Separation and determination of geometrical isomers of metal chelates of benzoylacetone and trifluoroacetylacetone by high-performance liquid chromatography

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Other Title
  • 高速液体クロマトグラフィーによるベンゾイルアセトン及びトリフルオロアセチルアセトンの金属キレートの幾何異性体の分離と定量
  • コウソク エキタイ クロマトグラフィー ニヨル ベンゾイルアセトン オヨビ ト

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Abstract

A simple and rapid method was established for the separation and determination of octahedral geometric isomers of cobalt (III), chromium(III), and rhodium (III) chelates of benzoylacetone (BA) and trifluoroacetylacetone (TFA) by high-performance liquid chromatography (HPLC). The HPLC separation of cis and trans isomers of the three BA chelates was performed on an alumina column (Woelm Alumina basic, 25μ, 4mm×50cm), using hexane-2-propanol (100:0.15) as the eluent. The separation of cis and trans isomers of the three TFA chelates was achieved on a silica gel column (Waters μ Porasil, 10μ, 3.9mm×30cm), using benzene-hexane (60:40) as the eluent. By maintaining the temperature of the column at (22.0±0.1)°C in a thermostat during HPLC operations, the reproducibilities of the retention times and the peak heights were improved (averaged1% and1.4 %, respectively), and the linear calibration curves were obtained in the concentration range of (10-610-3)mol/l for the twelve isomers studied. The average of the correlation coefficients of the calibration curves obtained for twelve isomers was 0.9995. The detection limits of the isomers were in the concentration range of (16)×10-6 mol/l and were (1.2×10-11, 2.8×10-12)mol for 2 μl of sample. The recovery and the coefficient of variation of the determination of these isomers were (96.1104) % (average 98.8%) and (0.62.8)% (average 1.3%), respectively.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 32 (10), 605-610, 1983

    The Japan Society for Analytical Chemistry

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