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[Preparation and simultaneous determination of corynoline and acetylcorynoline in the herb of Corydalis bungeana].
Zhongguo Zhong yao za zhi = Zhongguo zhongyao zazhi = China journal of Chinese materia medica Pub Date : 2004-05-14
Ge Huang 1 , Hong-juan Yang , Fa-mei Li
Affiliation  

OBJECTIVE To isolate and purify corynoline and acetylcorynoline from Corydalis bungeana and develop a reversed-phase HPLC method of determining the two components in C. bungeana. METHOD Alkaloids were isolated from the ethanolic extract with column gel chromatography, and identified on the basis of spectral analysis (UV, 1H-NMR, 13C-NMR) and physicochemical properties. For quantitative analysis of the two components, samples were separated on an ODS column with mobile phase of methanol-15 mmol.L-1 potassium dihydrogen phosphate/potassium phosphate dibasic (pH 6.70, 70:30). The flow rate was 0.8 mL.min-1, and the detection was set at 289 nm. RESULT The purity was 99.5% and 99.1% for corynoline and acetylcorynoline respectively. The calibration curves were linear in the range of 6.9-110.4 mg.L-1 corynoline and 8.7-139.5 mg.L-1 acetylcorynoline. The RSD was 2.1% and 2.7%, and the average recovery was 97.3% and 97.2% respectively. CONCLUSION The method of isolating and purifying corynoline and acetylcorynoline from Corydalis bungeana and the HPLC method of simultaneous determination of the two components have been developed. The HPLC method is simple, easy to perform and applicable to the content determination of corynoline and acetylcorynoline in C. bungeana of various origins.

中文翻译:

紫花延胡索中红霉素和乙酰基羟脯氨酸的制备及同时测定

目的从紫花延胡索中分离纯化紫苏碱和乙酰紫苏碱,建立反相高效液相色谱法测定杜鹃花中两种成分的方法。方法采用柱凝胶色谱法从乙醇提取物中分离出生物碱,并根据光谱分析(UV,1H-NMR,13C-NMR)和理化性质进行鉴定。为了对这两种成分进行定量分析,在ODS色谱柱上分离样品,其流动相为甲醇-15 mmol.L-1磷酸二氢钾/磷酸氢二碱(pH 6.70,70:30)。流速为0.8 mL.min-1,检测设置为289 nm。结果天冬氨酸和乙酰天冬氨酸的纯度分别为99.5%和99.1%。校准曲线在6.9-110.4 mg.L-1羟乙基胆碱和8.7-139.5 mg.L-1乙酰基羟乙基林之间呈线性关系。RSD为2.1%和2.7%,平均回收率分别为97.3%和97.2%。结论已开发了从紫花延胡索中分离纯化紫杉醇和乙酰紫杉醇的方法,以及同时测定这两种成分的HPLC方法。高效液相色谱法简便,易行,适用于各种产地梭状芽胞杆菌中胭脂红碱和乙酰胭脂碱的含量测定。
更新日期:2019-11-01
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