Institute of Antibiotics, Huashan Hospital, Fudan University, 12 M. Wulumuqi Road, Shanghai 200040, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Nov 15;878(30):3119-24. doi: 10.1016/j.jchromb.2010.09.021. Epub 2010 Oct 1.
A rapid and highly sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for simultaneous determination of cefoperazone sodium and sulbactam sodium in human plasma was developed. The analytes and internal standard (IS), cefuroxime sodium, were extracted from human plasma via liquid-liquid extraction with ethyl acetate and separated on a Waters Xterra C18 column within 3.5 min. Quantitation was performed on a triple quadrupole mass spectrometer employing electrospray ionization technique, operating in selected reaction monitoring (SRM) and negative ion mode. The precursor to product ion transitions monitored for cefoperazone, sulbactam and IS were m/z 644.1→528.0, 232.1→140.0, and 423.0→362.0, respectively. The assay was validated in the linear range of 0.1-20 μg/mL for cefoperazone and 0.02-4 μg/mL for sulbactam. The intra- and inter-day precisions (CV%) were within 8.39% for each analyte. The recoveries were greater than 87.3% for cefoperazone and 87.2% for sulbactam. Each analyte was found to be stable during all sample storage, preparation and analytical procedures. The method was successfully applied in a pharmacokinetic study of Sulperazon injection in six hospital-acquired pneumonia (HAP) patients.
建立了一种快速灵敏的液相色谱-串联质谱（LC-MS/MS）法，用于同时测定人血浆中的头孢哌酮钠和舒巴坦钠。分析物和内标（IS）头孢呋辛钠通过乙酸乙酯液-液萃取从人血浆中提取，在 Waters Xterra C18 柱上在 3.5 分钟内分离。定量采用电喷雾电离技术的三重四极杆质谱仪在选择反应监测（SRM）和负离子模式下进行。监测的头孢哌酮、舒巴坦和 IS 的前体到产物离子跃迁分别为 m/z 644.1→528.0、232.1→140.0 和 423.0→362.0。该测定法在头孢哌酮的线性范围为 0.1-20 μg/mL，舒巴坦的线性范围为 0.02-4 μg/mL。每个分析物的日内和日间精密度（CV%）均在 8.39%以内。头孢哌酮和舒巴坦的回收率均大于 87.3%。在所有样品储存、制备和分析过程中，每个分析物均稳定。该方法成功应用于六名医院获得性肺炎（HAP）患者中舒培唑注射液的药代动力学研究。
