Johnson L D, Waltz R H, Ussary J P, Kaiser F E
J Assoc Off Anal Chem. 1976 Jan;59(1):174-87.
Applications of an improved gel-solvent system for cleanup of pesticide residues by gel permeation chromatography (GPC) were investigated. Elution characteristics using Bio-Beads SX-3 gel and a toluene-ethyl acetate (1+3) elution solvent were determined for 16 nonionic chlorinated pesticides, 3 polychlorinated biphenyls (PCBs), 14 chlorophenoxy herbicide esters, and 7 organophosphate insecticides. Elution patterns for vegetable and animal lipids were also studied. Quantitative recoveries of the pesticides were achieved. No liquid-liquid partitioning cleanup steps were required with any type of nonionic chlorinated pesticide or sample matrix. Only GPC cleanup was required for the nonionic chlorinated pesticides, PCBs, and organophosphate pesticide residues in chicken and turkey fat samples. Electron capture and flame photometric detectors were used in the gas chromatographic method for the respective pesticides. Samples containing up to 0.5 g lipid each were processed at the rate of one every 30-40 min with the automated system. Results were in excellent agreement with those from accepted manual partitioning methods and were achieved with significant savings of both labor and chemicals.
研究了一种改进的凝胶 - 溶剂系统在凝胶渗透色谱法(GPC)净化农药残留中的应用。测定了使用Bio - Beads SX - 3凝胶和甲苯 - 乙酸乙酯(1 + 3)洗脱溶剂对16种非离子型氯化农药、3种多氯联苯(PCBs)、14种氯苯氧基除草剂酯和7种有机磷杀虫剂的洗脱特性。还研究了蔬菜和动物脂质的洗脱模式。实现了农药的定量回收。对于任何类型的非离子型氯化农药或样品基质,都无需液 - 液分配净化步骤。鸡肉和火鸡脂肪样品中的非离子型氯化农药、多氯联苯和有机磷农药残留仅需GPC净化。气相色谱法中分别使用电子捕获检测器和火焰光度检测器检测相应的农药。使用自动化系统,每30 - 40分钟处理一个含脂量高达0.5 g的样品。结果与公认的手动分配方法所得结果高度一致,且显著节省了人力和化学试剂。