Oliva J, Navarro S, Barba A, Navarro G
Technological National Center of Canning Industry (CTC), Murcia, Spain.
J Chromatogr A. 1999 Feb 12;833(1):43-51. doi: 10.1016/s0021-9673(98)00860-7.
A rapid gas chromatographic method for determination of residue levels of one insecticide (chlorpyrifos) and four fungicides (penconazole, fenarimol, vinclozolin and metalaxyl) in grapes, must and wine is described. An on-line microextraction method was used. The matrix, once extracted with a mixture of acetone-dichloromethane (1:1, v/v) was filtered and concentrated. Electron-capture detection for chlorpyrifos, penconazole, fenarimol and vinclozolin and mass-selective detection in the selected-ion monitoring mode for metalaxyl were utilised. No clean-up was necessary because there were no interferences in the area of interest of the chromatogram. Linearity of both detectors, in the range 0.02-2 ng/microliter, was checked. In all cases, the correlation coefficient was the same or superior to 0.997. Recoveries from spiked grapes, must and wine ranged from 78% to 101% (fortification level, 0.1-1 mg/kg). Limits of determination were between 0.01 mg/kg for metalaxyl and 0.001 mg/kg for vinclozolin.
描述了一种快速气相色谱法，用于测定葡萄、葡萄汁和葡萄酒中一种杀虫剂（毒死蜱）和四种杀菌剂（戊唑醇、粉锈宁、乙烯菌核利和甲霜灵）的残留量。采用了在线微萃取法。用丙酮 - 二氯甲烷（1:1，v/v）混合物萃取基质后，进行过滤和浓缩。对毒死蜱、戊唑醇、粉锈宁和乙烯菌核利用电子捕获检测，对甲霜灵采用选择离子监测模式下的质量选择性检测。由于色谱图感兴趣区域没有干扰，无需净化。检查了两种检测器在0.02 - 2 ng/微升范围内的线性。在所有情况下，相关系数均相同或优于0.997。加标葡萄、葡萄汁和葡萄酒的回收率在78%至101%之间（强化水平为0.1 - 1 mg/kg）。甲霜灵的测定限为0.01 mg/kg，乙烯菌核利的测定限为0.001 mg/kg。
