Barnhart E R, Patterson D G, Tanaka N, Araki M
Division of Environmental Health Laboratory Sciences, Centers for Disease Control, Atlanta, GA 30333.
J Chromatogr. 1988 Jul 8;445(1):145-54. doi: 10.1016/s0021-9673(01)84516-7.
To purify the tetrachlorobenzo-p-dioxins synthesized for chemical and biological reference standards, reversed-phase liquid chromatography on pyrenylethyl- and octadecylsilylated stationary phase (PYE and C18) columns was employed with 100% methanol. The pyrenylethyl phase satisfactorily separated isomers resulting from mixtures of reaction products which had not been adequately separated with conventional C18 or silica gel. The use of a single chromatographic mode, liquid chromatography, and a single mobile phase with columns of distinctly different properties, C18 and PYE, separates 20 of the 22 isomers from each other and from the 1246/1249 pair. (The observed properties of the two columns afford insight into steric and polarizability differences among isomers.)
为了纯化合成用作化学和生物学参考标准的四氯苯并对二恶英,采用100%甲醇在芘乙基和十八烷基硅烷化固定相(PYE和C18)柱上进行反相液相色谱法。芘乙基相能令人满意地分离反应产物混合物产生的异构体,而这些异构体用传统的C18或硅胶无法充分分离。使用单一的色谱模式(液相色谱)和单一的流动相,搭配性质明显不同的C18和PYE柱,可将22种异构体中的20种彼此分离,并与1246/1249对分离。(两根柱所观察到的性质有助于深入了解异构体之间的空间和极化率差异。)