目的: 建立UPLC-MS/MS法,同时测定风湿安泰片中18个特征性成分含量,并对测定结果进行化学计量学分析,为其质量控制提供依据。方法: 采用Waters BEH C18(100 mm×2.1 mm,1.7 μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.2 mL·min-1,柱温40 ℃,进样量1 μL;质谱采用电喷雾离子源(ESI),正离子检测,多反应监测(MRM)模式。结果: 所建方法在一定范围内线性关系良好(r≥0.998 6),平均加样回收率为90.2%~101.7%,RSD为1.1%~4.9%。39批次样品中麻黄碱(以盐酸麻黄碱计)、伪麻黄碱(以盐酸伪麻黄碱计)、绿原酸、紫丁香苷、士的宁、马钱子碱、小檗碱(以盐酸小檗碱计)、柚皮苷、桂皮醛、人参皂苷Re、人参皂苷Rg1、人参皂苷Rb1、朝藿定C、淫羊藿苷、川续断皂苷Ⅵ、甘草酸(以甘草酸铵计)、羌活醇、异欧前胡素的含量范围分别为20.23~141.75、10.50~121.69、215.24~697.34、8.46~42.42、135.24~363.32、91.29~242.87、19.65~80.31、22.57~105.05、4.69~86.88、10.32~241.15、3.36~65.07、10.79~390.69、6.51~86.29、4.10~89.75、195.55~566.37、96.98~448.95、0~132.41、7.09~232.71 μg·片-1。化学计量学结果显示,5个生产企业39批样品聚为3类,不同生产企业样品质量存在一定差异,筛选出影响质量的8个差异性标志物(柚皮苷、甘草酸、异欧前胡素、小檗碱、紫丁香苷、麻黄碱、伪麻黄碱、士的宁)。结论: 建立的方法简单、可行,结合化学计量学方法,可用于风湿安泰片的质量评价。
Objective: To establish an UPLC-MS/MS method to measure the content of 18 characteristic components in Fengshiantai tablets, and conduct chemometric analysis on the measurement results to provide a basis for quality control. Methods: The components were separated on Waters BEH C18(100 mm×2.1 mm, 1.7 μm) column with methanol and 0.1% formic acid aqueous solution as the mobile phase by gradient elution at a flow rate of 0.2 mL·min-1. The column temperature was set at 40 ℃. The injection volume was 1 μL. The detection was carried out by electrospray ionization(ESI), and electron spray ionization source was adopted in positive ion detection with multiple reaction monitoring mode(MRM). Results: The established methods showed a good linear relationship in a certain range (r≥0.998 3), whose average recovery rates of samples were 90.2%-101.7% with the RSD of 1.1%-4.9%. The content of ephedrine(calculated as ephedrine hydrochloride), chlorogenic acid, syringin, strychnine, brucine, berberine(calculated as berberine hydrochloride), naringin, cinnamaldehyde, ginsenoside Re, ginsenoside Rg1, epimedin C, icariin, asperosaponin Ⅵ, glycyrrhizic acid(calculated as glycyrrhizic acid ammonium salt), ginsenoside Rb1, notopterol, isoimperatorin in 39 batches of samples were 20.23-141.75 μg per tablet, 10.50-121.69 μg per tablet, 215.24-697.34 μg per tablet, 8.46-42.42 μg per tablet, 135.24-363.32 μg per tablet, 91.29-242.87 μg per tablet, 19.65-80.31 μg per tablet, 22.57-105.05 μg per tablet, 4.69-86.88 μg per tablet, 10.32-241.15 μg per tablet, 3.36-65.07 μg per tablet, 10.79-390.69 μg per tablet, 6.51-86.29 μg per tablet, 4.10-89.75 μg per tablet, 195.55-566.37 μg per tablet, 96.98-448.95 μg per tablet, 0-132.41 μg per tablet, 7.09-232.71 μg per tablet. The results of chemometrics showed that 39 batches of samples from 5 production enterprises were classify into three categories, and there were certain differeces in sample quality among different production enterprises, eight differential markers(naringin, glycyrrhizic acid, isoimperatorin, berberine, syringin,ephedrine, pseudoephedrine, strychnine) that caused quality differences were found. Conclusion: The established method is simple and feasible, combined with chemometric methods, and can be used for quality evaluation of Fengshiantai tablets.
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