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纸质出版日期:2013
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薛静, 叶正良, 李德坤, 等. 注射用丹参多酚酸中鞣质类物质的排除性检测[J]. 中国实验方剂学杂志, 2013,19(4):93-95.
XUE Jing, YE Zheng-liang, LI De-kun, et al. Exclusive Detection of the Tannin in Salvianolic Acid Extracts for Injection[J]. Chinese journal of experimental traditional medical formulae, 2013, 19(4): 93-95.
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×250 mm
5 μm)
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
5 μm)
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
5 μm)
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: HPLC was employed to detect the tannin in salvianolic acid extracts for injection. Method: Gallic acid
catechins and ellagic acid in salvianolic acid extracts for injection were analyzed using HPLC method before and after the hydrolysis. The chromatographic condition for gallic acid was as follows:the chromatographic column was Venusil XBP C18 (4.6 mm×250 mm
5 μm) with the flow rate of 0.8 mL·min-1
mobile phase was phosphoric acid-water (0.05:100) and methanol
column temperature was kept at 30℃ and the detector was set at 271 nm. The chromatographic condition for catechins was as follows:the chromatographic column was Venusil XBP C18 (4.6 mm×250 mm
5 μm) at the gradient elution mode with the flow rate of 0.8 mL·min-1
mobile phase was phosphoric acid-water (0.05: 100) and methanol
column temperature was kept at 30℃ and the detector was set at 271 nm. The chromatographic condition for ellagic acid was as follows:the chromatographic column was Venusil XBP C18(4.6 mm×250 mm
5 μm) with the flow rate of 1.0 mL·min-1
mobile phase was phosphoric acid-water (0.2:100) and acetonitrile
column temperature was kept at 40℃ and the detector was set at 254 nm. Result: There was no gallic acid in salvianolic acid extracts before and after the hydrolysis. But catechins and ellagic acid might exist in salvianolic acid extracts after the hydrolysis. With the corresponding standard product in salvianolic acid extracts after the hydrolysis and detected again
it proved that no catechins and ellagic acid existed in salvianolic acid extracts after the hydrolysis. Conclusion: No tannin exists in salvianolic acid extracts after the treatment of polyamide resin.
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