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目的建立高效液相色谱-串联质谱(HPLC-MS/MS)同时测定参乌健脑胶囊(SJC)中8种成分(葛根素、丹参酮IIA、二苯乙烯苷、芍药苷、人参皂苷Re、人参皂苷Rg1、毛蕊异黄酮苷、黄芩苷)的定量方法。方法选用YMC-Triart C18色谱柱,以甲醇-0.2%甲酸水溶液为流动相,梯度洗脱,体积流量为0.6 m L/min,柱温40℃。质谱条件:ESI源,采用多反应监测模式(MRM),以定量离子对峰面积进行定量。结果 SJC中葛根素、丹参酮IIA、二苯乙烯苷、芍药苷、人参皂苷Re、人参皂苷Rg1、毛蕊异黄酮苷、黄芩苷分别在20.31~20 310、25.66~25 660、20.45~20 450、50.79~50 790、50.57~50 570、50.38~50 380、10.32~10 320、25.74~25 740 ng/m L内线性关系良好(r≥0.999 0);精密度良好,重复性良好,RSD均小于2.0%;在室温条件下24 h内稳定;加样回收率为97.98%~102.48%,RSD小于1.6%。所测8种成分在6批样品中的质量分数依次为葛根素1.843~1.860 mg/g、丹参酮IIA 1.618~1.629 mg/g、二苯乙烯苷2.116~2.129 mg/g、芍药苷2.537~2.547mg/g、人参皂苷Re 0.034~0.041 mg/g、人参皂苷Rg1 0.048~0.055 mg/g、毛蕊异黄酮苷0.551~0.564 mg/g和黄芩苷2.333~2.346 mg/g。结论该方法快速、简便、重复性好,可用于同时测定SJC中多种成分。
OBJECTIVE To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) system for the simultaneous determination of eight components (puerarin, tanshinone IIA, stilbene glycoside, paeoniflorin, ginsenoside Re, Saponin Rg1, Caryophyllantin, baicalin). Methods YMC-Triart C18 column was used. The mobile phase consisted of methanol-0.2% formic acid as mobile phase. The volume flow rate was 0.6 m L / min and the column temperature was 40 ℃. Mass Spectrometry Conditions: ESI source using multiple reaction monitoring mode (MRM) to quantitate peak area with quantitation ions. Results SJC puerarin, tanshinone IIA, stilbene glycoside, paeoniflorin, ginsenoside Re, ginsenoside Rg1, calycosin and baicalin were 20.31 ~ 20 310,25.66 ~ 25 660,20.45 ~ 20 450,50.79 ~ 50790,50.57 ~ 50 570,50.38 ~ 50 380,10.32 ~ 10 320,25.74 ~ 25 740 ng / m L good linear relationship (r ≥ 0.9999); good precision, good reproducibility, RSD were less than 2.0% ; Stable at room temperature within 24 h; sample recovery was 97.98% ~ 102.48%, RSD less than 1.6%. The mass fraction of 8 components in 6 batches of samples were as follows: puerarin 1.843-1.860 mg / g, tanshinone IIA 1.618-1.629 mg / g, stilbene glycoside 2.116-2.129 mg / g, paeoniflorin 2.537-2.547 mg / g, 0.034 ~ 0.041 mg / g ginsenoside Re, 0.048 ~ 0.055 mg / g ginsenoside Rg1, 0.551 ~ 0.564 mg / g calycosin and 2.333 ~ 2.346 mg / g baicalin. Conclusion The method is rapid, simple and reproducible. It can be used for the simultaneous determination of various components in SJC.