超高效液相色谱-串联质谱法测定儿童患者血浆中的白消安  

Determination of Busulfan in Plasma from Pediatric Patients by UPLC-MS/MS

作　　者：柴慧霞 张海凤[2] 邵端芳[3] 权力 崔小岱[2] 刘嵘[3] CHAI Huixia;ZHANG Haifeng;SHAO Duanfang;QUAN Li;CUI Xiaodai;LIU Rong(Weifang Medical University,Weifang 261053;Experiment Center of the Institute,Capital Institute of Pediatrics,Beijing 100020;Dept.of Hematology,Capital Institute of Pediatrics,Beijing 100020;Institute of Molecular Medicine,Peking University,Beijing 100871)

机构地区：[1]潍坊医学院,山东潍坊261053 [2]首都儿科研究所实验中心,北京100020 [3]首都儿科研究所血液科,北京100020 [4]北京大学分子医学研究所,北京100871

出　　处：《中国医药工业杂志》2022年第6期876-882,共7页Chinese Journal of Pharmaceuticals

基　　金：国家自然科学基金项目(81501838);北京市人才基金项目(2014000021469G229)。

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法测定儿童患者血浆中的白消安(1)。采用ACQITY UPLC~?HSS T色谱柱(2.1 mm×50 mm,1.8μm),多反应监测模式,结合电喷雾离子源正离子分段扫描分析。结果显示,1在20~3000 ng/ml内线性关系良好,方法定量限为5 ng/ml。日内、日间精密度均小于5%,平均提取回收率为90%~110%,残留效应为0.01%。1的标准血浆样品于室温条件保存24 h后1的浓度下降了22%,提示不稳定,而其他贮存条件下(4、–20和–80℃),1周内1的浓度基本无变化。建立的方法所需的血浆样品量少,即使1μl血浆也可用于检测。该法快速、准确、可靠,可为1的儿科临床治疗和药动学研究提供参考。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of busulfan(1)in plasma from pediatric patients.The ACQITY UPLCHSS Tcolumn(2.1 mm×50 mm,1.8μm)was used,and the multiple reaction monitoring mode was adopted with the electrospray ion source for positive ion segmental scanning analysis.The results showed that it was linear for 1 in the range of 20-3000 ng/ml,and the quantification limit of the method was 5 ng/ml.The intra-and inter-day precisions were below 5%.The average extraction recoveries were 90%-110%,and the residual effect was 0.01%.The concentration of 1 decreased by 22%after storage at room temperature for 24 h,indicating that the plasma sample was unstable under this condition.While under the other storage conditions(4,–20 and–80℃),the concentrations of 1 were basically unchanged within one week.The established method required a small amount of plasma sample,and even 1μl of plasma could be used for detection.This method was fast,accurate and reliable,which provided a reference for pediatric therapy and pharmacokinetic studies of 1.

关 键 词：白消安 UPLC-MS/MS 血药浓度监测 儿童患者 

分 类 号：R969.1[医药卫生—药理学]