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目的改进测定血浆中甲硝唑含量的RP-HPLC法。方法采用Phenomenex C18分析拄(150mm×4.6mm,5μm),流动相为甲醇-水(25:75),流速1mL·min-1,柱温40℃,替硝唑为内标。血浆样品经pH9.5硼酸盐碱化后用3mL二氯甲烷-乙酸乙酯(1:1)提取浓集,在320nm处检测,按内标法定量。结果甲硝唑和替硝唑的tR分别是4.0、4.8min。甲硝唑0.0125～20μg·mL-1线性关系良好(r=0.9992);最低定量限为0.0125μg·mL-1;批内、批间RSD分别为2.63%～5.83%、4.52%～6.88%;方法回收率为95.67%～108.21%;萃取回收率为70.25%～77.76%。结论所建方法快速简便﹑灵敏准确,适用于甲硝唑肠溶片的人体药动学研究。
Objective To improve the determination of metronidazole in plasma by RP-HPLC method. Methods Phenomenex C18 was used to analyze the column (150 mm × 4.6 mm, 5 μm). The mobile phase consisted of methanol-water (25:75), flow rate 1 mL · min-1 and column temperature 40 ℃. Plasma samples were basified with borate at pH 9.5 and extracted with 3 mL of dichloromethane-ethyl acetate (1: 1), detected at 320 nm and quantified by internal standard method. Results The tR of metronidazole and tinidazole were 4.0 and 4.8 min, respectively. The linear range was 0.0125 ~ 20μg · mL-1 for metronidazole (r = 0.9992). The lowest limit of quantification was 0.0125μg · mL-1. The intra- and inter-batch RSD were 2.63% -5.83% and 4.52% -6.88% The recoveries of the method ranged from 95.67% to 108.21%. The extraction recoveries ranged from 70.25% to 77.76%. Conclusion The method is rapid, simple, sensitive and accurate and suitable for the study of human pharmacokinetics of metronidazole enteric-coated tablets.