UPLC-MS/MS法同时测定通关藤药材中3种皂苷的含量
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篇名: UPLC-MS/MS法同时测定通关藤药材中3种皂苷的含量
TITLE:
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 mL/min,柱温为40 ℃,进样量为5 μL,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/mL(r=0.999 7)、0.025~10 ng/mL(r=0.999 5)、0.025~10 ng/mL(r=0.998 9);定量限分别为0.1、0.025、0.025 ng/mL,检测险分别为0.05、0.012 5、0.012 5 ng/mL;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。
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-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 5 μL. 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.
期刊: 2018年第29卷第8期
作者: 王祁民,安静,李颖,马银玲,董占军
AUTHORS: WANG Qimin,AN Jing,LI Ying,MA Yinling,DONG Zhanjun
关键字: 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
KEYWORDS: Marsdenia tenacissima; Tenacissoside A; Tenacissoside H; Tenacissoside I; UPLC-MS/MS
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