摘要
目的评定液质联用法(HPLC-MS/MS)在测定人血浆中甲氨蝶呤(MTX)浓度时的不确定度。方法分析HPLC-MS/MS法测定人血浆中MTX浓度时的不确定度来源,计算不确定度并进行合成和扩展。结果人血浆中MTX低浓度(0.025μmol·L-1)和高浓度(0.653μmol·L-1)的扩展不确定度分别为0.0016μmol·L-1和0.034μmol·L-1(P=95%,k=2)。结论 HPLC-MS/MS法测定人血浆中MTX浓度的不确定度在低浓度时主要由回收率、曲线拟合、生物样品配制和基质效应引入,在高浓度时主要由生物样品配制、回收率和基质效应引入。
Objective To evaluate the uncertainty in the determination of methotrexate (MTX) in human plasma by HPLC-MS/MS. Methods The process of the MTX determination was analyzed and the uncertainty from various sources were calculated. The combined and expanded uncertainty were also evaluated. Results The expanded uncertainty of MTX at low (0.025 μmol · L - 1) and high (0.653 μmol ·L - 1) levels was 0.0016 μmol · L - 1 and 0.034 μmol · L - 1 (p = 95%, k = 2). Conclusion The uncertainty in the determination of MTX in human plasma by HPLC-MS/MS at low concentration is mainly caused by recovery, calibration curve fitting, sample preparation and matrix effect while at high concentration the uncertainty is mainly caused by sample preparation, recovery and matrix effect.
出处
《中南药学》
CAS
2016年第2期117-122,共6页
Central South Pharmacy
基金
国家自然科学基金(No.81301118)
多肽及小分子药物北京市重点实验室开放课题(No.2014DTYW03)