在电子轰击模式和选择离子监测下进行确证。所提出的MSPD方法用于分析一年中采集的48个样品。在10个样品中检测到腐霉利、乙烯菌核利、毒死蜱和毒虫畏，其含量低于西班牙政府允许的最大残留限量。
