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目的:建立一种灵敏、可靠的检测血清中硫酸头孢噻利含量的高效液相色谱-串联质谱法。方法:血清样品经酸化甲醇蛋白沉淀后,采用Extend C_(18)柱(250 mm×4.6mm,5μm)0.02 mol·L~(-1)乙酸铵-甲醇(65:35)为流动相,头孢唑啉为内标,应用高效液相色谱/大气压化学电离串联质谱法在多反应监测模式(MRM)下测定,硫酸头孢噻利和内标的定量离子对分别为m/z 523→396和m/z 455→323。结果:硫酸头孢噻利的回收率在94.0%～101.9%之间,硫酸头孢噻利在2.0～1000.0μg·L~(-1)范围内呈良好线性,日内RSD<9.2%,日间RSD<10.6%,定量检出限为2.0μg·L~(-1)。结论:本方法简便、灵敏、干扰少、特异性好,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 serum by high performance liquid chromatography-tandem mass spectrometry. Methods: The serum samples were precipitated with acidified methanol and the mobile phase consisted of 0.02 mol·L -1 ammonium acetate - methanol (65:35) with Extend C 18 column (250 mm × 4.6 mm, 5 μm) The internal standard of oxazoline was determined by high performance liquid chromatography / atmospheric pressure chemical ionization tandem mass spectrometry in multiple reaction monitoring mode (MRM). The quantitative ion pairs of cefoselir sulfate and internal standard were m / z 523 → 396 and m / z 455 → 323. Results: The recoveries of cefoselir sulfate ranged from 94.0% to 101.9%, and cefoselir sulfate showed a good linearity within the range of 2.0-1000.0 μg · L -1. The intraday RSD was less than 9.2% and the intraday RSD was < 10.6%, and the limit of quantification was 2.0 μg · L -1. Conclusion: The method is simple, sensitive, less interference and good specificity, which can be used in the clinical pharmacokinetics of cefoselis sulfate and the determination of blood concentration in the special clinical population.