CAJ | 학술논문

目的：建立简便、快速地测定人全血中西罗莫司血药浓度的HPLC-MS/MS方法。方法：全血样品经硫酸锌及含有子囊霉素（内标）的乙腈溶液沉淀后，取上清液20μL进样分析。采用Symmetry-C18色谱柱（2.1 mm×50 mm，3.5μm），流动相梯度洗脱，流速为0.5 mL·min-1，质谱采用电喷雾离子化电离源，经多反应监测模式检测。结果：西罗莫司和子囊霉素的保留时间分别为2.24 min和2.21 min，空白血浆中内源性物质不干扰测定；西罗莫司的血药浓度在1~30 ng· mL-1时，线性关系良好（r=0.9995）；日内、日间RSD值均小于10%，提取回收率为86.4%~90.4%。结论：本方法灵敏、准确、简单、快速，可用于西罗莫司的血药浓度监测和早期肝移植患者药代动力学研究。
목적：건립간편、쾌속지측정인전혈중서라막사혈약농도적HPLC-MS/MS방법。방법：전혈양품경류산자급함유자낭매소（내표）적을정용액침정후，취상청액20μL진양분석。채용Symmetry-C18색보주（2.1 mm×50 mm，3.5μm），류동상제도세탈，류속위0.5 mL·min-1，질보채용전분무리자화전리원，경다반응감측모식검측。결과：서라막사화자낭매소적보류시간분별위2.24 min화2.21 min，공백혈장중내원성물질불간우측정；서라막사적혈약농도재1~30 ng· mL-1시，선성관계량호（r=0.9995）；일내、일간RSD치균소우10%，제취회수솔위86.4%~90.4%。결론：본방법령민、준학、간단、쾌속，가용우서라막사적혈약농도감측화조기간이식환자약대동역학연구。
Objective:To establish a simple and rapid HPLC-MS/MS method for determination of sirolimus in human whole blood. Methods:The samples of whole blood were deproteinated by zinc sulfate and internal standard reconstituted in acetonitrile and separated by a Symmetry-C18 column (2.1 mm×50 mm, 3.5 μm) at the flow rate of 0.5 mL·min-1 with gradient elution. Detection was performed on a tandem mass spectrometry with electrospray ionization source in positive ionmode. Multiple reactions monitoring mode was used to quantify sirolimus and internal standard respectively. Results: The retention time of sirolimus and internal standard were 2.24 min and 2.21 min, respectively. The linear range of sirolimus was 1–30 ng·mL-1( r=0.999 5). The intra-day and inter-day RSD were both less than 10%. The extraction recoveries were 86.4%–90.4%. Conclusion:The method is sensitive, accurate, simple and rapid for monitoring of whole blood concentration of sirolimus and pharmacokinetic study in early liver tansplant recipients.