Department of Pathology and Laboratory Medicine, Emory University School of Medicine, Atlanta, GA 30322, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Mar 1;879(7-8):553-6. doi: 10.1016/j.jchromb.2011.01.005. Epub 2011 Jan 12.
A method for the determination of tranexamic acid (TXA) in human plasma and cerebral spinal fluid (CSF) was developed. Analyses were performed by ultra performance liquid chromatography with tandem mass spectrometry detection (UPLC-MS/MS) using ɛ-aminocaproic acid (ACA) as an internal standard. TXA and ACA were extracted from a 50 μL sample of plasma or CSF using a methanol protein crash protocol, and chromatographic separation was performed on an ACQUITY™ TQD mass spectrometer using a UPLC C18 BEH 1.7 μm column with a water and methanol gradient containing 0.1% formic acid. The detection and quantitation was performed by positive ion electrospray ionization using the multiple reaction monitoring (MRM) mode. The method was linear over the concentration range of 0.1-10.0 μg/mL, with lower limit of quantitation of 0.1 μg/mL for TXA. The intra- and inter-assay precision was less than 12% and 13% respectively at the plasma and CSF TXA concentrations tested. The present method provides a relatively simple and sensitive assay with short turn-around-time. The method has been successfully applied to assess the plasma and CSF concentrations of tranexamic acid achieved with only one dosing regimen of tranexamic acid in patients undergoing cardiopulmonary bypass surgery (CPB).
建立了一种同时测定人血浆和脑脊液中氨甲环酸（TXA）的方法。采用超高效液相色谱-串联质谱法（UPLC-MS/MS），以ε-氨基己酸（ACA）为内标，对样品进行分析。采用甲醇蛋白沉淀法从 50 μL 血浆或脑脊液样品中提取 TXA 和 ACA，采用 ACQUITY™ TQD 质谱仪，在 ACQUITY UPLC C18 BEH 1.7μm 色谱柱上，以含 0.1%甲酸的水-甲醇梯度洗脱，进行色谱分离。采用正离子电喷雾电离，多反应监测（MRM）模式进行检测和定量。该方法在 0.1-10.0μg/mL 浓度范围内呈线性，TXA 的定量下限为 0.1μg/mL。在测试的血浆和 CSF TXA 浓度下，日内和日间精密度均小于 12%和 13%。本方法提供了一种相对简单、灵敏、分析时间短的方法。该方法已成功应用于评估心脏体外循环手术（CPB）患者单次氨甲环酸给药后血浆和脑脊液中氨甲环酸的浓度。
