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目的建立一种同时测定人血浆中甲砜霉素(TAP)及其前药甲砜霉素甘氨酸酯(TG)的高效液相色谱法。方法采用高氯酸蛋白沉淀法处理血浆,色谱柱为Kromasil-C18反相柱(150 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(pH=2)-甲醇-乙腈(85∶12∶3,V/V/V),流速为1 mL·min-1,检测波长为224 nm。结果血浆中TAP和TG标准曲线线性范围均为0.5～100 mg·L-1,定量限浓度均为0.5 mg·L-1;高、中、低(50,10和1 mg·L-1)3种浓度的日间和日内变异均小于5.0%,准确度偏差小于5.0%。血浆经室温4 h、-70℃冷冻放置2 mo、冻融2次或高氯酸处理均显示TAP和TG稳定性较好。结论该方法灵敏、准确、简单、快速,可用于TAP和TG的药动学研究。
Objective To establish a high performance liquid chromatographic method for the simultaneous determination of thiamphenicol (TAP) and its precursor thiamphenicol glycinate (TG) in human plasma. Methods The plasma was treated with perchloric acid precipitation method. The column was Kromasil-C18 reversed-phase column (150 mm × 4.6 mm, 5 μm). The mobile phase consisted of phosphate buffer solution (pH = 2) : 3, V / V / V) with a flow rate of 1 mL · min-1 and a detection wavelength of 224 nm. Results The linear range of TAP and TG in plasma was 0.5-100 mg · L-1 and the limit of quantification was 0.5 mg · L-1. High, medium and low (50, 10 and 1 mg · L -1) The intra-day and intra-day variation of the three concentrations were less than 5.0% and the accuracy deviation was less than 5.0%. The plasma was stable at room temperature 4 h, frozen at -70 ℃ for 2 months, frozen-thawed twice or treated with perchloric acid. Conclusion The method is sensitive, accurate, simple and rapid and can be used for pharmacokinetic studies of TAP and TG.