HPLC-MS/MS法测定人血浆中替加环素浓度的不确定度评定

Uncertainty Evaluation of Content Determination of Tigecycline in Human Plasma by HPLC-MS / MS

目的:评定高效液相色谱-质谱联用法(HPLC-MS/MS)测定人血浆中替加环素(TGC)浓度的不确定度。方法:分析HPLC-MS/MS法测定人血浆中TGC浓度的整个过程,分别评定测量重复性、称量、工作液配制、生物样品配制、回收率、仪器允差和标准曲线拟和引起的不确定度大小,最后计算合成不确定度并进行扩展。结果:人血浆中替加环素低、中、高浓度的测定值和不确定度可分别表示为:(48.737±4.587),(396.067±19.096)和(1 489.000±103.563)ng·ml-1,(P=95%,k=2)。结论:HPLC-MS/MS法测定人血浆中TGC浓度的不确定度主要来源在低浓度时曲线拟合和高浓度时回收率。

Objective： To evaluate the uncertainty of tigecycline （TGC） determination in human plasma by HPLCJMS/MS. Methods： The whole process of TGC determination by HPLC-MS/MS in human plasma was analyzed and the uncertainty caused by re- peatability, weighing, standard solution preparation, biological sample preparation, recovery, instrument precision and calibration curve fitting were evaluated respectively and the combined and expanded uncertainty were calculated. Results： The measured value and the uncertainty of TGC determined at low, medium and high levels in human plasma could be expressed as （48. 737 ± 4.587 ）, （396.067 ± 19. 096） and （ 1489. 000 ± 103. 563 ） ng · ml - 1, respectively （ P = 95 %, k = 2）. Conclusion： The uncertainty of TGC in human plasma determined by the HPLC-MS/MS method is mainly caused by calibration curve fitting and recovery at low and high concentration.