Abstract：
Ceftriaxone (CTRX) is a commonly used cephalosporin antibiotic. It is suggested that monitoring plasma/serum concentrations is helpful for its safe use. This study aimed to develop and validate an analytical method for measuring CTRX concentrations in human serum according to International Conference on Harmonization guideline M10. Ten microliters of serum sample was purified using a salting-out assisted liquid-liquid extraction procedure with magnesium sulfate. The upper layer was then diluted threefold and analyzed using a liquid chromatography-tandem mass spectrometry-based method with a total run time of 12 min. The linear calibration curve was obtained over the concentration range 5-500 μg/ml. The within-run accuracy varied from 0.2 to 6.5%, and the precision was ≤8.0%. The between-run accuracy and precision ranged from 0.7% to 5.6% and ≤6.4%, respectively. Significant carryover was resolved by injecting four blanks after high-concentration CTRX samples. The recovery rates from spiked serum at low and high concentrations were 44.4 and 43.4%, respectively. Other factors, including selectivity, matrix effects, stability, dilution integrity and reinjection reproducibility also met the acceptance criteria. Serum concentrations in 14 samples obtained from two participants receiving 2 g/day of CTRX were successfully determined using this method.
摘要：
头孢曲松(CTRX)是一种常用的头孢菌素类抗生素。建议监测血浆/血清浓度有助于其安全使用。本研究旨在根据国际协调会议指南M10开发和验证一种用于测量人血清中CTRX浓度的分析方法。使用硫酸镁的盐析辅助液-液萃取程序纯化十微升血清样品。然后将上层稀释三倍,并使用基于液相色谱-串联质谱的方法进行分析,总运行时间为12分钟。在5-500μg/ml的浓度范围内获得线性校准曲线。运行中的精度从0.2％到6.5％不等，精密度≤8.0%。运行间准确度和精密度范围为0.7%至5.6%，≤6.4%，分别。通过在高浓度CTRX样品后注射四个空白来解决显著的残留。低浓度和高浓度加标血清的回收率分别为44.4和43.4％，分别。其他因素,包括选择性，矩阵效应，稳定性,稀释完整性和回注再现性也符合验收标准。使用该方法成功地测定了从接受2g/天CTRX的两名参与者获得的14个样品中的血清浓度。
