摘要
建立了超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定小鼠肿瘤部位阿霉素药物浓度的方法。样本经甲醇沉淀蛋白法处理,C 18色谱柱分离,采用甲酸水溶液(A)-甲醇(B)为流动相,梯度洗脱,以柔红霉素作为内标,在电喷雾离子化(ESI)正离子模式下检测,扫描方式为多反应监测(MRM),用于定量的离子对分别为m/z 544.2→m/z 397.2(阿霉素)和m/z 528→m/z 321(柔红霉素,内标)。结果表明:经优化测定组织匀浆后阿霉素标准曲线的线性范围为100~10000μg/L,线性关系良好(r>0.99);准确度、日内和日间精密度(RSD)、提取回收率均符合生物样品的分析要求。该方法专属性强、灵敏度高、操作简单、快速,适用于检测阿霉素在小鼠体内肿瘤部位的药物浓度。
Protein precipitation by methanol was used for the sample pretreatment,the chromatographic separation was carried out on a Shim-Pack GISS-HP C 18(100mm×2.1mm×3μm)using a mobile phase consisting of solvent A(0.1%formic acid in water)and solvent B(acetonitrile)for gradient elution.With daunorubicin as internal label,the samples were determined in a positive ion mode by electro-spray ionization(ESI).The compounds were quantitated by multiple reaction monitoring(MRM)using transition mass of m/z 544.2→m/z 397.2 for doxorubicin and m/z 528→m/z 321 for daunorubicin(internal label).The experiment results showed that the linear range of the calibration curve of doxorubicin was 100-10000μg/L and the linear relation of tissue homogenates was good(r>0.99).This method is highly specific,sensitive and rapid.Its accuracy,intra-day and inter-day precisions,recovery ratio can meet the requirements of the biological samples analysis.
作者
王婷
孙亮
王东亮
甘雅玲
胡西学
郭宏博
何芳菲
王昱青
蒋乔
Wang Ting;Sun Liang;Wang Dongliang;Gan Yaling;Hu Xixue;Guo Hongbo;He Fangfei;Wang Yuqing;Jiang Qiao(National Center for Nanoscience and Technology,Beijing 100190,China;Shimadzu(China)Co.,Ltd.,Beijing 100020,China)
出处
《分析仪器》
CAS
2020年第1期25-28,共4页
Analytical Instrumentation
关键词
超高效液相色谱-串联质谱
阿霉素
尾静脉注射
含量测定
Ultra high performance liquid choromatography-tandem mass spectrometry(UHPLC-MS/MS)
Doxorubicin
Tail intravenous injection
Determination
