Zhang Shuang-Qing, Chen Guo-Hua
Department of Pharmaceutics, School of Pharmacy, The University of Mississippi, MS 38677, USA.
Biomed Chromatogr. 2009 May;23(5):510-5. doi: 10.1002/bmc.1146.
A sensitive and specific ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for quantification of a newly developed anticancer agent NPD-103 has been established. An aliquot of human plasma sample (200 microL) was spiked with (13)C-labeled paclitaxel (internal standard) and extracted with 1.3 mL of tert-butyl methyl ether. NPD-103 was quantitated on a C(18) column with methanol-0.1% formic acid (75:25, v/v) as mobile phase using UPLC-MS-MS operating in positive electrospray ionization mode with a total run time of 3.0 min. For NPD-103 at the concentrations of 1.0, 5.0 and 10.0 microg/mL in human plasma, the absolute extraction recoveries were 95.58, 102.43 and 97.77%, respectively. The linear quantification range of the method was 0.1-20.0 microg/mL in human plasma with linear correlation coefficients greater than 0.999. The intra- and inter-day accuracy for NPD-103 at 1.0, 5.0 and 10.0 microg/mL levels in human plasma fell into the ranges of 95.29-100.00% and 91.04-94.21%, and the intra- and inter-day precisions were in the ranges of 8.96-11.79% and 7.25-10.63%, respectively. This assay is applied to determination of half-life of NPD-103 in human plasma.
已建立一种灵敏且特异的超高效液相色谱-串联质谱法（UPLC-MS-MS），用于定量一种新研发的抗癌药物NPD-103。取一份人类血浆样本（200微升），加入（13）C标记的紫杉醇（内标），并用1.3毫升叔丁基甲醚萃取。NPD-103在C（18）柱上进行定量分析，以甲醇-0.1%甲酸（75:25，v/v）作为流动相，采用正电喷雾电离模式运行的UPLC-MS-MS，总运行时间为3.0分钟。对于人类血浆中浓度为1.0、5.0和10.0微克/毫升的NPD-103，绝对萃取回收率分别为95.58%、102.43%和97.77%。该方法在人类血浆中的线性定量范围为0.1-20.0微克/毫升，线性相关系数大于0.999。人类血浆中1.0、5.0和10.0微克/毫升水平的NPD-103日内和日间准确度分别在95.29-100.00%和91.04-94.2%范围内，日内和日间精密度分别在8.96-11.79%和7.25-10.63%范围内。该分析方法用于测定NPD-103在人类血浆中的半衰期。
