用HPLC-MS/MS法检测大鼠乳腺微透析液中环磷酰胺的浓度  

Determination of cyclophosphamide in rat breast microdialysis fluid by HPLC-MS/MS method

作　　者：胡霜霜[1] 刘春生[1] 童卫杭[1] 曹淼[1] 吴城[1] 彭珑[1] 王丹[1] 

机构地区：[1]第二炮兵总医院药学部,北京100088

出　　处：《药学服务与研究》2015年第3期205-207,共3页Pharmaceutical Care and Research

基　　金：国家自然科学青年基金(81301662);中国博士后科学基金(2013M532151)

摘　　要：目的：建立HPLC-MS/MS法检测大鼠乳腺微透析液中环磷酰胺的浓度。方法：采用Cosmosil-C18色谱柱（150mm×4.6mm,5μm）,流动相：A相为0.1%甲酸溶液,B相为乙腈,0-1min A∶B=70∶30,1-1.5min A∶B=60∶40,1.5-5.5min A∶B=40∶60,5.5-8min A∶B=70∶30,梯度洗脱8min,流速为1ml/min。正离子多反应检测（MRM）方式进行检测,监测离子对：环磷酰胺m/z261.3→140.1,内标安替比林m/z 189.2→104.0。结果：环磷酰胺的线性范围为0.05-10μg/ml,最低定量限为0.05μg/ml。日间和日内RSD均〈15%,准确度和稳定性实验结果均符合生物样品的测定要求。结论：本方法灵敏度高,操作简便,适用于微透析样品中环磷酰胺的浓度测定。Objective：To establish a HPLC-MS/MS method for the determination of cyclophosphamide concentration in rat breast microdialysis fluid.Methods：The analysis was performed on Cosmosil-C18column（150mm×4.6mm,5μm）.The mobile phase was composed of 0.1%formic acid solution（A）-acetonitrile（B）in gradient elution at a flow rate of 1ml/min,0-1min A∶B=70∶30,1-1.5min A∶B=60∶40,1.5-5.5min A∶B=40∶60,5.5-8min A∶B=70∶30.Selected positive ion multiple reaction monitoring（MRM）of m/z261.3→140.1（cyclophosphamide）and m/z189.2→104.0（internal standard antipyrine）was performed.Results：Calibration curves were linear over the range of 0.05-10μg/ml for cyclophosphamide,the lowest detection limit was 0.05μg/ml.Intra-and inter-day precisions were less than 15%.The results of accuracy and stability tests all met the requirements for the determination of biological samples.Conclusion：This method is sensitive and easy for operation,and could be used for the determination of cyclophosphamide in microdialysis samples.

关 键 词：环磷酰胺 含量测定 微透析 色谱法 高效液相 质谱法 

分 类 号：R927.2[医药卫生—药学]