水杨苷对照品的制备工艺

Preparation process of Salicin reference substance

关键词:  白柳皮  水杨苷  提取  对照品

Key words:  white willow bark  salicin  extraction  reference substance

摘要:

从白柳皮中提取分离水杨苷，并通过纯化工艺，制备水杨苷对照品。采用大孔树脂分离、正丁醇萃取、重结晶方法从白柳皮中提取水杨苷，经熔点和比旋度测定、水杨苷元素分析、红外光谱、液相色谱-质谱联用和核磁共振谱进行水杨苷的鉴别，并采用HPLC-UV和HPLC-ELSD进行水杨苷纯度测定。结果表明，提取物经熔点和比旋度测定、水杨苷元素分析、红外光谱、液相色谱-质谱联用和核磁共振谱鉴定为水杨苷，提取的水杨苷对照品平均含量为99.19%，纯度大于99%，符合中药标准品（供含量测定用）的要求。

Abstract:

The present study was performed to extract and separate the salicin from the bark of white willow to prepare the purified salicin reference substance. The salicin was extracted with the macroporous rein separation, N-butyl alcohol extraction and recrystallized method . The purified salicin was identified by testing the melting point and specific rotation, elemental analysis, infrared spectrum, liquid chromatography tandem mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) spectrum. The purity of salicin was measured by HPLC-UV and HPLC-ELSD. The results indicated that the extract was identified as salicin after testing melting point and specific rotation, elemental analysis, infrared spectrum, LC-MS and NMR spectrum. The average content of extracted salicin reference substance is about 99.19% and the purity is more than 99%, which meet the requirement of traditional Chinese medicine reference standards (for determination use).