[关键词]
[摘要]
目的 首次建立止血调经颗粒甲醇提取物的HPLC指纹图谱,同时对其中芍药苷和毛蕊异黄酮葡萄糖苷的含量进行测定。方法 赛默飞UltimateTM U3000系列高效液相色谱仪;Thermo AcclaimTM 120 C18色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈-水,梯度洗脱;体积流量为1 mL/min;柱温30℃;检测波长254 nm;进样量10 μL。结果 止血调经颗粒甲醇提取物指纹图谱共标记了11个共有峰,10批样品的相似度均大于0.95;其中,指纹峰分别来自黄芪(1、5、7、10号峰)、党参(1号峰)、续断(2、3号峰)、白芍(4号峰)、当归(6号峰)、茜草(6、8、11号峰)和仙鹤草(9号峰),确定3个已知成分,分别为芍药苷、毛蕊异黄酮葡萄糖苷和芒柄花素;芍药苷和毛蕊异黄酮葡萄糖苷的质量分数分别为1 062.00、84.08 μg/g。结论 该方法重复性好,简便可靠,可用于止血调经颗粒的快速鉴别,为该复方制剂的质量控制提供有效手段。
[Key word]
[Abstract]
Objective To establish an HPLC fingerprint of methanol extract of Zhixue Tiaojing Granule (ZTG), and determine the content of paeoniflorin and calycosin-7-glucosid. Methods HPLC analysis was performed on an Thermo UltiMateTM U3000 LC system and carried out at 30℃ on a column of Thermo AcclaimTM 120 C18 (250 mm×4.6 mm, 5 μm). Gradient elution system was composed of water solution (phase A) and acetonitrile (phase B). Detection was performed at the wavelength of 254 nm, the mobile flow rate was 1 mL/min, the column temperature was 30℃, and sample volumn was 10 μL. Results The HPLC fingerprint for 10 batches of ZTG were obtained and the similarities for 10 batches of samples were all over 0.95. Eleven characteristic peaks were found and peaks were from Astragali Radix (peak 1, 5, 7, 10), Codonopsis Radix (peak 1), Dipsaci Radix (peak 2, 3), Paeoniae Radix Alba (peak 4), Angelicae Sinensis Radix (peak 6), Rubiae Radix et Rhizoma (peak 6, 8, 11), and Agrimoniae Herba (peak 9). Besides, three peaks were assigned include paeoniflorin, calycosin-7-glucosid, and formononetin. The content of paeoniflorin and calycosin-7-glucosid was 1 062 μg/g and 84.08 μg/g. Conclusion The method can be used for the quality control of ZTG with good precision, accuracy, and reproducibility.
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[基金项目]
长沙市2018年度第二批事前立项事后补助科技计划项目(重大专项):止血调经颗粒关键技术研究及产业化(kh1802009)