King J R, Nony R C, Bowman M C
J Chromatogr Sci. 1977 Jan;15(1):14-21. doi: 10.1093/chromsci/15.1.15.
An analytical method is described for determining residues of the synthetic estrogen diethylstilbestrol (DES) in animal chow at levels as low as 1 ppb. A methanol extract of the chow is subjected to a 3-step cleanup procedure including a Sephadex LH-20 column, liquid-liquid partitioning at pH 14 and 10.2, and a silica gel column. Residues of DES in the cleaned-up extract are analyzed directly by high-speed liquid chromatography or derivatized to pentafluoropropionyl-DES and assayed by electron-capture gas chromatography. Tests with 14C-DES were used to develop and validate the procedure. Ancillary data concerning extraction efficiencies of various solvents, comparisons of various derivatizing reagents, rates of trans-cis isomerization in two solvents, P-values of DES in various solvent-systems and thin-layer chromatographic behavior i
描述了一种分析方法，用于测定动物饲料中低至1 ppb水平的合成雌激素己烯雌酚（DES）残留量。饲料的甲醇提取物经过三步净化程序，包括Sephadex LH - 20柱、在pH 14和10.2下的液 - 液分配以及硅胶柱。净化后的提取物中的DES残留量直接通过高效液相色谱法分析，或衍生化为五氟丙酰 - DES并通过电子捕获气相色谱法测定。使用¹⁴C - DES进行测试以开发和验证该程序。关于各种溶剂的提取效率、各种衍生化试剂的比较、两种溶剂中反 - 顺异构化速率、DES在各种溶剂体系中的P值以及薄层色谱行为的辅助数据i
