固相萃取后采用液相色谱-质谱联用技术测定人血浆和尿液中的苯丙香豆素、华法林及其单羟基化代谢物。
Determination of phenprocoumon, warfarin and their monohydroxylated metabolites in human plasma and urine by liquid chromatography-mass spectrometry after solid-phase extraction.
作者信息
Ufer Mike, Kammerer Bernd, Kirchheiner Julia, Rane Anders, Svensson Jan-Olof
机构信息
Division of Clinical Pharmacology, Department of Laboratory Medicine, Karolinska Institute, Huddinge University Hospital, SE-141 86 Stockholm, Sweden.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 5;809(2):217-26. doi: 10.1016/j.jchromb.2004.06.023.
A high-performance liquid chromatography-mass spectrometry (HPLC-MS) method for the quantification of phenprocoumon, warfarin, and their known monohydroxylated metabolites in human plasma and urine was developed using a simple, selective solid-phase extraction scheme. Chromatographic separation was achieved on a reversed-phase Luna C18 column and step gradient elution resulted in a total run time of about 13 min. Limits of quantification (LOQ) were < or = 40 nM for the parent compounds and < or = 25 nM for the metabolites and the limit of detection (LOD) was < or = 2.5 nM for all analytes. Average recovery was 84% (+/- 3.7) and 74% (+/- 13.2) in plasma and urine, respectively. Intra- and inter-day coefficients of variation were < or = 8.6 and < or = 10.6% in plasma and urine, respectively. The method was successfully applied to the analysis of phenprocoumon samples from four healthy volunteers and should prove useful for future comparative studies of warfarin and phenprocoumon pharmacokinetics.
采用一种简单、选择性的固相萃取方案，开发了一种用于定量测定人血浆和尿液中苯丙香豆素、华法林及其已知单羟基化代谢物的高效液相色谱-质谱（HPLC-MS）方法。在反相Luna C18柱上实现色谱分离，采用梯度洗脱，总运行时间约为13分钟。母体化合物的定量限（LOQ）≤40 nM，代谢物的定量限≤25 nM，所有分析物的检测限（LOD）≤2.5 nM。血浆和尿液中的平均回收率分别为84%（±3.7）和74%（±13.2）。血浆和尿液中日内和日间变异系数分别≤8.6%和≤10.6%。该方法成功应用于四名健康志愿者的苯丙香豆素样品分析，应证明对未来华法林和苯丙香豆素药代动力学的比较研究有用。
Zotero 插件