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建立了测定人体血浆中环磷酰胺血药浓度的超高效液相色谱-串联质谱方法。样品经甲醇沉淀蛋白,高速离心分离提取,用Waters Acquity UPLC BEH C18色谱柱(50mm×2.1mm,1.7μm)分离,以0.1%甲酸水溶液∶乙腈=(80∶20)为流动相进行洗脱,流速0.4mL.min-1,采用电喷雾质谱正离子模式电离,检测离子(m/Z)对为140.0/106.0,外标法定量。本方法简便快速、准确可靠,环磷酰胺在2—100ng.mL-1的浓度范围内呈良好的线性关系,相关系数r为0.9999;检出限为1μg.L-1,回收率为98.4%—100.5%,相对标准偏差<2.5%。本方法适用于环磷酰胺的临床药动学研究。
A high performance liquid chromatography-tandem mass spectrometry method was established for the determination of cyclophosphamide in human plasma. Samples were precipitated with methanol and extracted by high speed centrifugation. The samples were separated on a Waters Acquity UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm) and eluted with 0.1% aqueous formic acid: acetonitrile (80:20) Flow rate 0.4mL.min-1, electrospray ionization mass spectrometry positive ion mode, the detection ion (m / Z) pairs of 140.0 / 106.0, external standard method. The method is simple and rapid, accurate and reliable, cyclophosphamide in the concentration range of 2-100ng.mL-1 showed a good linear relationship, the correlation coefficient r was 0.9999; detection limit of 1μg.L-1, the recovery rate was 98.4% -100.5%, relative standard deviation <2.5%. The method is suitable for clinical pharmacokinetics of cyclophosphamide.