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目的:建立高效液相-紫外(HPLC-UV)法测定人血浆中头孢噻利的浓度。方法:血浆样品经高氯酸沉淀蛋白处理后,用阿司匹林作为内标进行HPLC-UV检测;色谱柱采用Diamonsil C18(5μm,4.6 mm×150 mm)色谱柱;流动相为:乙腈+20 mmol/L醋酸铵(8+92,v/v),用冰醋酸调pH至5.20;检测波长为254 nm;结果:在选定的色谱条件下,头孢噻利与血液中的杂质分离良好。头孢噻利在血浆中的线性范围为0.2μg/ml~50.0μg/ml,最低检测浓度(LLOQ)为0.2μg/ml,日内和日间的精密度(RSD)均小于10%,准确度为96%~102%,提取回收率均大于80%。结论:该方法经考察符合生物样品的测定要求,可应用于人血浆中头孢噻利浓度的测定和药代动力学研究。
Objective: To establish a HPLC-UV method for the determination of ceftibrin in human plasma. Methods: The plasma samples were treated with perchloric acid precipitated protein and detected by HPLC-UV with aspirin as internal standard. The column was Diamonsil C18 (5μm, 4.6 mm × 150 mm) L ammonium acetate (8 + 92, v / v). The pH was adjusted to 5.20 with glacial acetic acid. The detection wavelength was 254 nm. Results: Under the selected chromatographic conditions, the separation of ceftibrin and blood impurities was good. The linear range of ceftibrin in plasma was 0.2μg / ml ~ 50.0μg / ml, the lowest detection concentration (LLOQ) was 0.2μg / ml, the intra- and inter-day precision was less than 10%, the accuracy was 96% ~ 102%, extraction recovery rate is greater than 80%. Conclusion: This method is suitable for the determination of ceftibride concentration and pharmacokinetics in human plasma after investigation and accords with the determination of biological samples.