UPLC-MS/MS法同时测定通关藤药材中3种皂苷的含量  

Simultaneous Determination of 3 Kinds of Saponins in Marsdenia tenacissima by UPLC-MS/MS

作　　者：王祁民 安静[1] 李颖[2] 马银玲[1] 董占军[1] WANG Qimin;AN Jing;LI Ying;MA Yinling;DONG Zhanjun(Dept.of Pharmacy,Hebei Provincial People’s Hospital,Shijiazhuang 050051,China;Graduate School,Hebei Medical University,Shijiazhuang 050017,China)

机构地区：[1]河北省人民医院药学部,石家庄050051 [2]河北医科大学研究生学院,石家庄050017

出　　处：《中国药房》2018年第8期1048-1051,共4页China Pharmacy

基　　金：河北省中医药管理局中医药类科研计划课题(No.冀中医药[2017]67号-2018073)

摘　　要：目的:建立同时测定通关藤药材中通关藤苷A、H、I含量的方法。方法:采用超高效液相色谱-串联质谱法,色谱柱为Phenomenex Kinetex XB-C18,流动相为0.1%甲酸溶液-乙腈(梯度洗脱),流速为0.2 m L/min,柱温为40℃,进样量为5μL,离子源为电喷雾离子源,多反应离子监测模式,正离子扫描,离子源喷射电压为5 500 V,雾化气压力为60 psi,加热气压力为60 psi,帘气压力为20 psi,去溶剂温度为600℃。结果:通关藤苷A、H、I检测质量浓度线性范围分别为0.1~10 ng/m L(r=0.999 7)、0.025~10 ng/m L(r=0.999 5)、0.025~10 ng/m L(r=0.998 9);定量限分别为0.1、0.025、0.025 ng/m L,检测险分别为0.05、0.012 5、0.012 5ng/m L;精密度、稳定性、重复性试验的RSD均小于4.0%;加样回收率分别为97.67%~99.00%(RSD=0.47%,n=6)、95.00%~101.67%(RSD=2.59%,n=6)、96.67%~103.33%(RSD=2.83%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于通关藤药材中通关藤苷A、H、I含量的同时测定。OBJECTIVE:To establish the method for simultaneous determination of tenacissoside A,tenacissoside H and tenacissoside I in Marsdenia tenacissima.METHODS:UPLC-MS/MS method was adopted.The determination was performed on a Phenomenex Kinetex XB-C18 column with mobile phase consisted of 0.1%formic acid solution-acetonitrile(gradient elution)at the flow rate of 0.2 mL/min.The column temperature was set at 40℃,and sample size was 5μL.Multiple reaction monitoring(MRM)mode was adopted with electrospray ion source as ion source,using positive ion scanning.Source jet voltage was 5 500 V,nebulizer pressure was 60 psi,heating pressure was 60 psi,curtain pressure was 20 psi and cone temp was set at 600℃.RESULTS:The linear ranges of tenacissoside A,tenacissoside H and tenacissoside I were 0.1-10 ng/mL(r=0.999 7),0.025-10 ng/mL(r=0.999 5),0.025-10 ng/mL(r=0.998 9),respectively;limited of quantation were 0.1,0.025,0.025 ng/mL,limited of detection were 0.05,0.012 5,0.012 5 ng/mL,respectively;RSDs of precision,stability and reproducibility tests were<4.0%.The recoveries were 97.67%-99.00%(RSD=0.47%,n=6),95.00%-101.67%(RSD=2.59%,n=6),96.67%-103.33%(RSD=2.83%,n=6).CONCLUSIONS:The method is simple,precise,stable and reproducible,and can be used for simultaneous determination of tenacissoside A,tenacissoside H and tenacissoside I in M.tenacissima.

关 键 词：通关藤 通关藤苷A 通关藤苷H 通关藤苷I 超高效液相色谱-串联质谱法 

分 类 号：R28[医药卫生—中药学]