Research & Development, Bristol-Myers Squibb Co., Route 206/Province Line Road, Lawrenceville, NJ 08543, United States.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Oct 1;879(27):2919-27. doi: 10.1016/j.jchromb.2011.08.025. Epub 2011 Aug 26.
A liquid chromatography-full scan high resolution accurate mass spectrometry (LC-HRMS) method for quantifying prednisone and prednisolone in human plasma using a quadrupole time-of-flight mass spectrometer (Q-TOF) was developed. Plasma samples were extracted using a liquid-liquid extraction procedure. Full scan data were acquired in the TOF only mode and extracted ion chromatograms were generated post-acquisition with the exact masses of the analytes. The calibration range was 5-2500 ng/mL, with a Lower Limit of Quantitation (LLOQ) of 5 ng/mL. The assay accuracy was between 98.4% and 106.3%. The between-run (inter-day) and within-run (intra-day) precision were within 1.7% and 2.9%, respectively. The matrix effect was between 0.98 and 1.10 for the six different lots of human plasma evaluated. Pooled incurred samples were analyzed by the method and the results matched those obtained from an LC-MS/MS method. In addition, qualitative information on phospholipids, and other endogenous components were also extracted from the full-scan data acquired.
建立了一种采用四极杆飞行时间质谱仪(Q-TOF)的液相色谱-全扫描高分辨精确质量测定法(LC-HRMS)，用于定量测定人血浆中的泼尼松和泼尼松龙。采用液液萃取法提取血浆样品。仅在飞行时间模式下采集全扫描数据，并在采集后生成具有分析物精确质量的提取离子色谱图。校准范围为 5-2500ng/mL，定量下限(LLOQ)为 5ng/mL。测定的准确度在 98.4%至 106.3%之间。批间(日间)和批内(日内)精密度分别在 1.7%和 2.9%范围内。在所评估的六种不同批次的人血浆中，基质效应在 0.98 至 1.10 之间。用该方法分析了经处理的 incurred 样品，结果与 LC-MS/MS 方法获得的结果相匹配。此外，还从采集的全扫描数据中提取了磷脂和其他内源性成分的定性信息。
