液质联用检测人尿液中莎巴比星及其代谢物M3浓度

发布时间：2019-07-09 12:14

【摘要】：目的:建立超高效液相色谱-质谱联用(UHPLC-MS/MS)测定尿液中莎巴比星及其代谢物M3浓度的方法,用于小细胞肺癌Ⅰ期临床尿液中药动学研究。方法:多柔比星作为内标,用氯仿进行液液萃取处理,选用ACQUITY UPLC BEH Shield RP18色谱柱(100 mm×2.1 mm,1.7μm)分离,流动相为0.1%甲酸水-乙腈(90∶10,V/V),流速0.3 m L·min~(-1)。采用ESI正离子方式进行检测,用于定量分析的检测离子为莎巴比星m/z 644.2→130.2、M3 m/z 646.2→130.1和多柔比星m/z 544.3→397.1。结果:莎巴比星和M3在2~200 ng·m L~(-1)范围内呈良好的线性拟合关系(r0.99)。在目标化合物出峰时间处,未观察到基质的内源性成分干扰,残留率可接受,并对方法的选择性、提取回收率、基质效应、精密度与准确度以及部分稳定性等进行了验证,均符合FDA和CFDA指导原则的要求,且该方法在临床预实验入组患者尿液药物分析中进行验证。结论:本方法可灵敏、准确、快速地测定尿液中莎巴比星和代谢物M3的浓度,能够满足临床药动学研究的需求。
文内图片：
图片说明：莎巴比星、M3及内标的质谱碎裂图
[Abstract]:Objective: to establish an ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) method for the determination of Sababisin and its metabolite M3 in urine for the kinetic study of traditional Chinese medicine in stage I clinical urine of small cell lung cancer. Methods: doxorubicin was used as internal standard and chloroform was used for liquid-liquid extraction. ACQUITY UPLC BEH Shield RP18 column (100 mm 脳 2.1 mm, 1.7 渭 m) was used to separate doxorubicin. The mobile phase was 0.1% formate water-acetonitrile (90 脳 10, V 鈮，

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