摘要
目的建立UPLC-MS/MS同时测定消癌平注射液中通关藤苷A、通关藤苷I、通关藤苷H的含量。方法采用Phenomenex Kinetex XB-C18色谱柱(2.1 mm×50 mm,2.6μm),以0.1%甲酸水-乙腈为流动相,梯度洗脱分离,流速为0.2 m L·min^(-1),通过电喷雾离子源,多反应监测(MRM),正离子模式。结果通关藤苷A、I、H分别在0.05~10 ng·m L^(-1),0.025~10 ng·m L^(-1),0.025~10 ng·m L^(-1)浓度内呈良好的线性关系,r>0.998,检测限为0.012 5~0.025 ng·m L^(-1),平均回收率分别为97.9%,95.7%,96.1%,RSD<3.4%。结论方法简单快速,准确灵敏,可用于消癌平注射液中通关藤苷A、I、H的定量测定。
OBJECTIVE To establish a method for the simultaneous determination of Tenacissoside A, Tenacissoside H and Tenacissoside I in Xiaoaiping injection by UPLC-MS/MS. METHODS The separation was performed on a Phenomenex Kinetex XB-C18 column（2.1 mm×50 mm, 2.6 μm） using the mobile phase of acetonitrile-0.1% formic acid solution at a flow rate of 0.2 m L·min^（-1） in gradient elution mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via electrospray ionization source in positive mode. RESULTS The linearity range of Tenacissoside A, Tenacissoside H and Tenacissoside I were 0.05-10 ng·m L^（-1）, 0.025-10 ng·m L^（-1）, 0.025-10 ng·m L^（-1）, respectively, with all correlation coefficient（r） 〉0.998. The limit detection was 0.012 5-0.025 ng·m L^（-1） and the recoveries were 97.9%, 95.7%, 96.1%, respectively, with RSD 〈3.4%. CONCLUSION The proposed UPLC-MS/MS method is simple, rapidness, accurate, and sensitivity, can be used for the quantitative determination of Tenacissoside A, Tenacissoside H and Tenacissoside I in Xiaoaiping injection.
作者
董占军
安静
王祁民
宋浩静
DONG Zhanjun, AN Jing, WANG Qimin, SONG Haojing(Department of Pharmacy, Hebei General Hospital, Shijiazhuang 050057, Chin)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2018年第3期396-398,共3页
Chinese Journal of Modern Applied Pharmacy
基金
河北省医学科学研究重点课题计划(20170245)
