化学発光検出高速液体クロマトグラフィーによるメタンフェタミンの定量(<特集>医療と分析化学)

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A method is described for the determination of methamphetamine (MP) by a high-performance liquid-chromatographic method using a peroxyoxalate chemiluminescence reaction. After MP was derivatized with 4-(N, N-dimethylaminosulphonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F), it was detected by a chemiluminescence method. Bis(2,4,6-trichlorophenyl) oxalate (TCPO) and hydrogen peroxide were used as postcolumn chemiluminescence reagents. The separation of the DBD-F derivative of MP was carried out using a reversed-phase column (GL Science, Lichrospher RP 18-5,4.6i.d.×250 mm) and an acetonitrile aqueous solution as the mobile phase (flow rate, 1.0ml/min). The optimum pH, temperature and reaction time for fluorogenic reactions of DBD-F and MP were 8,70℃, 30 min, respectively. The linear calibration graph was observed over the range of 5×10^<-9>〜5×10^<-6> M. The correlation coefficient for this line was 0.999. The detection limit (3σ) was 2×10^<-9> M (40fmol) and the relative standard deviation was 1.4% (n=6) for a concentration of 5×10^<-9> M. The effect of urine on the MP determination was investigated. The urine sample solutions were prepared by adding a 1×10^<-7> M or 1×10^<-8> M MP standard solution to a normal human urine. The relative chemiluminescence intensities were 98〜102% toward the chemiluminescence intensity of the MP standard solution.
社団法人日本分析化学会の論文
1997-12-05