Fogy I, Schmid E R, Huber J F
Z Lebensm Unters Forsch. 1979 Dec;169(6):438-43. doi: 10.1007/BF01126746.
It is shown that carbamate pesticides can be determined at the ppm level in different kinds of fruits and vegetables using high pressure liquid chromatography. The lower detection limit corresponding to a signal to noise ratio of three is between 0,025 and 0,25 ppm depending on the type of carbamate and plant material. In all cases it is below the maximum permissible value for pesticide residues. Due to the high separating power of high pressure liquid chromatography a simple sample pretreatment procedure can be used. The carbamates are extracted from the biological sample by dichloromethane and injected directly into the liquid chromatograph after replacing the extraction solvent by the mobile phase. In many cases a definite identification and quantitation of the carbamate is possible with a single chromatographic column. Some plants with a more complex matrix require a two-column operation in which the effluent fraction of the first column containing the pesticide is transferred by column switching to a second column in order to achieve a complete separation. The improved resolution in the two-column operation is caused by the relative enrichment effect of the fractionation and the increased column length.
结果表明,使用高压液相色谱法可以测定不同种类水果和蔬菜中百万分比浓度水平的氨基甲酸酯类农药。对应于信噪比为3的最低检测限在0.025至0.25 ppm之间,具体取决于氨基甲酸酯的类型和植物材料。在所有情况下,该检测限均低于农药残留的最大允许值。由于高压液相色谱具有高分离能力,因此可以采用简单的样品预处理程序。用二氯甲烷从生物样品中提取氨基甲酸酯类,并用流动相替换提取溶剂后直接注入液相色谱仪。在许多情况下,使用单一色谱柱就可以对氨基甲酸酯进行明确的鉴定和定量。一些基质较为复杂的植物需要进行双柱操作,其中通过柱切换将含有农药的第一柱流出物馏分转移至第二柱,以实现完全分离。双柱操作中分辨率的提高是由分馏的相对富集效应和增加的柱长导致的。