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目的建立一种灵敏、可靠的测定人血清中硫酸头孢噻利浓度的高效液相色谱二极管阵列检测方法。方法血清样品经酸化甲醇蛋白沉淀后,以0.02 mol·L~(-1)乙酸铵-甲醇(75:25,V/V)为流动相,色谱柱为Extend C_(18)柱(250 mm×4.6 mm,5μm),头孢唑林为内标,检测波长为254 nm,流速为0.5 mL·min~(-1)。结果硫酸头孢噻利的绝对回收率为79.9%~84.7%,方法回收率为91.7%~103.3%,日内精密度(RSD)<5.2%,日间精密度(RSD)<7.3%,硫酸头孢噻利质量浓度在0.02~1.0mg·L~(-1)时具有良好线性,定量检出限为0.02 mg·L~(-1)。结论本方法具有简便、灵敏、准确等优点,可用于硫酸头孢噻利的临床药动学研究及临床特殊人群的血药浓度测定。
Objective To establish a sensitive and reliable method for the determination of ceftiofur sulfate in human serum by high performance liquid chromatography (HPLC) diode array. Methods The serum samples were precipitated with acidified methanol. The mobile phase was 0.02 mol·L -1 ammonium acetate - methanol (75:25, V / V) and the column was Extend C 18 column (250 mm × 4.6 mm, 5 μm) and cefazolin as the internal standard. The detection wavelength was 254 nm and the flow rate was 0.5 mL · min ~ (-1). Results The absolute recovery of cefoselis sulfate was 79.9% ~ 84.7%, the recovery rate was 91.7% ~ 103.3%, the intra-day precision was lower than 5.2%, the intraday precision was lower than 7.3% The linear range was 0.02 ~ 1.0 mg · L -1 with a limit of quantification of 0.02 mg · L -1. Conclusion The method is simple, sensitive and accurate. It can be used in the clinical pharmacokinetics of cefoselis sulfate and the determination of blood concentration in clinical special population.