中国药房2018，Vol.29Issue(8)：1048-1051,4.DOI:10.6039/j.issn.1001-0408.2018.08.09
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
摘要
Abstract
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-C18column 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 5 μ L. 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Key words
Marsdenia tenacissima/Tenacissoside A/Tenacissoside H/Tenacissoside I/UPLC-MS/MS分类
医药卫生引用本文复制引用
王祁民,安静,李颖,马银玲,董占军..UPLC-MS/MS法同时测定通关藤药材中3种皂苷的含量[J].中国药房,2018,29(8):1048-1051,4.基金项目
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) （No.冀中医药〔2017〕67号-2018073）
