论文部分内容阅读
目的建立全血中西罗莫司的UPLC(超高效液相色谱)/MS/MS测定方法。方法全血样品中加入他克莫司(FK506)作内标,用叔丁基甲醚进行提取。以乙腈与含千分之五甲酸的水溶液为流动相(40∶50),色谱柱为Acquity UPLCTMBEHC8(50mm×2.1mm,1.7μm),流速0.5ml/min。三重四极杆质谱采用正离子模式,离子采集方式为多反应监测模式(MRM),离子源温度105℃,离子源电离电压为3300V,雾化气流速500L/h。采集离子(母离子/子离子)西罗莫司为931.2/864.1,FK506为822.0/577.0。结果西罗莫司在1～240μg/L浓度范围内呈良好的线性(r=0.9995)。日内、日间精密度均在15%以内,提取回收率大于75.0%,方法回收率为95.0%～98.5%,最低检测限为0.2μg/L。结论本方法灵敏、准确,适合临床西罗莫司的全血分析。
Objective To establish a UPLC (ultra performance liquid chromatography) / MS / MS method for determination of sirolimus in whole blood. Methods Whole blood samples were added with tacrolimus (FK506) as an internal standard and extracted with tert-butyl methyl ether. The mobile phase (40:50) consisted of acetonitrile and aqueous 5% methanoic acid. The chromatographic column was Acquity UPLC TM MBEHC8 (50 mm × 2.1 mm, 1.7 μm) at a flow rate of 0.5 ml / min. The triple quadrupole mass spectrometer used a positive ion mode. The ion collection mode was a multi-reaction monitoring mode (MRM). The temperature of the ion source was 105 ℃. The ionization voltage of the ion source was 3300V. The atomization gas flow rate was 500L / h. The collected ions (parent ions / daughter ions) were sirolimus 931.2 / 864.1 and FK506 822.0 / 577.0. Results Sirolimus showed a good linearity (r = 0.9995) at a concentration of 1-240 μg / L. The intra-day and inter-day precision were less than 15%, the recovery rate was more than 75.0%, the recovery rate was 95.0% ~ 98.5%, the lowest detection limit was 0.2μg / L. Conclusion The method is sensitive and accurate and suitable for clinical whole blood analysis of sirolimus.