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目的建立同时测定玄麦甘桔颗粒(玄参、麦冬、甘草、桔梗)中8种有效成分(哈巴苷、甘草苷、哈巴俄苷、桔梗皂苷D、甘草酸铵、麦冬皂苷D、麦冬黄烷酮A和麦冬黄烷酮B)的方法,并对市售不同厂家生产玄麦柑桔颗粒中上述8种有效成分进行定量分析。方法采用超高效液色谱相串联质谱(UPLC-MS/MS)法,Phenomenex Kenetix C18柱(50 mm×2.1 mm,5μm),流动相为乙腈和含0.1%甲酸的水溶液梯度洗脱,体积流量0.3 m L/min;质谱采用正负离子同时监测,多反应监测模式扫描,进样量5μL。结果玄麦柑桔颗粒中哈巴苷、甘草苷、哈巴俄苷、桔梗皂苷D、甘草酸铵、麦冬皂苷D、麦冬黄烷酮A和麦冬黄烷酮B分别在9~2 250、8~2 000、3.4~850、96~24 000、12.4~3 100、3.6~1 900、1.7~425、1.5~375 ng/m L内线性关系良好,加样回收率为97.2%~102.8%,RSD小于2.7%。8种成分在8批样品中的质量分数依次为哈巴苷32.8~107.6μg/g,甘草苷54.8~178.0μg/g,哈巴俄苷14.6~70.7μg/g,桔梗皂苷D 31.2~280.0μg/g,甘草酸铵106.4~287.9μg/g,麦冬皂苷D 0.1~0.6μg/g,麦冬黄烷酮A 0.01~0.07μg/g和麦冬黄烷酮B 0.03~0.17μg/g。结论建立的方法简单、高效、准确可靠,可用于同时测定玄麦甘桔颗粒中8种成分,为该制剂建立更全面的质量控制方法提供依据。
OBJECTIVE To establish a method for simultaneous determination of 8 active ingredients in Xuanmai Ganjie Granules (Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae, Radix Platycodonis) with Radix Glycyrrhizae, Glycyrrhizin, Harpagoside, Platycodin D, Glycyrrhizinate, Ophiopogon japonicus D Flavanone A and Ophiopogon flavone B) method, and the commercially available different manufacturers Xuan Mai citrus granules in the above eight active ingredients for quantitative analysis. Methods The mobile phase was a gradient elution of acetonitrile and 0.1% formic acid on a Phenomenex Kenetix C18 column (UPLC-MS / MS) with a mobile phase of 0.3 m L / min; mass spectrometry using positive and negative ions simultaneously monitoring, multi-reaction monitoring mode scanning, injection volume 5μL. Results Xuanmai citrus granules in habitacoside, glycyrrhizin, Harpagoside, platycodin D, glycyrrhizin, Ophiopogon japonicus D, Ophiopogon flavonoids A and Ophiopogon flavonoids B in 9 ~ 2 250,8 ~ 2 000,3.4 ~ 850,96 ~ 24 000,12.4 ~ 3 100,3.6 ~ 1 900,1.7 ~ 425,1.5 ~ 375 ng / m L good linearity, the recovery rate was 97.2% ~ 102.8% RSD is less than 2.7%. The mass fraction of eight components in eight batches of samples was 32.8-107.6 μg / g for habanero, 54.8-178.0 μg / g for liquiritin, 14.6-70.7 μg / g for harpagoside, 31.2-280.0 μg / g for platycodon, , 106.4-287.9 μg / g ammonium glycyrrhizinate, 0.1-0.6 μg / g Ophiopogon japonicus D, 0.01-0.07 μg / g Ophiopogon A, and 0.03-0.17 μg / g Ophiopogon B. Conclusion The established method is simple, efficient, accurate and reliable, and can be used for the simultaneous determination of eight components in Xuanmaiganqing Granules, providing a basis for the establishment of a more comprehensive quality control method.