共鳴ラマン検出のための脂肪族アルデヒドの誘導体化と高速液体クロマトグラフィー

概要

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A high performance liquid chromatography coupled with resonance Raman spectrometric detection was described. For Raman detection of eluates from an analytical column, it is necessary to convert into derivatives which exhibit the resonance Raman effect. Therefore, derivatization reagent was prepared by reacting 4-dimethylaminoazobenzene-4'-sulfonyl chloride (DABS chloride) with hydrazine. DABS hydrazine reacted with carbonyl groups selectively and these derivatives had a maximum absorption at 443 nm in the visible region. The resonance Raman spectra of DABS hydrazones were measured by means of a flow cell in chloroform solution. DABS hydrazones have revealed Raman band at 1135, 1336, 1392, 1421, and 1445 cm^<-1> in the resonance Raman spectra. HPLC separations of DABS hydrazones were accomplished on a Finepak SIL C_<18> column (4.6mmφ×250mm) and 80 % (v/v) acetonitrile/water as a mobile phase at a flow rate of 0.4 ml/min. Chromatograms were obtained by measuring the intensity of resonance Raman scattering at 1135cm^<-1> with 488.0 nm line of Ar^+ laser at 500 mW output. The calibration curve was linear in the range of 5 ppm to 100 ppm of acetaldehyde in aqueous solution. By this procedure, the R. S. D. was 7.3 % at 5 ppm of acetaldehyde.
社団法人日本分析化学会の論文
1985-06-05