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,5 μm),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 mL/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5 μL。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/mL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32.8～107.6 μg/g,甘草苷54.8～178.0 μg/g,哈巴俄苷14.6～70.7 μg/g,桔梗皂苷D 31.2～280.0 μg/g,甘草酸铵106.4～287.9 μg/g,麦冬皂苷D 0.1～0.6 μg/g,麦冬黄烷酮A 0.01～0.07 μg/g和麦冬黄烷酮B 0.03～0.17 μg/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 develop a UPLC-MS/MS method for simultaneously determining harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in Xuanmai Ganjie Granules (composed with Scrophulariae Radix, Ophiopogonis Radix, Glycyrrhizae Radix et Rhizoma, and Platycodonis Radix) from different pharmaceutical companies. Methods The chromatographic separation was achieved on Phenomenex Kenetix C₁₈ column (50 mm × 2.1 mm, 5 μm) by using a mobile phase consisted of acetonitrile and 0.1% formic acid water at the flow rate of 0.3 mL/min for gradient elution. Simultaneous monitoring of positive and negative ions and multiple reaction monitoring (MRM) scan mode were applied to the quantification of the components in Xuanmai Ganjie Granules; Sample volume was 5 μL. Results There was good linearity between the absorption peak area and the concentration for harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in the ranges of 9—2 250, 8—2 000, 3.4—850, 96—24 000, 12.4—3 100, 3.6—1 900, 1.7—425, and 1.5—375 ng/mL, respectively. The average recoveries were ranged from 97.2% to 102.8% (RSD ≤ 2.7%). The contents of harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in eight batches of samples were in the ranges of 32.8—107.6, 54.8—178.0, 14.6—70.7, 31.2—280.0, 106.4—287.9, 0.1—0.6, 0.01—0.07, and 0.03—0.17 μg/g, respectively. Conclusion The developed method is simple, effective, and credible for determining the eight components in Xuanmai Ganjie Granules. It provides more helpful information for the comprehensive quality evaluation of Xuanmai Ganjie Granules.

河北省卫生厅青年科技课题(ZL20140340);河北省中医药管理局指导性项目(2014152)