Nony C R, Bowman M C, Holder C L, Young J F, Oller W L
J Pharm Sci. 1976 Dec;65(12):1810-6. doi: 10.1002/jps.2600651229.
Chemical methods were developed for the trace analysis of the herbicide 2,4,5-trichlorophenoxyacetic acid, its glycineamide, and their alkaline hydrolyzable conjugates in mouse blood, urine, and feces. The salient elements of the methods are extraction of the free acids with benzene, methylation, cleanup on a silica gel column, and quantification via electron-capture GLC. Any unextracted conjugates remaining in the substrates are then subjected to alklaline hydrolysis, and the liberated 2,4,5-trichlorophenoxyacetic acid is assayed. Data are presented concerning recoveries of the compounds from the three spiked substrates. The utility of the procedures is illustrated by a preliminary pharmacolinetic study employing parallel electron-capture GLC and radioassays of the three substrates from mice injected with a single intravenous dose of 14C-2,4,5-trichlorophenoxyacetic acid. GLC characteristics and partition values of the the compounds and hydrolysis of the glycineamide under various conditions also are discussed.
已开发出化学方法用于痕量分析小鼠血液、尿液和粪便中的除草剂2,4,5-三氯苯氧乙酸、其甘氨酰胺及其可碱水解的共轭物。这些方法的主要步骤包括用苯萃取游离酸、甲基化、在硅胶柱上净化以及通过电子捕获气相色谱法定量。然后对底物中残留的任何未萃取共轭物进行碱水解,并测定释放出的2,4,5-三氯苯氧乙酸。给出了关于从三种加标底物中回收化合物的数据。通过一项初步药代动力学研究说明了这些程序的实用性,该研究采用平行电子捕获气相色谱法和放射性测定法,对单次静脉注射14C-2,4,5-三氯苯氧乙酸的小鼠的三种底物进行分析。还讨论了这些化合物的气相色谱特征和分配值以及甘氨酰胺在各种条件下的水解情况。