高效液相色谱法测定血清中甲氨蝶呤及其代谢物
HPLC determination of methotrexate and its metabolite in serum.
作者信息
Brandsteterová E, Seresová O, Miertus S, Reichelová V
机构信息
Department of Analytical Chemistry, Slovak Technical University, Bratislava, Czechoslovakia.
出版信息
Neoplasma. 1990;37(4):395-403.
Determination of methotrexate (MTX) residues in biological samples (serum, cerebrospinal fluid) was worked out using liquid-liquid and solid-phase extractions and high performance liquid chromatography (HPLC) with UV detection. Clinical samples from patients treated by low and high doses of MTX were analyzed using reversed-phase and ion-pair liquid chromatography, and buffer-methanolic mobile phases. Chromatographic conditions were optimized for the simultaneous determination of MTX and its metabolite and the minimal analysis time was recommended. The results were statistically evaluated, elimination curves and chromatograms have been demonstrated. Solid-phase extraction recovery was 93.1 +/- 1.5% and the determination limit for methotrexate in serum samples was 5.10(-7) mol/l and after the preconcentration of samples 5.10(-8) mol/l.
采用液-液萃取和固相萃取以及带紫外检测的高效液相色谱法（HPLC）测定生物样品（血清、脑脊液）中的甲氨蝶呤（MTX）残留。使用反相和离子对液相色谱法以及缓冲液-甲醇流动相分析了接受低剂量和高剂量MTX治疗患者的临床样品。对色谱条件进行了优化，以同时测定MTX及其代谢物，并推荐了最短分析时间。对结果进行了统计学评估，展示了消除曲线和色谱图。固相萃取回收率为93.1±1.5%，血清样品中甲氨蝶呤的测定限为5×10⁻⁷mol/l，样品预浓缩后为5×10⁻⁸mol/l。
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