[关键词]
[摘要]
目的 建立同时测定银黄制剂中10种成分(新绿原酸、绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素)的超高效液相色谱(UPLC)方法。方法 采用Acquiyt UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以乙腈-0.4%磷酸水溶液为流动相,梯度洗脱,体积流量0.4 mL/min,在326 nm波长处进行检测,柱温40℃,进样量1.0 μL。结果 银黄制剂中10种成分在考察线性范围内线性关系良好(r≥0.999 6),加样回收率均在97.43%~99.94%,RSD均小于2.0%。11批银黄制剂样品中新绿原酸、绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素质量分数分别在0.236~3.419、5.279~26.220、0.495~4.714、0.130~2.702、0.310~3.210、0.363~5.036、35.209~133.289、1.493~6.635、1.546~5.393、0.254~0.823 mg/g。结论 该方法简便,准确,快速,分离效果好,重复性好,可用于银黄制剂的质量控制,并为将来该制剂质量标准提升提供参考。
[Key word]
[Abstract]
Objective To develop an UPLC method for simultaneous determination the contents of 10 active constituents[neochlorogenic acid (NCA), chlorogenic acid (CA), cryptochlorogenic acid (CCA), isochlorogenic acid A (ICAA), isochlorogenic acid B (ICAB), isochlorogenic acid C (ICAC); bacicalin, wogonoside, baicalein, and wogonin] in Yinhuang preparations. Methods Analysis was performed on an Acquiyt UPLC BEH C18 chromatographic column (100 mm×2.1 mm, 1.7 μm) eluted with acetonitrile-0.4% phosphoric acid, gradient elution, and the flow rate was 0.4 mL/min, the detection wavelength was set at 326 nm, the column temperature was 40℃, and the injection volume was 1.0 μL. Results All calibration curves were linear (r≥0.999 6) over the tested ranges. The average recoveries (n=9) ranged from 97.43% to 99.94% with RSD value below 2.0%. The contents of 11 batches of NCA, CA, CCA, ICAA, ICAB, ICAC, bacicalin, wogonoside, baicalein, and wogonin were 0.236-3.419, 5.279-26.220, 0.495-4.714, 0.130-2.702, 0.310-3.210, 0.363-5.036, 35.209-133.289, 1.493-6.635, 1.546-5.393, and 0.254-0.823 mg/g. Conclusion This method is rapid, simple, sensitive, accurate, and reproducible, which can be used for quality control of Yinhuang preparation, and provide a reference for the formulation of quality standards to enhance in the future.
[中图分类号]
[基金项目]
贵州省科技厅社会攻关项目(黔科合成转字[2015]5213号)