Wang Lu, Zheng Xin, Zhong Wen, Chen Jia, Jiang Ji, Hu Pei
Peking Union Medical College Hospital, N°41 Damucang, Xidan, Xicheng District, Beijing 100032, PR China.
Peking Union Medical College Hospital, N°41 Damucang, Xidan, Xicheng District, Beijing 100032, PR China
J Chromatogr Sci. 2016 May-Jun;54(5):713-9. doi: 10.1093/chromsci/bmv243. Epub 2016 Feb 18.
Ceftizoxime sodium is a third-generation cephalosporin available for parenteral administration, which is mainly excreted through urine. A rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method was developed and validated for the determination of ceftizoxime in human serum and urine. The samples were purified by protein precipitation and separated on an XTerra Phenyl column (4.6 × 50 mm, 5 µm). Electrospray ionization in the positive ion mode and multiple reaction monitoring were used to monitor the ion transitions at m/z 383.9/227.0. The results revealed that the method had excellent selectivity. The linear range covered from 2.50 to 10,000 ng/mL in serum and from 0.500 to 50.0 µg/mL in urine, respectively. Intra-batch and inter-batch precisions (in terms of relative standard deviation) were all <15% and the accuracies (in terms of relative error) were within the range of ± 15%. The lower limit of quantification, stability and extraction recovery were also validated and satisfied the criteria of validation. Finally, the method was successfully applied to a pharmacokinetic study of Chinese elderly healthy subjects after intravenous administration. The Cmax values in serum were 34,721.3 ± 5,697.3 ng/mL. Serum concentrations declined with t1/2 of 2.57 ± 0.22 h.
头孢唑肟钠是一种可供肠胃外给药的第三代头孢菌素，主要通过尿液排泄。建立并验证了一种快速灵敏的超高效液相色谱-串联质谱法（UPLC-MS-MS），用于测定人血清和尿液中的头孢唑肟。样品通过蛋白沉淀法进行纯化，并在XTerra苯基柱（4.6×50 mm，5 µm）上进行分离。采用正离子模式下的电喷雾电离和多反应监测来监测m/z 383.9/227.0处的离子跃迁。结果表明该方法具有出色的选择性。血清中的线性范围分别为2.50至10,000 ng/mL，尿液中的线性范围为0.500至50.0 µg/mL。批内和批间精密度（以相对标准偏差计）均<15%，准确度（以相对误差计）在±15%范围内。还对定量下限、稳定性和提取回收率进行了验证，并满足验证标准。最后，该方法成功应用于中国老年健康受试者静脉给药后的药代动力学研究。血清中的Cmax值为34,721.3±5,697.3 ng/mL。血清浓度以2.57±0.22 h的t1/2下降。
