Cunliffe Jennifer M, Noren Carl F, Hayes Roger N, Clement Robert P, Shen Jim X
Schering-Plough Research Institute, Summit, NJ 07901, United States.
J Pharm Biomed Anal. 2009 Aug 15;50(1):46-52. doi: 10.1016/j.jpba.2009.03.034. Epub 2009 Apr 7.
A rapid and robust liquid chromatographic tandem mass spectrometric (LC-MS/MS) method for the determination of posaconazole concentrations in human plasma was validated. Posaconazole was extracted from human plasma using mixed-mode cation exchange solid phase extraction in a 96-well plate format followed by gradient separation on a fused-core Halo C18 column. The analyte and its corresponding internal standard were detected using a Sciex API 4000 triple quadrupole LC-MS/MS system equipped with a TurboIonSpray ionization source operated in the positive ion mode. The calibration range of the method was 5.00-5000ng/mL using a 50microL aliquot of plasma. The assay inter-run accuracy and precision were-4.6-2.8% and 2.3-8.7%, respectively (n=18). The results from method validation indicate the method to be sensitive, selective, accurate, and reproducible. The method was successfully applied to the routine analysis of clinical samples with the fused-core silica columns providing excellent reproducibility for greater than 1000 injections per column.
一种用于测定人血浆中泊沙康唑浓度的快速且可靠的液相色谱串联质谱（LC-MS/MS）方法得到了验证。泊沙康唑采用96孔板形式的混合模式阳离子交换固相萃取从人血浆中提取，随后在核壳型Halo C18柱上进行梯度分离。使用配备TurboIonSpray离子源并以正离子模式运行的Sciex API 4000三重四极杆LC-MS/MS系统检测分析物及其相应的内标。该方法使用50μL血浆等分试样的校准范围为5.00 - 5000ng/mL。批间分析的准确度和精密度分别为-4.6 - 2.8%和2.3 - 8.7%（n = 18）。方法验证结果表明该方法灵敏、选择性好、准确且可重现。该方法成功应用于临床样品的常规分析，核壳型硅胶柱对每根柱子超过1000次进样提供了出色的重现性。
