摘要
目的:建立测定人全血中西罗莫司浓度的超高压液相色谱-串联质谱(UPLC-MS/MS)方法。方法:色谱柱为Agilent SB-C_(18)(2.1 mm×50 mm,1.8μm),流动相为水(A)-乙腈(0.1%甲酸,B),流速0.3 mL/min,梯度洗脱。依维莫司为内标,电喷雾离子源,多反应离子监测模式,正离子模式检测。西罗莫司和依维莫司离子对m/z分别为936.5/409.5、980.6/389.3。同时采用该方法对我院血管瘤患儿西罗莫司血药浓度进行监测。结果:西罗莫司在0.625~40.000 ng/mL浓度范围内与相对峰面积线性关系良好(r=0.9997),日内、日间RSD均<10%,提取回收率91.95%~118.50%,基质效应81.67%~107.84%。结论:本方法灵敏、准确、快速,能满足临床常规监测西罗莫司血药浓度的需求。
Objective:To establish the ultra high pressure liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for determination of sirolimus in human whole blood.Methods:The analysis was carried out on the Agilent SB-C_(18)(2.1 mm×50 mm,1.8μm)column with gradient elution.The mobile phase was water(A)-acetonitrile(0.1%formic acid,B)at a flow rate of 0.3 mL/min.Everolimus was used as internal standard.The determination was performed on a triple quadrupole tandem mass spectrometer by multiple reactions monitoring mode via electrospray ionization source.The quantitative ion transition m/z of sirolimus and everolimus were 936.5/409.5 and 980.6/389.3.Meanwhile,the blood concentration of sirolimus in children with hemangioma was monitored by this method.Results:Sirolimus showed good linearity(r=0.999,7)in relative peak area over the concentration range of 0.625 to 40.000 ng/mLwith intra-day and inter-day RSD less than 10%,extraction recoveries from 91.95%to 118.50%and matrix effects from 81.67%to 107.84%.Conclusion:The method is sensitive,accurate and rapid for monitoring of whole blood concentration of sirolimus,which can meet the needs of routine clinical monitoring of sirolimus blood concentration.
作者
林志燕
黄晓会
杨萍
Lin Zhiyan;Huang Xiaohui;Yang Ping(Xinhua Hospital Affiliated to Shanghai Jiao Tong University School of Medicine,Shanghai 200092,China)
出处
《儿科药学杂志》
CAS
2022年第11期14-18,共5页
Journal of Pediatric Pharmacy
关键词
西罗莫司
超高压液相色谱-串联质谱
血管瘤
儿童
治疗药物监测
sirolimus
ultra high pressure liquid chromatography-tandem mass spectrometry
hemangioma
children
therapeutic drug monitoring
