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目的:利用高效液相色谱法对注射用丹参多酚酸中的鞣质类成分进行排除性检测。方法:采用高效液相色谱法检测水解前后丹参多酚酸样品中没食子酸、儿茶素和鞣花酸。没食子酸液相色谱条件:色谱柱Venusil XBP C18(4.6 mm×250mm,5μm),流动相甲醇-0.05%磷酸水溶液(5∶95)等度洗脱,流速0.8 mL.min-1,柱温30℃,检测波长271 nm。儿茶素液相色谱条件:色谱柱Venusil XBP C18(4.6 mm×250 mm,5μm),流动相甲醇-0.05%磷酸水溶液梯度洗脱,流速0.8 mL.min-1,柱温30℃,检测波长271 nm。鞣花酸液相色谱条件:色谱柱Venusil XBP C18(4.6 mm×250 mm,5μm),流动相乙腈-0.2%磷酸溶液(18∶82),流速1.0 mL.min-1,柱温40℃,检测波长254 nm。结果:水解前后的丹参多酚酸样品的色谱图中,在没食子酸标准品的色谱峰位置,没有相应峰出现;水解后样品中,儿茶素、鞣花酸标准品位置的附近有可疑峰存在,水解后的样品中加入相应对照品再次测定,可确认可疑峰并非儿茶素和鞣花酸的峰。结论:丹参原药材在经过制剂工艺中的聚酰胺树脂柱处理后,其中的鞣质类成分已经被除去,得到的注射用丹参多酚酸中没有鞣质类成分或含量极低。
OBJECTIVE: To determine the content of tannins in Salvia miltiorrhiza polyphenols for injection by HPLC. Methods: The contents of gallic acid, catechin and ellagic acid in Salvia miltiorrhiza polyphenols sample before and after hydrolysis were determined by HPLC. Gallic acid liquid chromatography conditions: column Venusil XBP C18 (4.6 mm × 250mm, 5μm), mobile phase methanol -0.05% phosphoric acid solution (5:95) isocratic elution, flow rate 0.8 mL.min-1, column temperature 30 ℃, detection wavelength 271 nm. Catechin HPLC conditions: column Venusil XBP C18 (4.6 mm × 250 mm, 5μm), mobile phase methanol -0.05% phosphoric acid aqueous solution gradient elution, flow rate 0.8 mL.min-1, column temperature 30 ℃, detection wavelength 271 nm. Ellagic acid liquid chromatography conditions: column Venusil XBP C18 (4.6 mm × 250 mm, 5μm), mobile phase acetonitrile -0.2% phosphoric acid solution (18:82), flow rate 1.0 mL.min-1, column temperature 40 ℃, Detection wavelength 254 nm. Results: There was no corresponding peak in the chromatogram of Salvia miltiorrhiza polyphenols samples before and after hydrolysis. In the samples after hydrolysis, there were suspicious peaks in the vicinity of the standard of catechin and ellagic acid Presence of hydrolyzed samples by adding the corresponding reference substance again measured to confirm that the suspicious peak is not catechin and ellagic acid peak. Conclusion: The original medicinal materials of Salvia miltiorrhiza Bunge have been removed after the polyamide resin column of the preparation process has been processed. There is no tannin component in the Salvia miltiorrhiza polyphenols for injection or the content is extremely low.