Dorlo Thomas P C, Hillebrand Michel J X, Rosing Hilde, Eggelte Teunis A, de Vries Peter J, Beijnen Jos H
Department of Pharmacy & Pharmacology, Slotervaart Hospital/The Netherlands Cancer Institute, Louwesweg 6, 1066 EC Amsterdam, The Netherlands.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Apr 1;865(1-2):55-62. doi: 10.1016/j.jchromb.2008.02.005. Epub 2008 Feb 20.
A sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the quantification of miltefosine is presented. A 250 microL human EDTA plasma aliquot was spiked with miltefosine and extracted by a solid-phase extraction method. Separation was performed on a Gemini C18 column (150 mm x 2.0 mm I.D., 5 microm) using an alkaline eluent. Detection was performed by positive ion electrospray ionization followed by triple-quadrupole mass spectrometry. The assay has been validated for miltefosine from 4 to 2000 ng/mL using 250 microL human EDTA plasma samples. Results from the validation demonstrate that miltefosine can be accurately and precisely quantified in human plasma. At the lowest level, the intra-assay precision was lower than 10.7%, the inter-assay precision was 10.6% and accuracies were between 95.1 and 109%. This assay is successfully used in a clinical pharmacokinetic study with miltefosine.
本文介绍了一种用于定量米替福新的灵敏且特异的液相色谱-串联质谱（LC-MS/MS）分析方法。取250微升人乙二胺四乙酸（EDTA）血浆样品，加入米替福新，采用固相萃取法进行提取。使用碱性洗脱液在Gemini C18柱（150毫米×2.0毫米内径，5微米）上进行分离。通过正离子电喷雾电离，随后进行三重四极杆质谱检测。该分析方法已使用250微升人EDTA血浆样品，在4至2000纳克/毫升的米替福新浓度范围内进行了验证。验证结果表明，米替福新可在人血浆中进行准确且精确的定量。在最低水平时，批内精密度低于10.7%，批间精密度为10.6%，准确度在95.1%至109%之间。该分析方法已成功应用于米替福新的临床药代动力学研究。
