固定相24：β-酮醯胺-金屬錯合物鍵結矽膠之吸附及液相層析選擇研究

Stationary Phases 24: Adsorption and Liquid Chromatographic Selectivity of β-Ketoamide-metal Complex Chemically Bonded Silica

吳鎰州(Y. Z. Wu) ； 郭陳叡(C. R. Kou) ； 駱宏鼎(H. D. Luoh) ； 鄧朝岡(T. G. Den)

《化學》 49卷3期 (1991/09) Pp. 207-216

https://doi.org/10.6623/chem.1991027

摘要

本文爲用自製之β-酮醯胺-銅(或鐵)化學鍵結矽膠作支體，對一系列供電子樣品作吸附及高效液相層析研究。所自製之β-酮醯胺-銅(或鐵)固定相爲用[3-(2-氨基乙基)氨基丙基]三甲氧基矽烷與矽膠(共兩種型式，100～200 mesh型爲吸附用，10 μm型爲高效液相層析用)耦合，接著再與diketene反應，最後再與銅或鐵離子鍵結而成。在吸附應用上，此產品可在批次法下對甲醇溶劑中之hydrazine，phenylhydrazine，2,4- dinitrophenyl-hydrazine，Acetylacetone，Pyridine，triphenylphosphine等樣品作選擇吸附，每克最大吸附量對hydrazine及acetylacetone最佳，約爲0.24~0.27 mmol，其他被吸附樣品則爲0.01 ~ 0.03 mmol之間，但對dimetylsulfide，naphthalene，9-methylanthracene，hydrazone衍生物等則無明顯吸附。在高效液相層析上，正逆相層析分離在此錯合體固定相上可明顯看出對酮類丶pyridine丶醌類等樣品有較強之滯留，並可與在無金屬之β-酮醯胺基固定相上比較出。

並列摘要

The adsorption and high performance liquid chromatographic selectivity of several electron rich compounds on .β-ketoamidecopper or iron complex chemically bonded silica is investigated. The title products were prepared by the coupling of [3-(2-aminoethyl) aminopropyl] trimethoxysilane and silica (100-200 mesh for batch adsorption, or 10 urn for HPLC), followed by the reaction with diketene and finally bonded with Cu(II) or Fe(III). In application, hydrazine, phenylhydrazine, 2,4-dinitrophenylhydrazine, acetylacetone, pyridine and triphenylphosphine in methanol solvent can be adsorbed by these support materials, and no significant affinity is observed for dimethylsulfide, hydrazone derivative, naphthalene and 9-methylanthracene. The maximun sample uptake capacities are found in range from 0.24 to 0.27 mmol/g for hydrazine or acetylacetone, and from 0.01 to 0.03 mmol/g for phenylhydrazine, 2,4-dinitrophenylbydrazine, triphenylphosphine or pyridine. In HPLC, reversed phase and normal phase liquid chromatography of ketones, quinones or pyridine have effective strong retentions on these complex ststionary phases, when compared with another nonmetallic ,B-ketoamide stationary phase.