Shigeta Kensuke, Kikuchi Masafumi, Tanaka Masaki, Takasaki Shinya, Oishi Hisashi, Sado Tetsu, Matsuda Yasushi, Noda Masafumi, Okada Yoshinori, Mano Nariyasu, Yamaguchi Hiroaki
Faculty of Pharmaceutical Sciences, Tohoku University, Sendai, Japan.
Department of Pharmaceutical sciences, Tohoku University Hospital, Sendai, Japan.
Biomed Chromatogr. 2020 Aug;34(8):e4853. doi: 10.1002/bmc.4853. Epub 2020 May 22.
Sirolimus is used on patients after solid organ transplantation and on lymphangioleiomyomatosis (LAM) patients, and therapeutic drug monitoring is required in clinical practice. We have previously reported an accurate method for quantitative determination of sirolimus, but its sample preparation step was complicated. In this study, we developed a modified liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method for sirolimus quantification. A supported liquid extraction cartridge was used to purify sirolimus from whole blood and ion suppression was mostly prevented. The validation results met the acceptance criteria. This method was compared with the antigen conjugated magnetic immunoassay (ACMIA) and our previously reported method, using whole blood samples from LAM patients. Comparison of the Bland-Altman plots of the currently developed method and the previous method revealed no significant difference between the two methods (mean bias, -2.02%; 95% CI, -7.81-3.78). The values obtained using ACMIA were significantly higher than those obtained using the current method by 13.87% (95% CI, 6.49-21.25) owing to cross-reactivity. The degrees of cross reactivities in LAM patients and in organ transplant patients were similar, and our LC/ESI-MS/MS method precisely measured the blood concentrations of sirolimus.
西罗莫司用于实体器官移植后的患者以及淋巴管平滑肌瘤病(LAM)患者,临床实践中需要进行治疗药物监测。我们之前报道了一种准确测定西罗莫司的方法,但其样品制备步骤较为复杂。在本研究中,我们开发了一种改进的液相色谱/电喷雾电离串联质谱(LC/ESI-MS/MS)方法用于西罗莫司定量。使用固相萃取柱从全血中纯化西罗莫司,大部分抑制了离子抑制作用。验证结果符合验收标准。使用LAM患者的全血样本,将该方法与抗原偶联磁免疫分析(ACMIA)以及我们之前报道的方法进行了比较。当前开发的方法与之前方法的布兰德-奥特曼图比较显示,两种方法之间无显著差异(平均偏差,-2.02%;95%置信区间,-7.81-3.78)。由于交叉反应性,使用ACMIA获得的值比使用当前方法获得的值显著高13.87%(95%置信区间,6.49-21.25)。LAM患者和器官移植患者中的交叉反应程度相似,我们的LC/ESI-MS/MS方法精确测量了西罗莫司的血药浓度。